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Techniques for Measuring the Electrical Resistivity

of Bulk Materials

Mary Anne Tupta


Keithley Instruments, Inc.

A GREATER MEASURE OF CONFIDENCE

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A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Resistivity Measurement Overview

• ____ resistivity
Definition of electrical __ ____of a_____
material____ ______
• Methods for making resistivity_____ _____of conductors, insulators, and
measurements
semiconductors ____ _____
• Key considerations for selecting equipment
_____ _____ for measuring resistivity
• Sources of measurement errors and ways to optimize resistivity measurements
____ _____

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What is the Electrical Resistivity of a Material?

____ __ ____ _____ ____ ______


The electrical resistance of a material……
_____ _____
• is a basic material property;
____ _____
• defines how well the material will conduct an electric current;
_____ _____
• is a common electrical measurement.
____ _____
Ohm’s law relates the current (I) and the applied voltage (V) to the material
resistance (R) as follows:

V=IR

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What is the Electrical Resistivity of a Material?

____
Electrical Resistivity __ ____
= longitudinal _____
electrical ____ ______
resistance of a uniform rod of unit
_____ _____
length and unit cross-sectional area:
____ _____
A
  R_____
_____
L
____ _____
Current Source ρ = resistivity (Ω-cm)
R = resistance: V/I (Ω)
Voltmeter
V A = cross-sectional area of
L
sample (cm2)
L = distance between two
A
leads of voltmeter (cm)
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Typical Resistivity Values

____ __ ____ _____ ____ ______


The electrical resistivities of solid_____
materials_____
span over many magnitudes.
____ _____
Three classifications of materials based on their resistivities:
_____ _____
Classification ____
Type _____
of Electrical Typical Resistivities
Conductor
Metals Good electrical 10-6 Ω-cm
conductors
Insulators Low electrical 109 to 1020 Ω-cm
conductivity
Semiconductors Intermediate levels of 10-3 to 107 Ω-cm
conductivity

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Comparison of Simplified Energy Bands

____ __ ____ _____ ____ ______


_____ _____
____ _____
Conduction Band

Conduction Band
_____ _____ Conduction Band

Energy
____ _____
Energy Gap
Energy Gap

Valence Band
Valence Band
Valence Band

Metal Insulator Semiconductor

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Measuring____
the __ ____ _____of____
Resistivity ______
Conductors:
_____ _____
Metals and Superconductors (very low resistance)
____ _____
_____ _____
Graphene and other
____ Nanomaterials
_____
(low voltage and low power - use same techniques)

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Measuring the Resistivity of Conductors

____
Basic Test Procedure: __ ____ _____ ____ ______Voltmeter

_____ _____ V
1. Source current (I) through the
____ _____
sample using one pair of leads. L
_____ _____ w
2. Measure the voltage drop (V)____
across_____
t Sample
a second pair of leads a known
distance (L) apart.

3. Calculate the resistivity (ρ) of the Current Source


sample using the cross-sectional
area (A=wt) and the distance
between the voltmeter leads. V wt
   cm
I L
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Sources of Error when Measuring Low Resistance

____ __ ____ _____ ____ ______


• Test lead resistance
• Thermoelectric voltages
_____ _____
• Low frequency noise ____ _____
• External noise sources _____ _____
• Johnson noise ____ _____
• Voltmeter not sensitive enough

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Eliminate Lead Resistance by Using the 4-Wire Method

2-Wire Method
____ 4-Wire
__ ____ _____ ____ Method
______
I I
_____ _____
____ _____
_____ _____
V V
____ _____

RLead RLead
RLead RLead

RSample
RSample
Measured Resistance: Measured Resistance:
VM/I = RSample + 2RLead VM/I = RSample
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Thermoelectric Voltages

Voltmeter
Copper Test Leads
____ __ ____ _____ ____ ______ Voltmeter
Metal A V _____ _____CopperMetal
Test Leads
A V
____ _____
_____ _____
____ _____ Sample
Sample – Metal B
T1 Metal B T2

Current Source Temperature Gradient

Thermoelectric voltages are generated when dissimilar metals (Metal A and


Metal B) in the circuit are at different temperatures (T1 and T2).

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Ways to Reduce Thermoelectric Voltages

____ __ ____ _____ ____ ______


• Construct test circuits using the same materials for interconnects.
_____ _____
• Minimize temperature gradients within the test circuit.
____ _____
• Allow the test equipment to warm up.

_____ _____
Use an offset compensation method.
____ _____

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Use the Current Reversal Method


to Eliminate Voltage Offsets (VEMF)

____
Measurement __ ____
with Positive Polarity_____ ____ ______
Measurement with Negative Polarity
_____ _____
VEMF
____ _____ VEMF
_____ _____
I+ V____
M+ _____ I- VM-
R R

VM+ = VEMF + IR VM- = VEMF - IR


Voltage Measurement:
VM   VM  VEMF  IR  (VEMF  IR)
VM    IR
2 2
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Use the Delta Mode Method to Eliminate


Voltage Offsets and Noise

____ __ ____ _____


The ____ ______
Delta method consists of
_____ _____
alternating the current source polarity
and using a moving average of voltage
____ _____
readings to calculate the resistance.
_____ _____
Averaging reduces the noise
____ _____
bandwidth and therefore the noise.

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External Noise Sources

• External Noise ____


Sources = interferences
__ ____ _____ created
____by motors,
______ computer screens,
or other electrical equipment
_____ _____

____ _____
Control these External Noise Sources by:
– Shielding and filtering _____ _____
____ _____
– Remove or turn-off the noise source
– When using DC instruments, integrate each measurement for an integer number of
power line cycles. The line cycle noise will “average out” when the integration time
is equal to an integration number of power line cycles.

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Johnson Noise

• Johnson Noise –____


places__
a fundamental
____ _____ limit on resistance
____ measurements.
______
_____ _____
• In any resistance, thermal energy produces the motion of charged particles.
____ _____
This charge movement results in Johnson noise.
_____ _____
____ _____
• The formula for the voltage noise generated:
where k=Boltzmann’s constant, T= temp in K, rms V  4kTRB
B=noise bandwidth in Hz, R=resistance of sample in ohms

• Reduce by:
1. Reduce the measurement bandwidth –digital filtering (averaging readings) or
analog filtering

2. Reduce temperature of the device
3. Reduce the sample resistance (usually not practical)
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Use a Nanovoltmeter to Measure Voltage Drops

When measuring the____ __ ____


resistances _____ ____
of conductors or other______
low power materials, very
small voltages are measured, typically
_____ in the microvolt and nanovolt range.
_____
____
To measure these very small voltage _____
drops, use a sensitive voltmeter such as a
nanovoltmeter. _____ _____
Verify the____ _____
product specifications to make sure the
measurement resolution and accuracy will be able to
perform the sensitive measurement of your application.
Model 2182A Nanovoltmeter

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Review of Measurement Considerations for Measuring


the Resistivity of Conductors Voltmeter

• ____ __ ____
Make a 4-wire measurement _____
to eliminate the____ ______ L

lead resistance from affecting_____


the measurement
_____ Sample

accuracy.
____ _____
Current Source

• _____ _____
Use an offset compensation technique to
eliminate voltage offsets and reduce
____noise:
_____
Current Reversal Method or Delta Method.

• Eliminate external noise sources and use line


cycle integration.

continued . . .

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Review of Measurement Considerations (continued)

• Reduce Johnson noise by reducing the


____ __averaging
____ _____ ____ ______
 4kTRB
measurement bandwidth,
_____ _____
readings, and reducing the temperature of rms V
the sample.
____ _____
_____ _____
• Use a sensitive voltmeter, such as a
____ _____
nanovoltmeter, to measure the low Model 2182A
voltages.  Nanovoltmeter

• Use a low noise, bipolar current source that


can perform current reversals.

Model 6221 AC + DC Model 6220 DC


Current Source Current Source

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____ __ ____ _____ ____ ______


_____ _____
____ _____
_____ _____ of Insulators
Measuring the Resistivity
____ _____
(High Resistance)

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Resistivity Measurements of Insulators

____
The resistance of an __ ____
insulator is _____ ____ ______
Sample
measured by: _____ _____ Resistance
I
____ _____
1. Applying a voltage to the sample R
for a specified time period _____
Voltage
_____
V A Ammeter
____
Source_____

2. Measuring the resulting current

3. Calculating the resistivity using


Ohm’s Law and geometrical
V
considerations
R
I
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Volume Resistivity of Insulator

LO
____
Volume Resistivity is a__ ____ of_____
measure the ____ ______
A
_____
leakage current directly through _____
a material.
____ _____ HI
Test Procedure for Volume Resistivity:
_____of _____
1. Place sample between 2 electrodes area (A). Electrode t
____ _____ Sample
2. Apply potential difference (V) between the 2 electrodes.
HI
Voltage
3. Wait specified time (60 seconds) and measure current (I) Source
using sensitive ammeter. LO

4. Calculate resistivity based on the area of the electrodes


V A
and thickness of the sample (t). Units are Ω-cm.

I t
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Surface Resistivity of Insulator


I

____ __ ____ _____ ____


Electrode ______
HI HI V w
 
L
_____ _____A
Sample w
LO ____ _____ I L
LO
_____ _____
____ _____
Surface Resistivity is defined as the electrical resistance of the surface of an
insulator.

Test Procedure for Surface Resistivity:


1. Place two electrodes a known distance (L) apart on sample.
2. Apply potential difference (V) between electrodes.
3. Wait specified time and measure current (I) with ammeter.
4. Calculate resistivity using width (w) of material and distance (L) between the
electrodes. The units are ohms or ohms per square.

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Sources of Error When Measuring High Resistance

• Improper Measurement
____ __Instrumentation
____ _____ ____ ______
• Electrification Time
• Test Voltage
_____ _____
• Background Currents ____ _____
• Electrodes and Geometrical_____ _____
Considerations
• Electrostatic Interference ____ _____
• Humidity

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Use Sensitive Ammeter and Proper Cabling

Measuring the resistance


____ of insulators
__ ____ usually ____
_____ involves______
measuring current in the
1E-9 and 1E-12 current range.
_____ _____
____
When measuring very small current, _____
<100nA, it is important to use a sensitive
ammeter, such as an electrometer or picoammeter.
_____ _____
Electrometers and picoammeters____ _____
have sub-picoamp (1E-12) sensitivity.

Model 6517B Electrometer/


Voltage Source

The 6517B has 1E-15 A Sensitivity!

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Time Dependency of High Resistance Measurement

• Apply 250V ____ __ ____ _____ ____


250V Step ______
Response of Antistatic Bag
• Wait 60s _____ _____
• Measure Current
• Calculate Resistivity ____ _____
_____ _____
At 5 s, current=
1.5x10-10 ____ _____

At 60 s, current=
2.5x10-12

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Test Voltage

____ __ ____ _____ ____ ______


• _____ are
Resistivity measurements of insulators _____
dependent on the applied voltage.
____ _____

_____ _____ V
In general, as the voltage increases,
the resistivity decreases
____ _____

• Sometimes the voltage may be varied intentionally to determine the voltage
dependence of an insulator.

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Background Currents

When measuring very high resistances, background currents can cause


erroneous readings. ____ __ ____
Background may_____ ____ ______
be due to:
• charge stored in the material _____ _____
• static or triboelectric charge ____ _____
• piezoelectric effects
_____ _____
____
Background currents can be equal _____
or greater than the current stimulated by the
applied voltage.

If background current is same polarity as measured current, then resultant


current reading will be much higher than the true value.

If background current is the opposite polarity, these unwanted currents may


cause a reverse polarity current reading. This can cause the calculated
resistance to be negative!

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Alternating Polarity Method

____ __ ____ _____ ____ ______


_____ _____
Positive Voltage ____ _____
Applied and
Exponential Current _____ _____
Measured.
____ _____

Negative Voltage
Applied and
Exponential
Current Measured.

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Electrodes

Electrodes for use____ __ ____material:


on an insulating _____ ____ ______
_____ _____
• Has good contact to the material:
____ paint_____
on electrodes or use flat metal plates
with conductive rubber
_____ _____

____ _____
Should be much lower resistance than the sample and should not contaminate
the sample

• Enables easy calculation of resistivity from the geometrical considerations


Where:
Aelectrode

ρ=Volume Resistivity
R A=area of electrode on sample
t t=thickness of sample
R=measured resistance V/I
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Volume Resistivity with the


Model 8009 Resistivity Test Fixtures
Top Electrode
Electrodes ____ __ ____ _____ ____ ______
Test
_____ _____
Sample ____ _____
HI
_____
HI _____
Voltage
Ammeter A
____ Source
_____
LO
LO 0V Ring
Guard

Center Electrode
Volume resistivity is a measure of the leakage
current through the material, between the top
electrode and center bottom electrode. The outside Model 8009 Resistivity Test Chamber
ring electrode is guard.

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Surface Resistivity with the Model 8009

____is__
The Surface Resistivity ____ _____ ____
measured ______
by placing two electrodes on the_____ Electrodes
_____
surface of the test sample, applying 0V Guard
____ _____
a potential difference between them, Test
_____Sample
and measuring the resulting current. _____
____ _____ R
Notice the surface resistivity (R) is HI HI
measured between the bottom
Center Electrode and the Ring Ammeter A
Electrode.
LO LO

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Model 65 High Resistivity Measurement Package

____ __ ____ _____ ____ ______


8009 Resistivity
Test Fixture
_____ _____
____ _____
_____ _____
____ _____
6524 Software

6517B Electrometer/Voltage Source

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Electrostatic Interference and Shielding

Shield
____ __ ____ _____ ____ ______
_____ _____
____ _____
HI _____ _____ HI
Ammeter ____ _____
Sample
Voltage
Source
LO
LO

Connect Shield to LO terminal of Picoammeter or Electrometer

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Review of Measurement Considerations for Measuring


the Resistivity of Insulators

____ __ ____ _____ ____ ______


1. Use a picoammeter or electrometer for low current
measurements. _____ _____
2. ____
Use the same electrification time _____
for each test to compare
results. _____ _____ Model 6517B
3. Use the same applied voltage for test comparisons.
____ _____
4. Use the Alternating Polarity Technique to reduce the effects of
background currents.
5. Use proper electrodes and take geometrical considerations
into account.
6. Use electrostatic shielding to avoid errors due to electrostatic
interference.
7. Use an environmentally controlled room.
Model 8009

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____ __ ____ _____ ____ ______


_____ _____
____ _____
_____ _____
Measuring____ the_____
Resistivity of
Semiconductors

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Measuring Resistivity of Semiconductors

____ __ ____ _____ ____ ______


The two most common methods _____for measuring the
_____
resistivity of semiconductor materials are:
____ _____
• Four-Point Collinear Probe Method
• van der Pauw Resistivity Method
_____ _____
____ _____
Both of these methods use a 4-wire method to
eliminate both the lead resistance and the contact Photo courtesy of Lucas Signatone

resistance from affecting measurement accuracy.

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4-Point Collinear Probe Method

Test Procedure: ____ __ ____ _____ ____ ______


HI LO
_____ _____
1. Place probes in center of wafer.
2. Source current from probes 1____
to 4. _____
3. Measure voltage between probes 2 and 3.
4. Calculate resistivity: _____ _____ HI
V
LO
Measure

 V ____ _____ Voltage


Source Current

Between 2
tk From 1 To 4 And 3
ln 2 I
4-Point
Where: Collinear
ρ= volume resistivity (ohm-cm) 1 2 3 4
Probe
V=voltage measured between 2 and 3
I=source current (A)
t = sample thickness (cm) Wafer
k=correction factor
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Sources of Measurement Error

____
1. Lead and contact __ ____
resistance _____ ____ ______
_____ _____
2. ____method
Voltage offsets (use current reversal _____to reduce)
_____ _____
3. Instrumentation ____ _____
4. Issues with high resistance materials

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Test Set-Up Showing Circuit Resistances


Source Current
HI LO
____ __ ____ _____ ____ ______
_____ _____
RL=Lead Resistance
HI LO ____ _____
V RC=Contact Resistance
RL1 R
_____
R
_____
RS=Semiconductor Resistance
L2R L3 L4
____ _____

1 2 3 4
RC1 RC2 RC3 RC4 Only the voltage drop due to RS2 is
V
measured by the voltmeter.
RS1 RS2 RS3
Measure Voltage
Between 2 And 3
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Instrumentation for Mid-Range Resistances


(100mohm to <1Mohm)

Use a standard DC____ __source


current ____ _____
(bipolar ____current
to perform ______
_____
reversals) to force the current and a DMM _____
to measure the voltage
drop. ____ _____
OR
_____ _____
Use a SourceMeter which can source the current and measure the
voltage drop. ____ _____
ALSO
Use a commercially available 4-point probe head.

Photo courtesy of Lucas Signatone

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Commercially Available Automatic Resistivity System

____ __ ____ _____ ____ ______


_____ _____
____ _____
_____ _____
____ _____

Photo courtesy of Lucas Signatone

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Issues for High Range Resistances (up to 1E12 ohms)

____ probe
• Use a 4-point collinear __ ____ _____
that has ____
excellent ______
isolation between the
probes to avoid leakage current_____
errors _____
• Use a current source with high output _____ (1E14) to avoid loading
____impedance
errors
_____ _____
• Use a current source with a built-in guard to reduce the effects of shunt
capacitance ____ _____
• Use voltmeters with high input impedance (1E14 ohms)
• Use shielding to avoid errors due to electrostatic interference
• Use differential electrometer method to avoid issues of common mode
current

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Common Mode Current Errors When Measuring High R


Current
Source
____ __ ____ HI _____ R____ ______ C

_____ _____
AC
____ _____
_____LO_____
Voltmeter Common
____ _____ Mode
Current
V RV
i
RIN
Contact AC When the resistance of the sample,
Resistance RS2, becomes on the same order of
HI LO
1 2 3 4
magnitude as the isolation spec
(input LO to chassis) of the current
RC1 RC2 RC3 RC4 source and voltmeter, then common
RS1 RS2 RS3 mode current will flow affecting the
measurement accuracy.
Sample Resistance
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Making Differential Four-Point Probe Measurements


(For Very High Resistances >1Mohm)
HI LO
____ __ ____ _____ ____ ______
_____ _____
Voltmeter
____ _____
_____V _____
HI ____ _____LO

X1 X1
Buffer Buffer
HI LO HI LO

1 2 3 4
RC1 RC2 RC3 RC4

RS1 RS2 RS3

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van der Pauw Resistivity Method

____ __ ____ _____ ____ ______Force


van der Pauw resistivity is a 4-probe technique that Current
_____ _____
involves applying a current and measuring a voltage
____ _____
using four small contacts on a circumference of a flat,
arbitrarily-shaped sample. 1
_____ _____
Test Procedure: ____ _____ 4 2
• Force Current (I) on adjacent terminals
Measure
• Measure Voltage (V) on an opposite pair of adjacent Voltage
3
terminals
• Repeat measurements around sample V
• Calculate resistivity

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van der Pauw Resistivity Method

____
• vdp configuration __for
is useful ____ _____ ____
measuring ______
very small samples _____ _____
Force
____ _____ Current
• Easy to measure Hall voltage using an _____
_____
electromagnet to apply the B field B
____ _____ 1

• Force I and Measure V on opposite 4 2


terminals Measure
3 Voltage

Hall Configuration

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van der Pauw Resistivity

V5
____ __ ____ _____ ____ ______
1 2
V3
1
_____ _____
2 1 2 1 2
V7

4 3 4
____ _____
3 4 3 4 3

V1 _____ _____
____ _____
V6

1 2 1 2 1 2 1 2
V4 V8

4 3 4 3 4 3 4 3

V2

A series of 8 measurements are performed around the periphery of the sample to


compensate for offsets and are combined mathematically to compute the resistivity.

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Switching to Perform vdp Measurements

1
____
Use a switch matrix to __ ____ _____ ____ ______ Sample

automatically switch the current


_____ _____
source and voltmeter between all
4 2

four terminals of the sample. ____ _____ 3

_____ _____
Choose a switch system that will
not degrade the measurements.
____ _____ 1 2 3 4
1
Current
Source
Use offset compensation
technique – current reversals – to 2

eliminate voltage offsets due to


the switch.
3
V Voltmeter
Use same configuration to
measure the Hall voltage using 4

an electromagnet. Switch Matrix

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High Resistance vdp Measurements

Model 7065 Hall____


Effect__
Card
____ _____ ____ ______
Configuration
_____ _____
Matrix Card that switches ____ _____
current source and _____ _____
voltmeter to the 4 terminals
of the sample.
____ _____

Has unity gain buffers on


the card to avoid problems
with isolation or needing to
use an electrometer to
measure the voltage drops

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Using Four SMUs to Measure High R Samples

Model 4200-SCS with 4 SMUs and 4 preamps


____ __ ____ _____ ____ ______
– Input impedance >1016 
_____ _____
– Accurate low current sourcing, pA
____ _____SMU1 i SMU2
– No leakage errors due to mechanical I Source
V Measure
switches _____ _____
1 2
– Includes software to automate____ _____ V Difference
measurements and calculate resistivity 4 3
SMU4 SMU3
Common V Measure

Model 4200-SCS Semiconductor


Characterization System

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A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Making Good Measurements on High Resistance


Samples

• ____
Use electrostatic __ ____
shielding _____electrical
to minimize ____ ______
interference
– Shield the DUT and all sensitive
_____circuitry
_____
– Use shielded cabling
– Connect the shield to the low____
terminal_____
of the system
_____ _____
• Use guarding to reduce the effects of leakage current in system
– Guarded current source ____ _____
– Guarded voltmeters
– Use triax cable instead of coax cable

• Allow sufficient settling time


– Source I and measure V as a function of time to determine appropriate settling time
– A diamond sample can take several minutes for settling

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A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Settling Time of a 1012Ω Resistance Sample

____ __ ____ _____ ____ ______


_____ _____
____ _____
_____ _____
____ _____

Wait at least
20 seconds
for a settled
measurement

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A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Summary

____ __ ____ _____ ____ ______


•Use an appropriate method for measuring the resistivity. The method will
_____ _____
depend on if the material is a conductor, insulator, or semiconductor.
____ _____
•Choose the appropriate instrumentation.
_____ _____
____ _____
•Apply the proper measurement techniques to avoid measurement errors.

54 © Copyright 2010 Keithley Instruments, Inc.


A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Reference Materials
www.keithley.com
____ __ ____ _____ ____ ______
Low Level Measurements Handbook, 6th Edition
_____ _____
Application Notes: Hall effect,____ _____
van der Pauw
method, four-point collinear_____
probe method,
_____
insulator resistivity, low voltage measurements,
low current measurements, etc. ____ _____

White Papers: Delta method, current reversal


techniques, etc.

55 © Copyright 2010 Keithley Instruments, Inc.


A GREATER MEASURE OF CONFIDENCE | www.keIthley.com

Contact Keithley with Your Questions


Worldwide Headquarters Europe:
Within the USA: (+1) 888-KEITHLEY Germany: (+49) 89-84930740
____ __ ____
Outside the USA: (+1) 440-248-0400 _____ ____
United ______
Kingdom: (+44) 118-9297500
_____ _____ France: (+33) 1-64532020
Email: applications@keithley.com
____ _____ Asia:
_____ _____
Additional offices: www.keithley.com China: (+86) 10-82255011
Japan: (+81) 3-57337555
____ _____Korea: (+82) 2-574-7778
Taiwan: (+886) 3-572-9077

For additional information on this topic and free reference material,


visit http://www.keithley.com.

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