CN107008984A - A kind of surface metalation and method for welding for electronic packaging composite material - Google Patents

A kind of surface metalation and method for welding for electronic packaging composite material Download PDF

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Publication number
CN107008984A
CN107008984A CN201710192150.0A CN201710192150A CN107008984A CN 107008984 A CN107008984 A CN 107008984A CN 201710192150 A CN201710192150 A CN 201710192150A CN 107008984 A CN107008984 A CN 107008984A
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sic
welding
plating
surface metalation
composite material
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CN107008984B (en
Inventor
刘桂武
张相召
乔冠军
骆文强
刘磊
邵海成
徐紫巍
王明松
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Jiangsu Hongpu Electronic Material Technology Co ltd
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Jiangsu University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B23K1/206—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/008—Soldering within a furnace
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/48—Coating with alloys
    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel

Abstract

The invention belongs to welding technology field, it is related to a kind of high-volume fractional SiCpThe surface metalation and method for welding of/Al composites.Composite deposite Ni P SiC are made by rational technique in the present invention, by adding SiC particulate into coating, you can to effectively reduce the thermal expansion coefficient difference between matrix and coating, the adhesion of lifting coating that can also be appropriate, in addition, relatively only in SiCpThe upper surface nickel plating of/Al composites is welded, and SiC particulate is added in coating can improve soldering strength to a certain extent.Low-melting-point glass solder (SnO ZnO P2O5Glass solder) there is preferable wetability with SiC ceramic, the requirement that glass is used as partial pressure of oxygen in solder welding conditions is relatively low, soldering efficiency can effectively be improved, reduce cost, therefore surface metalation and this soldering processes are combined, good soldered fitting can be obtained, the application in Electronic Packaging field is met.

Description

A kind of surface metalation and method for welding for electronic packaging composite material
Technical field
The invention belongs to high-volume fractional SiCpThe welding of/Al composites, is related to a kind of high-volume fractional SiCp/ Al is multiple The surface metalation and method for welding of condensation material.
Background technology
High-volume fractional SiCp/ Al composites are because with highly thermally conductive, high intensity, good wearability and adjustable expanding system The advantages of number (CTE), has a wide range of applications in automobile, Aero-Space, electronics industry.Although excellent performance, due to composite wood The presence of high-volume fractional SiC particulate and aluminum substrate surface film oxide in material, seriously hinder wetting of the solder on mother metal and Sprawl, and then have impact on the brazing property of matrix material.
For this problem, Many researchers are selected in SiCp/ Al composite material surfaces carry out chemical nickel plating, such as China specially A kind of sharp ZL201110259096.X " aluminum silicon carbide composite material Electroless nickel-phosphor plating process "；Such as Chinese patent " 201510051866.X a kind of high-volume fractional silicon-carbide particle reinforced aluminium-base composite material method for welding " uses Al-5Si- SiC of the 24Cu-1.5Zn-1Ti solders in plating nickel on surfacepSoldering research is done on/Al composites；Chinese patent ZL201010526125.X " a kind of intermediate temperature solder of soldering aluminum silicon carbide composite material and preparation and method for welding " uses Ag- SiC after Cu-Sn-Ni solder strip soldering chemical nickel platingsp/ Al composites and kovar alloy carry out soldering；Chinese patent A kind of SiC of ZL201110415109.8 " method of aluminum silicon carbide composite material solderability chemical nickel plating " chemical nickel platingp/ Al is multiple Aluminium nitride electronic ceramic substrate is welded using common plumber's solder in condensation material surface.Chinese patent ZL201010520717.0 " one The intermediate temperature solder of kind soldering aluminum silicon carbide composite material and preparation and method for welding " is using the weldering of 40Al-40.7Ag-19.3Cu eutectics Expect the face of weld all AlN ceramic of nickel plating and SiC/Al composites.
In welding process, wetting and the weldability of solder and matrix material can be improved after finding nickel plating, but simultaneously Occur in that the problem of some are new, the bond strength of matrix and coating not enough, in particular with the rise of welding temperature, due to matrix Cause nickel coating easily to fall off with the difference of coating thermal coefficient of expansion and reduce weld strength.The application is in order to solve nickel plating SiCpThis problem that/Al composite plate welds occur, selection introduces a certain amount of SiC particulate to be made compound in nickel coating Coating Ni-P-SiC, you can with the difference for the thermal coefficient of expansion for effectively reducing matrix and coating, the knot of coating can also be strengthened With joint efforts.
In addition in welding process, for SiCpThe solder of/Al composite solderings mainly has Al bases, Sn bases, Ag bases.Root According to above-mentioned middle welding patent, and documents below：Document " Wang Peng, Xu Dongxia, Chen Long, Niu Jitai high-volume fractionals SiCp/ 6063Al composites vacuum brazing technique and wetting mechanism research heat processing techniques, 2014,03:155-157 " uses Al- Si-Cu-Mg-Ni quinary alloy solders are to 60%SiCp/ 6063Al composites carry out vacuum brazing；" height increases document, Li Qing Jump, Zhao Zuliang, Niu Jitai high-volume fractionals SiCpThe vacuum brazing technique research heat of/6063Al composites and kovar alloy Processing technology, 2015,17:189-191 " studies high-volume fractional using Ag57.6-Cu22.4-In10-Sn10 solders are used SiCpThe vacuum brazing technique of/Al composites and kovar alloy；Document " Fan Xiaojie, Xu Dongxia, Niu Jitai, Wang Dongbin, Chen Si Outstanding .Sn-Ag-Cu-Bi lead-free brazings compare SiC to different volumesp/ 6063Al composites vacuum soldered joint tissue and performance Influence material Leaders, 2015,16:89-93 " research Sn-Ag-Cu-Bi lead-free brazings compare SiC to different volumesp/6063Al The influence of composite vacuum soldered joint tissue and performance.In comparison with the present application, Al base solders are oxidizable, Sn for above-mentioned solder Base solder welding temperature is too low, and Ag base solder costs are higher, with larger use limitation.
In a word, in comparison with the present application, above-mentioned soldering processes or solder selection can realize high-volume fractional SiCp/ Al is multiple The soldering of condensation material, but Ni layers between matrix thermal coefficient of expansion mismatch, the interface binding power defect such as loosely, postwelding easily exists Interface induces crackle, and the various limitations (welding temperature is high, oxidizable or cost is higher etc.) of metal solder in addition all become Limit the principal element of such method application.Therefore how by researching and developing suitable glass solder and optimization soldering processes, into For high-volume fractional SiCpThe wide variety of technical bottleneck of/Al composites.
The content of the invention
The invention reside in the surface metalation and method for welding there is provided a kind of electronic packaging composite material, it is therefore an objective to improves High-volume fractional SiCp/ Al composite soldered fitting performances, the particularly characteristic such as the intensity of joint, corrosion resistance.
To achieve these goals, the present invention, which is adopted the following technical scheme that, is achieved, and one kind is used for Electronic Packaging The surface metalation and method for welding of composite, the preparation of its surface metalation are made up of following steps：
1st, it is a kind of for electronic packaging composite material method for surface metallation, including：
(1) composite plating bath is prepared：By commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid with one Determine concentration proportioning to be well mixed, then add a certain amount of SiC particulate, be configured to the Ni-P-SiC plating solutions of certain pH value.
(2) sample pretreatment：By high-volume fractional SiCp/ Al composites use deionization after carrying out oil removing, sensitization, activation Water is cleaned.
(3) plating：The sample handled well in step (2) is put into the composite plating bath configured in step (1), one is placed in Composite Coatings are carried out in the magnetic agitation water-bath of constant temperature degree.
Nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate in above-mentioned preparation composite plating bath, Ni-P-SiC plating solutions Concentration with lactic acid is respectively：25g/L, 30g/L, 20g/L, 15g/L and 30g/L, SiC concentration are 3g/L, Ni-P-SiC plating solutions PH value be 4-6.
Above-mentioned sample pretreatment, wherein oil removing：Acetone, ultrasonic 10min；Sensitization：50ml/L HCl+25g/L SnCl2 In solution, 15s, room temperature；Activation：25ml/L HCl+0.25g/L PdCl2In solution, 20s, room temperature.
Above-mentioned plating, its plating temperature is 80-90 DEG C, plating time：15-60mim.
To achieve these goals, the present invention, which is adopted the following technical scheme that, is achieved, and one kind is used for Electronic Packaging The surface metalation and soldering processes of composite, its soldering processes are made up of following steps：
(1) to-be-welded pieces through surface metalation are placed in absolute ethyl alcohol and be cleaned by ultrasonic 15 minutes.
(2) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate organic binder bond, after being sufficiently stirred for To uniform paste.
(3) paste solder is coated uniformly on using manual application or the method for silk-screen printing by cleaned to-be-welded pieces On.
(4) two coated to-be-welded pieces surfaces are in contact and alignd and be put into graphite jig, and in two coatings The steel part of certain pressure can be applied by being placed on good part to be welded.
(5) graphite jig assembled is placed in vacuum (vacuum≤1 × 10 in vacuum drying oven-2Pa) or under argon gas protection enter Row soldering, certain temperature is heated to certain firing rate, and after after held for some time, 300 are cooled to certain cooling velocity DEG C, blow-on is sampled when then cooling to room temperature with the furnace.
Above-mentioned appropriate binding agent is the composite solution of terpinol and ethyl cellulose, and wherein terpinol is solvent, and Terpinol：Ethyl cellulose：Eutectic SnO-ZnO-P2O5The mass ratio of glass solder is 9:1:10.
Above-mentioned certain pressure is 3-10kPa.
Above-mentioned programming rate is 5-10 DEG C/min, and brazing temperature is 500-600 DEG C, and soaking time is 10-30min, cold But speed is 3-5 DEG C/min.
The application mainly passes through high-volume fractional SiCp/ Al composite material surfaces metallize and using middle temperature glass solder profit With vacuum protection soldering composite.By to high-volume fractional SiCp/ Al composite material surfaces metallize, and improve glass solder To the wettability of composite, by adding appropriate SiC particulate into metallization coating, it can effectively reduce matrix and plating The coefficient of thermal expansion differences of layer, the appropriate adhesion for lifting coating.To ensure to obtain good soldered fitting, in brazing process, To-be-welded pieces need to apply certain pressure, while welding atmosphere is needed for vacuum or argon gas protection.
Compared with prior art, the present invention has advantages below：(1) composite deposite Ni-P- is made by rational technique SiC, by adding SiC particulate into coating, you can to effectively reduce the thermal expansion coefficient difference between matrix and coating, may be used also With the adhesion of appropriate lifting coating, in addition, relatively only in SiCpThe upper surface nickel plating of/Al composites is welded, coating Middle addition SiC particulate can improve soldering strength to a certain extent.(2) for relatively several conventional metals base solders, eutectic glass Glass solder (SnO-ZnO-P2O5Glass solder) there is preferable wetability with SiC ceramic, glass is used as oxygen in solder welding conditions The requirement of partial pressure is relatively low, can effectively improve soldering efficiency, reduces cost, therefore surface metalation is mutually tied with this soldering processes Close, good soldered fitting can be obtained, the application in Electronic Packaging field is met.
Brief description of the drawings
Fig. 1 is high-volume fractional SiCp/ Al composite material surface Ni-P-SiC coating SEM schemes.
Fig. 2 is high-volume fractional SiCp/ Al composite material surface Ni-P-SiC coating cross section SEM schemes, and illustrates SiC ceramic It is uniformly distributed among coating.
When Fig. 3 is SiC concentration 3g/L after the scraping pattern of composite deposite and correspondence acoustical signal figure, composite deposite scraping experiment Pattern and correspondence acoustic signal intensity, illustrate composite deposite and SiCp/Al composites has good binding ability.
Embodiment
With reference to specific embodiment, the present invention is further elaborated.It is of the present invention a kind of for Electronic Packaging The surface metalation step of composite includes：
(1) composite plating bath is prepared：By commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid with one Determine concentration proportioning to be well mixed, then add SiC particulate, be configured to the Ni-P-SiC plating solutions of certain pH value.
(2) sample pretreatment：By high-volume fractional SiCp/ Al composites use deionization after carrying out oil removing, sensitization, activation Water is cleaned.
(3) plating：The sample handled well in (2) is put into the composite plating bath configured in (1), certain temperature is placed in Composite Coatings are carried out in magnetic agitation water-bath.
Nickel sulfate in preparation composite plating bath of the present invention, Ni-P-SiC plating solutions, sodium hypophosphite, trisodium citrate, The concentration of sodium acetate and lactic acid is respectively：25g/L, 30g/L, 20g/L, 15g/L and 30g/L, SiC concentration 3g/L, composite plating bath PH is 4-6.
Sample pretreatment of the present invention, wherein oil removing：Acetone, ultrasonic 10min；Sensitization：50ml/L HCl+25g/L SnCl2In solution, 15s, room temperature；Activation：25ml/L HCl+0.25g/L PdCl2In solution, 20s, room temperature.
Plating of the present invention, its plating temperature is 80-90 DEG C, plating time：15-60mim.
A kind of soldering processes for electronic packaging composite material of the present invention include：
(1) to-be-welded pieces through surface metalation are placed in absolute ethyl alcohol and be cleaned by ultrasonic 15 minutes.
(2) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate organic binder bond, after being sufficiently stirred for To uniform paste.
(3) paste solder is coated uniformly on using manual application or the method for silk-screen printing by cleaned to-be-welded pieces On.
(4) two coated to-be-welded pieces surfaces are in contact and alignd and be put into graphite jig, and in two coatings The steel part of certain pressure can be applied by being placed on good part to be welded.
(5) graphite jig assembled is placed in vacuum (vacuum≤1 × 10 in vacuum drying oven-2Pa) or under argon gas protection enter Row soldering, certain temperature is heated to certain firing rate, and after after held for some time, 300 are cooled to certain cooling velocity DEG C, blow-on is sampled when then cooling to room temperature with the furnace.
Appropriate binding agent of the present invention be terpinol+ethyl cellulose solution, wherein terpinol be solvent, and pine Oleyl alcohol：Ethyl cellulose：Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g, application certain pressure is 3-10kPa, heating Speed is 5-10 DEG C/min, and brazing temperature is 500-600 DEG C, and soaking time is 10-30min, and cooling velocity is 3-5 DEG C/min.
Case study on implementation 1
(1) by commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid respectively with 25g/L, 30g/ L, 20g/L, 15g/L and 30g/L concentration are well mixed, and then add 3g/L SiC particulate, are configured to the Ni-P-SiC that PH is 4 Plating solution.
(2) by high-volume fractional SiCpAfter/Al composites first have children outside the state plan oil removing through acetone, 50ml/L HCl+25g/L are placed in SnCl2It is sensitized, is then putting and 25ml/L HCl+0.25g/L PdCl in solution2Activated in solution, it is dry with deionized water rinsing Only it is placed in the composite plating bath configured in (1).Finally it is placed in magnetic agitation water-bath and carries out Composite Coatings, regulation temperature is 80 DEG C, plating time is 60min.
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate terpinol+ethyl cellulose solution (pine Oleyl alcohol：Ethyl cellulose:Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g), uniform paste is obtained after being sufficiently stirred for.With Paste is covered in the high-volume fractional SiC of metalized by manual application or method for printing screenp/ Al composite material surfaces On.
(4) the tape welding fitting surface for coating completion is in contact and alignd and be put into graphite jig, and in sample to be connected It is upper to place the steel part for applying 10kPa pressure；The graphite jig assembled is placed in vacuum drying oven (vacuum≤1 × 10-2) or argon Pa Soldering is carried out under gas shielded, 400 DEG C are heated with 10 DEG C/min, then is heated to 5 DEG C/min after 530 DEG C, insulation 30min, with 5 DEG C/min cooling velocity to 400 DEG C, then with 3 DEG C/min cooling velocity to 300 DEG C, blow-on when then cooling to room temperature with the furnace Sampling.
Case study on implementation 2
(1) by commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid respectively with 25g/L, 30g/ L, 20g/L, 15g/L and 30g/L concentration are well mixed, and then add 3g/L SiC particulate, are configured to the Ni-P-SiC that PH is 4 Plating solution.
(2) by high-volume fractional SiCpAfter/Al composites first have children outside the state plan oil removing through acetone, 50ml/L HCl+25g/L are placed in SnCl2It is sensitized, is then putting and 25ml/L HCl+0.25g/L PdCl in solution2Activated in solution, it is dry with deionized water rinsing Only it is placed in the composite plating bath configured in (1).Finally it is placed in magnetic agitation water-bath and carries out Composite Coatings, regulation temperature is 90 DEG C, plating time is 30min.
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate terpinol+ethyl cellulose solution (pine Oleyl alcohol：Ethyl cellulose:Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g), uniform paste is obtained after being sufficiently stirred for.With Paste is covered in the high-volume fractional SiC of metalized by manual application or method for printing screenp/ Al composite material surfaces On.
(4) the tape welding fitting surface for coating completion is in contact and alignd and be put into graphite jig, and in sample to be connected It is upper to place the steel part for applying 5kPa pressure；The graphite jig assembled is placed in vacuum drying oven (vacuum≤1 × 10-2) or argon gas Pa Protection is lower to carry out soldering, and 400 DEG C are heated with 10 DEG C/min, then is heated to 5 DEG C/min after 500 DEG C, insulation 15min, with 5 DEG C/ Min cooling velocity is to 400 DEG C, then with 3 DEG C/min cooling velocity to 300 DEG C, and blow-on takes when then cooling to room temperature with the furnace Sample.
Case study on implementation 3
(1) by commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid respectively with 25g/L, 30g/ L, 20g/L, 15g/L and 30g/L concentration are well mixed, and then add 3g/L SiC particulate, are configured to the Ni-P-SiC that PH is 6 Plating solution.
(2) after high-volume fractional SiCp/Al composites first being had children outside the state plan into oil removing through acetone, 50ml/L HCl+25g/L are placed in SnCl2It is sensitized, is then putting and 25ml/L HCl+0.25g/L PdCl in solution2Activated in solution, it is dry with deionized water rinsing Only it is placed in the composite plating bath configured in (1).Finally it is placed in magnetic agitation water-bath and carries out Composite Coatings, regulation temperature is 90 DEG C, plating time is 15min.
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate terpinol+ethyl cellulose solution (pine Oleyl alcohol：Ethyl cellulose:Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g), uniform paste is obtained after being sufficiently stirred for.With Paste is covered in the high-volume fractional SiC of metalized by manual application or method for printing screenp/ Al composite material surfaces On.
(4) the tape welding fitting surface for coating completion is in contact and alignd and be put into graphite jig, and in sample to be connected It is upper to place the steel part for applying 3kPa pressure；The graphite jig assembled is placed in vacuum drying oven (vacuum≤1 × 10-2) or argon gas Pa Protection is lower to carry out soldering, and 400 DEG C are heated with 10 DEG C/min, then is heated to 5 DEG C/min after 580 DEG C, insulation 30min, with 5 DEG C/ Min cooling velocity is to 400 DEG C, then with 3 DEG C/min cooling velocity to 300 DEG C, and blow-on takes when then cooling to room temperature with the furnace Sample.
Case study on implementation 4
(1) by commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid respectively with 25g/L, 30g/ L, 20g/L, 15g/L and 30g/L concentration are well mixed, and then add 3g/L SiC particulate, are configured to the Ni-P-SiC that PH is 6 Plating solution.
(2) after high-volume fractional SiCp/Al composites first being had children outside the state plan into oil removing through acetone, 50ml/L HCl+25g/L are placed in SnCl2It is sensitized, is then putting and 25ml/L HCl+0.25g/L PdCl in solution2Activated in solution, it is dry with deionized water rinsing Only it is placed in the composite plating bath configured in (1).Finally it is placed in magnetic agitation water-bath and carries out Composite Coatings, regulation temperature is 85 DEG C, plating time is 40min.
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate terpinol+ethyl cellulose solution (pine Oleyl alcohol：Ethyl cellulose:Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g), uniform paste is obtained after being sufficiently stirred for.With Paste is covered in the high-volume fractional SiC of metalized by manual application or method for printing screenp/ Al composite material surfaces On.
(4) the tape welding fitting surface for coating completion is in contact and alignd and be put into graphite jig, and in sample to be connected It is upper to place the steel part for applying 10kPa pressure；The graphite jig assembled is placed in vacuum drying oven (vacuum≤1 × 10-2) or argon Pa Soldering is carried out under gas shielded, 400 DEG C are heated with 10 DEG C/min, then is heated to 5 DEG C/min after 600 DEG C, insulation 10min, with 5 DEG C/min cooling velocity to 400 DEG C, then with 3 DEG C/min cooling velocity to 300 DEG C, blow-on when then cooling to room temperature with the furnace Sampling.
Case study on implementation 5
(1) by commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid respectively with 25g/L, 30g/ L, 20g/L, 15g/L and 30g/L concentration are well mixed, and then add 3g/L SiC particulate, are configured to the Ni-P-SiC that PH is 5 Plating solution.
(2) by high-volume fractional SiCpAfter/Al composites first have children outside the state plan oil removing through acetone, 50ml/L HCl+25g/L are placed in SnCl2It is sensitized, is then putting and 25ml/L HCl+0.25g/L PdCl in solution2Activated in solution, it is dry with deionized water rinsing Only it is placed in the composite plating bath configured in (1).Finally it is placed in magnetic agitation water-bath and carries out Composite Coatings, regulation temperature is 80 DEG C, plating time is 15min.
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds appropriate terpinol+ethyl cellulose solution (pine Oleyl alcohol：Ethyl cellulose:Eutectic SnO-ZnO-P2O5Glass solder=9g:1g:10g), uniform paste is obtained after being sufficiently stirred for.With Paste is covered in the high-volume fractional SiC of metalized by manual application or method for printing screenp/ Al composite material surfaces On.
(4) the tape welding fitting surface for coating completion is in contact and alignd and be put into graphite jig, and in sample to be connected It is upper to place the steel part for applying 10kPa pressure；The graphite jig assembled is placed in vacuum drying oven (vacuum≤1 × 10-2) or argon Pa Soldering is carried out under gas shielded, 400 DEG C are heated with 10 DEG C/min, then is heated to 5 DEG C/min after 590 DEG C, insulation 30min, with 5 DEG C/min cooling velocity to 400 DEG C, then with 3 DEG C/min cooling velocity to 300 DEG C, blow-on when then cooling to room temperature with the furnace Sampling.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention Any simple modification, change that technical spirit is made to above example, still fall within the protection domain of technical solution of the present invention It is interior.

Claims (7)

1. a kind of surface metalation and method for welding for electronic packaging composite material, it is characterised in that comprise the following steps that：
(1) composite plating bath is prepared：By commercially available nickel sulfate, sodium hypophosphite, trisodium citrate, sodium acetate and lactic acid with certain dense Degree proportioning is well mixed, then adds a certain amount of SiC particulate, is configured to the Ni-P-SiC plating solutions of certain pH value；
(2) plating：The sample pre-processed is put into the composite plating bath configured in step (1), the magnetic of certain temperature is placed in Composite Coatings are carried out in power stirring water-bath, the to-be-welded pieces through surface metalation are obtained；
(3) commercially available eutectic SnO-ZnO-P is taken2O5Glass solder, adds organic binder bond, uniform paste is obtained after being sufficiently stirred for；
(4) paste solder is coated uniformly on using the method for manual application or silk-screen printing cleaned through surface metalation In to-be-welded pieces；
(5) two coated to-be-welded pieces surfaces are in contact and alignd and be put into graphite jig, and it is coated at two The steel part of certain pressure can be applied by being placed on part to be welded；
(6) graphite jig assembled is placed in vacuum or the lower progress soldering of argon gas protection in vacuum drying oven, with certain firing rate Certain temperature is heated to, after after held for some time, 300 DEG C is cooled to certain cooling velocity, then cools to room temperature with the furnace Shi Kailu is sampled.
2. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is：In the Ni-P-SiC plating solutions, nickel sulfate, sodium hypophosphite, trisodium citrate, the concentration difference of sodium acetate and lactic acid For：25g/L, 30g/L, 20g/L, 15g/L and 30g/L, SiC concentration are 3g/L, and the pH value of Ni-P-SiC plating solutions is 4-6.
3. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is, described sample pretreatment refers to：By high-volume fractional SiCp/ Al composites carry out oil removing, sensitization, activate after spend from Sub- water cleaning；Wherein oil removing：Acetone, ultrasonic 10min；Sensitization：50ml/L HCl+25g/L SnCl2In solution, 15s, room temperature； Activation：25ml/L HCl+0.25g/L PdCl2In solution, 20s, room temperature.
4. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is, described plating, its plating temperature is 80-90 DEG C, plating time：15-60mim.
5. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is, described binding agent is terpinol and the composite solution of ethyl cellulose, wherein terpinol is solvent, and terpinol：Second Base cellulose：Eutectic SnO-ZnO-P2O5The mass ratio of glass solder is 9:1:10.
6. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is, described certain pressure is 3-10kPa.
7. a kind of surface metalation and method for welding for electronic packaging composite material as claimed in claim 1, its feature It is, vacuum≤1 × 10-2Pa, programming rate is 5-10 DEG C/min, and brazing temperature is 500-600 DEG C, and soaking time is 10-30min, cooling velocity is 3-5 DEG C/min.
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US5246890A (en) * 1992-08-03 1993-09-21 Corning Incorporated Non-lead sealing glasses
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