CN108620767A - A kind of composite soldering and preparation method thereof for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys - Google Patents
A kind of composite soldering and preparation method thereof for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys Download PDFInfo
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- CN108620767A CN108620767A CN201810434005.3A CN201810434005A CN108620767A CN 108620767 A CN108620767 A CN 108620767A CN 201810434005 A CN201810434005 A CN 201810434005A CN 108620767 A CN108620767 A CN 108620767A
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Manufacture Of Alloys Or Alloy Compounds (AREA)
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Abstract
It is a kind of for being brazed the composite soldering and preparation method thereof of quartzy short fiber reinforced silicon dioxide composite material and Invar alloys, be related to a kind of composite soldering and preparation method thereof.It is to solve existing welding SiO2f/SiO2Composite material and Invar alloys, connector lead to the problem of a large amount of frangible compounds at 400 DEG C or more using active solder soldered fitting microstructure, which is by Cu powder, few layer graphene and TiH2Composition.Method：One, Cu powder, TiH2Powder is weighed；Two, CuTi solders growth in situ graphene；Three, VFG/Cu powder and TiH2Mechanical mixture.15MPa, increase rate 200% are increased to by original 5MPa using the shearing strength of solder brazing rear joint of the present invention.The present invention is used for solder field.
Description
Technical field
The present invention relates to a kind of composite solderings and preparation method thereof.
Background technology
Aerospace field develops rapidly in recent years, and people are higher and higher to the degree of concern of its advanced material, to advanced
More stringent requirements are proposed for ceramic matric composite.Quartz has the characteristics that high transparency, high rigidity, highly corrosion resistant, makes it
It is widely used in fields such as electronics, communication, optical instruments.But fracture toughness and bending strength cannot meet space flight
The requirement of aviation harsh conditions.SiO2f/SiO2(SiO2The SiO of Short Fiber Reinforcement toughening2Ceramic matric composite) it is gradual by people
It explores and, it is by Ludox melting infiltration sintering method, and using SiO 2-ceramic as matrix, control of two-dimensional braided quartz fibre is to increase
It is strong mutually to obtain.It is insensitive to crackle, thermal shock resistance properties is excellent, at the same to centimetre, the wideband wave transparent performance of millimeter wave it is fabulous,
Therefore one of the ideal material being increasingly becoming in antenna house manufacturing process.
In antenna house assembling process, need SiO2f/SiO2The shell of composite material realizes connection with metallic matrix, because
This reliable connection is can to make its widely applied premise.There is the Invar alloys of very low coefficient of thermal expansion in room temperature, at
For the first choice of becket in antenna house.SiO is realized usually using the methods of mechanical connection, activity bonding and welding2f/SiO2It is multiple
Condensation material is reliably connected with Invar alloys.Mechanical connection has simple principle, needs to increase answering for composite material parts structure
Miscellaneous degree so that mechanical connection is unable to get extensive use.Though bonded joint can be to avoid the complexity of structure design, connector
It cannot be satisfied the in-flight heatproof requirement of antenna house.Active vacuum brazing is the high activity member in liquid solder when passing through high temperature
Element reacts with base material and forms effective metallurgical binding, to obtain reliable fine and close connector.
Realize SiO2f/SiO2The difficulty that composite material is connected with Invar be their chemical key class, constitution element and
There are larger differences for coefficient of thermal expansion etc..SiO2f/SiO2Composite material is in preparation process, due to the standing with unit with silicon oxygen bond
The formation of body reticular structure and the formation for repeatedly impregnating the high surface of compound rear surface energy, this causes ceramic material surfaces difficulty to be moistened
It is wet, it is therefore desirable to realize that active element reacts with ceramic interface and obtains stable interface layer.SiO2f/SiO2Composite material with
Connector will generate larger residual stress to Invar alloys in cooling procedure, and reason is the two coefficient of thermal expansion and springform
Amount differs greatly.It is relatively low in the coefficient of thermal expansion of room temperature condition, Invar alloys；Increased with temperature, coefficient of thermal expansion drastically on
It rises.However, being brazed SiO using active element2f/SiO2When composite material is with Invar alloys, the soldered fitting microstructure of acquisition
In there are a large amount of frangible compounds, with SiO2f/SiO2Composite material, Invar alloy elastics modulus and coefficient of thermal expansion are equal
There is larger gap, and induces residual thermal stress in cooling procedure, severe exacerbation soldering joint strength.
Invention content
The present invention is to solve existing welding SiO2f/SiO2Composite material and Invar alloys, connector are adopted at 400 DEG C or more
A large amount of frangible compounds are led to the problem of with active solder soldered fitting microstructure, are provided a kind of for being brazed quartzy staple fiber
Enhance silicon dioxide composite material (SiO2f/SiO2Composite material) with the composite solderings and preparation method thereof of Invar alloys.
The composite soldering that the present invention is used to be brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys be by
Cu powder, few layer graphene and TiH2Composition.
The purity of the Cu is that the grain size of 99.0%~99.9%, Cu powder is 300 mesh, TiH2Purity be 99% or more,
TiH2Particle size be 48~52 μm, the number of plies of few layer graphene (VFG) is 8~12 layers, graphene a diameter of 10~
90nm。
The above-mentioned preparation for being brazed quartzy short fiber reinforced silicon dioxide composite material and the composite soldering of Invar alloys
Method includes the following steps：
One, Cu powder, TiH2Powder is weighed：50%~80% Cu powder and 20%~50% is weighed by atomic percent
TiH2Powder is cleaned using acetone ultrasound；
Two, CuTi solders growth in situ graphene：Cu powder after step 1 is cleaned equably is laid on silicon chip surface, will
The silicon chip for being loaded with Cu powder is put on the warm table of PECVD device；1Pa is evacuated to hereinafter, being passed through H2；With 10~30 DEG C/min's
Speed is warming up to 550~650 DEG C of growth temperature, stops being passed through H later2, it is changed to be passed through CH4With Ar gases, Ar and CH is adjusted4's
Flow-rate ratio is continuously heating to 750~850 DEG C, opens radio frequency, and plasma sputtering stops after 40~90 minutes, closes penetrate successively
Frequently, heating and gas are passed through always Ar gases in cooling procedure, and the flow of Ar is 20~50sccm, and pressure is maintained
400~600Pa is cooled to room temperature, obtains the Cu powder (VFG/Cu powder) of few layer graphene doping；
Three, VFG/Cu powder and TiH2Mechanical mixture：The Cu powder and TiH for few layer graphene doping that step 2 is obtained2Powder
1.5~5h of ball milling after the mixing of end, obtains composite soldering.
Further, the flow-rate ratio of Ar and CH4 is (70~95) in step 2:(5~30).
The present invention is reacted using the Ti elements in the graphene and solder of Cu powder surface vertical-growth, graphene edge
C atom active highers preferentially combined with Ti, so as to improve joint interface tissue, inhibit excessive brittle intermetallic in connector
The formation of object, effectively improves SiO2f/SiO2The microstructure of composite material and Invar alloy-junctions, greatly improves SiO2f/
SiO2The mechanical property of composite material and Invar alloy-junctions.
In addition, the present invention adds TiH2, the supply of Ti contents is realized, while the atomic ratio of fixed Ti and Cu is 23:
77, it is prepared for adulterating the composite soldering of few layer graphene.
Beneficial effects of the present invention：
The solder of the present invention is for soldering connection SiO2f/SiO2Composite material and fusing point for Invar alloys are suitable, wetting
Property is good, and can meet 400 DEG C of requirements of soldered fitting.Comparison finds have using brazing seam structure after the connection of single CuTi solders
There are more Cu-Ti compounds, and uses Cu-Ti, Ti-Fe, Ti-Ni metal in the brazed seam after the connection of VFG/CuTi composite solderings
Between compound be suppressed, there is the Cu based solid solutions area of large area, show preferable plastic deformation ability.By inspection
It surveys, 15MPa, increase rate 200% is increased to by original 5MPa using the shearing strength of solder brazing rear joint of the present invention.
The solder of the present invention is brazed SiO at 930 DEG C under the conditions of heat preservation 10min2f/SiO2Composite material and Invar alloys,
The connector room temperature shearing strength of acquisition up to 13~17MPa, compared to AgCuTi solder connectors intensity 500 DEG C of retention rates by
50% is increased to 70%, has superior high-temperature behavior.
Description of the drawings
Fig. 1 is SiO prepared by embodiment 12f/SiO2The electromicroscopic photograph of composite material；
Fig. 2 is the electromicroscopic photograph of single CuTi solders.
Specific implementation mode
Technical solution of the present invention is not limited to act specific implementation mode set forth below, further includes between each specific implementation mode
Arbitrary combination.
Specific implementation mode one：Present embodiment for be brazed quartzy short fiber reinforced silicon dioxide composite material with
The composite soldering of Invar alloys is by Cu powder, few layer graphene and TiH2Composition.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：The purity of the Cu powder is
The grain size of 99.0%~99.9%, Cu powder is 300 mesh.It is other same as the specific embodiment one.
Specific implementation mode three：The present embodiment is different from the first embodiment in that：The TiH2Purity be
99% or more, TiH2Particle size be 48~52 μm.It is other same as the specific embodiment one.
Specific implementation mode four：The present embodiment is different from the first embodiment in that：Few layer graphene (VFG)
The number of plies be 8~12 layers, a diameter of 10~90nm of graphene.It is other same as the specific embodiment one.
Specific implementation mode five：Present embodiment for be brazed quartzy short fiber reinforced silicon dioxide composite material with
The preparation method of the composite soldering of Invar alloys, includes the following steps：
One, Cu powder, TiH2Powder is weighed：50%~80% Cu powder and 20%~50% is weighed by atomic percent
TiH2Powder is cleaned using acetone ultrasound；
Two, CuTi solders growth in situ graphene：Cu powder after step 1 is cleaned equably is laid on silicon chip surface, will
The silicon chip for being loaded with Cu powder is put on the warm table of PECVD device；1Pa is evacuated to hereinafter, being passed through H2；With 10~30 DEG C/min's
Speed is warming up to 550~650 DEG C of growth temperature, stops being passed through H later2, it is changed to be passed through CH4With Ar gases, Ar and CH is adjusted4's
Flow-rate ratio is continuously heating to 750~850 DEG C, opens radio frequency, and plasma sputtering stops after 40~90 minutes, closes penetrate successively
Frequently, heating and gas are passed through always Ar gases in cooling procedure, and the flow of Ar is 20~50sccm, and pressure is maintained
400~600Pa is cooled to room temperature, obtains the Cu powder of few layer graphene doping；
Three, VFG/Cu powder and TiH2Mechanical mixture：The Cu powder and TiH for few layer graphene doping that step 2 is obtained2Powder
1.5~5h of ball milling after the mixing of end, obtains composite soldering.
Present embodiment lacks layer by plasma auxiliary chemical vapor deposition (PECVD) method in Cu powder surface vertical-growth
Graphene (VFG), and using addition TiH during preparing composite soldering2Method realize Ti contents supply, be prepared for mixing
The composite soldering of miscellaneous few layer graphene.
The composite soldering of present embodiment is brazed SiO at 910 DEG C under the conditions of heat preservation 10min2f/SiO2Composite material with
Invar alloys, the connector room temperature shearing strength of acquisition is up to 6~10MPa.
The composite soldering of present embodiment is brazed SiO at 950 DEG C under the conditions of heat preservation 10min2f/SiO2Composite material with
Invar alloys, the connector room temperature shearing strength of acquisition is up to 11~14MPa.
The composite soldering of present embodiment is brazed SiO at 930 DEG C under the conditions of heat preservation 10min2f/SiO2Composite material with
Invar alloys, the connector room temperature shearing strength of acquisition is up to 13~17MPa.
Specific implementation mode six：Present embodiment is unlike specific implementation mode five：Atomic percent is pressed in step 1
Than weighing 77% Cu powder and 23% TiH2Powder.It is other identical as specific implementation mode five.
Specific implementation mode seven：Present embodiment is unlike specific implementation mode five：Radio-frequency power is in step 2
140~160W.It is other identical as specific implementation mode five.
Specific implementation mode eight：Present embodiment is unlike specific implementation mode five：Ar and CH in step 24Stream
Amount is than being (70~95):(5~30).It is other identical as specific implementation mode five.
Specific implementation mode nine：Present embodiment is unlike specific implementation mode five：Ar and CH in step 24Stream
Amount is than being 80:20.It is other identical as specific implementation mode five.
Specific implementation mode ten：Present embodiment is unlike specific implementation mode five：What is prepared in step 3 is compound
Solder is powdered.It is other identical as specific implementation mode five.
Elaborate below to the embodiment of the present invention, following embodiment under based on the technical solution of the present invention into
Row is implemented, and gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.
Embodiment 1：
The present embodiment is for being brazed SiO2f/SiO2The preparation method of composite material and the composite soldering of Invar alloys, including
Following steps：
One, select the purity of Cu powder for 99.9%, TiH2The purity of powder is 99%.The grain size of Cu powder is 300 mesh, TiH2's
Size is about 50 μm.77% Cu powder and 23% TiH are weighed by atomic percent2Powder；
Two, the powder weighed and silicon chip are put into acetone, carry out ultrasonic wave (supersonic frequency is 20KHz) and cleans 10min.
After powder and silicon chip natural air drying, Cu powder is equably laid on silicon chip surface；
Three, silicon chip that step 2 is loaded with to Cu powder is put on the warm table of PECVD device and is evacuated to 1Pa hereinafter, being passed through
H2, flow 30sccm, maintenance pressure is in 450Pa；It is warming up to 600 DEG C of growth temperature with the speed of 15 DEG C/min, is stopped later
It is passed through H2, it is changed to be passed through CH4With Ar gases, Ar and CH is adjusted4Flow-rate ratio, adjust CH4Flow is 10sccm, and Ar flows are
90sccm, and pressure is maintained into 900Pa；700 DEG C are continuously heating to, radio frequency, radio-frequency power 200W are opened, plasma splashes
It penetrates and stops after sixty minutes, close radio frequency, heating, gas etc. successively, be passed through Ar gases always in cooling procedure, the flow of Ar is
30sccm, and pressure is maintained into 500Pa, it is cooled to the Cu powder (VFG/Cu powder) that room temperature obtains few layer graphene doping；
Four, step 3 is obtained into VFG/Cu powder and TiH2Ball milling 2h after powder mixing, obtains composite soldering；
Five, the greasy dirt of Invar alloy welding surfaces, oxide are cleaned out with mechanical chipping method, then by Invar
Alloy is put into acetone, is carried out ultrasonic wave (supersonic frequency is 20KHz) and is cleaned 10min；
Six, by composite soldering pressed powder that step 4 obtains and be processed by the equal sheet of weldering surface area；
Seven, by after the material natural air drying after cleaning, according to being SiO from top to bottom2f/SiO2Composite material, composite soldering
The form of tabletting and Invar alloys is assembled, and the pressure that surface applies 2MPa is fixed.
Eight, the workpiece assembled is put into vacuum furnace, when vacuum degree is 1 × 10-3When Pa, start with 10 DEG C/min
Speed be heated to 930 DEG C, keep the temperature 10min, then cool to 400 DEG C with the speed of 10 DEG C/min, cool to room with the furnace thereafter
Temperature completes SiO2f/SiO2The soldering of composite material and Invar alloys.
SiO manufactured in the present embodiment2f/SiO2The electromicroscopic photograph of composite material is as shown in Figure 1.Using single CuTi solders as
Control, electromicroscopic photograph are as shown in Figure 2.Brazing seam structure has more Cu-Ti compounds after single CuTi solders connection, and uses
Cu-Ti, Ti-Fe, Ti-Ni intermetallic compound are suppressed in brazed seam after the connection of VFG/CuTi composite solderings, are occurred big
The Cu based solid solutions area of area, shows preferable plastic deformation ability.
After tested, the present embodiment SiO2f/SiO2The connector room temperature shearing strength of composite material and Invar alloys reaches
15MPa。
Embodiment 2：
The present embodiment and the difference of embodiment 1 are：In step 8, the workpiece assembled is put into vacuum furnace
In, when vacuum degree is 1 × 10-3When Pa, start to be heated to 950 DEG C with the speed of 10 DEG C/min, keep the temperature 10min, then with 10 DEG C/
The speed of min cools to 400 DEG C, cools to room temperature with the furnace thereafter, that is, completes SiO2f/SiO2Composite material and Invar alloys
Soldering.Other parameters and step are same as Example 1.
After tested, the present embodiment SiO2f/SiO2The connector room temperature shearing strength of composite material and Invar alloys reaches
13MPa。
Claims (10)
1. a kind of composite soldering for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys, feature
It is that the composite soldering is by Cu powder, few layer graphene and TiH2Composition.
2. according to claim 1 a kind of for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar conjunctions
The composite soldering of gold, it is characterised in that：The purity of the Cu powder is that the grain size of 99.0%~99.9%, Cu powder is 300 mesh.
3. according to claim 1 or 2 a kind of for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar
The composite soldering of alloy, it is characterised in that：The TiH2Purity be 99% or more, TiH2Particle size be 48~52 μm.
4. according to claim 3 a kind of for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar conjunctions
The composite soldering of gold, it is characterised in that：The number of plies of few layer graphene is 8~12 layers, a diameter of 10~90nm of graphene.
5. described in claim 1 for being brazed the compound of quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
The preparation method of solder, it is characterised in that this approach includes the following steps：
One, Cu powder, TiH2Powder is weighed：50%~80% Cu powder and 20%~50% TiH are weighed by atomic percent2
Powder is cleaned using acetone ultrasound；
Two, CuTi solders growth in situ graphene：Cu powder after step 1 is cleaned equably is laid on silicon chip surface, will be loaded with
The silicon chip of Cu powder is put on the warm table of PECVD device；1Pa is evacuated to hereinafter, being passed through H2；With the speed of 10~30 DEG C/min
It is warming up to 550~650 DEG C of growth temperature, stops being passed through H later2, it is changed to be passed through CH4With Ar gases, Ar and CH is adjusted4Flow
Than being continuously heating to 750~850 DEG C, opening radio frequency, plasma sputtering stops after 40~90 minutes, closes radio frequency successively, adds
Heat and gas, are passed through always Ar gases in cooling procedure, and the flow of Ar is 20~50sccm, and pressure is maintained 400~
600Pa is cooled to room temperature, obtains the Cu powder of few layer graphene doping；
Three, VFG/Cu powder and TiH2Mechanical mixture：The Cu powder and TiH for few layer graphene doping that step 2 is obtained2Powder is mixed
1.5~5h of ball milling after conjunction obtains composite soldering.
6. according to claim 5 for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
The preparation method of composite soldering, it is characterised in that weigh 77% Cu powder and 23% TiH by atomic percent in step 12Powder
End.
7. according to claim 5 or 6 for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
Composite soldering preparation method, it is characterised in that in step 2 radio-frequency power be 140~160W.
8. according to claim 7 for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
The preparation method of composite soldering, it is characterised in that Ar and CH in step 24Flow-rate ratio be (70~95):(5~30).
9. according to claim 8 for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
The preparation method of composite soldering, it is characterised in that Ar and CH in step 24Flow-rate ratio be 80:20.
10. according to claim 9 for being brazed quartzy short fiber reinforced silicon dioxide composite material and Invar alloys
The preparation method of composite soldering, it is characterised in that the composite soldering prepared in step 3 is powdered.
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| CN112427759A (en) * | 2020-10-27 | 2021-03-02 | 哈尔滨工业大学 | ZrC-SiC ceramic and TC4 titanium alloy brazing method |
| CN113307647A (en) * | 2021-04-16 | 2021-08-27 | 长春工业大学 | Indirect brazing method of aluminum nitride ceramic copper-clad plate |
| CN114178738A (en) * | 2021-12-08 | 2022-03-15 | 浙江亚通焊材有限公司 | Active solder for brazing ceramic and stainless steel and solder paste |
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| CN114178738A (en) * | 2021-12-08 | 2022-03-15 | 浙江亚通焊材有限公司 | Active solder for brazing ceramic and stainless steel and solder paste |
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