CN107447087B - A kind of segmented dehydrogenation process method for cutting down package casing - Google Patents

A kind of segmented dehydrogenation process method for cutting down package casing Download PDF

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Publication number
CN107447087B
CN107447087B CN201710424083.0A CN201710424083A CN107447087B CN 107447087 B CN107447087 B CN 107447087B CN 201710424083 A CN201710424083 A CN 201710424083A CN 107447087 B CN107447087 B CN 107447087B
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plating
nitrogen
package casing
segmented
dehydrogenation
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CN107447087A (en
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申忠科
刘思栋
董鸣
董一鸣
夏庆水
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CETC 55 Research Institute
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CETC 55 Research Institute
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D3/00Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02Extraction of non-metals
    • C21D3/06Extraction of hydrogen

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The present invention discloses a kind of segmented dehydrogenation process method that can cut down package casing, is controlled mainly for the internal hydrogen content after package casing sealing cap, including toasts two process sections after baking and plating before plating;When heating, as the pure nitrogen gas of positive pressure to be atmosphere relative to the external world, pressure limit controls between 97-103KPa equipment, takes away part by frequent inflation/deflation and hydrogen is precipitated;Air impact is excluded by prepurging before nitrogen charging heating, specially pumping furnace chamber vacuum is to 10Pa hereinafter, then fill purity nitrogen to 50MPa or more, then is evacuated to 10Pa again hereinafter, recycling twice.The method of the present invention may be implemented to control the hydrogen contents of all kinds of kovar alloy shells in 500ppm hereinafter, and shell solderability is not influenced by big after dehydrogenation, solder soaks well on coating.

Description

A kind of segmented dehydrogenation process method for cutting down package casing
Technical field
The present invention is a kind of segmented dehydrogenation process method that can cut down package casing, is mainly used in can cut down package casing In the control of middle hydrogen content, belong to electronic encapsulation shell material processing technology.
Background technique
Kovar alloy, also referred to as teleoseal are field of power electronics, especially electronic encapsulation shell field using extremely Extensive material, with processing performance is good, linear expansion coefficient is matched with some conventional encapsulation materials and certain temperature undertissue Many advantages, such as with good stability.
Hydrogen content is to an important indicator in package casing quality requirement.Potential hazard existing for hydrogen includes: gradually Generating steam causes steam to accelerate electronic component corrosion failure, generation black brittleness tissue to cause low temperature damage, make containing excessive Obtaining certain is that sensitive material hydrogenates and loses original performance and cause the functional deterioration of the semiconductor chips such as GaAs and device.Cause This, needs the hydrogen content in strict control package casing.
But in package casing manufacturing process, it is certain thickness that kovar alloy generally requires plating after shell molding Ni layers and Au layers, the processes such as plating are difficult to avoid that introducing hydrogen from physical chemistry angle.And durings shell metallurgy, annealing etc., May also be using hydrogen shield atmosphere etc., these can also introduce hydrogen, need using certain dehydrogenation process removal shell remaining hydrogen. Method conventional at present is that have 125 DEG C of baking 168h after plating or even longer, 250 DEG C of baking 48h or even longer etc..But Gold-plated back casing long term high temperature baking, on the one hand influencing efficiency and increase equipment cost can greatly increase if 168h or more is toasted It is production cycle, also higher to equipment requirement.On the other hand, existing data is all provable under long term high temperature, coating bottom Ni It can gradually diffuse into Au layers, reach after Au layer surface because the baking oxidation solderability that shell subsequent device mounts to caused by is big It is big to reduce.
Shell dehydrogenation is needed by long-term baking, but long-time high temperature causes plating weldability to become very poor after plating, and Achieve the purpose that dehydrogenation sufficiently (target be < 500ppm) and plating weldability is influenced small, has any problem.
Summary of the invention
The present invention proposes that a kind of segmented dehydrogenation process method that can cut down package casing, the first purpose are abundant control pipes Shell hydrogen content meets hydrogen content < 500ppm by regulations examination related in GJB548B-2005;It is another object of the present invention to make The plating weldability of dehydrogenation rear casing is not influenced by big.
Technical Solving of the invention: one kind can cut down the segmented dehydrogenation process method of package casing, including plating front baking Toast two process sections after roasting and plating, when heating, equipment is as the pure nitrogen gas of positive pressure to be atmosphere, pressure limit control relative to the external world System takes away part by frequent inflation/deflation and hydrogen is precipitated between 97-103KPa;Air shadow is excluded by prepurging before nitrogen charging heating It rings, specially pumping furnace chamber vacuum is to 10Pa hereinafter, then fill purity nitrogen to 50MPa or more, then is evacuated to 10Pa again hereinafter, circulation two It is secondary.
Beneficial effects of the present invention: the hydrogen content control that all kinds of kovar alloy shells may be implemented in the method for the present invention exists 500ppm hereinafter, and shell solderability is not influenced by big after dehydrogenation, solder soaks well on coating.
Detailed description of the invention
Fig. 1 is baking process curve graph before the present invention plates.
Fig. 2 is baking process curve graph after present invention plating.
Specific embodiment
A kind of segmented dehydrogenation process cutting down package casing chooses the thick wall shell conduct that certain wall thickness is up to 5mm Typical Representative, embodiment are as follows:
1) it by the shell before being electroplated after the assembly is completed, is placed in vacuum brazing furnace or same function device, by invention Step prepurging described in content;
2) when prepurging is completed, and final nitrogen charging is to 70MPa or more, heating is opened;
3) furnace chamber nitrogen pressure range is set as 97-103KPa, and stove automatically adjusts charge and discharge nitrogen according to program;
4) heating stepses set heating rate as 10 DEG C/min, after rising to 250 DEG C of heat preservation 10min, then with 5 DEG C/min's Heating rate rises to 300 DEG C, keeps the temperature 48h, closes heating, furnace cooling.Heating, heat preservation and temperature-fall period are pure 99% or more It is carried out in nitrogen atmosphere, sees attached drawing 1;
5) 50 DEG C are cooled to the furnace hereinafter, opening fire door, taking-up shell is electroplated;
6) it after the completion of being electroplated, to being toasted after the plating of shell row within 72h, is carried out in nitrogen drying box;
7) Baking out step after plating sets 10 DEG C/min of heating rate, after rising to 100 DEG C of heat preservation 5min, then 5 DEG C/min 120 DEG C are risen to, 48h is kept the temperature, sees attached drawing 2;
8) 50 DEG C are cooled to the furnace hereinafter, opening fire door, taking-up shell completes dehydrogenation.
Baking process section before plating refers to the state when after shell items are installed residual electricity plates a process before plating.This Process section carries out in vacuum brazing furnace, and technology characteristics are 10 DEG C/min of heating rate, after rising to 250 DEG C of heat preservation 10min, then uses The heating rate of 5 DEG C/min rises to 300 DEG C, keeps the temperature 48h, closes heating, furnace cooling.Heating, heat preservation and temperature-fall period exist It is carried out in 99% or more purity nitrogen atmosphere;Under the conditions of 300 DEG C, the parameter of 48h is kept the temperature, is that the synthesis obtained after numerous tests is examined Consider the more excellent parameter of efficiency and dehydrogenation effect, can sufficiently remove can cut down the intracorporal hydrogen of base very much.
The present invention and common process Contrast on effect:
The following table 1 is above-mentioned same shell, respectively 250 DEG C after the method for the present invention and conventional plating, 48h baking method hydrogen contains Examination correlation data is measured, each group has been selected three samples.It can be observed that dehydrogenation effect of the present invention is substantially better than tradition side Method.
250 DEG C after the present invention and plating, 48h baking conventional method influences solderability: it is common to have chosen a kind of chip attachment Au-Sn solder nitrogen atmosphere, soldering chain-conveyer furnace, 340 DEG C of heat preservation 5min under the conditions of carried out wetting and spreading test, Invention and solder situation after conventional method dehydrogenation, comparison discovery present invention adverse effect caused by shell solderability are obvious It is small.
1. two methods hydrogen content data comparison of table
Wherein 1-3 is the complete direct data for detecting hydrogen content and obtaining of sealing cap after dehydrogenation of the present invention;4-6 is after dehydrogenation of the present invention Sealing cap is complete to carry out 150 DEG C, after 240h hours high-temperature storage again, detects the data of hydrogen content;7-9 be conventional method plating after 250 DEG C, 48h dehydrogenation directly detects the data that hydrogen content obtains;10-12 is 250 DEG C after plating, after 48h dehydrogenation sealing cap it is complete carry out again 150 DEG C, After 240h hours high-temperature storage, the data of hydrogen content are detected.
The present invention influences to exclude furnace chamber residual air, and prepurging operation need to be carried out before heating operation, specially takes out true Sky is opened after nitrogen valve fills purity nitrogen to 50MPa to 10Pa hereinafter, close vacuum, closes nitrogen valve and be evacuated down to 10Pa again hereinafter, so Circulation carries out normal inflated with nitrogen and heating stepses after twice again.
The present invention retains in furnace chamber in order to avoid the hydrogen that hydrogen overflows formation in baking process, and content excessively influences can The positive reaction balance for cutting down further dehydrogenation in material, needs to set soldering oven nitrogen pressure range between 97-103KPa, that is, is lower than Nitrogen valve, which automatically opens, when 97KPa is filled with nitrogen, and nitrogen valve closes exhaust valve opening when being discharged to 97KPa when being higher than 103KPa It is automatic to close exhaust valve open nitrogen valve, it moves in circles.
The above-mentioned nitrogen pressure control of the present invention, is the formulation in practical external atmosphere pressure 95KPa, needs the entire mistake of furnace chamber Journey keeps nitrogen pressure is relatively extraneous to be that positive pressure prevents from outside air from entering causing to aoxidize to baking part, so minimum pressure should be On external atmosphere pressure.Meanwhile more frequently inflation/deflation is conducive to take away the hydrogen of part precipitation, so highest nitrogen pressure and Interval between high-low pressure all should not be too large, and occurrence is referred to variation of the present invention.
The baking process stage after plating of the invention refers to after plating after the completion of plating Ni plating Au technique within 72h, if retaining after plating Time dehydrogenation again too long, the shallow-layer absorption hydrogen that electroplating process generates may diffuse to inside, and baking removal difficulty increases.This work The skill stage need to only carry out in nitrogen drying box, 10 DEG C/min of heating rate, and 5min, then 5 DEG C/min liter are kept the temperature when rising to 100 DEG C To 120 DEG C, 48h is kept the temperature.Drying box also can be selected when condition is inadequate herein directly to heat in air atmosphere, solderability is influenced Less.

Claims (5)

1. one kind can cut down the segmented dehydrogenation process method of package casing, toasts it is characterized in that including that plating is preceding and toast two after plating Process section;When heating, equipment as the pure nitrogen gas of positive pressure to be atmosphere relative to the external world, pressure limit control 97-103KPa it Between, part is taken away by frequent inflation/deflation, hydrogen is precipitated;Air impact is excluded by prepurging before nitrogen charging heating, specially pumping furnace chamber is true Sky to 10Pa hereinafter, then fill purity nitrogen to 50MPa or more, then be evacuated to 10Pa again hereinafter, circulation twice.
2. one kind according to claim 1 can cut down the segmented dehydrogenation process method of package casing, it is characterized in that affiliated Baking process before plating refers to before plating after the completion ofs shelving equal, plating start before stage;It is carried out in vacuum brazing furnace, heating speed Rate is 10 DEG C/min, after rising to 250 DEG C of heat preservation 10min, then after rising to 300 DEG C with the heating rate of 5 DEG C/min, heat preservation 48h.
3. a kind of segmented dehydrogenation process method that can cut down package casing according to claim 1, it is characterized in that affiliated plating Baking process afterwards refers to after plating after plating within 72h;It carries out, 10 DEG C/min of heating rate, rises in nitrogen drying box To 100 DEG C of heat preservation 5min, then 5 DEG C/min rises to 120 DEG C, keeps the temperature 48h.
4. a kind of according to claim 1 can cut down the segmented dehydrogenation process method of package casing, it is characterized in that need to set Nitrogen valve, which automatically opens, for nitrogen pressure range between 97-103KPa, that is, when being lower than 97KPa is filled with nitrogen, and is higher than Nitrogen valve is closed when 103KPa, air pressure is down to 97KPa again, then drain tap is automatically closed and opens nitrogen by drain tap opening Valve inflation, moves in circles.
5. baking process method after plating according to claim 3, it is characterized in that referring to that plating Ni plating Au technique is complete after the plating At being carried out within rear 72h.
CN201710424083.0A 2017-06-07 2017-06-07 A kind of segmented dehydrogenation process method for cutting down package casing Active CN107447087B (en)

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CN108438579A (en) * 2018-03-23 2018-08-24 江苏安邦电化有限公司 A kind of N-butyl raw material finished product storage tank nitrogen seal device
CN109207692A (en) * 2018-09-06 2019-01-15 合肥圣达电子科技实业有限公司 A kind of package casing manufacturing method controlling inside cavity hydrogen content
CN110193500B (en) * 2019-05-07 2020-06-16 中国石油天然气集团有限公司 Coiled tubing dehydrogenation system and coiled tubing dehydrogenation method using same
CN110592630A (en) * 2019-10-24 2019-12-20 中电国基南方集团有限公司 Sectional type dehydrogenation method for silicon-aluminum packaging shell

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CN101839340A (en) * 2009-11-14 2010-09-22 襄樊新立恒星活塞环有限责任公司 Piston ring and surface spongy tin plating technique thereof

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