IEC 60749-7:2011
(Main)Semiconductor devices - Mechanical and climatic test methods - Part 7: Internal moisture content measurement and the analysis of other residual gases
Semiconductor devices - Mechanical and climatic test methods - Part 7: Internal moisture content measurement and the analysis of other residual gases
IEC 60749-7:2011 specifies the testing and measurement of water vapour and other gas content of the atmosphere inside a metal or ceramic hermetically sealed device. The test is used as a measure of the quality of the sealing process and to provide information about the long-term chemical stability of the atmosphere inside the package. It is applicable to semiconductor devices sealed in such a manner but generally only used for high reliability applications such as military or aerospace. This test is destructive. This second edition cancels and replaces the first edition published in 2002 and constitutes a technical revision. This second edition has been completely re-written so as to align it with the text of the latest versions of MIL-STD-750, method 1018 and MIL-STD-883, method 1018. The main change is the removal of the two alternative methods formerly designated method 2 and method 3.
Dispositifs à semiconducteurs - Méthodes d'essais mécaniques et climatiques - Partie 7: Mesure de la teneur en humidité interne et analyse des autres gaz résiduels
La CEI 60749-7:2011 spécifie les essais et les mesures de la teneur en vapeur d'eau et en autres gaz de l'atmosphère à l'intérieur d'un dispositif métallique ou céramique scellé hermétiquement. L'essai est utilisé en tant que mesure de la qualité du procédé de scellement et en vue de fournir des informations sur la stabilité chimique à long terme de l'atmosphère à l'intérieur du boîtier. Il est applicable à tous les dispositifs à semiconducteurs scellés de cette manière mais généralement réservés pour les applications à haute fiabilité comme dans les domaines militaire et spatial. Le présent essai est destructif. Cette deuxième édition annule et remplace la première édition parue en 2002, dont elle constitue une révision technique. Cette seconde édition a été complètement remaniée de manière à l'aligner sur le texte des dernières versions de la MIL-STD-750, méthode 1018 et la MIL-STD-883, méthode 1018. La modification principale est la suppression des deux méthodes alternatives, anciennement désignées méthode 2 et méthode 3.
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IEC 60749-7 ®
Edition 2.0 2011-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Semiconductor devices – Mechanical and climatic test methods –
Part 7: Internal moisture content measurement and the analysis of other residual
gases
Dispositifs à semiconducteurs – Méthodes essais mécaniques et climatiques –
Partie 7: Mesure de la teneur en humidité interne et analyse des autres gaz
résiduels
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IEC 60749-7 ®
Edition 2.0 2011-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Semiconductor devices – Mechanical and climatic test methods –
Part 7: Internal moisture content measurement and the analysis of other residual
gases
Dispositifs à semiconducteurs – Méthodes essais mécaniques et climatiques –
Partie 7: Mesure de la teneur en humidité interne et analyse des autres gaz
résiduels
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
CODE PRIX L
ICS 31.080.01 ISBN 978-2-88912-532-6
– 2 – 60749-7 IEC:2011
CONTENTS
FOREWORD . 3
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Test apparatus . 5
4.1 Mass spectrometer method . 5
4.2 Mass spectrometer . 5
4.2.1 Spectra range . 5
4.2.2 Detection limit . 6
4.2.3 System calibration . 6
4.2.4 Calibration for other gases . 6
4.2.5 Daily calibration check . 7
4.2.6 Substitution . 7
4.2.7 Precision tuning . 7
4.2.8 Record keeping . 7
4.3 Vacuum opening chamber . 7
4.4 Piercing arrangement . 7
4.5 Pressure-sensing device . 7
5 Procedure . 8
6 Failure criteria . 9
7 Implementation . 9
8 Summary . 10
Bibliography . 11
60749-7 IEC:2011 – 3 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
SEMICONDUCTOR DEVICES –
MECHANICAL AND CLIMATIC TEST METHODS –
Part 7: Internal moisture content measurement
and the analysis of other residual gases
FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote
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8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
indispensable for the correct application of this publication.
9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of
patent rights. IEC shall not be held responsible for identifying any or all such patent rights.
International Standard IEC 60749-7 has been prepared by IEC technical committee 47:
Semiconductor devices.
This second edition cancels and replaces the first edition published in 2002 and constitutes a
technical revision. This second edition has been completely re-written so as to align it with the
text of the latest versions of MIL-STD-750, method 1018 and MIL-STD-883, method 1018.
The main change is the removal of the two alternative methods formerly designated method 2
and method 3.
– 4 – 60749-7 IEC:2011
The text of this standard is based on the following documents:
FDIS Report on voting
47/2087/FDIS 47/2098/RVD
Full information on the voting for the approval of this standard can be found in the report on
voting indicated in the above table.
This publication has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 60749 series, under the general title Semiconductor devices –
Mechanical and climatic test methods, can be found on the IEC website.
The committee has decided that the contents of this publication will remain unchanged until
the stability date indicated on the IEC web site under "http://webstore.iec.ch" in the data
related to the specific publication. At this date, the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
60749-7 IEC:2011 – 5 –
SEMICONDUCTOR DEVICES –
MECHANICAL AND CLIMATIC TEST METHODS –
Part 7: Internal moisture content measurement
and the analysis of other residual gases
1 Scope
This International Standard specifies the testing and measurement of water vapour and other
gas content of the atmosphere inside a metal or ceramic hermetically sealed device. The test
is used as a measure of the quality of the sealing process and to provide information about
the long-term chemical stability of the atmosphere inside the package. It is applicable to
semiconductor devices sealed in such a manner but generally only used for high reliability
applications such as military or aerospace. This test is destructive.
2 Normative references
The following referenced documents are indispensable for the application of this document.
For dated references, only the edition cited applies. For undated references, the latest edition
of the referenced document (including any amendments) applies.
None
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
parts per million by volume
ppmv
the concentration of one substance in another substance expressed as a ratio of parts of the
one substance in a million parts of the other substance, measured by volume
4 Test apparatus
4.1 Mass spectrometer method
This method measures the water vapour content of the device atmosphere by mass spectro-
metry. The apparatus is detailed below.
4.2 Mass spectrometer
The mass spectrometer shall be capable of meeting the requirements of 4.2.1 to 4.2.2 and
shall be calibrated in accordance with 4.2.3 to 4.2.8.
4.2.1 Spectra range
The mass spectrometer shall be capable of reading a minimum spectra range of 1 AMU to
100 AMU (atomic mass units).
– 6 – 60749-7 IEC:2011
4.2.2 Detection limit
The mass spectrometer shall be capable of reproducibly detecting the specified moisture
content for a given volume package with a signal-to-noise ratio of 20:1 (i.e. for a specified
limit of 5 000 ppmv, 0,01 ml, the mass spectrometer shall demonstrate a 250 ppmv minimum
detection limit to moisture for a package volume of 0,01 ml). The smallest volume shall be
considered the worst case.
4.2.3 System calibration
The mass spectrometer shall be calibrated annually with a moisture level in the 4 500 ppmv to
5 500 ppmv range, with a moisture level in the 2 000 ppmv to 3 000 ppmv range and with a
moisture level in the 7 000 ppmv to 8 000 ppmv range using the same sensitivity factor. This
calibration needs to be performed for each calibrator volume to demonstrate a linear response
and to detect offset. A minimum of three data points for each moisture level shall be collected.
Package simulators which have the capability of generating at least three known volumes of
gas ±10 % on a repetitive basis by means of a continuous sample volume purge of known
moisture content ±5 % shall be used. Moisture content shall be established by the standard
generation techniques (i.e. double pressure, divided flow, or cryogenic method). The dew
point hygrometer shall be recalibrated a minimum of once a year using equipment traceable to
national standards or by a suitable commercial calibration services laboratory using
equipment traceable to national standards. The dew point hygrometer shall be capable of
measuring the dew point temperature to within an accuracy of ±0,2 °C. The system shall have
a pressure sensor to measure the pressure in line with the temperature dew point sensor to
an accuracy of ±300 Pa for the range of pressure being used. In addition, the test laboratory
shall have a procedure to calculate the concentration of moisture, in units of parts per million
by volume, from the dew point temperature measurement and the pressure measurement.
Gas analysis results obtained by this method shall be considered valid only in the moisture
range or limit bracketed by at least two (volume or concentration) calibration points (i.e. 5 000
ppmv between 0,01 ml to 0,1 ml or 1 000 ppmv to 5 000 ppmv between 0,01 ml to 0,1 ml). A
best fit curve shall be used between volume calibration points. Systems not capable of
bracketing may use an equivalent procedure as approved by the customer or certifying body.
Corrections of sensitivity factors deviating greater than 10 % from the mean between
calibration points shall be required.
NOTE It is recommended that the percentage of water vapour contained in a gas flowing through the gas
humidifier be compared to the dew point sensor reading for accuracy of the sensor. The following equation may be
used to calculate the per cent of water vapour contained in a gas flowing through the gas humidifier.
100 (P )
v
(1)
%H O=
P +P
g a
where
P is the vapour pressure of water in the GPH based on water temperature in degrees celsius (°C);
v
P is the gauge pressure;
g
P is the atmospheric pressure.
a
4.2.4 Calibration for other gases
Calibration shall be required for all gases found in concentrations greater than 0,01 % by
volume. As a minimum, this shall include all gases listed in Item b) of Clause 5. The
applicable gases shall be calibrated at approximately 1 % concentrations requirements, with
the exception of the following:
– fluorocarbons, which may use a concentration of approximately 200 ppmv;
– ammonia, which may use a concentration of approximately 200 ppmv;
– hydrogen, which may use a concentration of approximately 200 ppmv;
– nitrogen, which may use a concentration of approximately 80 %;
– helium, which may use a concentration of approximately 10 %; and
60749-7 IEC:2011 – 7 –
– oxygen, which may use a concentration of approximately 20 %.
4.2.5 Daily calibration check
The system calibration shall be checked on the day of test prior to any testing. This shall
include checking the calibration by admitting a sample with a moisture level in the 4 500 ppmv
to 5 500 ppmv range at the required volumes and comparing the result with the dew point
hygrometer. The resulting moisture reading shall be within 250 ppmv of the moisture level in
the calibration sample. Calibration performed on the day of test prior to any testing may be
substituted for this calibration check. Calibration records shall be kept on a daily basis.
NOTE Equipment error needs to be determined and subtracted from the allowed maximum deviation of 250 ppmv.
The calibration check shall be performed using the same conditions used for testing devices (e.g. background
pressure, background environment, time between sample inlets, package simulator volume, etc.).
4.2.6 Substitution
Any calibration performed on the day of test, and prior to any testing may be substituted for
this calibration check.
4.2.7 Precision tuning
Precision tuning shall be performed following significant maintenance or repair of the ion
source.
4.2.8 Record keeping
A record of all changes made to the sensitivity factors shall be maintained.
4.3 Vacuum opening chamber
The test apparatus shall incorporate a vacuum opening chamber which can contain the device
and a vacuum transfer passage connecting the device to the mass spectrometer according to
4.2. A vacuum transfer passage shall efficiently (without significant loss of moisture from
adsorption) transfer the gas from the device to the mass spectrometer ion source for
measurement.
For initial certification of systems or extension of suitability, device temperature on systems
using an external fixture shall be characterized by placing a thermocouple into the cavity of a
blank device of similar mass, internal volume, construction, and size. This shall be a means
for proving the device temperature that has been maintained at 100 °C ± 5 °C for the
minimum 10 min. This also applies to devices prebaked in an external oven but tested with
the external fixture to adjust for any temperature drop during the transfer. These records shall
be maintained by the test laboratory.
4.4 Piercing arrangement
The test apparatus shall contain a piercing arrangement functioning within the opening
chamber or transfer passage according to 4.3, which can pierce the specimen housing
(without breaking the mass spectrometer chamber vacuum and without disturbing the package
sealing medium), thus allowing the specimen's internal gases to escape into the chamber and
mass spectrometer.
NOTE A sharp-pointed piercing tool, actuated from outside the chamber wall via a bellows to permit movement is
used to pierce both metal and ceramic packages. For ceramic packages, or devices with thick metal lids, the
package lid or cover should be locally thinned by abrasion to facilitate localized piercing.
4.5 Pressure-sensing device
A pressure-sensing device shall be located in the transfer passage to measure the pressure
rise in the transfer passage during the test. This pressure sensor is used to read a relative
pressure change when the device is punctured. This relative pressure change indicates the
– 8 – 60749-7 IEC:2011
relative quantity of gas in the device when comparing the test results of one device to another
device. The significance of the reading is not intended to be absolute. Although the pressure
gauge reading is reported, the pressure gauge is for indication only.
5 Procedure
All devices shall be pre-baked for 16 h to 24 h at 100 °C ± 5 °C prior to the test. Ovens shall
have a means to indicate if a power interruption occurs during the pre-baking period and for
how long the temperature drops below 100 °C ± 5 °C. Devices whose temperature drops
below 100 °C ± 5 °C for more than 1 h shall undergo another pre-bake to begin a minimum of
12 h later.
A maximum 5 min transfer time from pre-bake to hot insertion into apparatus shall be allowed.
If 5 min is exceeded, the device shall be returned to the pre-bake oven and pre-bake
continued until device reaches 100 °C ± 5 °C.
The system shall be maintained at a stable temperature equal to or above the device
temperature. The fixturing in the vacuum opening chamber shall position the specimen as
required by the piercing arrangement according to 4.4 and maintain the device at
100 °C ± 5 °C for a minimum of 10 min prior to piercing.
After device insertion, the device and chamber shall be pumped down and baked out at a
temperature of 100 °C ± 5 °C until the background pressure level will not prevent achieving
the specified measurement accuracy and sensitivity. The background vacuum spectra shall be
acquired and shall later be subtracted from the sample spectra. After pump down, the device
case or lid shall be punctured and the following properties of the released gases shall be
measured using the mass spectrometer.
a) The water-vapour content of the released gases, as a percent by unit volume or ppmv of
the total gas content.
b) The proportions (by volume) of the other following gases: nitrogen, helium, Mass 69
(fluorocarbons), oxygen, argon, hydrogen, carbon dioxide, methane, ammonia, and other
solvents, if available. Calculations shall be made and reported on all gases present. Data
reduction shall be performed in a manner, which will preclude the cracking pattern
interference from other gas species in the calculations of moisture content. Data shall be
corrected for any system dependent matrix effects such as the presence of hydrogen in
the internal ambient.
c) The increase in chamber pressure as the gases are released by piercing the device
package. A pressure change of ±25 % from expected for that package volume and
pressurization may indicate that
• the puncture was not fully accomplished,
• the device package was not sealed hermetically, or
• does not contain the normal internal pressure.
d) The test laboratory should provide comments describing the spectra of unknowns or
gases that are present but not in sufficient concentration to be identified or quantified with
reasonable certainty.
e) If the test laboratory has reason to believe that the test results may be invalid due to
reasons such as improper puncture of the device or equipment malfunction, the results
shall be reported as ‘no test’ with additional comments provided. The device may be
replaced with another.
NOTE The device should be hermetic in accordance with IEC 60749-8, and free from any surface contaminants
which may interfere with accurate water vapour content measurement. The internal gas analysis laboratory is not
required to test for hermeticity in accordance with IEC 60749-8. It is recommended that samples submitted for
testing should include information about the manufacturing process, including sealing pressure, sealing gas, free
internal cavity volume, lid thickness at puncture site, lid material, and the location of the puncture site.
60749-7 IEC:2011 – 9 –
6 Failure criteria
The failure criteria are as follows.
a) A device shall be considered a failure if the water vapour content exceeds 5 000 ppmv,
unless otherwise detailed in the relevant procurement specification;
b) A device shall be considered a failure if the content of other gases exceeds the maximum
value detailed in the relevant procurement specification;
c) A device being tested in a batch system which exhibits an abnormally low total gas
content, as defined in Item c) of Clause 5, shall constitute a hermeticity failure not an
internal gas analysis failure. Such a device may be replaced by another device from the
same population; if the replacement device exhibits normal total gas content for its type,
neither it nor the original device shall constitute a failure for this cause.
7 Implementation
Suitability for performing analysis using this test method is granted by the qualifying authority
for specific limits and volumes. The calibration procedures and the suitability survey of this
test method are designed to guarantee ±20 % lab-to-lab correlation in making a determination
whether the sample passes or fails the specified limit. Water vapour contents reported either
above or below the range of suitability are not certified as correlatable values. This out of
specification data has meaning only in a relative sense and only when one laboratory's results
are being compared. The specification limit of 5 000 ppmv shall apply to all package volumes
(unless otherwise specified), with the following correction factors permitted, to be used by the
manufacturer provided they are documented and shown to be applicable:
a) For package volumes less than 0,01 ml internal free volume which are sealed while
heated in a f
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