CN105364246B - A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing - Google Patents

A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing Download PDF

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CN105364246B
CN105364246B CN201510968183.0A CN201510968183A CN105364246B CN 105364246 B CN105364246 B CN 105364246B CN 201510968183 A CN201510968183 A CN 201510968183A CN 105364246 B CN105364246 B CN 105364246B
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sio
matric composite
ceramic matric
solder
pretreated
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CN105364246A (en
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亓钧雷
罗大林
马蔷
林景煌
陈树林
冯吉才
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Harbin Institute of Technology
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Harbin Institute of Technology
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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
    • B23K1/008—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
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Ceramic Products (AREA)

Abstract

A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing, the present invention relates to material welding field.The invention solves the problems that existing SiO2The fused quartz of amorphous is difficult to be soaked by active solder in ceramic matric composite, and then influences SiO2The problem of joint mechanical property of ceramic matric composite and solder bonding metal.Method：First by sand paper to SiO2Ceramic matric composite, solder and metal material are polished, are cleaned by ultrasonic, then using corrosive liquid to SiO2Ceramic matric composite welding surface is corroded, finally by the SiO after corrosion2Ceramic matric composite, solder and metal material stack and are put into vacuum furnace brazing successively.The present invention is used for surface corrosion SiO2The method of ceramic matric composite assistant brazing.

Description

A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing
Technical field
The present invention relates to material welding field.
Background technology
It is severe particularly in the research and development process of aerospace industry advanced material in the development of advanced composite material The service condition at quarter is good to light weight, resistance to elevated temperatures, good mechanical performance advanced Ceramic Matrix Composites Fabricated is constantly proposed more High requirement, this causes the advanced composite material using fibre-woven composite as representative to get growing concern for.And make For a kind of crucial protection and electric component, SiO2Ceramic matric composite is obtained extensively on the antenna house of aerospace craft Using.Antenna house assembling and in use, cover body composite is necessarily required to realize in its end and metal material effectively connects Connect, so as to obtain finished product member.
At present, sintering metal powder, diffusion welding (DW), transition liquid-phase combination and vacuum brazing are normal as ceramics-to-metals joining Method.Wherein, the method for vacuum brazing is most widely used, because this method is simple to operate, and cost is low and joint matter Amount is high.Vacuum brazing refers to that workpiece heat is carried out in vacuum chamber, is mainly used in requirement quality high product and oxidizable material Welding.In Process of Vacuum Brazing, weldment and solder heat, less than mother metal fusion temperature, utilize liquid to higher than solder fusing point State solder wetting mother metal, fills play movement and is connected weldment with mother metal phase counterdiffusion realization.However, the fused quartz of amorphous is difficult to Soaked by active solder, and then influence SiO2The joint mechanical property of ceramic matric composite and solder bonding metal.
The content of the invention
The invention solves the problems that existing SiO2The fused quartz of amorphous is difficult to be soaked by active solder in ceramic matric composite, enters And influence SiO2The problem of joint mechanical property of ceramic matric composite and solder bonding metal, and a kind of surface corrosion SiO is provided2 The method of ceramic matric composite assistant brazing.
A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing, is specifically followed the steps below 's：
First, by SiO2Ceramic matric composite, solder and metal material are polished with sand paper respectively, then clear with acetone successively 10min~20min is washed, pretreated SiO is obtained2Ceramic matric composite, pretreated solder and pretreated gold Belong to material；
2nd, with corrosive liquid to pretreated SiO2Ceramic matric composite is corroded, corrosion depth be 0.01mm~ 5mm, 10min~20min is cleaned after corrosion with acetone, the SiO after being corroded2Ceramic matric composite；
Described corrosive liquid is the hydrofluoric acid that mass percent is 1%~48% and mass percent is 1%~70% The mixed liquor of nitric acid, the nitric acid that the hydrofluoric acid that described mass percent is 1%~48% is 1%~70% with mass percent Volume ratio be 1:(1~5)；
Or described corrosive liquid be NaOH that mass percent is 10%~50% and mass percent be 10%~ 50% KOH mixed liquor, the NaOH and mass percent that described mass percent is 10%~50% are 10%~50% KOH volume ratio be 1:(1~5)；
3rd, the SiO that pretreated solder is placed in after corrosion2Ceramic matric composite and pretreated metal material Between surface to be welded, part to be welded is obtained, part to be welded is placed in vacuum brazing furnace, 5 × 10 are evacuated to vacuum brazing furnace- 4Pa~5 × 10-3Pa, is then warming up to 500 DEG C~1200 DEG C by vacuum brazing furnace temperature, and is 500 DEG C~1200 in temperature 5min~30min is incubated at DEG C, temperature is finally cooled to by room temperature by 500 DEG C~1200 DEG C with 5 DEG C/min~10 DEG C/min, i.e., Complete surface corrosion SiO2The method of ceramic matric composite assistant brazing.
The present invention can make SiO by using corrosive liquid2The amorphous Si O of ceramic matric composite surface hardly possible wetting2It is rotten Erosion, so as to significantly improve active solder in SiO2Ceramic matric composite wettability of the surface, and formed in ceramic side Unique pinning effect, pinning effect can alleviate joint residual stress, so that the mechanical property of joint is improved, it is final to realize SiO2The high-quality connection of ceramic matric composite and metal.Such a method is simple, and efficiently, cost is low, is easy to industrial metaplasia Production.
The beneficial effects of the invention are as follows：
1st, the present invention is by corroding amorphous substance, so as to promote solder in SiO2The wetting on ceramic matric composite surface Sprawl, realize SiO2The high-quality connection of ceramic matric composite and metal.
2nd, the present invention can be matched simply by regulating and controlling the concentration and mixed liquor of corrosive liquid, and then obtain different corrosion The ceramics of effect, so as to obtain the soldered fitting of different performance.
3rd, the method corroded in the present invention to ceramic matric composite surface using corrosive liquid is simple, efficient, cost It is low.
4th, the present invention is by first corroding, the process welded afterwards, the pinning effect of uniqueness can be formed in ceramic side, so as to alleviate Joint residual stress, improves the mechanical property of joint.
The present invention is used for a kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing.
Brief description of the drawings
Fig. 1 is the SiO that embodiment one is obtained2f/SiO2Ceramic matric composite and metal Nb connector seam organization Scanning electron microscopic picture.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it Between any combination.
Embodiment one：A kind of surface corrosion SiO described in present embodiment2Ceramic matric composite assistant brazing Method, specifically follow the steps below：
First, by SiO2Ceramic matric composite, solder and metal material are polished with sand paper respectively, then clear with acetone successively 10min~20min is washed, pretreated SiO is obtained2Ceramic matric composite, pretreated solder and pretreated gold Belong to material；
2nd, with corrosive liquid to pretreated SiO2Ceramic matric composite is corroded, corrosion depth be 0.01mm~ 5mm, 10min~20min is cleaned after corrosion with acetone, the SiO after being corroded2Ceramic matric composite；
Described corrosive liquid is the hydrofluoric acid that mass percent is 1%~48% and mass percent is 1%~70% The mixed liquor of nitric acid, the nitric acid that the hydrofluoric acid that described mass percent is 1%~48% is 1%~70% with mass percent Volume ratio be 1:(1~5)；
Or described corrosive liquid be NaOH that mass percent is 10%~50% and mass percent be 10%~ 50% KOH mixed liquor, the NaOH and mass percent that described mass percent is 10%~50% are 10%~50% KOH volume ratio be 1:(1~5)；
3rd, the SiO that pretreated solder is placed in after corrosion2Ceramic matric composite and pretreated metal material Between surface to be welded, part to be welded is obtained, part to be welded is placed in vacuum brazing furnace, 5 × 10 are evacuated to vacuum brazing furnace- 4Pa~5 × 10-3Pa, is then warming up to 500 DEG C~1200 DEG C by vacuum brazing furnace temperature, and is 500 DEG C~1200 in temperature 5min~30min is incubated at DEG C, temperature is finally cooled to by room temperature by 500 DEG C~1200 DEG C with 5 DEG C/min~10 DEG C/min, i.e., Complete surface corrosion SiO2The method of ceramic matric composite assistant brazing.
The beneficial effect of present embodiment is：
1st, present embodiment is by corroding amorphous substance, so as to promote solder in SiO2Ceramic matric composite surface Wetting and spreading, realizes SiO2The high-quality connection of ceramic matric composite and metal.
2nd, present embodiment can be matched simply by regulating and controlling the concentration and mixed liquor of corrosive liquid, and then obtain difference The ceramics of corrosive effect, so as to obtain the soldered fitting of different performance.
3rd, the method corroded in present embodiment to ceramic matric composite surface using corrosive liquid it is simple, efficient, Cost is low.
4th, present embodiment is by first corroding, the process welded afterwards, and the pinning effect of uniqueness can be formed in ceramic side, so that Alleviate joint residual stress, improve the mechanical property of joint.
Embodiment two：Present embodiment from unlike embodiment one：SiO described in step one2 Ceramic matric composite is SiO2f/SiO2Ceramic matric composite, SiO2f/Al2O3Ceramic matric composite or fiber reinforcement pottery Porcelain based composites.It is other identical with embodiment one.
Embodiment three：Unlike one of present embodiment and embodiment one or two：Institute in step one The solder stated is TiZrCuNi, TiZrCu, AgCuTi, TiCuNi, TiNi or TiNiNb.Other and embodiment one or two It is identical.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Institute in step one The solder stated is paillon foil.It is other identical with embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Institute in step one The metal material stated is metal Nb, titanium alloy TC 4, Invar alloys or GH99 alloys.It is other with the phase of embodiment one to four Together.
Embodiment six：Unlike one of present embodiment and embodiment one to five：It is rotten in step 2 Erosion depth is 0.05mm.It is other identical with embodiment one to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：It is rotten in step 2 Erosion depth is 0.05mm~5mm.It is other identical with embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：It is right in step 3 Vacuum brazing furnace is evacuated to 1 × 10-3Pa~5 × 10-3Pa.It is other identical with embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：In step 3 so Vacuum brazing furnace temperature is warming up to 600 DEG C afterwards, and 5min~30min is incubated in the case where temperature is 600 DEG C.Other and specific implementation Mode one to eight is identical.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：In step 3 so Vacuum brazing furnace temperature is warming up to 860 DEG C afterwards, and 5min~30min is incubated in the case where temperature is 860 DEG C.Other and specific implementation Mode one to nine is identical.
Embodiment 11：Unlike one of present embodiment and embodiment one to ten：In step 3 Then vacuum brazing furnace temperature is warming up to 500 DEG C~1200 DEG C, and temperature be insulation 5min at 500 DEG C~1200 DEG C~ 15min.It is other identical with embodiment one to ten.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：
A kind of surface corrosion SiO described in the present embodiment2The method of ceramic matric composite assistant brazing, be specifically according to What following steps were carried out：
First, by SiO2Ceramic matric composite, solder and metal material are polished with sand paper respectively, then clear with acetone successively 15min is washed, pretreated SiO is obtained2Ceramic matric composite, pretreated solder and pretreated metal material；
2nd, with corrosive liquid to pretreated SiO2Ceramic matric composite is corroded, and corrosion depth is 0.05mm, rotten 15min is cleaned with acetone after erosion, the SiO after being corroded2Ceramic matric composite；
The mixing for the nitric acid that described corrosive liquid is the hydrofluoric acid that mass percent is 40% and mass percent is 1% Liquid, the volume ratio for the nitric acid that the hydrofluoric acid that described mass percent is 40% is 1% with mass percent is 1:1；
3rd, the SiO that pretreated solder is placed in after corrosion2Ceramic matric composite and pretreated metal material Between surface to be welded, part to be welded is obtained, part to be welded is placed in vacuum brazing furnace, 5 × 10 are evacuated to vacuum brazing furnace- 3Pa, is then warming up to 860 DEG C by vacuum brazing furnace temperature, and is incubated 10min in the case where temperature is 860 DEG C, finally with 5 DEG C/min Temperature is cooled to room temperature by 860 DEG C, SiO is obtained2f/SiO2The connector of ceramic matric composite and metal Nb, that is, complete table Corrode SiO in face2The method of ceramic matric composite assistant brazing.
SiO described in step one2Ceramic matric composite is SiO2f/SiO2Ceramic matric composite；
Solder described in step one is AgCuTi paillon foils；
Metal material described in step one is metal Nb.
The SiO that the present embodiment is obtained2f/SiO2The shearing resistance of ceramic matric composite and metal Nb connector at room temperature is strong Spend for 51.2MPa, SiO of the AgCuTi solders after corrosion prepared by step 22Ceramic matric composite moistened surface angle is 29.3°。
Fig. 1 is the SiO that embodiment one is obtained2f/SiO2Ceramic matric composite and metal Nb connector seam organization Scanning electron microscopic picture；As seen from the figure, amorphous structure is corroded in ceramic matrix.

Claims (2)

1. a kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing, it is characterised in that it is according to following steps Carry out：
First, by SiO2Ceramic matric composite, solder and metal material are polished with sand paper respectively, are then cleaned successively with acetone 10min~20min, obtains pretreated SiO2Ceramic matric composite, pretreated solder and pretreated metal Material；
SiO described in step one2Ceramic matric composite is SiO2f/SiO2Ceramic matric composite；
Metal material described in step one is metal Nb, titanium alloy TC 4, Invar alloys or GH99 alloys；
Solder described in step one is TiZrCuNi, TiZrCu, AgCuTi, TiCuNi, TiNi or TiNiNb；
2nd, with corrosive liquid to pretreated SiO2Ceramic matric composite is corroded, and corrosion depth is 0.01mm~5mm, rotten 10min~20min is cleaned with acetone after erosion, the SiO after being corroded2Ceramic matric composite；
The mixed liquor for the nitric acid that described corrosive liquid is the hydrofluoric acid that mass percent is 40% and mass percent is 1%, institute The volume ratio for the nitric acid that the hydrofluoric acid that the mass percent stated is 40% is 1% with mass percent is 1:1；
3rd, the SiO that pretreated solder is placed in after corrosion2Ceramic matric composite and pretreated metal material are to be welded Between junction, part to be welded is obtained, part to be welded is placed in vacuum brazing furnace, 5 × 10 are evacuated to vacuum brazing furnace-4Pa~5 ×10-3Pa, is then warming up to 860 DEG C by vacuum brazing furnace temperature, and is incubated 10min~30min in the case where temperature is 860 DEG C, most Temperature is cooled to by 860 DEG C by room temperature with 5 DEG C/min~10 DEG C/min afterwards, that is, completes surface corrosion SiO2Ceramic matric composite The method of assistant brazing.
2. a kind of surface corrosion SiO according to claim 12The method of ceramic matric composite assistant brazing, its feature exists Solder described in step one is paillon foil.
CN201510968183.0A 2015-12-21 2015-12-21 A kind of surface corrosion SiO2The method of ceramic matric composite assistant brazing Active CN105364246B (en)

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CN110240494A (en) * 2019-06-28 2019-09-17 大连大学 A kind of fiber reinforcement Cf/SiC composite plate weld connector
CN112548252B (en) * 2020-11-30 2022-06-21 哈尔滨工业大学 Method for regulating and controlling surface structure of carbon fiber reinforced composite material and metal brazing through electric corrosion
CN112548253B (en) * 2020-11-30 2022-03-25 哈尔滨工业大学 Method for brazing fiber reinforced composite material and metal in selective hot corrosion auxiliary mode

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JP3266041B2 (en) * 1996-05-22 2002-03-18 株式会社島津製作所 Member joining method and optical measuring device manufactured by this method
CN101407420B (en) * 2008-11-04 2011-06-22 西安交通大学 Method for preparing non-grain boundary phase porous silicon nitride ceramic based on carbothermal reduction
CN101935226B (en) * 2010-08-31 2012-09-26 中国航空工业集团公司北京航空材料研究院 Process for soldering SiO2f/SiO2 composite ceramic and metal material
CN102167609B (en) * 2010-12-23 2012-10-10 中国人民解放军国防科学技术大学 Quartz/quartz-boron nitride high-temperature wave-permeable material
CN102350553B (en) * 2011-06-29 2013-06-05 哈尔滨工业大学 Welding method of high-volume-content ceramic reinforced Al-base composite material
CN102924110B (en) * 2012-10-24 2014-01-08 中国航空工业集团公司北京航空材料研究院 Method for brazing SiO2f/SiO2 composite ceramic and metal material
CN104475898B (en) * 2014-12-26 2016-04-27 哈尔滨工业大学 The foreign material method for welding of porous interlayer structure brazed seam

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