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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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ASTM Standard D570-10. 3. 3. 3. temperature tolerance must be +/-2 °C and the RH tolerance must be +/-3%RH.00001g or 0.4 Perforated stainless steel trays or wire mesh baskets used for holding samples and for placement into ovens. 3 Apparatus 3.) 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.5 Large aluminum plate or disk used for heat sink capability. Test Method to Measure Fluid Permeation through MEMS Packaging Materials. formulated under the cognizance of the JC-14. Test Method for the Measurement of Water Absorption Characteristics for Semiconductor Plastic Molding Compounds. Test Method A120B (Revision of A120A) . 2 Normative references J-STD-020. DIN EN ISO 62: 2008. 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. 3.1 Analytical balance capable of resolution of either 0.001% of sample weight. SEMI MS10-0812. 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.1 Subcommittee on Reliability test methods for packaged Devices. Within the chamber working area.2 High temperature oven capable of maintaining uniform temperatures from 100 °C – 250 °C +/-2 °C.3 Temperature / humidity chamber(s) capable of maintaining temperatures of 30 °C – 85 °C and relative humidity’s from 60%RH – 85%RH. 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. Standard Test Method for Water Absorption of Plastics. JEDEC Standard No. 3. SEMI G66-0811.6 Desiccator for holding dry samples. Plastics Determination of Water Absorption. Moisture/Reflow Sensitivity Classification for Nonhermetic Solid State Surface Mount Devices.

1.05r (1) for a coupon of length L.1. 5. the free surface area in the thickness dimension must be less than 5% of the flat-sided free surface area of the sample.1.JEDEC Standard No.1 Prepare samples by using proper processing parameters as recommended by the material supplier.2 Process and cure the samples using recommended processing conditions per the manufacturer’s specification.0mm. which is to measure the sample weight in air and immersed in a liquid with known density (alcohol.1 Measure the linear dimensions of the prepared sample to the nearest ±0. In this way. 5. both internal and surface. etc.2 Absorption measurements below 100 °C 5. The linear dimensions must be accurately measured to within ±0. One accurate way of determining the volume is to use Archimedes’s principle. the following relation must be met: h < 0. 5. Test Method A120B (Revision of A120A) . h.2.1 Sample preparation 5. 5. samples may be sectioned and finely polished from larger bulk specimens.1 Test samples must be flat parallel-sided discs or coupons.02mm. and width W. 4. 0.3 – 1. NOTE Calculating the volume by measuring the linear dimensions is never accurate.). The error is smaller when the sample is big. and thickness h. It is recommended that the maximum sample thickness not exceed 1.4 The prepared samples should be inspected for voids by Acoustic Microscopy (AM) or x-ray. For a disc of radius r. using the appropriate geometric relationship based on the sample shape. volume of a sample with irregular shape can also be determined.1 To approximate one-dimensional diffusion behavior with edge effects limited to less than 5% of the total diffusional moisture mass uptake. 5 Procedure 5. Record the sample thickness.1.02mm.0mm. Vol. and calculate the sample volume. The ideal samples must be 95% of theoretical maximum density. 22-A120B Page 2 4 Test samples 4. because the time to achieve moisture saturation at temperatures below 60°C will be excessively long for slow diffusing compounds. IPA. Care must be taken to maintain near- parallel sided flatness for samples prepared in this manner.3 To obtain the appropriate sample thickness as given by relations (1) or (2).1.05 (W × L) h < (2) (W + L) Recommended sample thickness should be in the range from 0.

JEDEC Standard No. Read Points: At the desired read point.5.2.2. Remove the sample(s) from the bake oven and immediately cool by placing in contact with the heat sink of 3. remove the sample(s) from the bake oven. as per J-STD-020. The sample weight measurement be made within a few minutes after removal of the sample from the temperature / humidity chamber. weigh the sample(s) using the analytical balance equipment in 3. place them in a clean. devices should be weighed within 30 minutes after removal from oven NOTE As per J-STD-020. If condensed water should contact a sample. and measure the sample weight and record as WetW(t). small sample(s) (less than 1.5 Place the sample(s) into a stainless steel holder and transfer to a temperature / humidity chamber stabilized at a pre-set temperature and humidity.2.2. Time delays longer than 5 minutes after removal from the temperature / humidity chamber could affect the sample weight measurements.5 mm total height). Continue until the sample(s) have lost all their moisture as determined by the dry weight in 5. 5.1 and determine the dry weight per 5. If more than one sample is to be measured.4% when stored at 85°C/85% RH. devices should be weighed within 30 minutes after removal from oven. Most sample(s) will reach saturation between 0. The dry weight is determined when no further weight loss is observed. Within 30 minutes after removal of the sample(s) from the bake oven. At accumulative times. immediately dry the sample using Nitrogen or dry air. Read Points: The X-axis (time) read points.5 mm total height). remove the sample(s) from the container and determine their weight using the analytical balance equipment in 3. shallow container so that the sample bodies do not touch each other. The sample should then be returned to the chamber for re-equilibration and another data point taken at a later time.2. The Y-axis (weight gain) should start with ‘‘0’’and increase to the saturated weight gain. For the early readings.2 The dry weight of the sample shall be determined.002% difference.3 Weigh the sample according to 3. as per J-STD-020.3. remove the sample from the temperature / humidity chamber. should be selected for plotting the absorption curve. small sample(s) (less than 1. less than 0. cool as per 5. dry. 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.1. Within 30 minutes after weighing the samples. shallow container so that the sample bodies do not touch each other. Return the sample(s) to the bake oven for the desired time. 5. Devices shall be kept at room ambient between removal from the oven or chamber and weighing and subsequent reinsertion into the oven or chamber. place them in a clean. points should be relatively short (24 hours or less) because the curve will have a steep initial slope. dry.2 Absorption measurements below 100 °C (cont’d) 5. Later readings may be spread out further (10 days or more) as the curve becomes asymptotic.1 and record weight as DryW(1). 22-A120B Page 3 5. the samples and heat sink should be placed into a desiccator to limit moisture uptake during the weight measurements. Within 30 minutes after removal from the oven.2. after two consecutive measurements with a minimum baking interval of 12 hours.4.2.3% and 0. Within 30 minutes after weighing the samples. 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. Test Method A120B (Revision of A120A) . Note: As per J-STD-020. Return the sample(s) to the temperature/humidity chamber for the desired time.

2. WetW(f) 5. 22-A120B Page 4 5.002% from the previous measurement.2. 5.7 Record the final wet weight of the sample as.6.2.8 Bake the sample again at 125°C until dry as determined per 5.2.1 Additional weight gain after a 24 hour period is less than 0. DryW(2).2.10 Record the reversible saturated moisture mass as.2. 5. M(t) = {WetW(t) – DryW(1)}. 5. NOTE 1 An alternative method to estimate the reversible saturated moisture mass can be determined by an intercept approach as shown in Figure 2. 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.JEDEC Standard No.6.2.6 Place the sample back into the temperature / humidity chamber and continue weight measurements until either of the following conditions are met: 5.2 A plot of the moisture mass gain. 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. = {WetW(t) –DryW(1)} d(M)/dt = constant Moisture Mass Time Figure 1 — Example of linearly increasing moisture mass gain 5.2. MSat = {WetW(f) – DryW(2)}.2 Absorption measurements below 100 °C (cont’d) 5.2. Test Method A120B (Revision of A120A) .9 Record the second dry weight as.

22-A120B Page 5 5.2 Absorption measurements below 100 °C (cont’d) = {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.

3..2 using different temperature and humidity conditions. 5.% RH ) C Sat (T. NOTE 1 Equation (4) is recognized as an approximation to the analytical closed form solution. 22-A120B Page 6 5.JEDEC Standard No.3 Solubility and diffusivity calculation 5.%RH) (mg) = reversible saturated moisture mass at temperature T and %RH as determined in 5.04919h 2 D(T ) = (4) t 0.2 Using the moisture mass gain curve.3 Repeat sorption measurements 5. length. calculate the moisture diffusivity from: 0.2. it will provide an accurate approximation to less than a few percent error.3.10 5. An alternate method for determining D(T) is to use a best fit curve fitting approach of the experimental weight gain data.1 Calculate the solubility at the given temperature and humidity by using: M Sat (T .2 to 5. i.3.%RH) = = (Msat/M(mass))ρ (ρ=density) (3) Vol Where: C Sat(T. and zo are the width. and 85 °C/60%RH. and thickness of the sample. yo.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.e. respectively.5. The following environmental conditions shall be used: 30 °C/60%RH. Mt/MSat = 0.%RH) = the moisture solubility at temperature T and %RH (mg/cm3 ) Vol = sample volume (cm3) M Sat(T.3. however. 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 π6 l =0 m = 0 n =0 (5)  (2l + 1)  2  (2m + 1)  2  (2n + 1)  2     where Leqv = π 2   +   +   x o   y o   z o   Here xo. Test Method A120B (Revision of A120A) .5 Where: D(T) = the diffusivity at temperature T (mm2/s) h = sample thickness (mm) t0. 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. 60 °C/60%RH.

4. WSat.3.4.4.4. immediately cool per 5.2. is achieved as determined by a calculation using a previously determined diffusivity at 85 °C.4. 5. see 7.2 Remove the sample from the temperature/humidity chamber. of the absorption diffusivities determined in 5. cool as per 5.5 Repeat steps 5.6.2.4. Test Method A120B (Revision of A120A) .4. 22-A120B Page 7 5. Equation (5) may also be used as an alternative method.1. 5. WSat.4 Remove the sample after a recorded elapsed period of time.4 Desorption measurements above 100 °C 5.3 and 5. JEDEC Standard No.2.1 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.2.3 Immediately place the sample into a bake oven stabilized at a temperature greater than 100 °C.1 to 5.5 is now defined as the time at which the desorbed mass of moisture is equal to one-half the saturated mass.3. 5. 5.6 Calculate D(T) using equation (4). and record the saturated sample weight.4.7 Reset bake oven to a higher bake temperature and repeat measurements following 5. The sample shall be transferred into a stainless steel holder that has been preheated and stabilized at the set bake temperature. 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.4.4.3. 5. and measure the sample weight per 5.4.4. Estimated weight losses can be assessed by using the following equation: ∞  (2n + 1) 2 π 2 Dt  8 1  (2n + 1) 2 exp− Mt = 1−  (6) M Sat π2 n =0  h2  5.4 until the sample is dry. where t0.

7 Calculation of functional fit for solubility 7.JEDEC Standard No.1.2 Parameters Es and So are obtained from a curve fit of a plot of ln(CSat/P) vs. 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 = Boltzman’s constant. Measurements above the Tg of the material should be reported as a separate activation energy and pre-exponential factor. 1/T 7. it is recommended that a minimum of three temperatures are used differing by 20-30C for both above and below Tg.2 For accurate determination of the activation energy.1 The solubility can be fitted to the following equation: E  C Sat (T .3 For accurate determination of the activation energy (eV).1 The activation energy (eV) for moisture diffusion is calculated from the slope of a plot of ln{D(T)} vs.1 Diffusion of moisture may show a dependency on the Tg (Glass Transition Temperature) of the material. 6. Test Method A120B (Revision of A120A) . T = temperature in °K 7. 8. 1/T where T is in degrees Kelvin. it is recommended that a minimum of three temperatures are used differing by 20-30C for both above and below Tg. 22-A120B Page 8 6 Calculation of functional fit for moisture diffusivity 6. P ) = PS o exp s  (8)  kT  Where: So = pre-exponential factor (mg/cm3•Pa) 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.1.617x10-5 eV/°K 6.

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 9 8 Report results 8.

Replaced “DIN53495” with current version “DIN EN ISO 62:2008” & Added SEMI MS10-0812. 8 Section 7.2 Absorption measurements below 100°C (cont’d).Changed “Tg” to “Tg (Glass Transition Temperature)” for clarification. JESD22- A120B. Added “for both above and below Tg” for clarification. it is included. 7 Removed repeat of “6 Calculations of functional fit for moisture diffusivity (cont’d)”.1 – Added “= (Msat/M(mass))ρ (ρ=density)” to equation 3 for clarification. JESD22-A120A (January 2008). compared to its predecessor. “D(T)” to “D(T) (Diffusivity at Temperature)” & “CSat(T. Updated “D570-98” to “D570-10”.1 – Changed “activation energy” to “activation energy (eV)” to help clarify what “eV” is in equations. 2 Section 5. 6 Section 5. 3 Removed repeat of “5 Procedure (cont’d)” & “5.2.1 – Changed “Do” to “Do (Pre-exponential Factor for Fitted Lines)”. 5 Removed repeat of “5 Procedure (cont’d)”.Changed “activation energy” to “activation energy (eV)” to help clarify what “eV” is in equations.%RH) (Solubility at a given temperature and humidity)” for clarification. Updated read points for “dry weight” data to the more specific procedure and clarification approved in J-STD-020D.1 .Changed from “water sorption” to “moisture sorption”. 3 Sections 5. Section 5.2 – Updated procedure to determine “dry weight” to the more specific procedure and clarification approved in J-STD-020D. 4 Removed repeat of “5 Procedure (cont’d)” & “5. If the change to a concept involves any words added or deleted (excluding deletion of accidentally repeated words). “Ea” to “Ea (Activation Energy (eV))”.2. Test Method A120B (Revision of A120A) .3 .5 – Removed redundant paragraph regarding transfer of sample(s) in stabilized chamber that has been preheated. 8 Section 8. 7 Section 6. Updated “SEMI G66-96” to “SEMI G66-0811”.2. 7 Section 6.3. 1 2 Normative references – Added J-STD-020. 3 Section 5.1.3.3 & 5.1.3 – Changed “It is suggested that the sample be” to “The sample shall be”. Page Description of change 1 1 Scope .4 – Added “by Acoustic Microscopy (AM) or x-ray” inspection techniques for voids. 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.JEDEC Standard No.4.3 – Changed “Suggested environmental conditions are” to “The following environmental conditions shall be used”.%RH)” to “CSat(T. 5 Section 5. Some punctuation changes are not included. 6 Removed repeat of “5 Procedure (cont’d)”.2 Absorption measurements below 100°C (cont’d).

All comments will be collected and dispersed to the appropriate committee(s). Recommendations for correction: 3. Suite 220 Arlington.907. please complete this form and return to: JEDEC Fax: 703. clause number Test method number Clause number The referenced clause number has proven to be: Unclear Too Rigid In Error Other 2. I recommend changes to the following: Requirement. Individuals or companies are invited to submit comments to JEDEC.7583 Attn: Publications Department 2500 Wilson Blvd. If you can provide input. VA 22201-3834 1. Other suggestions for document improvement: Submitted by Name: Phone: Company: E-mail: Address: City/State/Zip: Date: .Standard Improvement Form JEDEC JESD22A120B The purpose of this form is to provide the Technical Committees of JEDEC with input from the industry regarding usage of the subject standard.