Solved with COMSOL Multiphysics 5.

F r e e z e - Dr y i ng
Introduction
Freeze-drying, or lyophilization, is a dehydration process that is often used to preserve
a perishable food or material. It is also frequently used as a way to remove water from
goods, making them lighter and easier to transport.

Lyophilization is widely recognized as an important technique in many industries. It

is used, for example, in the pharmaceutical industry for the preservation of antibiotics,
in the manufacturing of semiconductor ceramics, and by preservation initiatives, such
as in the restoration of water-damaged documents. And of course, the process is widely
used in the food industry, to preserve tasty snacks that can last up to 30 years. The wet
substance is frozen and ice (or some other frozen solvent) is removed through
sublimation in the presence of a high vacuum.

Freeze-drying uses a technique called sublimation, where a frozen liquid passes directly
from a frozen state and into a gaseous state. This ability for a solid to skip the liquid
phase and pass directly into the gaseous phase can be explained by a phase diagram,
where a substances state under different pressure and temperature conditions is
described. As is shown in a phase diagram, at very low pressures and temperatures, a
solid can pass directly into the gaseous stage without passing through the intermediary
liquid phase.

This example models the process of ice sublimation in a vial under vacuum-chamber
conditions, a test case for many freeze-drying setups. The model uses the Deformed
Geometry interface to compute the coupled heat and mass balances to handle the
advancing vapor-ice interface.

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Model Definition
In this example, you model the process of sublimation of pure water ice in a vial.
Figure 1 depicts the model geometry.

Figure 1: Vial model geometry.

The geometry is axisymmetric but the boundary condition presented in Equation 1

below is not. For this reason, the model must be built in 3D. Because y = 0 is a
symmetry plane, only half of the structure is represented to save computational cost.

IDEAL GAS ASSUMPTION AND MEAN MOLAR MASS

Ice occupies the domain located at the bottom. The remaining space contains vapor
generated by sublimation. It is supposed to be close to vacuum, initially at a dry air
partial pressure p0 of 20 Pa. At such a low pressure value, the vapor can be considered
as an ideal gas with a water partial pressure:

p water = cRT

where c is the concentration of water in the vapor (mol/m3), R is the gas constant (J/
(molK)) and T is temperature (K). The total pressure in the vapor domains is given by:

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p = p 0 + p vap

Hence, the mean molar mass of vapor, Mvap, is:

p 0 M air + p water M water

M vap = -----------------------------------------------------------
p

The values of Mair and Mwater are 29 g/mol and 18 g/mol, respectively.

H E A T TR A N S F E R
You solve the heat conduction equation in both the ice and vapor phases:

T
C p ------- = ( kT )
t

Here, Cp is the specific heat capacity (J/(kgK)) and k is the thermal conductivity (W/
(mK)). The density, (kg/m3), in the vapor domain is calculated using the mean
molar mass of vapor, Mvap, and the ideal gas approximation:

M vap p
= -----------------
RT

A boundary heat source is added to the interface in order to handle possible external
heating, for example, by radiation. In this model, the boundary heat source is set to
5000 W/m2.

The heat flux at the vial bottom is

x 2 y 2
Q in = ( 5.5 10 W/m ) ------- + -------
3 2
(1)
R0 R0

for x > 0, and zero otherwise. This distribution simulates the influence of possible
uneven heating of the tray, and of the vial bottom shape.

Finally, the temperature and vapor concentration at the vial exit are constrained to
fixed values that represent the conditions in the vacuum chamber, including the vapor
condenser effect.

M A S S TR A N S P O R T
In freeze-drying processes, the transport of vapor is only due to diffusion, and you
model it by the equation:

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c
= ( D c )
t

where D is the diffusion coefficient, here equal to 0.05 m2/s. The inward flux of water
vapor at the interface is:

ice
n N v = c ------------------ V s
M water

where Vs is the interface normal velocity, defined later, in Equation 2.

ICE-VAPOR INTERFACE
The thermodynamic equilibrium implies that the temperature at the interface satisfies:

p eq
T = --------
Rc

where the equilibrium vapor pressure, peq, is approximated (Ref. 1) by the following
function of the interface temperature T (here referring to the temperature value in
kelvin):

p eq = exp 9.550426 ------------------------- + 3.53068 log T 0.00728332 T

5723.265
T

Simultaneous heat and mass balances at the sublimation interface lead to the Stefan
condition for the interface velocity:

Qs
V s = -------------- (2)
ice L

where Qs is the jump in the normal heat flux at the interface (W/m2), and L is the
latent heat of ice sublimation, equal to 2.84106 J/kg.

Results
To make the simulation more interesting, a heater is placed under the vial so that it
covers only half of the bottom of the container, producing uneven heating. In the
beginning of the simulation (Figure 2), there is ice on the bottom of the container,
while the remaining space in the container is composed of vapor that has been created
by sublimation.

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As the ice continues to sublime, the temperature and flux distribution in the model can
be measured. After a period of t = 1800 s, the melting ice has the proportions shown
in Figure 3.

Figure 2: Initial state.

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Figure 3: Temperature and heat flux at the end of the drying time period.

You can see from this visualization that the melting front has a concave curved shape
that is higher around the outside edges of the vial wall. Additionally, because the
heating is uneven at the bottom of the vial, the interface level is slightly lower, near
x > 0. As the ice becomes a vapor, the mass of the solid decreases and therefore the
mesh of the solid must change as well.

Notes About the COMSOL Implementation

To set up the application in COMSOL Multiphysics, use the Deformed Geometry
interface to track the ice surface, and then compute coupled mass and heat balances on
the moving mesh. Figure 4 shows the initial mesh (left) and the deformed mesh at the

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end of the simulation (right).

Figure 4: Initial swept mesh (left) and deformed mesh at the end of the simulation (right).

Develop the solution in two steps. First, precompute the initial state by a stationary
analysis. Then, use the solution obtained as the initial value for the transient analysis of
drying.

In Equation 2 for the interface velocity, Qs corresponds to the jump in the normal heat
flux at the interface. This quantity can be precisely evaluated through the Lagrange
multiplier for temperature, T_lm. This variable is available when weak constraints are
enabled in the region of interest, as is the case here with the fixed temperature
constraint at the melting front.

Reference
1. D.M. Murphy and T. Koop, Review of the vapour pressures of ice and supercooled
water for atmospheric applications, Quarterly J. Royal Meteorological Soc., vol. 131,
issue 608, pp. 15391565, 2005.

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Application Library path: Heat_Transfer_Module/Phase_Change/

freeze_drying

Modeling Instructions
From the File menu, choose New.

NEW
1 In the New window, click Model Wizard.

MODEL WIZARD
1 In the Model Wizard window, click 3D.
2 In the Select physics tree, select Chemical Species Transport>Transport of Diluted
Species (tds).
3 Click Add.
4 In the Select physics tree, select Heat Transfer>Heat Transfer in Fluids (ht).
5 Click Add.
6 In the Select physics tree, select Mathematics>Deformed Mesh>Deformed Geometry
(dg).
7 Click Add.
8 Click Study.
9 In the Select study tree, select Preset Studies for Selected Physics Interfaces>Stationary.
10 Click Done.

STUDY 1

Step 1: Stationary
1 In the Model Builder window, under Study 1 click Step 1: Stationary.
2 In the Settings window for Stationary, locate the Physics and Variables Selection
section.
3 In the table, enter the following settings:

Physics interface Solve for Discretization

Deformed Geometry (dg) physics

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GLOBAL DEFINITIONS

Parameters
1 On the Home toolbar, click Parameters.
2 In the Settings window for Parameters, locate the Parameters section.
3 Click Load from File.
4 Browse to the applications Application Library folder and double-click the file
freeze_drying_parameters.txt.

DEFINITIONS

Analytic 1 (an1)
1 On the Home toolbar, click Functions and choose Local>Analytic.
2 In the Settings window for Analytic, type p_eq in the Function name text field.
3 Locate the Definition section. In the Expression text field, type
exp(9.550426-5723.265/T+3.53068*log(T)-0.00728332*T).

4 In the Arguments text field, type T.

5 Locate the Units section. In the Arguments text field, type K.
6 In the Function text field, type Pa.
7 Locate the Plot Parameters section. In the table, enter the following settings:

Argument Lower limit Upper limit

T 193.15 273.15

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8 Click the Plot button.

The equilibrium vapor pressure just defined should look like the figure below.

Variables 1
1 On the Home toolbar, click Variables and choose Local Variables.
2 In the Settings window for Variables, locate the Variables section.
3 Click Load from File.
4 Browse to the applications Application Library folder and double-click the file
freeze_drying_variables.txt.

GEOMETRY 1
1 In the Model Builder window, under Component 1 (comp1) click Geometry 1.
2 In the Settings window for Geometry, locate the Units section.
3 From the Length unit list, choose mm.

Cylinder 1 (cyl1)
1 On the Geometry toolbar, click Cylinder.
2 In the Settings window for Cylinder, locate the Size and Shape section.
3 In the Radius text field, type 5.

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4 In the Height text field, type 20.

5 Click to expand the Layers section. Clear the Layers on side check box.
6 Select the Layers on bottom check box.
7 In the table, enter the following settings:

Layer name Thickness (mm)

Layer 1 8

8 Right-click Component 1 (comp1)>Geometry 1>Cylinder 1 (cyl1) and choose Build

Selected.

Cone 1 (cone1)
1 On the Geometry toolbar, click Cone.
2 In the Settings window for Cone, locate the Size and Shape section.
3 In the Bottom radius text field, type 5.
4 In the Semi-angle text field, type 45.
5 Locate the Position section. In the z text field, type 20.
6 Right-click Component 1 (comp1)>Geometry 1>Cone 1 (cone1) and choose Build
Selected.

Cylinder 2 (cyl2)
1 On the Geometry toolbar, click Cylinder.
2 In the Settings window for Cylinder, locate the Size and Shape section.
3 In the Radius text field, type 4.
4 In the Height text field, type 2.
5 Locate the Position section. In the z text field, type 21.
6 Right-click Component 1 (comp1)>Geometry 1>Cylinder 2 (cyl2) and choose Build
Selected.

Block 1 (blk1)
1 On the Geometry toolbar, click Block.
2 In the Settings window for Block, locate the Size section.
3 In the Width text field, type 10.
4 In the Depth text field, type 5.
5 In the Height text field, type 23.
6 Locate the Position section. In the x text field, type -5.

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7 In the y text field, type -5.

8 Right-click Component 1 (comp1)>Geometry 1>Block 1 (blk1) and choose Build
Selected.

Difference 1 (dif1)
1 On the Geometry toolbar, click Booleans and Partitions and choose Difference.
2 Select the objects cone1, cyl1, and cyl2 only.
3 In the Settings window for Difference, locate the Difference section.
4 Find the Objects to subtract subsection. Select the Active toggle button.
5 Select the object blk1 only.
6 Click the Build All Objects button.
7 Click the Zoom Extents button on the Graphics toolbar.
These steps create a geometry similar to that in Figure 1.
Before defining the materials, configure the physics to indicate which are the solid
and vapor domains. This allows COMSOL Multiphysics to flag what material
properties you need to enter.

H E A T TR A N S F E R I N F L U I D S ( H T )

Heat Transfer in Fluids 1

1 In the Model Builder window, under Component 1 (comp1)>Heat Transfer in Fluids (ht)
click Heat Transfer in Fluids 1.
2 In the Settings window for Heat Transfer in Fluids, locate the Thermodynamics, Fluid
section.
3 From the Fluid type list, choose Ideal gas.
4 From the Gas constant type list, choose Mean molar mass.
5 From the Specify Cp or list, choose Ratio of specific heats.

Heat Transfer in Solids 1

1 On the Physics toolbar, click Domains and choose Heat Transfer in Solids.
2 Select Domain 1 only.

MATERIALS
You can now define the two materials involved in the model: ice and water vapor.

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Material 1 (mat1)
1 In the Model Builder window, under Component 1 (comp1) right-click Materials and
choose Blank Material.
2 In the Settings window for Material, type Ice in the Label text field.
3 Locate the Geometric Entity Selection section. Click Clear Selection.
4 Select Domain 1 only.
5 Locate the Material Contents section. In the table, enter the following settings:

Property Name Value Unit Property group

Thermal conductivity k k_ice W/(mK) Basic
Density rho rho_ice kg/m Basic
Heat capacity at constant pressure Cp Cp_ice J/(kgK) Basic

Material 2 (mat2)
1 In the Model Builder window, right-click Materials and choose Blank Material.
2 In the Settings window for Material, type Water Vapor in the Label text field.
3 Select Domains 24 only.
4 Locate the Material Contents section. In the table, enter the following settings:

Property Name Value Unit Property group

Thermal conductivity k 0.02 W/(mK) Basic
Ratio of specific heats gamma 1.3 1 Basic
Mean molar mass Mn M_vap kg/mol Basic

TR A N S P O R T O F D I L U T E D S P E C I E S ( T D S )
1 In the Model Builder window, under Component 1 (comp1) click Transport of Diluted
Species (tds).
2 Select Domains 24 only.
3 In the Settings window for Transport of Diluted Species, locate the Transport
Mechanisms section.
4 Clear the Convection check box.
In freeze-drying processes, mass transfer by convection is often neglected.

Transport Properties 1
1 In the Model Builder window, under Component 1 (comp1)>Transport of Diluted
Species (tds) click Transport Properties 1.

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2 In the Settings window for Transport Properties, locate the Diffusion section.
3 In the Dc text field, type D_vap.

Initial Values 1
1 In the Model Builder window, under Component 1 (comp1)>Transport of Diluted
Species (tds) click Initial Values 1.
2 In the Settings window for Initial Values, locate the Initial Values section.
3 In the c text field, type c_init.

Concentration 1
1 On the Physics toolbar, click Boundaries and choose Concentration.
2 Select Boundary 13 only.
3 In the Settings window for Concentration, locate the Concentration section.
4 Select the Species c check box.
5 In the c0,c text field, type c_c.

Flux 1
1 On the Physics toolbar, click Boundaries and choose Flux.
2 Select Boundary 6 only.
3 In the Settings window for Flux, locate the Inward Flux section.
4 Select the Species c check box.
5 In the N0,c text field, type V_s*(c-rho_ice/M_vap).

Symmetry 1
1 On the Physics toolbar, click Boundaries and choose Symmetry.
2 Select Boundaries 5, 8, and 11 only.

H E A T TR A N S F E R I N F L U I D S ( H T )

Heat Transfer in Fluids 1

1 In the Model Builder window, under Component 1 (comp1)>Heat Transfer in Fluids (ht)
click Heat Transfer in Fluids 1.
2 In the Settings window for Heat Transfer in Fluids, locate the Model Inputs section.
3 In the pA text field, type p.

Initial Values 1
1 In the Model Builder window, under Component 1 (comp1)>Heat Transfer in Fluids (ht)
click Initial Values 1.

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2 In the Settings window for Initial Values, locate the Initial Values section.
3 In the T text field, type T_init.

Heat Flux 1
1 On the Physics toolbar, click Boundaries and choose Heat Flux.
2 In the Settings window for Heat Flux, locate the Boundary Selection section.
3 From the Selection list, choose All boundaries.
4 Remove Boundary 3 from the selection list.
5 Locate the Heat Flux section. Click the Convective heat flux button.
6 In the h text field, type h_wall.
7 In the Text text field, type T0.

Heat Flux 2
1 On the Physics toolbar, click Boundaries and choose Heat Flux.
2 Select Boundary 3 only.
3 In the Settings window for Heat Flux, locate the Heat Flux section.
4 In the q0 text field, type Q_in.

Temperature 1
1 On the Physics toolbar, click Boundaries and choose Temperature.
2 Select Boundary 6 only.
3 In the Settings window for Temperature, locate the Temperature section.
4 In the T0 text field, type p_eq(T)/(R_const*c).
5 In the Model Builder windows toolbar, click the Show button and select Advanced
Physics Options in the menu.
6 Click to expand the Constraint settings section. Locate the Constraint Settings
section. From the Apply reaction terms on list, choose Individual dependent variables.
7 Select the Use weak constraints check box.
By activating weak constraints, the Lagrange multiplier for temperature is made
available at the melting front. You can use it to evaluate precisely the heat flux jump
between the adjacent vapor and ice domains.

Temperature 2
1 On the Physics toolbar, click Boundaries and choose Temperature.
2 Select Boundary 13 only.
3 In the Settings window for Temperature, locate the Temperature section.

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4 In the T0 text field, type T_c.

Boundary Heat Source 1

1 On the Physics toolbar, click Boundaries and choose Boundary Heat Source.
2 Select Boundary 6 only.
3 In the Settings window for Boundary Heat Source, locate the Boundary Heat Source
section.
4 In the Qb text field, type 5000.

Symmetry 1
1 On the Physics toolbar, click Boundaries and choose Symmetry.
2 Select Boundaries 2, 5, 8, and 11 only.

DEFORMED GEOMETRY (DG)

1 In the Model Builder window, under Component 1 (comp1) click Deformed Geometry
(dg).
2 In the Settings window for Deformed Geometry, locate the Frame Settings section.
3 From the Geometry shape order list, choose 1.
Despite a slight loss in numerical precision, changing the geometry shape order to
1 provides more stability to the model.

Free Deformation 1
1 On the Physics toolbar, click Domains and choose Free Deformation.
2 Select Domains 1 and 2 only.

Prescribed Mesh Displacement 2

1 On the Physics toolbar, click Boundaries and choose Prescribed Mesh Displacement.
2 Select Boundaries 3 and 9 only.

Prescribed Normal Mesh Velocity 1

1 On the Physics toolbar, click Boundaries and choose Prescribed Normal Mesh Velocity.
2 Select Boundary 6 only.
3 In the Settings window for Prescribed Normal Mesh Velocity, locate the Normal Mesh
Velocity section.
4 In the vn text field, type V_s*sign(dg.nZg).
The variable V_s is the front velocity normal component assuming that the interface
normal vector is directed upwards. To ensure that the velocity field is correctly
oriented for this interior boundary, multiply V_s by sign(dg.nZg).

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Prescribed Mesh Displacement 1

1 In the Model Builder window, under Component 1 (comp1)>Deformed Geometry (dg)
click Prescribed Mesh Displacement 1.
2 In the Settings window for Prescribed Mesh Displacement, locate the Prescribed
Mesh Displacement section.
3 Clear the Prescribed z displacement check box.

MESH 1
In the Model Builder window, under Component 1 (comp1) right-click Mesh 1 and choose
Swept.

Size
1 In the Model Builder window, under Component 1 (comp1)>Mesh 1 click Size.
2 In the Settings window for Size, locate the Element Size section.
3 From the Predefined list, choose Extra fine.
4 Click the Build All button.
Now you can see a mesh similar to that shown in below.

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STUDY 1

Step 2: Time Dependent

1 On the Study toolbar, click Study Steps and choose Time Dependent>Time Dependent.
2 In the Settings window for Time Dependent, locate the Study Settings section.
3 Click Range.
4 In the Range dialog box, type 1[min] in the Step text field.
5 In the Stop text field, type 30[min].
6 Click Replace.
7 In the Model Builder window, click Study 1.
8 In the Settings window for Study, locate the Study Settings section.
9 Clear the Generate default plots check box.

Solution 1
1 On the Study toolbar, click Show Default Solver.
2 In the Model Builder window, expand the Solution 1 node, then click Time-Dependent
Solver 1.
3 In the Settings window for Time-Dependent Solver, click to expand the Time
stepping section.
4 Locate the Time Stepping section. From the Steps taken by solver list, choose
Intermediate.
Temperature and concentration are highly interdependent in this model. Hence,
indicate that the physics are fully coupled and choose a direct solver for more
robustness.
5 Right-click Study 1>Solver Configurations>Solution 1>Time-Dependent Solver 1 and
choose Fully Coupled.
6 Right-click Study 1>Solver Configurations>Solution 1>Time-Dependent Solver
1>Direct and choose Enable.
7 On the Study toolbar, click Compute.

RESULTS
Only half of the vial geometry has been built for the calculations. In the next steps,
mirror plots are defined to visualize the entire geometry in post-processing plots.

Data Sets
1 On the Results toolbar, click More Data Sets and choose Mirror 3D.

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2 In the Settings window for Mirror 3D, locate the Plane Data section.
3 From the Plane list, choose xz-planes.
4 Click the Plot button.
5 Right-click Results>Data Sets>Mirror 3D 1 and choose Duplicate.
6 In the Settings window for Mirror 3D, locate the Data section.
7 From the Data set list, choose Study 1/Solution Store 1.

3D Plot Group 1
1 On the Results toolbar, click 3D Plot Group.
2 In the Settings window for 3D Plot Group, type Sublimation Interface in the
Label text field.
3 Locate the Data section. From the Data set list, choose Mirror 3D 2.

Sublimation Interface
1 Right-click Results>Sublimation Interface and choose Slice.
2 In the Settings window for Slice, click Replace Expression in the upper-right corner
of the Expression section. From the menu, choose Model>Component 1>Heat Transfer
in Fluids>Temperature>T - Temperature.
3 Locate the Plane Data section. In the Planes text field, type 1.
4 Locate the Coloring and Style section. From the Color table list, choose ThermalLight.
5 In the Model Builder window, right-click Sublimation Interface and choose Isosurface.
6 In the Settings window for Isosurface, click Replace Expression in the upper-right
corner of the Expression section. From the menu, choose
Model>Geometry>Coordinate (Geometry)>Zg - Zg-coordinate.
7 Locate the Levels section. From the Entry method list, choose Levels.
8 In the Levels text field, type Z0.
9 Locate the Coloring and Style section. Clear the Color legend check box.
10 Right-click Sublimation Interface and choose Arrow Volume.
11 In the Settings window for Arrow Volume, click Replace Expression in the upper-right
corner of the Expression section. From the menu, choose Model>Component 1>Heat
Transfer in Fluids>Domain fluxes>ht.tfluxx,...,ht.tfluxz - Total heat flux (Material).
12 Locate the Coloring and Style section. From the Color list, choose Black.
13 Right-click Sublimation Interface and choose Streamline.
14 In the Settings window for Streamline, locate the Streamline Positioning section.

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15 From the Positioning list, choose Magnitude controlled.

16 Right-click Sublimation Interface and choose Volume.
17 In the Settings window for Volume, locate the Expression section.
18 In the Expression text field, type dom==1.
The expression dom==1 plots the ice domain and the remaining regions in different
colors.
19 Locate the Coloring and Style section. From the Color table list, choose GrayScale.
20 Select the Reverse color table check box.
21 Clear the Color legend check box.
22 Right-click Results>Sublimation Interface>Volume 1 and choose Deformation.
Use the Deformation feature to shift the second plot.
23 In the Settings window for Deformation, locate the Scale section.
24 Select the Scale factor check box.
25 In the associated text field, type 1.
26 Locate the Expression section. In the x component text field, type -15.
27 In the y component text field, type 0.
28 In the z component text field, type 0.
29 On the Sublimation Interface toolbar, click Plot.
30 Click the Zoom Extents button on the Graphics toolbar.
To create the plot shown in Figure 3, follow these steps:
31 In the Model Builder window, click Sublimation Interface.
32 In the Settings window for 3D Plot Group, locate the Data section.
33 From the Data set list, choose Mirror 3D 1.
34 On the Sublimation Interface toolbar, click Plot.
35 Click the Zoom Extents button on the Graphics toolbar.
To create the plot shown in Figure 4, reproduce the following steps:

3D Plot Group 2
1 On the Home toolbar, click Add Plot Group and choose 3D Plot Group.
2 In the Settings window for 3D Plot Group, type Mesh Comparison in the Label text
field.
3 Click to expand the Title section. From the Title type list, choose None.

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Mesh Comparison
1 Right-click Results>Mesh Comparison and choose Mesh.
2 In the Settings window for Mesh, locate the Data section.
3 From the Data set list, choose Study 1/Solution 1.
4 From the Time (s) list, choose 0.
5 Locate the Color section. From the Color table list, choose GrayScale.
6 Clear the Color legend check box.
7 Right-click Results>Mesh Comparison>Mesh 1 and choose Duplicate.
8 In the Settings window for Mesh, locate the Data section.
9 From the Time (s) list, choose 1800.
10 Right-click Results>Mesh Comparison>Mesh 2 and choose Deformation.
11 In the Settings window for Deformation, locate the Expression section.
12 In the x component text field, type 15.
13 Locate the Scale section. Select the Scale factor check box.
14 On the Mesh Comparison toolbar, click Plot.
15 Click the Zoom Extents button on the Graphics toolbar.

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