JEDEC

STANDARD

Test Method for the Measurement of

Moisture Diffusivity and Water
Solubility in Organic Materials Used
in Electronic Devices

JESD22-A120B
(Revision of JESD22-A120A, January 2008)

JULY 2014

JEDEC SOLID STATE TECHNOLOGY ASSOCIATION

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 JEDEC Standard No. 22-A120A
Page 1

STANDARD TEST METHOD FOR THE MEASUREMENT OF MOISTURE DIFFUSIVITY

AND WATER SOLUBILITY IN ORGANIC MATERIALS USED IN ELECTRONIC DEVICES

(From JEDEC Board Ballot JCB-14-30, formulated under the cognizance of the JC-14.1 Subcommittee on
Reliability test methods for packaged Devices.)

1 Scope

The purpose of this test method is to provide a means for determining the moisture sorption properties of
organic materials used in the packaging of electronic devices.

This specification details the procedures for the measurement of characteristic bulk material properties of
moisture diffusivity and water solubility in organic materials used in the packaging of electronic devices.
These two material properties are important parameters for the effective reliability performance of plastic
packaged surface mount devices after exposure to moisture and subjected to high temperature solder
reflow.

2 Normative references

J-STD-020, Moisture/Reflow Sensitivity Classification for Nonhermetic Solid State Surface Mount
Devices.

ASTM Standard D570-10, Standard Test Method for Water Absorption of Plastics.

SEMI G66-0811, Test Method for the Measurement of Water Absorption Characteristics for
Semiconductor Plastic Molding Compounds.

DIN EN ISO 62: 2008, Plastics Determination of Water Absorption.

SEMI MS10-0812, Test Method to Measure Fluid Permeation through MEMS Packaging Materials.

3 Apparatus

3.1 Analytical balance capable of resolution of either 0.00001g or 0.001% of sample weight.
3.2 High temperature oven capable of maintaining uniform temperatures from
100 C 250 C +/-2 C.
3.3 Temperature / humidity chamber(s) capable of maintaining temperatures of 30 C 85 C and
relative humiditys from 60%RH 85%RH. Within the chamber working area, temperature
tolerance must be +/-2 C and the RH tolerance must be +/-3%RH.
3.4 Perforated stainless steel trays or wire mesh baskets used for holding samples and for placement
into ovens.
3.5 Large aluminum plate or disk used for heat sink capability.
3.6 Desiccator for holding dry samples.

Test Method A120B

(Revision of A120A)
JEDEC Standard No. 22-A120B
Page 2

4 Test samples

4.1 Test samples must be flat parallel-sided discs or coupons. The linear dimensions must be
accurately measured to within 0.02mm.

4.1.1 To approximate one-dimensional diffusion behavior with edge effects limited to less than 5% of
the total diffusional moisture mass uptake, the free surface area in the thickness dimension must
be less than 5% of the flat-sided free surface area of the sample. For a disc of radius r, and
thickness h, the following relation must be met:

h < 0.05r (1)

for a coupon of length L, and width W,

0.05 (W L)
h < (2)
(W + L)

Recommended sample thickness should be in the range from 0.3 1.0mm. It is recommended
that the maximum sample thickness not exceed 1.0mm, because the time to achieve moisture
saturation at temperatures below 60C will be excessively long for slow diffusing compounds.

5 Procedure

5.1 Sample preparation

5.1.1 Prepare samples by using proper processing parameters as recommended by the material supplier.

5.1.2 Process and cure the samples using recommended processing conditions per the manufacturers
specification.

5.1.3 To obtain the appropriate sample thickness as given by relations (1) or (2), samples may be
sectioned and finely polished from larger bulk specimens. Care must be taken to maintain near-
parallel sided flatness for samples prepared in this manner.

5.1.4 The prepared samples should be inspected for voids by Acoustic Microscopy (AM) or x-ray, both
internal and surface. The ideal samples must be 95% of theoretical maximum density.

5.2 Absorption measurements below 100 C

5.2.1 Measure the linear dimensions of the prepared sample to the nearest 0.02mm. Record the
sample thickness, h, and calculate the sample volume, Vol, using the appropriate geometric
relationship based on the sample shape.

NOTE Calculating the volume by measuring the linear dimensions is never accurate. The error is smaller
when the sample is big. One accurate way of determining the volume is to use Archimedess principle,
which is to measure the sample weight in air and immersed in a liquid with known density (alcohol, IPA,
etc.). In this way, volume of a sample with irregular shape can also be determined.

Test Method A120B

(Revision of A120A)
 JEDEC Standard No. 22-A120B
Page 3

5.2 Absorption measurements below 100 C (contd)

5.2.2 The dry weight of the sample shall be determined, as per J-STD-020, first by baking the sample
for 24 hours at 125 +5/-0 C and continue baking and weigh the sample every 12 hours until no
further weight loss is observed to ensure that the sample(s) are dry. The dry weight is determined
when no further weight loss is observed, less than 0.002% difference, after two consecutive
measurements with a minimum baking interval of 12 hours. Within 30 minutes after removal
from the oven, weigh the sample(s) using the analytical balance equipment in 3.1 and determine
the dry weight per 5.2.4. Note: As per J-STD-020, small sample(s) (less than 1.5 mm total
height), devices should be weighed within 30 minutes after removal from oven

NOTE As per J-STD-020, small sample(s) (less than 1.5 mm total height), devices should be weighed
within 30 minutes after removal from oven. Remove the sample(s) from the bake oven and immediately
cool by placing in contact with the heat sink of 3.5. If more than one sample is to be measured, the samples
and heat sink should be placed into a desiccator to limit moisture uptake during the weight measurements.

5.2.3 Weigh the sample according to 3.1 and record weight as DryW(1). Read Points: At the desired
read point; remove the sample(s) from the bake oven. Within 30 minutes after removal of the
sample(s) from the bake oven, remove the sample(s) from the container and determine their
weight using the analytical balance equipment in 3.1. Within 30 minutes after weighing the
samples, place them in a clean, dry, shallow container so that the sample bodies do not touch each
other. Return the sample(s) to the bake oven for the desired time. Continue until the sample(s)
have lost all their moisture as determined by the dry weight in 5.2.2.

5.2.5 Place the sample(s) into a stainless steel holder and transfer to a temperature / humidity chamber
stabilized at a pre-set temperature and humidity.

At accumulative times, remove the sample from the temperature / humidity chamber, cool as per
5.2.3, and measure the sample weight and record as WetW(t).

Read Points: The X-axis (time) read points, as per J-STD-020, should be selected for plotting the
absorption curve. For the early readings, points should be relatively short (24 hours or less)
because the curve will have a steep initial slope. Later readings may be spread out further (10
days or more) as the curve becomes asymptotic. The Y-axis (weight gain) should start with
0and increase to the saturated weight gain. Most sample(s) will reach saturation between 0.3%
and 0.4% when stored at 85C/85% RH. Devices shall be kept at room ambient between removal
from the oven or chamber and weighing and subsequent reinsertion into the oven or chamber.

Care should be taken that no condensed moisture from the chamber walls comes into contact with
a sample during removal from the temperature / humidity chamber. If condensed water should
contact a sample, immediately dry the sample using Nitrogen or dry air. The sample should then
be returned to the chamber for re-equilibration and another data point taken at a later time.

The sample weight measurement be made within a few minutes after removal of the sample from
the temperature / humidity chamber. Time delays longer than 5 minutes after removal from the
temperature / humidity chamber could affect the sample weight measurements.

Within 30 minutes after weighing the samples, place them in a clean, dry, shallow container so
that the sample bodies do not touch each other. Return the sample(s) to the temperature/humidity
chamber for the desired time.

Test Method A120B

(Revision of A120A)
JEDEC Standard No. 22-A120B
Page 4

5.2 Absorption measurements below 100 C (contd)

5.2.6 Place the sample back into the temperature / humidity chamber and continue weight
measurements until either of the following conditions are met:

5.2.6.1 Additional weight gain after a 24 hour period is less than 0.002% from the previous measurement.

5.2.6.2 A plot of the moisture mass gain, M(t) = {WetW(t) DryW(1)}, versus time shows a linearly increasing
moisture mass gain with time or dM/dt = constant after an initial decreasing change in moisture mass with
time as depicted in Figure 1.
= {WetW(t) DryW(1)}

d(M)/dt = constant
Moisture Mass

Time
Figure 1 Example of linearly increasing moisture mass gain

5.2.7 Record the final wet weight of the sample as, WetW(f)

5.2.8 Bake the sample again at 125C until dry as determined per 5.2.2.

5.2.9 Record the second dry weight as, DryW(2).

5.2.10 Record the reversible saturated moisture mass as, MSat = {WetW(f) DryW(2)}.

NOTE 1 An alternative method to estimate the reversible saturated moisture mass can be determined by
an intercept approach as shown in Figure 2. Using this method the intercept point between the weight gain
curve and a linear extrapolation of the linear varying portion of the weight gain curve can be used to
estimate the reversible Fickian moisture weight gain response.

Test Method A120B

(Revision of A120A)
 JEDEC Standard No. 22-A120B
Page 5

5.2 Absorption measurements below 100 C (contd)

= {WetW(t) DryW(1)}
d(M)/dt = constant
Moisture Mass

Intercept Point
MSat

Time
Figure 2 Alternative intercept method to estimate the reversible Fickian moisture mass

Test Method A120B

(Revision of A120A)
JEDEC Standard No. 22-A120B
Page 6

5.3 Solubility and diffusivity calculation

5.3.1 Calculate the solubility at the given temperature and humidity by using:

M Sat (T ,% RH )
C Sat (T,%RH) = = (Msat/M(mass)) (=density) (3)
Vol

Where: C Sat(T,%RH) = the moisture solubility at temperature T and %RH (mg/cm3 )

Vol = sample volume (cm3)

M Sat(T,%RH) (mg) = reversible saturated moisture mass at temperature T and

%RH as determined in 5.2.10

5.3.2 Using the moisture mass gain curve, calculate the moisture diffusivity from:

0.04919h 2
D(T ) = (4)
t 0.5

Where: D(T) = the diffusivity at temperature T (mm2/s)

h = sample thickness (mm)

t0.5 = the sorption half-time (measured in seconds) defined as the time at which
the sorbed mass of moisture is equal to one-half the saturated mass,
i.e., Mt/MSat = 0.5.

NOTE 1 Equation (4) is recognized as an approximation to the analytical closed form solution, however,
it will provide an accurate approximation to less than a few percent error. An alternate method for
determining D(T) is to use a best fit curve fitting approach of the experimental weight gain data. The
following solution for rectangular or square samples can be used:

512 exp( D t Leqv )

(2l + 1) 2 (2m + 1) 2 (2n + 1) 2
Mt
= 1
M Sat 6 l =0 m = 0 n =0
(5)
(2l + 1) 2 (2m + 1) 2 (2n + 1) 2

where Leqv = 2 + +
x o y o z o

Here xo, yo, and zo are the width, length, and thickness of the sample, respectively. The value of
D(T) determined by a curve fitting technique using equation (5) should be compared to the value
determined by equation (4) as a reference check.

5.3.3 Repeat sorption measurements 5.2 to 5.3.2 using different temperature and humidity conditions.
The following environmental conditions shall be used: 30 C/60%RH, 60 C/60%RH, and 85
C/60%RH.

Test Method A120B

(Revision of A120A)
 JEDEC Standard No. 22-A120B
Page 7

5.4 Desorption measurements above 100 C

5.4.1 Place sample into a chamber maintained at 85 C/60%RH or 85 C/85%RH for 168 hrs or until
the saturated sample weight, WSat, is achieved as determined by a calculation using a previously
determined diffusivity at 85 C.

5.4.2 Remove the sample from the temperature/humidity chamber, cool as per 5.2.3, and record the
saturated sample weight, WSat.

5.4.3 Immediately place the sample into a bake oven stabilized at a temperature greater than 100 C.

The sample shall be transferred into a stainless steel holder that has been preheated and stabilized
at the set bake temperature.

5.4.4 Remove the sample after a recorded elapsed period of time, immediately cool per 5.2.3, and
measure the sample weight per 5.2.4.

5.4.5 Repeat steps 5.4.3 and 5.4.4 until the sample is dry.

Appropriate times for recording weight losses can be determined by using a first order
extrapolation of the value for the diffusivity by using an Arrhenius fit, see 7.1, of the absorption
diffusivities determined in 5.3.2.

Estimated weight losses can be assessed by using the following equation:

(2n + 1) 2 2 Dt
8 1
(2n + 1) 2 exp
Mt
= 1 (6)
M Sat 2 n =0 h2

5.4.6 Calculate D(T) using equation (4), where t0.5 is now defined as the time at which the desorbed
mass of moisture is equal to one-half the saturated mass. Equation (5) may also be used as an
alternative method.

5.4.7 Reset bake oven to a higher bake temperature and repeat measurements following 5.4.1 to 5.4.6.

Test Method A120B

(Revision of A120A)
JEDEC Standard No. 22-A120B
Page 8

6 Calculation of functional fit for moisture diffusivity

6.1 The activation energy (eV) for moisture diffusion is calculated from the slope of a plot of
ln{D(T)} vs. 1/T where T is in degrees Kelvin. Report the best fit line as:
E
D (T ) = Do exp a (7)
kT

Where: Do = the pre-exponential factor for fitted line (mm2/s)

Ea = activation energy (eV)
k = Boltzmans constant, 8.617x10-5 eV/K

6.1.1 Diffusion of moisture may show a dependency on the Tg (Glass Transition Temperature) of the
material. Measurements above the Tg of the material should be reported as a separate activation
energy and pre-exponential factor.

6.1.2 For accurate determination of the activation energy, it is recommended that a minimum of three
temperatures are used differing by 20-30C for both above and below Tg.

7 Calculation of functional fit for solubility

7.1 The solubility can be fitted to the following equation:

E
C Sat (T , P ) = PS o exp s (8)
kT

Where: So = pre-exponential factor (mg/cm3Pa)

Es = activation energy (eV)
P = (%RH/PSat *100) is the partial pressure of water vapor (Pa) where PSat is
the saturated water vapor pressure at temperature T as obtained from
steam tables.
T = temperature in K

7.2 Parameters Es and So are obtained from a curve fit of a plot of ln(CSat/P) vs. 1/T

7.3 For accurate determination of the activation energy (eV), it is recommended that a minimum of
three temperatures are used differing by 20-30C for both above and below Tg.

Test Method A120B

(Revision of A120A)
 JEDEC Standard No. 22-A120B
Page 9

8 Report results

8.1 The following information shall be tabulated:

a) Mold compound identification

b) Test temperatures and relative humiditys

c) Do (Pre-exponential Factor for Fitted Lines)

d) Ea (Activation Energy (eV))

e) D(T) (Diffusivity at Temperature)
f) CSat(T,%RH) (Solubility at a given temperature and humidity)

Test Method A120B

(Revision of A120A)
JEDEC Standard No. 22-A120B
Page 10

Annex A (informative) Differences between JESD22-A120B and JESD22-A120A

This table briefly describes most of the changes made to entries that appear in this standard, JESD22-
A120B, compared to its predecessor, JESD22-A120A (January 2008). If the change to a concept involves
any words added or deleted (excluding deletion of accidentally repeated words), it is included. Some
punctuation changes are not included.

Page Description of change

1 1 Scope - Changed from water sorption to moisture sorption.
1 2 Normative references Added J-STD-020, Updated D570-98 to D570-10, Updated
SEMI G66-96 to SEMI G66-0811, Replaced DIN53495 with current version
DIN EN ISO 62:2008 & Added SEMI MS10-0812.
2 Section 5.1.4 Added by Acoustic Microscopy (AM) or x-ray inspection techniques
for voids.
3 Removed repeat of 5 Procedure (contd) & 5.2 Absorption measurements below
100C (contd).
3 Section 5.2.2 Updated procedure to determine dry weight to the more specific
procedure and clarification approved in J-STD-020D.
3 Sections 5.2.3 & 5.2.5 Removed redundant paragraph regarding transfer of sample(s) in
stabilized chamber that has been preheated. Updated read points for dry weight data
to the more specific procedure and clarification approved in J-STD-020D.
4 Removed repeat of 5 Procedure (contd) & 5.2 Absorption measurements below
100C (contd).
5 Removed repeat of 5 Procedure (contd).
5 Section 5.3.1 Added = (Msat/M(mass)) (=density) to equation 3 for clarification.
Section 5.3.3 Changed Suggested environmental conditions are to The following
environmental conditions shall be used.
6 Removed repeat of 5 Procedure (contd).
6 Section 5.4.3 Changed It is suggested that the sample be to The sample shall be.
7 Section 6.1 Changed activation energy to activation energy (eV) to help clarify
what eV is in equations.
7 Removed repeat of 6 Calculations of functional fit for moisture diffusivity (contd).
7 Section 6.1.1 - Changed Tg to Tg (Glass Transition Temperature) for clarification.
8 Section 7.3 - Changed activation energy to activation energy (eV) to help clarify
what eV is in equations. Added for both above and below Tg for clarification.
8 Section 8.1 Changed Do to Do (Pre-exponential Factor for Fitted Lines), Ea to
Ea (Activation Energy (eV)), D(T) to D(T) (Diffusivity at Temperature) &
CSat(T,%RH) to CSat(T,%RH) (Solubility at a given temperature and humidity) for
clarification.

Test Method A120B

(Revision of A120A)
Standard Improvement Form JEDEC JESD22A120B

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