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Vacuum Technology Simplified

First Edition

Mr. Anshuman Punj

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Notices
Knowledge and best practice in this field are constantly changing. As new
research and experience broaden our understanding, changes in research
methods, professional practices or medical treatment may become necessary.
Practitioners and researches must always rely on their own experience and
knowledge in evaluating and using any information, method, compounds or
experiments described herein. In using such information or methods they
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About the Author

Mr. Anshuman Punj


CEO of Supervac Industries
Hi I am Anshuman Punj. I am a post-graduate
mechanical engineer and an MBA by qualification.
(B.Tech.-Mechanical Engineering, M.Tech.-Tool
Design, MBA-specialization in Materials
Management). I have worked at various management
positions in the private sector as well as a consultant
Design for Tooling. (Eicher Goodearth, Modi Xerox
and Hero Motors). This was followed by an illustrious career in the Indian
Railways as a Class 1 officer. Coming across the upcoming and challenging
field of vacuum deposition, I quit the government service in order to develop
several ground breaking vacuum coating materials that could be manufactured
in-country. Today, I am the CEO of Supervac Industries, a highly successful
Indian company that manufactures and supplies vacuum consumables
(vacuum pump oils, graphite foil and suspension, boron nitride powder and
suspension, high vacuum silicone grease, ceramic evaporation boats) to a large
number of customers around the world. I head Supervac Industries which is
known world-wide for its high quality and reasonably priced products. With 17
years of experience in the Vacuum Industry, I regularly write articles and blogs
on Vacuum products and applications.
Experience
Director at Indian Railways, Marketing Engineer at Modi Xerox Ltd, Marketing
Engineer at Eicher Goodearth Pvt. Ltd.
Education
Masters Degree at Delhi Institute of Tool Engineering, High Schooling from
SBM Senior Secondary School.
Volunteer at Goonj, Indian Vacuum Society, BCI
Content

Preface

Part I Vacuum Pump Oil


1. Leakage Detection and Prevention in Vacuum Systems
2. Top 20 Questions About Rotary Vacuum Pumps and Oils
3. Molecular Distilled Vacuum Pump Oil: Explanation and Advantages
4. How to Reduce Vacuum Time
5. Graphite Foil Top 10 Questions Answered
6. Silicone Vacuum Grease Explained
7. Vacuum Oil Equivalents
Part II Diffusion Pump Oil
8. Boiling Temperature of Diffusion Pump Oil Explained
9. Know All About Diffusion Pump Part-1
10. Know All About Diffusion Pump Part-2
11. How To Get Maximum Life From Your Diffusion Pump Oil
Part III Evaporation Boat
12. Pin Holes: 5 Ways to Eliminate Them
13. Evaporation Boat: How it is made
14. Evaporation Boat: Get Your Moneys Worth Out Of It
Part I

Vacuum Pump Oil


Chapter 1: Leakage Detection and Prevention in Vacuum Systems
Leaks pose biggest challenge to engineers handling vacuum systems.
Leakages cripple the work and are invariably time consuming to detect.

This chapter is about two major issues related to leakage Detection and
Prevention.

Leakage Detection

Following are three methods of leakage detection

1. Physical Verification: This


should be used if even roughing
vacuum (1 x 10-1 Torr) cannot be
reached in the vacuum system. In
this method the person has to move
around the vacuum system slowly,
paying attention to any hissing or
whistling sound. This sound
indicates location of leak. Though
method is very simple, in this
method experience of the person is
very important and this way of
leakage detection is suitable only
for detecting large leaks.

2. Pirani Gauge and Solvent Method:


If vacuum climbs above roughing stage then obviously the leakage is small.
For such leaks this method is used. In this method vacuum pumps are
allowed to operate to reach a stable vacuum level. At this point a solvent,
normally acetone, is sprayed (generally with a syringe) at the suspect joint.
Since system is under vacuum if a leak exists at that joint then solvent is
quickly drawn in. As we understand pirani gauge is very sensitive to change
of gas compositions. Pirani gauge attached with the system therefore quickly
picks up presence of solvent and its reading changes (vacuum drop). After a
while the reading returns to the previous reading as solvent has been sucked
away by vacuum pumps.
If there is no change in reading of Pirani gauge then next suspect joint is tried
and so on till leakage is detected.
This is a very inexpensive method as it requires no special equipment.
Expertise is however required for proper results.
3. Helium Leak Detector: Though
expensive this is by far the most
accurate of leakage detection
methods. In this method a helium
leak detector is employed. Using a
bottle of Helium gas, Helium is
squirted at the suspect joint by a
nozzle. Since system is under
vacuum, if a leak exists then helium
is quickly drawn into vacuum
system. After this a spectrometer is
used to detect helium.

Spectrometer consists of the following:-

(a) An ionizer to ionize gas


(b) Analyzer to separate the gas and
(c) A detector to detect the composition of gas.

The spectrometer is connected to


vacuum line from which vacuum
pumps are drawing away the air.
Since spectrometer has an excellent
sensitivity, by using the spectrometer,
even minutest of leakages can be
detected.
If spectrometer does not detect any
helium, then next suspect joint is tried,
and by hit and trial, the leakage is
identified.

Precaution
Since Helium is a light gas care needs to be exercised during leak detection to
move from top to bottom of vacuum system and not the other way round. This
is because Helium squirted at a lower joint can always quickly travel up and
enter system from an upper leaking joint. This can absolutely sabotage the
procedure.

As the saying goes prevention is better than the cure. It is better if we are able
to prevent leakage in the first place.

Based on my engineering background and experience of about 20 years


in vacuum line a few practical tips for leakage prevention are given below-
1. Proper Maintenance of Gauges: Many
times faulty gauges result in assumption of a
leak. Since gauges are highly sensitive
equipment hence maintaining these properly
is very important. This will prevent any false
alarms and wastage of precious production
time in hunting a leak.

2. Virtual Leak: Many times the design of


system is such that from some part air is not
able to escape freely. This results in pressure
differential within vacuum chamber. For example, vacuum chamber may
have been pumped down to 1 x 10-5 Torr but a part of chamber from which
free escape of air is not possible may have vacuum of only 1 x 10 -2 Torr.
Slowly when the vacuum will be equalized in the chamber, then this will show
as a vacuum drop, resulting in time wastage on leak hunting. To prevent this,
proper system design is important and if such a pocket exists in chamber
from which free flow of air is not possible then that part must be given more
openings for faster evacuation.

3. Water Vapour: As vacuum engineers know, water vapor is most difficult to


be pumped out. Because of the polar nature of water molecules, they stick
to the walls of system forming strongly attached multiple layers. With time
water vapor will be released from walls and cause vacuum drop. To take care
of this, cryo panels are used in vacuum systems to freeze water vapor.
Another way is to push inert gas in vacuum system at high speed. This
dislodges water molecules and with inert gas these water molecules are also
drawn away by vacuum pumps. Argon and helium are cheaper in the list of
inert gasses and are therefore commonly used for this purpose. One could
however use any other inert gas also like Neon, Xenon, Krypton or Radon.

4. Proper Maintenance of O
Rings: Since metal to metal
surface contact is unable to hold
vacuum so O rings are employed
to seal vacuum. Using good
quality Viton O rings with good
compressibility solves problems of
leakage to a large extent. Another
precaution is to discard O rings if
they harden, soften too much or
swell up.
5. Use of high vacuum silicone
grease: Good quality Vacuum
grease applied to O rings goes a long
way in preventing leakages. This is
because not only does it provide
additional vacuum sealing but also
protects the O rings from hardening
and damage. This grease should have
a very low vapour pressure and
excellent tackiness. Supervac
manufactures High Vacuum Silicone
Grease SV-G9 which is widely used
by vacuum industry all over the world.

6. Baking: - If Possible the vacuum system should be baked at a temperature


of 250o C for minimum 12 hours under vacuum from time to time. This expels
the volatile gasses attached to vacuum system walls.

Conclusion

Leakage in a vacuum system is a nightmare, but observing a few basic


precautions like proper care of pumps, replacement of O rings as they age,
application of Vacuum grease and cleaning of flange surfaces etc. go a long
way in containing the problem.
If a leakage occurs then immediate action to detect it before it snowballs into
a major problem is important. Also people performing leakage detection
should be adequately trained and given required tools to be able to solve the
problem quickly and save precious production time.
Chapter 2: Top 20 Questions about Rotary Vacuum Pumps and
Oils
Q.1 What is a Roughing Pump?
Ans. A Roughing Pump is nothing but an ordinary Rotary vacuum pump which
is used to evacuate the vacuum system initially. After a roughing pump creates
vacuum of minimum 110-2 Torr, the valve systems changes settings and
pumps like Booster Pump and Diffusion Pump are connected to system to
create higher vacuum.

Q.2 What should be the basic properties of rotary vacuum pump oil?
Ans. Rotary vacuum pump oil must have following properties:-
1. Low vapor pressure of less than 110-3 Torr.
2. Should have viscosity between 65 to 80 cst at 40oC.
3. Should not contain corrosive elements like sulphur.
4. Should be resistant to oxidation.
5. Viscosity of the oil should not change much with change of temperature.

Q.3 Which is better synthetic rotary vacuum pump oil or mineral vacuum
pump oil?
Ans. Synthetic rotary vacuum pump oils give higher vacuum, create vacuum
faster and have longer working life. In addition, synthetic rotary vacuum pump
oil preserves and protects the pump interiors. So these next generation
synthetic oils are superior to commonly used organic rotary vacuum pump oils.
The latter is used only where cost is an issue. Supervac Industries
manufactures both synthetic as well as mineral rotary vacuum pump oils
SV-68 and SV-77 respectively.
Q.4 Can I use simple hydraulic oil for my rotary vacuum pump in place of
rotary vacuum pump oil?
Ans. No, you should never do that as this can seriously damage your rotary
pump. Rotary vacuum pump oil is not an ordinary lubricant. It is a special fluid
manufactured with thermal and oxidative stability. Unlike hydraulic oil, rotary
vacuum pump oil has a low vapor pressure. It is therefore absolutely different
from normal hydraulic oil or motor oil.
Q.5 Can I use simple motor/engine oil for my Rotary Vacuum Pump?

Ans. Never ever use motor/engine oil for your Rotary vacuum pump. People
tend to make this mistake so very often only to end up regretting eventually.
Motor oils are lubricants designed for automobile engines which work under
different principles whereas rotary vacuum pump oils are specialty fluids
manufactured keeping in mind the requirements of a vacuum pump. Motor oils
have a different viscosity from vacuum pump oils and have no vacuum
properties at all. Motor oils carry various additives like rust inhibitors and anti-
corrosion compounds. When put in the rotary pump, under low pressure and
high temperature, these additives separate from the base fluid and cling to the
insides of the pump as sticky/gummy solids. This affects the vacuum pressure
and harms the pump. Under high temperature of the vacuum pump, motor
oils/hydraulic oils start releasing vapors, thus bringing down the vacuum,
whereas good quality rotary vacuum pump oils do not release any vapors.
Supervac manufactures high quality Synthetic Rotary Vacuum Pump Fluid- SV-
77, which is a boon in terms of vacuum formation and pump maintenance.

Q.6 Do Roughing/rotary pumps need topping up of vacuum pump oil?


Ans. Rotary vacuum pumps lose a small amount of vacuum oil in the form of oil
mist. This loss is pronounced in initial (roughing) phase. To make up for this
loss of oil it is advisable to top up rotary vacuum pump oil from time to time.
Q.7 Will Rotary vacuum pump oil used in Kinney pump and Stroke pump
( both are roughing pumps) be the same or different?
Ans. Vacuum pumps as well as vacuum pump oils are made as per international
specifications. So a good rotary vacuum pump oil will be suitable for all/any
rotary vacuum pump made anywhere in the world and by any manufacturer.
Just like the same petrol works for cars made by Honda, Suzuki, Audi, Toyota
or any other brand.
Q.8 What is a two stage rotary vacuum pump?
Ans. A Rotary vacuum pump works by mechanically compressing and pushing
out the air from inlet to outlet. The outlet pressure therefore has to be higher
than atmospheric pressure for exhaust to take place. In two stages rotary pump
the outlet of one chamber is connected to inlet of next chamber. This increases
the compression and makes the air exhaust possible.
Majority of rotary pumps are two stage rotary pumps.
Q.9 How do I know that I need to change the oil of my rotary pump?
Ans. In vacuum industry practices for vacuum oil change vary widely.

Usually one of these three reasons trigger oil change:-


1. Rotary pump starts taking longer to create vacuum or is unable to reach the
desired vacuum level.
2. Color of oil changes from transparent or golden yellow to dark brown
indicating oxidation.
3. Some engineers prefer to change oil after a fixed number of working hour
which are either recommended by manufacturer or are based on experience.

Q.10 Can I recycle my rotary vacuum pump oil?


Ans. No, rotary vacuum pump oil cannot be recycled. This is because vacuum
pump oils work under very demanding conditions. Used vacuum oil, even if
recycled, will still be carrying various contaminants. For the safety of expensive
vacuum pump, used oil is best discarded.
Q.11 What are the reasons of noise in rotary vacuum pump?
Ans. Normally rotary pumps work noiselessly.
Noise in rotary vacuum pump could be because of following reasons:-

1. Excessive gas load because of some leak in system. This may also be
accompanied be release of oil mist from pump.
2. Some foreign object lodged in rotary pump. This will cause intermittent,
loud noise.
3. Worn out ball bearings. This causes continuous noise.

Q.12 What is the normal working temperature of a rotary vacuum pump?


Ans. Normal working temperature of rotary pump is about 80o C.

Q.13 My rotary pump overheats sometimes. Is this serious?


Ans. Yes, this is serious as pump can get seriously damaged if temperature of
pump exceeds 100oC. Rotary pumps need to be run in well-ventilated areas
and in case of extremely hot climates, as is common in India, use a fan to cool
the pump externally. Overheated pumps will not give the required vacuum and
thus unduly affect either the working of diffusion pump or the entire process.
Also, the oil in an overheated pump will turn less viscous (too thin) and will not
lubricate the pump interiors well; thereby leading to pump failure.

Q.14 What is gas ballast in rotary vacuum pump?


Ans. Since rotary vacuum pump creates vacuum by positive displacement and
compression of air so during operation of this pump some water vapors
condense to water and mix with vacuum oil. This reduces the vacuum.
Some pumps are equipped with gas ballast mechanism. This mechanism allows
some air to flow into compression portion of pump cycle, diluting the water
vapor. This causes fewer tendencies of water vapors to condense. This is called
gas ballasting.
Q.15 Do vane type rotary pump and piston type rotary pump require
different rotary vacuum pump oils?
Ans. In both vane type rotary pump and piston type rotary pumps, function of
vacuum oil is to provide lubrication. At the same time for both these pumps the
rotary vacuum pump oil should have a low vapor pressure and good viscosity
stability.
Since both types of pumps require same characteristics of vacuum oil so the
same vacuum oil is used for both these types of pumps.

Q.16 How do piston pumps work?

Ans. Piston pump is a type of Rotary


Vacuum Pump. This pump works on a
principle of drawing in and compressing of
gas to exhaust it to atmosphere. It has an
eccentric circular piston that rotates
around the cylinder to create vacuum.
This pump requires a Rotary Vacuum
pump oil seal between the metal surfaces
of the piston to separate the incoming and
exhausting gas in the pump. The circular
piston, rotating around the pump sucks in
air from the chamber, compresses it and
drives it out from the pump to create
vacuum. Rotary Vacuum Pump oil
provides lubrication also.
Q.17 What is a dry rotary vacuum pump. Compared to oil-sealed pump,
is it economical to use?
Ans. A dry pump does not depend on Rotary Vacuum Pump Oil for its operation.
In this pump a set of spirals draw air in to the center of spiral, continuously
compressing it. Air thus compressed finally exits from the center of spiral. These
spirals are normally made of Ceramic materials.
Because of very high cost this pump is not very popular in vacuum industry and
is used only where oil free vacuum is essential.
Q.18 Oil rotary vacuum pump or dry vacuum pump Which works out
cheaper?
Ans. A conventional rotary vacuum pump using rotary vacuum pump oil works
out cheaper. Dry pump have a very high cost because of ceramic components
used in them. Dry pumps are mainly used in industries like semiconductor
industry where cost is not of much importance.
Q.19 What is Holding Pump?

Ans. Holding pump is a simple rotary vacuum


pump of small capacity. Its function is to create
holding vacuum for diffusion pump, hence the
name holding pump. It is invariably connected
to diffusion pump and not directly to the vacuum
chamber.

Q.20 Why should I buy rotary vacuum pump oil from Supervac
Industries?
Ans. Supervac Industries, New Delhi, India is a reputed and trusted supplier of
Rotary Vacuum pump oil. More than 90% of companies using vacuum
systems in India are buying vacuum consumables from Supervac
Industries for more than 15 years.
.

Chapter 3: Molecular Distilled Vacuum Pump Oil: Explanation and


Advantages
Term molecular distilled vacuum oil (or MD oil) is often used in specifications of
vacuum oils especially for rotary vacuum pump oils. But very less literature is
available on molecular distillation which creates confusion amongst
maintenance engineers as to what exactly is Molecular distillation and how is it
different from fractional distillation (which is a common way of distilling liquids).
This blog post elaborates the process of molecular distillation in vacuum oils.

What is Molecular distillation?


It is special liquid-liquid separation
technology, which is quite different
from fractional distillation. In
molecular distillation we make use of
the difference of molecular mean
free path of different substances.

What is Molecular Mean Free


Path?
As we understand molecular mean
free path is the average path
travelled by a molecule between
two strikes.

The Process
In molecular distillation the liquid to
be distilled is made to flow in a very
thin layer in laminar flow on a heated
surface. Due to heating, the liquid
molecules go into vapor phase.
Because of difference in mean free paths the lighter molecules will travel farther.
A condensation surface is placed at an appropriate distance. Lighter molecules
having longer mean free path are able to travel to the condensation surface
where they condense and are guided on a separate path and removed. Heavy
particles in the meantime stay close to the heated surface and are guided on a
different path, separating the two. This process is carried out in vacuum.
Often molecular distillation is repeated 2 or 3 times and the resultant vacuum
oil is called Double Molecular Distilled Vacuum Oil or Triple Molecular Distilled
Vacuum Oil.

Molecular distillation is used in the manufacture of vacuum oils like:-

1. Rotary Vacuum Pump Oil


2. Diffusion Pump Oil
3. Booster Pump Oil

Why are Molecular distilled vacuum oils superior to normal vacuum


oils?
Molecular distilled vacuum oils offer the following advantages:

1. For rotary vacuum pump-


When the rotary pump starts it is at room temperature but it quickly reaches its
working temperature of about 80oC. At this temperature non-molecular distilled
oil will start releasing vapors of volatile impurities which will affect the vacuum
level adversely and increase the vacuum time. In molecular distilled rotary
vacuum pump oil the volatile impurities have already been removed so no
vacuum drop will take place.

2. For diffusion vacuum pump-


In diffusion pump oil if different fractions of oil start evaporating at different
temperatures then the desired vacuum level will never be achieved. Molecular
distilled diffusion pump oils have oil of only one boiling temperature (single cut
oil) so the desired vacuum level is achieved in a short time.

3. Both in Rotary and Diffusion Pump Oils volatile impurities will quickly be
released in vacuum so the oil level will drop and the vacuum pump therefore
will need frequent topping up. But not so with Molecular distilled oil.

Conclusion

My advice to all vacuum engineers is to use only molecular distilled vacuum oils
as they ensure optimal system performance.
Chapter 4: How to Reduce Vacuum Time
Introduction

In todays competitive scenario a lot of stress is laid on increasing productivity


by using machine time effectively. In case of Vacuum coating, process time is
difficult to reduce without
compromising on quality (NOT
acceptable). So reducing
vacuum time (time required to
create desired level of vacuum
before starting operation) is the
only option. For example- For a
batch metallizer where cycle
time is 30 minutes a saving of 3
minutes in vacuum time can
increase productivity by as
much as 10%. Production
engineers therefore are always on a lookout for fine tuning the procedures to
reduce vacuum time.

In this chapter various steps to reduce vacuum time have been discussed.

These are detailed as under:-

1. Good Quality Rotary Vacuum Pump Oil:

It is quite surprising that some


engineers continue to use automotive oils or hydraulic oils to run Rotary
Vacuum Pump. These oils have a lot of volatile impurities which are released
when Rotary vacuum pump goes to its normal working temperature of about
800C. This results in rotary pump taking longer time to create vacuum and never
achieving its full capacity to create vacuum. Also these oils have a lot of sulphur
and other impurities that attack vacuum seals causing vacuum time to increase
further.

Since rotary vacuum pump forms the foundation of vacuum system using wrong
oils over here affects the ultimate vacuum and vacuum time adversely. Good
quality rotary vacuum pump oils like Premium Quality Synthetic Rotary Vacuum
Pump Oil SV-77 can cut down vacuum time considerably and improve the
ultimate vacuum also.

2. Use of Vacuum Grease:

Humble Vacuum Grease plays a very important role in sealing minor leakages.
Minor leakages mostly go
undetected but increase
vacuum time. Using good
quality vacuum grease like High
Vacuum Silicone Grease SV-
G9 on all O-rings and oil seals
can go a long way in reducing
vacuum time. This is
particularly important on O-
rings like main O-ring of
vacuum chamber. For details
please read a detailed blog post
on this subject here.

3. Vacuum Chamber Cleaning:

Properly cleaned vacuum chamber can reduce vacuum time by up to 15

4. Good Quality Diffusion Pump Oil:

Since Diffusion pump is responsible for


creation of high vacuum, so good quality
diffusion pump oil goes a long way in
improving efficiency of vacuum system.
Silicone oils are preferable over messy
and out dated hydrocarbon diffusion pump
oils. Next generation Diffusion pump oils
like High Vacuum Silicone Diffusion Pump
Oil SV-SIGMA create very high vacuum
quickly reducing overall vacuum time.

5. Baking of Vacuum Chamber:


Vacuum Chamber contains a lot of absorbed gasses and moisture on its
surface. These get released under vacuum, increasing the cycle time. Baking
the vacuum chamber at minimum temperature of 150o C for at least 4 hours
under vacuum can result in removal of these gasses causing improvement of
vacuum time by 10% to 15%.

Metallizer

6. Timely Change of Vacuum Oils:

Many times because of tight production schedule or to save cost, vacuum oils
are not changed on time. This results in vacuum time going up. Vacuum oils
therefore must be changed as per frequency specified by manufacturer.
Sometimes, the process gases tend to deteriorate the vacuum oil. This can be
checked by observing the color of the oil. If it is dark and not transparent or even
golden yellow in color, it is time to discard that oil and go for a fresh charge.
7. Air Conditioning:

Moisture in vacuum chamber is most difficult of gasses to remove as water


being polar in nature forms layers of absorbed moisture and these layers are
held by static charge so difficult to remove.
Air conditioning of metallizing area reduces the moisture and hence helps in
improving vacuum time. As an alternative to air conditioner, dehumidifier can
also be used.

Moisture on the vacuum chamber surface


8. Pre Treatment of substrate to be coated:

Substrate to be coated also has absorbed


gasses and moisture on its surface. This gets
released under vacuum. Release of gasses is
further accelerated because of heat created by
the heat source like evaporation boat or
tungsten wire etc. which are employed to
evaporate Aluminum.
Pre Treatment of substrate may involve
heating of substrate under vacuum prior to
metallizing or simply storing it properly in low
humidity atmosphere.

9. Vacuum Chamber Design:


Proper design of vacuum chamber is essential for minimizing the vacuum time.
Although this is a very detailed subject but following two basic precautions are
necessary:

(a) Vacuum chamber shouldnt be a source of virtual leaks. Many times the
design of system is such that from some part of vacuum chamber air is not able
to escape freely. This results in pressure differential within vacuum chamber.
For example, vacuum chamber may have been pumped down to 1 x 10-5 Torr
but a part of chamber from which free escape of air is not possible may have
vacuum of only 1 x 10-2 Torr. Slowly when the vacuum will be equalized in the
chamber, then this will show as a vacuum drop, resulting in time wastage with
respect to vacuum time.

(b) Pumping system should be connected to vacuum chamber as much as


possible in the center of vacuum chamber to draw air out faster and more
effectively

10. Design of Pumping System:

Pumping system should always be designed taking into consideration the


volume of vacuum chamber and gas load of the process. Sometimes to reduce
costs pumping system capacity is sacrificed. This proves counterproductive.
Also pumping system must have a Booster Pump between Rotary Vacuum
Pump and Diffusion Pump to increase the pumping speed.

Conclusion:

If above mentioned ideas are applied diligently, vacuum time can be reduced
and productivity increased by 10-15%. Not only this, implementing these ideas
will also result in improvement in quality of metallization.
Chapter 5: Graphite Foil Top 10 Questions Answered
Q.1 Is there an alternative to graphite foil for metallizing?

Ans. Graphite foil is highly


conducting, flexible, compressible
and relatively inexpensive. It
serves to plug the gap between the
evaporation boat and the copper
clamp and so prevents any
sparking that may take place.
There is no alternate to graphite foil
as no other material meets all these
criterion.

Q.2 How should I determine what size of graphite tape I should be using?
Ans. Size of graphite tape is defined by the thickness and width. Choice of
thickness of graphite tape is based on condition (wear) of copper clamps. In
new machines thickness of 0.2mm is normally used. As copper clamps keep
wearing, thickness of graphite tape can be increased to 0.35mm and then
0.5mm.
Width of graphite tape is determine by the size of evaporation boats.

Q.3 Why use expensive Graphite Foil for a Metallizer?

Ans. Inside a vacuum chamber, Graphite foil is used as an electrically


conducting gasket between the Evaporation Boat and the Copper Clamp. Here,
it performs various important functions:
1. It has to let very high electrical current pass without any resistance
2. It has to protect the costly Evaporation Boat from overheating and
cracking and
3. It has to protect the Copper clamp from overheating and melting.

For all these functions to be performed efficiently, the graphite foil must be of
top quality packing in denser amounts of graphite per sq.cm. as well as be
very pure. Sadly, often for the sake of cost cutting or out of sheer ignorance,
cheap, low quality, plumber grade graphite foil is used which leads to disastrous
consequences. Plumber grade graphite foil cannot perform the aforementioned
functions. This low quality graphite foil is not 100% pure since it is made with
binders like resins, adhesives and rubber compounds which start releasing
vapors when heated. These vapors bring down the vacuum and also cling to
the substrate, thus affecting the quality of metallizing.
Placement of Graphite Foil

Q.4 What is the work of graphite foil in metallizing?


Ans. Graphite foil is placed between evaporation boat and copper clamp. Its
work is to fill any gaps between the two and provide smooth current flow. In
absence of graphite foil there will be sparking between evaporation boat and
clamp resulting in damage to clamp and boat and power wastage.

Q.5 How is graphite tape (used in metallizers) made?


Ans. A good quality graphite tape is prepared by exfoliating graphite powder
and then compressing it under high pressure in a power press. This graphite
tape does not have any binders and is therefore most suitable for use in
Metallizers.
Q.6 Why is graphite foil used with ceramic evaporation boat in
metallizing?
Ans. Evaporation boats get current from copper clamps and get heated up.
Since surface of neither evaporation boat nor copper clamp is perfect so small
gaps are left which cause sparking.

Graphite foil is put between boat and clamp. This fills any gaps. Further graphite
foil is highly conductive so it prevents sparking and ensures copper heating of
evaporation boats.

Q.7 What are the basic properties of graphite foil used in a metallizer?

Ans. A graphite foil used in metalizing should have following properties-


1. It should be made of high quality graphite powder not having any
impurities.
2. Graphite foil should have been made without using any binders, resins
etc. graphite content in this foil should be more than 99%.
3. Graphite foil should have high compressibility.

Q.8 What is the difference between special purpose graphite foil used in
metallizing and normal graphite foil?
Ans. Graphite foil used in metallizer is of very high purity (more than 99%) as it
is required to transmit very high current (up to 700 amp).

Q. 9 What is the difference between crinkled graphite tape and plain


graphite tape? Which is better?
Ans. Crinkled graphite tape is corrugated as shown below whereas plain
graphite tape has a uniform cross section.

Plain graphite tape is better because of its uniform cross section it provides
better contact between evaporation boats and copper clamps.
Q.10 Some suppliers supply graphite foil in very long rolls of
30m/50m/100m whereas Supervac supplies in 500mm length. Why is it so?
Ans. Graphite foils supplied by Supervac are
made from 100% pure graphite powder which is
pressed into the form of foil by a patented
process of exfoliation.
Other suppliers who do not have this technology
add binders to graphite powder so that it can be
rolled into long rolls of 30/50/100 meters.
Needless to say binders affect the performance
of graphite foil adversely.
Chapter 6: Silicone Vacuum Grease Explained
What is Grease?

Grease is a lubricant in a semi-solid state. It is


generally applied to those machinery parts where
liquid lubricants would not stay and need to be
applied only occasionally.

Water Resistant Sealant for Joints

It also works as a sealant to keep out moisture and other unwanted materials
from the system.

How is grease made?

Grease is made with a base oil or lubricant mixed with a thickener. The quality
and properties of grease are therefore primarily determined by the following
factors-
1. The base oil
2. The thickener
3. Special purpose additives, if any

How is the base oil in grease important?


We all know that lubricants can oxidize. But do you know that greases can
oxidize too? That is because of the base oil that makes up the grease.

Good base oil = Good grease


Low Quality base oil = Low Quality grease
Oxidized base oil = Oxidized grease

Hydrocarbon base oil in grease, when oxidized, will produce carbonization


leading to progressive hardening and crust formation. This can lead to
substantial damage to the moving machine parts as well as permanently ruin
the o-rings and seals.
What is the Drop Point in grease?
Generally, grease breaks down when subjected to
temperatures that exceed its melting point or the
Drop Point. This is that critical temperature where
the gel structure of the grease breaks down and
turns into liquid form. The base oil, thickener and the
additives separate. This transformation is always
irreversible. On cooling, it regains neither its
consistency fully nor its former performance.

When heated beyond its Drop point, grease softens,


leaks and bleeds into the system. For vacuum
systems this spells disaster.

So does it mean that the Drop Point of a grease


is determined by its base oils boiling point?
Yes, primarily. It also depends to an extent on the proportion and quality of the
thickener used. How a particular grease will behave under extreme conditions
like high pressure and temperature depends upon the properties of the base
lubricant in it.

Does the grease have a low temperature too?


Yes, just like the melting or Drop point, grease has a low temperature too at
which it stiffens. At this cold or low temperature grease becomes too hard to be
of any use for the moving components. Instead of lubricating them, hardened
grease can damage the o-rings and seals or the moving parts like bearings etc.
by stiffening and jamming them.

Again, the base oil determines the lowest temperature of grease.


Are all greases alike?
No, the difference in the components makes greases differ from one another.
There are hydrocarbon greases as well as silicone greases.
Synthetic Multi-Purpose Grease

Then there are synthetic multi-purpose greases. Within these 3 categories too,
greases differ based on the type and grade of the base oil used. Different
industries require grease that caters to their specific needs. For example,
Dielectric grease is used by the electrical industry; special automotive greases
are used by the automotive industry;

Food grade grease is required in machines where it is likely to come in contact


with edible ingredients and so on.0

How does silicone grease differ from hydrocarbon grease?

As the name suggests, the basic difference lies in the type of base oil in both.
Hydrocarbon based greases are mineral oil based while silicone grease has
silicone oil as the base oil. Hydrocarbon based grease is used primarily by the
automotive industry and mechanisms requiring high frictional lubrication which
makes use of greases thixotropic property. Silicone grease on the other hand
is most suited for lubrication as well as a sealant because of its water resistant
property. Unlike hydrocarbon based grease, silicone grease does not damage
rubber seals and O-rings. Also the latter are very thermally stable; so they can
withstand extreme working temperatures.

What is special about Supervac Silicone Vacuum Grease- SV-G9?


The following merits of High Vacuum
Silicone Grease- SV-G9 qualify it as top
quality high vacuum grease:

1. SV-G9 is made especially for the vacuum


coating industry keeping in mind the
parameters of the vacuum systems.
2. Its base oil is good quality silicone
vacuum oil with a temperature range of -
25 C to 250 C.
3. Its also called high vacuum grease because it has been designed
for systems requiring vacuum up to 10-9 Torr
4. SV-G9 lubricates and preserves the O-rings and seals and doesnt let them
swell or soften up with heat.
5. It contains no additives. Because of this, no unwanted vapors are released
into the vacuum chamber that can adhere to the substrate as impurities.
6. It is stiffer than normal silicone greases;
hence, even in very high temperatures,
it remains non-runny and maintains its
consistency.
7. Its an excellent water-proof sealant for
the joints which keeps out the moisture
from the system; so, is a must-have for
all the vacuum systems.
8. It has very good tackiness so it adheres
to the surface sealing the vacuum.
9. It has extremely low vapor pressure and
hence it is extremely suitable for
vacuum applications.
10. It is resistant to attack of most acids, alklies and water.

Formulated from high quality silicone vacuum oil as the base oil, SV-G9 is ideal
for the vacuum coating industry. Whats more, SV-G9 is very competitively
priced. It comes in the packing of 100g and 1 kg.
Supervac High Vacuum Silicone Grease SV-G9
SV-G9 is exact equivalent of Dow vacuum grease and exhibits all the qualities
of the latter minus the high cost. Vacuum coaters, world over, are using this
product with utmost satisfaction.
Chapter 7: Vacuum Oil Equivalents
A lot of confusion exists in the vacuum industry.
Reasons-
1. Engineers do not know which oil is equivalent to the oil supplied by their
plant manufacturer.
2. Equipment manufacturers rarely give detailed specifications of vacuum oil
to be used.
3. Equipment manufacturers keep changing their recommendation from time
to time.
4. The vacuum oils supplied by equipment
manufacturers are prohibitively costly
which is a big drain on the very
profitability of operations.
5. Availability of oil recommended by the
plant manufacturer may not be there in
the country of user.

User of equipment therefore is forced to pay through the nose and also keep
huge inventory of vacuum oil.

6. Sometimes vacuum oil being used goes out of production leaving users in
the lurch, For example production of DC-704 was discontinued and
equipment manufacturers never bothered to inform users of a replacement.
Users were left wondering what to use in place of DC-704.

Users of Vacuum equipment are most of the time wondering What if a database
existed which clearly told me which vacuum oil can be substituted by what
vacuum oil. Even better if this database gave
him transparent, easy to understand reason.s as
to why one vacuum oil is alternative to the other
vacuum oil. This would surely save a lot of money
and botheration for vacuum equipment users.
Based on my exhaustive and in-depth study of
vacuum oils, I have prepared an extensive list of
vacuum oils being used by the vacuum industry
and their equivalents/replacement. The list also
details the important properties of these oils because of which these are
substitutes.

DIFFUSION PUMP OIL

Common Properties
Equivalent
Supervac Grade that make them
Oils
Interchangeable

SV-Sigma High Vacuum


Silicone Diffusion Pump
Oil 1. Silicone Diffusion Pump
Oil.
1. DC-704 2. Ultimate vacuum of the
2. CVC-4 order of 1 x 10-7 Torr.
3. Hivac F4 3. Boiling
4. Ulvoil D31 Temperature 2200C
5. Indomet 4. Gasses being pumped
Tetra out are corrosive or
have high moisture.
5. Long service life.
SV-Sigma + Ultrahigh
Vacuum Silicone Diffusion
Pump Oil 1. Silicone Diffusion Pump
oil.
2. Ultimate vacuum of the
order of 1 x 10-9 Torr.
1. DC-705,
3. Boiling temperature
2. Hivac F5.
2550C.
4. Gives very clean
vacuum.
5. Very long service life.

SV-Sigma Fast Silicone


Diffusion Pump Oil 1. Silicone Diffusion Pump
Oil.
2. Ultimate Vacuum of the
order of 1 x 10-6 Torr.
1. DC-702. 3. Boiling temperature
1900C
4. Vacuum is created very
fast.
5. Long service life.

SV-Delta Diffusion Pump


1. Hydrocarbon Diffusion
Oil
Pump Oil.
1. Lion S 2. Ultimate Vacuum of the
2. Lion A order of 1 x 10-5 Torr.
3. Ulvoil D11. 3. Boiling Temperature
4. CVP 300 2350C.
5. CONVOIL 20 4. Economy of operation
is very important.
5. Service life 3-6 months.
ROTARY VACUUM PUMP OIL

Common Properties
Supervac Grade Equivalent Oils that make them
Interchangeable

1. Can create vacuum


1. GS-77 of the order of 6 x
SV-77 Rotary Vacuum Pump 2. LVO 200 10-4 Torr.
Oil 3. LVO 210 2. Water white
4. LVO 240 Synthetic Oil
5. LVO 260 3. Vacuum is created
6. LVO 300 very fast.
7. LVO 310 4. Can pump out
8. Molycoat L- corrosive gasses
1668FG and high moisture.
9. MD 505 5. Down time of pump
10. Eurolube is very low as oil
A-6, BV-4 has very low level
of impurities
1. R4
2. R7
3. Ultragrade19
4. AdixenA120
5. Mobil DTE Oil
6. MD502
1. Can create vacuum
7. MD504
of the order of 1 x
SV-68Rotary Vacuum Pump 8. N62
10-3 Torr.
Oil 9. VM 68
2. Organic Distilled oil.
10. MR 200
3. Economy of
11. LVO 100
operation is of
12. LVO 110
paramount
13. LVO 120
importance.
14. LVO 130
4. Rotary Pump is not
15. Molycoat L-
a front line pump
0610
and is backing a
16. VM 100
Diffusion or Booster
17. KV100
pump
18. N62
5. Operating
19. CVC 70/19
conditions are not
20. INLAND 19
very demanding.
21. Alcatel
Adixen A 200
22. Alcatel
Adixen A 120
23. NEOVAC
MR-200
These are not meant
1) Hydraulic for Vacuum Pumps
Oils, and can seriously
2) Automotive damage vacuum
oils pump. NEVER USE
THESE for Vacuum
3) Turbine oils
Pump.
BOOSTER PUMP OIL

Common Properties
Equivalent
Supervac Grade that make them
Oils
Interchangeable

1. Silicone Booster
SV-JS Silicone Vapour Jet Pump Oil.
Booster Pump Oil 2. Ultimate vacuum of
the order of 1 x 10-
5
Best in the Torr.
world. No 3. Can pump out
equivalent corrosive gasses
exists and high moisture.
4. Creates vacuum
very fast.
5. Gives long service
life and ensures low
down time.
SV-JH Organic Vapour Jet
Booster Pump Oil 1. Hydrocarbon
Booster Pump Oil.
2. Ultimate Vacuum of
1) Apiezon the order of 5 x 10-
booster 4
Torr.
pump oil AP 3. Economical to use.
201 4. Service life 4-6
months.
5. Creates vacuum
fast.
Conclusion-

Common Properties
Equivalent
Supervac Grade that make them
Grease
Interchangeable

1. Water proof and


moisture resistant.
2. Very low vapor
pressure.
SV-G9 High Vacuum 3. Corrosion inhibitor.
Silicone Grease 4. SV-G9 can withstand
temperatures as low as
-25C to as high as
1. MOLY KOTE
250 C.
M44
5. Will not catch fire.
6. Will not be runny at
high temperatures.
7. Will not form solid
deposits on the
vacuum system in low
temperatures.
In todays competitive scenario it is important that production costs are
optimized. Most of the times we are not at liberty to buy exorbitantly priced oils
from equipment manufacturer; neither can we keep a huge inventory of
vacuum oil just because it is not easily available in the country of operation.
Supervac therefore came up with manufacture of vacuum oils that are-

Reasonably priced
Excellent substitutes for costly vacuum oils
World class quality manufactured using cutting edge technology
Have very long service life
Delivered immediately
Available world over
Part II

Diffusion Pump Oil


Chapter 8: Boiling Temperature of Diffusion Pump Oil Explained
A lot of confusion exists in the vacuum industry about certain things, for
example-
What should the optimum temperature be set in diffusion pump heaters so
as to get maximum level of vacuum in shortest possible time?
How can the temperature in diffusion pumps be set in such a way that the
engineers are able to get maximum life from costly diffusion pump oil?
Is boiling temperature of silicone diffusion pump oil different from
hydrocarbon diffusion pump oil?
Before attempting to understand optimum boiling temperature of diffusion
pump oil, let us take a brief look about working of diffusion pump.
Since efficiency of diffusion pump depends solely on the working cycle of
diffusion pump oil (diffusion pump has no moving parts) so this is evident that a
higher diffusion pump temperature will mean a higher ultimate vacuum.
Obviously a question comes to mind at this stage that why dont we increase
the boiling temperature to highest possible level. Answer to this is that
increasing the temperature of diffusion pump oil involves financial implications
(cost increase) because of the following reasons
1. Diffusion pump oil works in very difficult environment where there is vacuum
and high temperature. So to increase the boiling temperature, superior
(obviously costlier) oil will be required which is capable of withstanding these
adverse conditions.
2. At higher temperature O-rings and oil seals may give way so better quality
sealing material is required (Costly again).
3. For handling higher temperature, construction of diffusion pump also has to
be stronger.
4. For attaining higher temperature higher energy charges will be incurred.
5. For obtaining higher temperature longer time is required so vacuum time
increases.

Decision about boiling temperature is basically a balance between level of


vacuum required and cost incurred. Our guideline in line with the established
practice in the industry is as below

Vacuum Temperature in Supervac Equivalent


S.No
Required Diffusion Pump Products Products

10-9 to 10- DC-705


1 245C SV-SIGMA+
10 Torr Hivac F5

DC-704
10-7 to 10-8 CVC4
2 220C SV-SIGMA
Torr Hivac F4
Ulvoil D31

10-5 to 10-6 SV-SIGMA


3 180C DC-702
Torr FAST
Some Myth no.1: Boiling temperature of hydrocarbon diffusion pump oil
is different from boiling temperature of silicone diffusion pump oil This
myth is baseless as boiling temperature of both hydrocarbon and silicone
diffusion pump oil is same. For example- Well known hydrocarbon diffusion
pump oils like Supervac SV-DELTA, Lion S, Ulvoil D11 and CVP300, all have
boiling temperature of 220oC.Some myths are prevalent in the industry about
diffusion pump oils. These are clarified as under-

Myth no.2: My diffusion pump has been designed for


hydrocarbon/silicone diffusion pump oil only This is also false. You can
use any diffusion pump oil (hydrocarbon or silicone) in any diffusion pump
based on your requirement. For details about merits of hydrocarbon and silicone
diffusion pump oil please read my blog post- Silicone Diffusion Pump Oil vs.
Hydrocarbon Diffusion Pump Oil

SV Sigma SV - Delta

Myth no.3: My equipment manufacturer asks me to use only a particular


brand of diffusion pump oil which is exorbitantly priced Your equipment
manufacturer is trying to fleece you. For details about equivalent vacuum oils
manufactured by reputed and established manufacturers anywhere in the world
please read our blog post at- Vacuum Oil Equivalents. In case you dont find it
there then please contact us. We will help you find an equivalent product.
Myth no.4: There is no need of topping up Absolutely false and dangerous
myth prevailing in the industry. Topping up at regular intervals is of utmost
importance to get proper vacuum and avoiding damage to the equipment.

Myth no.5: Charging less diffusion pump oil in diffusion pump


reduces vacuum time Absolutely false. Charging less oil than required will
cause back streaming, burning of diffusion pump oil and damage to costly
equipment.

Myth no.6: My diffusion pump oil works at 170oC Diffusion pumps do not
work at temperature below 180oC. Your oil supplier is supplying you cheaper
vapor jet booster pump oil.

Conclusion:-
Based on the information given above I am sure that you will be able to
choose the right diffusion pump oil as per your requirement. For example- if
level of vacuum required is only up to 10-5 Torr and equipment is old then
hydrocarbon diffusion pump oil will work more economical. Similarly if vacuum
level required is 10-7 Torr then there is no point in using SV-SIGMA+.
Furthermore by using simple precautions like frequent topping up you can get
a much longer life and value for money from your diffusion pump oil.
Chapter 9: Know All About Diffusion Pump Part-1
Q.1 How does a diffusion pump work?
Ans. A diffusion pump works on the principle of gas diffusion to create vacuum.
In a diffusion pump, diffusion pump oil is heated to its boiling temperature. Vapor
of this oil is compressed in a vertically tapering hollow cone as it moves up.
Simultaneously this oil vapor escapes from jets along the height of hollow cone.
Oil vapor escaping at great speed traps air and then collides with water cooled
wall of Diffusion Pump and moves down. Trapped air is released at bottom of
Diffusion Pump. This creates differential pressure in diffusion pump. Pressure
at top is minimum (high Vacuum) and at bottom is maximum (low Vacuum) from
bottom of diffusion pump the air is sucked by rotary pump.

Q.2 Is a diffusion pump made only in cylindrical shape?


Ans. Diffusion Pump has been successfully made in rectangular shape also. In
fact rectangular shaped Diffusion Pump has an advantage that its inlet
connected to Vacuum Chamber can be of larger area and Diffusion Pump itself
can be adjusted to occupy less space. This also works with Diffusion Pump Oil
as a working medium just like cylindrical Diffusion Pump.

Q.3 I understand that Turbo molecular pump (TMP) is an alternative to


diffusion pump. Is it better or worse than diffusion pump?

Ans. Turbo molecular pump works on the principal of positive displacement. In


this pump a series of inclined blades are mounted on a
shaft which rotates at very high speed. These are called
Rotors. Fixed blades or stators are fixed in such a way that
Rotors and Stators alternate. Because of rotation of shaft
and incline rotors push air down to next row of Stators.
Stators too are inclined in same direction and push this air
to next row of Rotors and so on to exit, where a Rotary
Pump draws away the air.
Though this pump creates good vacuum and can be used
in place of Diffusion Pump but its applications are limited
to critical applications like semiconductor coatings. This is
because of its high cost, more requirement of maintenance and the fact that
since this pump cannot be made of large size because of mechanical
considerations, a diffusion pump can be replaced only by a couple of Turbo
molecular pumps. Diffusion Pump on the other hand has no moving parts and
requires almost no maintenance other than Diffusion Pump Oil change, is
cheaper in cost and can be built in almost any size.

Q.4 Why is topping up required for Diffusion Pump Oil?


Ans. In a Diffusion Pump, DP oil evaporates to produce diffusion action. Since
oil is in vapor state so part of it is lost by leakage, some of this oil vapor is also
sucked away by Rotary Pump. It is therefore important that lost diffusion pump
oil is leveled up by topping.
Not topping up will result in overheating of the remaining oil and loss of oil as
explained above will further speed up, causing a drop in vacuum. In extreme
cases Hydrocarbon Diffusion Pump Oil may burn to tar like substance and
Silicone diffusion Pump oil may turn into grey colored crystals.

Belt Driven Rotary Vacuum Pump

Q.5 Why can a diffusion pump not work alone and requires a rotary pump
as backing pump?
Ans. A diffusion pump merely creates a vacuum gradient where top of diffusion
pump has a higher vacuum and bottom of diffusion pump has much lower
vacuum. A diffusion pump has no moving parts to force air out, so though lower
portion of Diffusion pump has a low vacuum but since it is still better than
atmospheric pressure so air will not flow out.
This lower portion of diffusion pump is connected to rotary vacuum pump. Since
vacuum in lower portion of Diffusion Pump is lower than what Rotary Vacuum
Pump Oil is able to create so Rotary Pump evacuates the diffusion pump and
diffusion pump is able to work.

Q.6 How can I get more life from my expensive Diffusion Pump Oil?
Ans. Diffusion pump oil is one of the costly consumables of the metallizer. With
a few precautions, its life can be prolonged and money saved.
1. Never open the pump when the oil is still hot. Exposing the hot oil to air
changes its viscosity, making it thick gel-like.
2. Take care to top up the oil in the pump in a timely way so as to avoid
accidental over heating of the oil.
3. Keep a timely watch on the pressure and heater gauges.
4. Back streaming of vapors from the vacuum chamber and/or Rotary pump
letting its vapors in to the Diffusion pump are two reasons for the DP oil to
get contaminated. This can be prevented by installing filters above the
chevron baffle of the DP and on the line in between the rotary and the
diffusion pump. These filters must be cleaned from time to time.
5. Silicone DP oil decomposes on coming in contact with even trace elements
of alkali metals e.g., sodium, potassium, cesium etc. Do not allow them
and/or their vapors to come in contact with the DP oil.
6. Keep a check on the water flow through the cooling lines for proper cooling
of the hot oil inside the diffusion pump.

Q.7 Do I need to open & clean jets of my diffusion pump every time I
change oil in it?
Ans. If you are using a good quality silicone diffusion pump oil then there is no
need of cleaning jets every time you change oil cleaning be done once in 4 to 5
years. However if you are using hydrocarbon diffusion pump oil then cleaning
is a must every time you change oil.

Q.8 Is DC-702/DC-704/DC-705 Diffusion pump oil still available? If not


then what is the alternative?

Ans. DC-702/DC-704/DC-705 these oils are


no longer available in the entire world as the
manufacturer Dow corning stopped the
production of these oils more than a year back.

SV Sigma SV Sigma+ SV Sigma Fast

Supervac Industries supplies SV-SIGMA, SV-SIGMA+ and SV-SIGMA FAST as


alternatives of DC-704, DC-705 and DC-702 respectively. These oils are being
used by a large number of customers in more than 20 countries.
Q.9 I observed whitish deposits in my
diffusion pump. What could this be? It is
serious?
Ans. On overheating silicone diffusion pump
oil turns into whitish grey silicone crystals.
Yes, this is serious. You need to check cooling
for diffusion pump and also make sure that
level of diffusion pump oil never falls below
minimum level. This requires topping up from
time to time. Also a faulty temperature gauge
not allowing heater cut-off to take place, can
be responsible for the oil overheating.
Silicone crystals
Q.10 What is back streaming in diffusion pump?
Ans. If the pressure is too high in the diffusion pump then the emerging diffusion
pump oil vapor from the jets trying to move down collides with air molecules in
the pump. This results in no vapor going down the pump. Contrary to this, the
vapor itself starts rising up the pump along with the air and raises pressure
instead of reducing it. This undesirable process is called back streaming.
Because of back streaming Diffusion Pump Oil can travel to vacuum chamber
or can even be removed by Rotary Vacuum pump. If it enters Rotary Pump then
it contaminates Rotary Vacuum Pump Oil also.
Chapter 10: Know All About Diffusion Pump Part-2

.
Q.11 What is the alternative of CVC4 diffusion pump oil.
Ans. Supervac Industries, New Delhi manufactures silicone diffusion pump oil
SV-SIGMA. This oil is a perfect alternative of CVC4. Infact, SV-SIGMA has a
much larger satisfied customer base and has been in use much before CVC4
started getting promoted.

Q.12 Can somebody supply me DC-702/DC-704/DC-705 diffusion pump


oil?
Ans. Dow Corning the company that manufactured DC-702/DC-704/DC-705
has stopped production of this oil since last 2 years as such this oil is not
available. Supervac Industries a leading supplier of vacuum oils worldwide
supplies the following-
1) SV-SIGMA FAST which is an alternative of DC-702.
2) SV-SIGMA which is an alternative of DC-704.
3) SV-SIGMA PLUS which is an alternative of DC-705.

SV Sigma SV Sigma+ SV Sigma Fast

Even when DC-702/DC-704/DC-705 was available a large number of


customers were using SV-SIGMA, SV-SIGMA+ and SV-SIGMA FAST
because of considerable technological and cost advantage.

Q.13 Do I need to clean jets of my diffusion pump, every time I change


diffusion pump oil in it?
Ans. If you are using good quality silicone diffusion pump oil then you need not
waste precious machine time in cleaning of jets every time you change diffusion
pump oil. Cleaning them once in about 5 to 7 years is enough.

Q.14 I am using silicone diffusion pump oil. Can I top up with hydrocarbon
diffusion pump oil?
Ans. No, Silicone diffusion pump oil should never be mixed with hydrocarbon
diffusion pump oil. So if you are using silicone diffusion pump oil then top up
with silicone diffusion pump oil and if you are using hydrocarbon diffusion pump
oil then top up with hydrocarbon diffusion pump oil.
Q.15 What should be the basic properties of silicone diffusion pump oil?
Ans. Silicone diffusion pump oil should have very low vapor pressure, should
have high thermal stability and should be resistant to oxidation. These are very
basic properties of silicone diffusion pump oil.

Q.16 What should the be basic properties of Hydrocarbon diffusion


pump oil?
Ans. Hydrocarbon D.P. Oil should have
very low vapor pressure, should have high
thermal stability and should be resistant to
oxidation. These are very basic properties
of hydrocarbon D.P. oil. Apart from these
qualities, hydrocarbon diffusion pump oil
should not have aromatic compounds and
artificial additives as these may turn to gel
form or black tar like substance and harm
the pump interiors.

Q.17 What is Holding Pump?


Ans. Holding pump is a simple rotary vacuum pump of small capacity. Its
function is to create holding vacuum for diffusion pump, hence the name
Holding Pump. It is invariably connected to diffusion pump and not to the
vacuum chamber.

Q.18 Can I use diffusion pump without using a rotary pump in my vacuum
system?
Ans. No, Diffusion pump cannot be used alone. Reasons are explained below.
A diffusion pump merely creates a vacuum gradient along its length where
vacuum in top portion connected to vacuum chamber is very high and vacuum
at the bottom of diffusion pump is low. Since even this low vacuum is better than
atmospheric pressure so diffusion pump cannot discharge in atmosphere.
Rotary pump therefore is added to evacuate the air from bottom portion of
diffusion pump.
Q.19 What is stalling of Diffusion Pump?
Ans. A Diffusion pump works on the principle of gas diffusion. This pump
requires Diffusion Pump Oil, which evaporates, gets compressed and then
escapes through jets, trapping air on its path down to the bottom of Diffusion
Pump and from there the air is evacuated by a Rotary Pump or a Booster Pump-
Rotary Pump combination.

For this arrangement to work, vacuum of minimum 10-1Torr in required to be


maintained in the main body of Diffusion Pump. Otherwise the Diffusion Pump
Oil escaping from jets in gaseous form collides with too much air available and
further raises pressure in Diffusion Pump body. This stops creation of vacuum
and is called Stalling of Diffusion Pump.
Q.20 What is the work of baffles in a diffusion pump?

Ans. Baffles are provided at the top of diffusion


pump. They stop diffusion pump oil from
escaping into vacuum chamber. Baffles should
be properly water cooled to perform their
function effectively.
Chapter 11: How To Get Maximum Life From Your Diffusion Pump
Oil
Diffusion Pump Oil is one of the costliest consumables required by vacuum
users. In the present day scenario of cut throat competition, engineers are under
a lot of pressure to reduce costs without compromising on quality. Based on my
experience of almost 20 years in the vacuum line, I have compiled a list of dos
and donts as to how one can get maximum life from the diffusion pump oil. For
the benefit of our valued customers, the facts are given below
1. Topping up at regular intervals is most important factor in getting maximum
life from Diffusion Pump Oil. Care should be taken to top up the oil in the pump
in a timely manner. In the absence of topping up, volume of oil in the Diffusion
Pump reduces, whereas heaters keep producing the same amount of heat. This
causes overheating and accelerated loss of DP oil. This further reduces the
volume of oil, which in turn causes more overheating and loss of DP oil is further
accelerated and so on.

Diagram of Diffusion Pump

2. Keep track of the water flow through the cooling lines. Check the inlet and
outlet water temperature as well as the flow rate. Lines can become clogged or
scaled over time. As Diffusion Pump oil vapor can only condense on coming in
contact with cold walls of DP. Any reduction in cooling causes overheating and
increase of pressure inside DP. This may result in loss of oil by back streaming.
3. Strange as it may sound a very low fore- pressure can also cause loss of DP
oil. This can be prevented by switching on heaters before fore pressure
becomes too low.
4. Faulty gauges for pressure/heater too, can cause accidental overheating of
the oil or the oil not getting the required heating. Check that all the gauges are
functioning properly.
5. Silicone diffusion Pump Oils have a life of about 4 times that of Hydrocarbon
Diffusion Pump Oils. Also Silicone Diffusion Pump oil does not blacken and clog
the jets of DP so Silicone DP oil works out more economical in the long
run.6. Poorly working Rotary Pump will put extra burden on diffusion pump. It
must be ensured that Rotary pump is working properly to get full life from
Diffusion Pump Oil.
7. Do not expose the oil to air when it is heated. Doing so will affect the viscosity
of the oil it thickens and vacuum reduces. To avoid air exposure valves must
be checked from time to time.
8. To avoid having the oil migrate into the vacuum chamber, a cold cap should
be fitted at the top of the nozzle assembly inside the diffusion pump. This cold
cap condenses the vapor in that area.
9. A concentric circular chevron baffle should be present at the mouth of the
pump. It allows air molecules to wander in, but traps the heavier oil vapors as
they try to escape.
10. There should be no gross vacuum leaks as this will result in deterioration of
oil quickly. Vacuum leaks also cause the pressure to drop and in extreme cases
may cause stalling of Diffusion Pump. Stalling will cause loss and deterioration
of diffusion pump oil. Such leaks can be plugged by applying silicone vacuum
grease to O rings and joints.
11. Sometimes back streaming of contaminants from the vacuum chamber
takes place causing the oil to form sludge. This is preventable by installing filters
above the chevron baffle of the diffusion pump.
12. Silicone diffusion pump oil starts to decompose if it comes in contact with
even trace elements of alkali metals (e.g. hydroxides of sodium, potassium,
cesium etc.). If process requires use of these then care should be exercised to
prevent them reaching silicone DP oil.
13. In processes like PVD, coatings requiring plasma or transparent metalizing,
gas load can cause vacuum of diffusion pump to fall below 10-1Torr. This can
result in back streaming of DP Oil or even stalling. This is preventable by
reducing the process speed or increasing the capacity of backing pumps.
Part III

Evaporation Boat
Chapter 12: Pin Holes: 5 Ways to Eliminate Them
Pin holes, sometimes also referred as pin windows, are the areas where no
metal has been deposited. These can be a big problem for quality Metallizing
especially in yarn grade metalizing where a pin hole can cause the thread to
break.
Reasons for formation of pin holes and how to avoid them-

1) If there was a particle on film that got removed after metallization, it will leave
a pin hole. This can be easily identified by careful examination as this pin hole
will also have an area of thinner metallization around it caused by shadow of
particle in the path of metal for deposition.

Pin Holes in Metallizing

Solution: Storing the film roll properly, away from dust goes a long way in solving
this problem. For this, vertical stacking of rolls in custom made wooden pallets
with core ends jutting out for handling of roll is the best possible way.
2) Spitting from boats may also cause pin holes; this is easily inferred by heat
damage to film around pin hole.
Solution: Controlling the wire feed and adjusting current to boats can solve this
problem.
3) Excessive tension while winding of film will also cause pin holes. This can be
inferred by examining the film. Here, pin holes will be elongated in the direction
of pull.
Pin Holes in Film Metallizing
Solution: Avoiding this problem requires adjustment of winding tension to the
appropriate value.

4) Residue of some solvent or masking oil on film can also cause pin holes.
These pin holes are clean and are also called pick off. These are formed by
removal of Metal from film because the solvent did not let metal adhere to the
film.

Pin Holes in Roll to Roll Metallizing


Solution: Storing the film where solvent vapors are present should be avoided.
Also, if in any application masking oil has to be put on the film; care should be
taken for its proper removal as well.
Hence, cleaning and properly storing the film solves this problem.
5) Aluminum wire that is oxidized on surface is another reason of pin holes as
Aluminum oxide will not deposit properly. This is evident by a uniform pattern of
pin holes.

Solution: Use of fresh Aluminum wire or ultrasonic cleaning of wire if wire is old,
goes a long way in solving this problem.
Pin holes on metallized film can be studied effectively by placing metallized film
on a flat surface below which a strong light source has been placed on a diffuser
to spread the light uniformly. A large area of film can be quickly scanned in this
way.
Chapter 13: Evaporation Boat: How it is made
GENERAL PROPERTIES
Evaporation Boats are ceramic components required for vacuum deposition of
various types of metals e.g. aluminum, copper, silver etc. over various
substrates.

ALFA Evaporation Boat (Supervac Industries)

They are of two types


1. A) 2 Component Boat This type of boat is made with Titanium Diboride
(Conductor) and Boron Nitride (Insulator).

2. B) 3 Component Boat This is made with Titanium Diboride


(Conductor), Boron Nitride (Insulator) and Aluminum Nitride (Insulator).

Two Component boat is longer lasting and of better quality. In three component
boat, Aluminum Nitride is added to bring down the cost. But consequently, it is
lower in life and quality as well. Hence, users prefer 2 component boats to 3
component ones.
Production of Evaporation Boats is very expensive, involving heavy, costly
machinery, raw materials and running energy costs. Also it is protected by
patent laws. Therefore, very few companies in the world are producing it.

THE PROCESS
There are 5 basic steps in the production of Evaporation Boats:
1. Preparing the powders First of all, the powder particles are brought down
to the desired size through milling.
2. Blending of the raw materials The powders are mixed together in the
desired ratio and blended thoroughly for the sake of uniformity in the raw
material.
3. Hot-pressing The blended raw material is then hot-pressed at a very high
temperature (More than 1500C)
with a pressure of more than 150
tons. This delivers a big block of
ceramic.

4. Machining The hot-pressed


ceramic block is then cut into boats
with a diamond cutter. Each boat is
ground for a smooth finish and
dimensional accuracy. A cavity is
ground into each boat.
5. Quality control Each and every boat is measured for resistivity. After final
inspection, boats are packed for shipping.

ALFA Boats come in various sizes and resistivity.


Supervac Industries make Evaporation Boats known with the trade name
ALFA ONE are made in various sizes and resistivity as per the customers
requirement. ALFA ONE boats come with Supervac Industries stamp of world-
class quality and reliability.
Chapter 14: Evaporation Boat: Get Your Moneys worth out Of It
In the present time of intense competition, it is natural that engineers are trying
hard to optimize the use of every resource to reduce costs. In
Metalizing, Evaporation Boats undoubtedly contribute most in variable cost. It
is therefore important that maximum life is derived from Evaporation Boats
without affecting the quality of Metalizing.
Based on my knowledge of Engineering, experience of nearly 20 years in
vacuum line and interaction with actual users, I have compiled a list of measures
which if implemented can enhance the life of Evaporation boats by about 25%
so that you get your moneys worth out of it.
These have been summarized as under
1) Initial heating of the new boats also called break in must always be slow to
get proper life from Boats. Reason? New boats will always have some absorbed
moisture. If the boat is heated quickly in this condition, the moisture, converted
into steam having much higher volume will have little time to escape and can
cause cracks because of high pressure build up.
2) At the end of the cycle it must be ensured that all the Aluminum or any other
metal being metalized has evaporated completely before heating is switched
off. Otherwise residual metal will seep into the pores of boats; now differential
cooling rates of boat and metal will crack the boat.
3) Care must be exercised that before the vacuum is broken, boats must have
cooled down. This is because sudden contact with cold air can cause boat
breakage. About 5 minutes is enough for boats to cool down.
4) Worn out copper clamps also are a big reason for boats not performing to
their full capacity. Non uniform wear of clamp causes sparking between clamp
and boat; this overheats and cracks the boat.
5) A good quality graphite foil is very important factor in enhancing the life of
Boat. To save money, sometimes Metallizers use poor quality plumbing grade
graphite foil. This foil contains many impurities and binders and offers
resistance to the flow of current. This causes the ends of boat to overheat and
break. Supervac supplies 100% pure graphite foil free of binders. This is made
with the patented process of Exfoliation. This foil gives you the following
outstanding benefits

A) Offers no resistance to the flow of current.


B) Saves costly power.
C) Enhances the life of Boats.

6) There is one more major factor inter linking the life of evaporation boat with
graphite foil. Good quality graphite foil has good compressibility. This allows a
proper electrical contact in boats and clamp before heating begins and
expansion of boats in heated condition. Poor quality graphite foil on the other
hand will not allow expansion of boats in heated condition putting additional
stress and subsequent breakage of boats.
7) Aluminum of purity 99% or more is required to avoid premature cracking.
Impure aluminum will have impurities which will have different boiling
temperatures; this will lead to an unstable pool of metal in boat cavity. This in
turn results in non-uniform heating of Evaporation Boat leading to thermal stress
and breakage.
8) Age of aluminum wire also affects boat life. With age, aluminum oxidizes and
Aluminum oxide thus formed causes spitting and excessive heating of Boats.
Freshly made or cleaned wire works best.
9) Hardness of Aluminum should be maintained in proper range if required by
tempering as a very hard wire is likely to puncture the boats.
10) Aluminum wire should be fed in such a way that it meets boat in the center
widthwise and in between 1/3 to lengthwise. This ensures proper pool
formation and increases the life of boats

11) Feed of aluminum wire must be regulated to ensure that some aluminum is
always available as molten pool on the surface of Boat. This makes sure that
boat is uniformly heated and increases the life of boat.
12) Power to boat must be so regulated that aluminum melts just before
touching the boat, otherwise it will cause an indentation in boat cavity, hastening
the failure of boat.
13) It has been observed that Boats made of Titanium Diboride and Boron
Nitride (also called 2 components or dimet) work out to be more economical
than boats where Aluminum nitride is also used in addition to the 2 ceramic
powders mentioned above to reduce the cost. Three component boats, though
cheaper in cost, have a markedly shorter life.
14) Experience shows that normal rectangular boats with cavity work out
cheaper than Triangular or elliptical boats or boats without cavity or laser
grooves on surface.

15) Good quality boats, manufactured by reputed companies like Supervac,


having density of the order of 98% of theoretical density have very low porosity.
This reduces aluminum seepage in boats and enhances life of boat. These
boats work out much more economical than those supplied by phony
importers/ unknown companies having no quality standards.
16) Contrary to popular myth, using boats with initial resistivity higher then
recommended by manufacturer does not give more life. In fact this wastes
power, causes overheating and premature cracking of boats.
17) Experience proves that spring loaded end support for boats works best for
optimizing the life of boats as it provides a proper contact and allows expansion
of boats on heating.
18) Level of vacuum in system is also very important for getting proper life from
boat. Working at vacuum above 1x 10-4 Torr is detrimental to the health of Boats
as they get oxidized and damaged.( For getting high level of vacuum in shortest
possible time Supervac Sigma+ Diffusion Pump oil and Supervac SV-77
Rotary Vacuum Pump Oil can be used.)
Points mentioned above are quite easy to implement and best of all do not cost
an extra rupee. This however can result in a saving of about Rs. 9, 00,000/- per
year per metallizer (a typical metallizer uses about 300 boats per month, costing
about Rs.1, 000 per boat. Saving is 300 x12 x1000 x25% = Rs.9, 00,000/-). This
is not all; implementation of these actions will also lead to better metalizing
quality, better maintained plant and saving of costly power also.
About Supervac Industries

Back in 1994 when vacuum coating industry of this country was in its nascent
stage, there were absolutely no reliable manufacturers and suppliers of vacuum
oils and other vacuum products in India. These were entirely imported. That is
when Supervac started manufacturing vacuum consumables indigenously.
With core values of High Quality at Sensible Rates, Supervac kept Customer
Satisfaction as the focal point of its growth. Today, 20 years later, we have
grown much bigger, with our products being exported to 30+ countries, but our
core values remain the same. Founded and headed by a post-graduate
mechanical engineer, Supervac Industries has two manufacturing units in
India
one in Hoshiarpur (Punjab) and another in Hyderabad (Andhra Pradesh).
The central marketing office is located in a major commercial center of New
Delhi, India. Consistent customer trust in brand Supervac is proof of our quality
and our claim of being no.1 manufacturer and supplier in India of a complete
range of vacuum consumables.
Products

Diffusion Pump Oils-


1. Diffusion Pump Oil: SV-Sigma
2. Diffusion Pump Oil: SV-Sigma+
3. Diffusion Pump Oil: SV-Sigma Fast
4. Diffusion Pump Oil: SV-Delta (Hydrocarbon)
Booster Pump Oils-
1. Vapor Jet Booster Pump Oil: SV-JS (Silicone)
2. Vapor Jet Booster Pump Oil: SV-JH (Hydrocarbon)
3. Roots Blower Pump Oil: SV-90S (Silicone)
4. Roots Blower Pump Oil: SV-90H (Hydrocarbon)
Rotary Vacuum Pump Oils-
1. Rotary Vacuum Pump Oil: SV-77 (Synthetic)
2. Rotary Vacuum Pump Oil: SV-68 (Hydrocarbon/Mineral)
Boron Nitride Powder-
1. Boron Nitride Powder: SV-BNP
2. Ultra Pure Boron Nitr:ide Powder: SV-BNP+
Boron Nitride Suspension-
1. Boron Nitride Suspension: Boronox
2. Boron Nitride Suspension: Boronox+
Ceramic Products-
1. Evaporation Boats:- Alpha One (Available in Different Sizes)
2. Graphite Foil/Tape: SV-GF (Available in Different Sizes)
3. Graphite Suspension/Paint: Graphinox
High Vacuum Silicone Grease: SV-G9

Very large scale production, patented processes and a very long service life
makes Supervac products extremely cost effective.
Technology
Supervac uses cutting-edge technology to ensure highest level of quality
conforming to international standards. We have purchased many technologies
from laboratories of international repute in order to bring the latest of worlds
technologies to our customers. Many our production processes are patented.
Quality and Innovation

Total reliability of products is maintained by 100% checks in each stage of


manufacturing. Strict adherence to the required specifications is maintained.
Supervac offers complete batch traceability of their products.

Our dedicated R&D team constantly strives to better the products, enabling the
company to deliver world-class products to our customers and thus keeping us
many steps ahead of our competitors.

Supervac Industries export their products to more than 20 different countries


in the world. More than 500 companies in India requiring application of vacuum
are sourcing products from us since many years. Customer confidence in the
form of repeated orders, is the biggest testimony to the high quality of products
manufactured by Supervac Industries.
Contact Details

Address:
B-21, Flatted Factory Complex,
Jhandewalan, New Delhi-110055 (India)
Phone number:
+91-11-2353 7331, +91-11-4355 4966, +91-11-4356 4967
Email:
info@SuperVacOils.com, sales@SuperVacOils.com
Contact Person:
Mr. Anshuman Punj
Contact Number:
+91-9810144936

Connect with us

Twitter: https://twitter.com/Supervacoils
Facebook: https://www.facebook.com/supervacindustries/
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LinkedIn: https://www.linkedin.com/company/supervac-industries
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