CN107457499A - A kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite - Google Patents

A kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite Download PDF

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Publication number
CN107457499A
CN107457499A CN201710674127.5A CN201710674127A CN107457499A CN 107457499 A CN107457499 A CN 107457499A CN 201710674127 A CN201710674127 A CN 201710674127A CN 107457499 A CN107457499 A CN 107457499A
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composite
solder
silicon carbide
welded
soldering
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CN107457499B (en
Inventor
钟志宏
温群
李华鑫
王志泉
宋奎晶
朱志雄
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Hefei University of Technology
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Hefei University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/008Soldering within a furnace
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/20Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40Making wire or rods for soldering or welding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/16Composite materials, e.g. fibre reinforced
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00Materials to be soldered, welded or cut
    • B23K2103/50Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
    • B23K2103/52Ceramics

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite, wherein the raw material and proportioning for silicon carbide ceramics and its high temperature brazing solder of composite are:The 30wt% of high purity titanium 20, the 80wt% of HIGH-PURITY SILICON 70, boron carbide or carborundum addition quality are high purity titanium and 0 10wt% of HIGH-PURITY SILICON gross mass.The present invention utilizes vacuum brazing technique (brazing temperature:1350~1430 DEG C;Soaking time:5~45min;Weld thickness:10~200 μm) prepare carborundum soldered fitting.It it is 1380 DEG C, soaking time 20min in welding temperature, weld thickness is 30 μm, B4When C additions are 5wt%, optimal soldered fitting is obtained, the maximum room temperature shear strength of joint reaches 114MPa, has stronger practical value.

Description

A kind of high-temp solder preparation method and pricker for silicon carbide ceramics and its composite Welding
Technical field
The present invention relates to a kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite, Belong to the connection area of silicon carbide ceramics and its composite.
Background technology
Carborundum and its composite are most widely used a kind of ceramic structure materials in current industry, in aviation, boat My god, automobile, have application in machine-building and nuclear industry.With in recent years science and technology and industrial economy rapid development, It is increasing to the demand of silicon carbide ceramics and its composite material structural member, study the connection of carborundum and also go deep into therewith.Carbon The extensive use of SiClx promotes the development of carborundum welding technique, while carbonization has been expanded in the development of carborundum welding technique again The application field of silicon, therefore the welding technique of carborundum just turns into one of focus studied at present.
Small (ρ=the 3.22g/cm of density of pure carborundum3), fusing point is high, high-temperature physics stable chemical performance, intensity hardness It is high.By long-term production practices and scientific experiment, carborundum and its composite are preferable candidate materials, are widely used in machine Tool manufacture, Aero-Space and nuclear industry etc., such as ballistic resistant sheet, aeroengine combustor buring room and nuclear fusion stack cladding structure material Deng on critical component.However, the machining property of silicon carbide ceramics and its composite is poor, it is difficult to which straight forming prepares chi Very little big or complex-shaped composite material component by material connection, it is necessary to be realized, so the interconnection technique of carbofrax material It is most important.But the interconnection technique of carborundum still imperfection, the practical application of carborundum is limited, especially towards extreme The silicon carbide ceramics of Service Environment and its interconnection technique of composite material structural member.Therefore, the higher pricker of temperature in use need to be developed Material and its soldering processes, to meet the system of the carborundum and its composite material structural member used under the operating modes such as high temperature resistant, Flouride-resistani acid phesphatase Standby demand.
The content of the invention
In order to avoid above-mentioned the shortcomings of the prior art, it is used to be carbonized it is an object of the invention to provide one kind The high-temp solder preparation method and soldering processes of silicon ceramic composite materials.
The present invention is used for the high-temp solder preparation method of silicon carbide ceramics and its composite, and its raw material and proportioning are:
High purity titanium (Ti) 20-30wt%,
HIGH-PURITY SILICON (Si) 70-80wt%,
(the gross mass sum of high purity titanium and HIGH-PURITY SILICON is 100%.)
Boron carbide or carborundum addition quality are high purity titanium and the 0-10wt% of HIGH-PURITY SILICON gross mass.
The present invention is used for the high-temp solder preparation method of silicon carbide ceramics and its composite, comprises the following steps:
Step 1:By the high purity titanium of proportional quantity and HIGH-PURITY SILICON mixed smelting, furnace cooling, brazing filler metal alloy block is solidified as;
Step 2:Step 1 gained brazing filler metal alloy block is processed into powder (average grain diameter 1mm), then passes through ball mill or powder Solder powder of the broken crusher machine into 5-20 μm of average grain diameter;
Step 3:The solder powder that step 2 is obtained mixes with boron carbide powder or silicon carbide powder, obtains composite soldering.
In step 1, the melting is non-consumable electric arc melting or vacuum induction melting.The non-consumable electric arc melting be Melting 4-6 times in argon gas atmosphere;The vacuum induction melting is in vacuum≤10-21500-1700 DEG C of Pa, smelting temperature condition Lower insulation 20-120min.
In step 3, the mode for being combined by ball milling or mixed by way of mechanical agitation adds ultrasonic disperse.
In step 3, the particle diameter of boron carbide powder or silicon carbide powder is 0.5-10 μm.
The present invention is used for the soldering processes of the high-temp solder of silicon carbide ceramics and its composite, comprises the following steps:
Step 1:Pretreatment
Silicon carbide ceramics and its composite are cut into the material to be welded of definite shape with slicer, use diamond suspension The surface to be connected for treating wlding material is polished, and is subsequently placed in absolute ethyl alcohol and is cleaned by ultrasonic, and is then cleaned and is blown with cotton It is dry, obtain the material to be welded of pretreatment;Weigh required composite soldering, the amount of weighing to ensure weld thickness as 10~200 μm, to Absolute ethyl alcohol is added in composite soldering and forms the solder suspension that solder mass concentration is 80%;
Step 2:By material and the solder suspension to be welded of pretreatment, according to material to be welded ,/solder suspension/treats wlding The order of material is assembled, and is subsequently placed into vacuum drying oven and is welded.
Step 3:Soldering
In vacuum 10-2Below Pa, it is warming up to 1350~1430 DEG C of brazing temperature and is incubated 5~45min, then cooling.
In step 3, heating rate is 5-30 DEG C/min.
In step 3, the mode of the cooling is furnace cooling, or is down to 500 DEG C with 5-15 DEG C/min rate of temperature fall, Furnace cooling afterwards.500 DEG C wherein are down to 5 DEG C/min rate of temperature fall, the effect of rear furnace cooling is optimal, is primarily due to cold But speed is reduced, and joint thermal stress is released, strength of joint lifting.
The present invention utilizes vacuum brazing technique (brazing temperature:1350~1430 DEG C;Soaking time:5~45min;Brazed seam is thick Degree:10~200 μm) prepare carborundum soldered fitting.It it is 1380 DEG C, soaking time 20min in welding temperature, weld thickness is 30 μm, B4When C additions are 5wt%, optimal soldered fitting is obtained, the maximum room temperature shear strength of joint reaches 114MPa, there is stronger practical value.
Compared with prior art, beneficial effects of the present invention are embodied in:
Present invention employs different melting technique (electric arc melting, vacuum induction melting) to have prepared a kind of new titanium Silicon alloy high-temp solder, to solve the problems, such as that silicon carbide ceramics and its composite braze-welded structure part temperature in use are low.
The present invention is connected using SiC particulate disperse enhancing titanium silicon high-temp solder to silicon carbide ceramics and its composite, with And reaction in-situ forms TiB2Silicon carbide ceramics and its composite are connected with SiC enhancing titanium silicon high temperature composite solderings, this hair It is bright compared with the past, high intensity can be obtained and resistant to elevated temperatures carborundum and its composite braze-welded structure part, solve carbonization One technical barrier of the engineer applied of silicon and its composite.
Brief description of the drawings
Fig. 1 is the assembling schematic diagram of material and solder to be welded in soldering processes.
Fig. 2 is the global tissue pattern (Ti-Si+5wt.% of the silicon carbide/carbon SiClx joint of boron carbide particles enhancing B4C).Wherein a is joint entirety pattern, and b is respectively contact cross-section amplification pattern.From figure 2 it can be seen that brazed seam situ is given birth to Into SiC and TiB2And Dispersed precipitate, play a part of activeness and quietness joint.
Fig. 3 is the global tissue pattern (Ti-Si+1wt.%SiC) of the silicon carbide/carbon SiClx joint of SiC particulate enhancing.From As can be seen that SiC addition alleviates the problem of mother metal is with intermediate layer thermal expansion coefficient difference in Fig. 3, formd in weld seam Substantial amounts of titanium silicon eutectic structure, does not find micro-crack in brazed seam.
Fig. 4 is soldered fitting shear strength test schematic diagram.
Embodiment
Below in conjunction with specific embodiment to technical scheme explanation for further analysis.
Embodiment 1:The preparation of high temperature composite soldering
It is used for silicon carbide ceramics in the present embodiment and its high-temp solder preparation method of composite is as follows:
1st, the high purity titanium of proportional quantity and HIGH-PURITY SILICON are mixed and utilizes furnace cooling after non-consumable electric arc melting, be solidified as pricker Expect alloy block, block is overturn and continues melting, five times repeatedly;High purity titanium and HIGH-PURITY SILICON are configured to by mass percentage:High purity titanium 24wt.%, HIGH-PURITY SILICON 76wt.%.
2nd, step 1 gained brazing filler metal alloy block is mechanically smashed, the alloy smashed is worn into average grain by rear Yong Yan Portland Footpath is less than 1mm powder, then ball mill ball mill grinding into average grain diameter be 10 μm of solder powder.
3rd, the solder powder and B obtained step 24C powder (0.5 μm of particle diameter) and absolute ethyl alcohol are added super by mechanical agitation The scattered mode of sound mixes, and obtains composite soldering.B4The quality of C powder is the 3wt.% of solder powder quality.
Embodiment 2:The preparation of high temperature composite soldering
It is used for silicon carbide ceramics in the present embodiment and its high-temp solder preparation method of composite is as follows:
1st, the high purity titanium of proportional quantity and HIGH-PURITY SILICON are mixed and carries out vacuum induction melting (vacuum is 10-2Below Pa, melt Refine 1700 DEG C of temperature, soaking time 20min), furnace cooling, it is solidified as brazing filler metal alloy block;High purity titanium and HIGH-PURITY SILICON press quality hundred Ratio is divided to be configured to:High purity titanium 22wt.%, HIGH-PURITY SILICON 78wt.%.
2nd, step 1 gained brazing filler metal alloy block is mechanically smashed, the alloy smashed is worn into average grain by rear Yong Yan Portland Footpath is less than 1mm powder, then ball mill ball mill grinding into average grain diameter be 20 μm of solder powder.
3rd, the solder powder and B obtained step 24C powder (5 μm of particle diameter) is mixed by way of ball milling, is obtained compound Solder.B4The quality of C powder is the 5wt.% of solder powder quality.
Embodiment 3:The preparation of high temperature composite soldering
It is used for silicon carbide ceramics in the present embodiment and its high-temp solder preparation method of composite is as follows:
1st, the high purity titanium of proportional quantity and HIGH-PURITY SILICON are mixed and utilizes non-consumable electric arc melting, furnace cooling, be solidified as pricker Expect alloy block, block is overturn and continues melting, five times repeatedly;High purity titanium and HIGH-PURITY SILICON are configured to by mass percentage:High purity titanium 20wt.%, HIGH-PURITY SILICON 80wt.%.
2nd, step 1 gained brazing filler metal alloy block is mechanically smashed, the alloy smashed is worn into average grain by rear Yong Yan Portland Footpath is less than 1mm powder, then ball mill ball mill grinding into average grain diameter be 10 μm of solder powder.
3rd, the solder powder and SiC powder (1 μm of particle diameter) and absolute ethyl alcohol obtained step 2 adds ultrasound by mechanical agitation Scattered mode mixes, and obtains composite soldering.The quality of SiC powder is the 1wt.% of solder powder quality.
Embodiment 4:The preparation of high temperature composite soldering
It is used for silicon carbide ceramics in the present embodiment and its high-temp solder preparation method of composite is as follows:
1st, the high purity titanium of proportional quantity and HIGH-PURITY SILICON are mixed and carries out vacuum induction melting (vacuum is 10-2Below Pa, melt Refine 1500 DEG C of temperature, soaking time 60min), furnace cooling, it is solidified as brazing filler metal alloy block;High purity titanium and HIGH-PURITY SILICON press quality hundred Ratio is divided to be configured to:High purity titanium 30wt.%, HIGH-PURITY SILICON 70wt.%.
2nd, step 1 gained brazing filler metal alloy block is mechanically smashed, the alloy smashed is worn into average grain by rear Yong Yan Portland Footpath is less than 1mm powder, then ball mill ball mill grinding into average grain diameter be 5 μm of solder powder.
3rd, the solder powder and SiC powder (2 μm of particle diameter) and absolute ethyl alcohol obtained step 2 adds ultrasound by mechanical agitation Scattered mode mixes, and obtains composite soldering.The quality of SiC powder is the 0.5wt.% of solder powder quality.
Embodiment 5:Soldering processes
The soldering processes for being used for the high-temp solder of silicon carbide ceramics and its composite in the present embodiment are as follows:
The 1st, silicon carbide ceramics and its composite are cut into 15mm × 10mm × 4mm material to be welded with inside diameter slicer, The face to be connected that wlding material is treated with 3 μm of diamond suspension liquid is polished 1h, then they are placed in absolute ethyl alcohol Row is cleaned by ultrasonic, and is then cleaned with cotton and hair-dryer dries up;Weigh the composite soldering 24Ti-76Si+5wt.%B of preparation4C 0.06g (corresponding 30 μm of weld thickness), adds absolute ethyl alcohol and prepares the suspension that solder mass fraction is 80%.
2nd, by material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, then each part for assembling completion is put into vacuum tungsten coil furnace.
3rd, vacuum tungsten coil furnace is warming up to 1380 DEG C, and heating rate is 10 DEG C/min, and 20min, Zhi Housui are incubated at 1380 DEG C Stove cools down.
The soldering joint strength that the present embodiment obtains can reach 114MPa.
Embodiment 6:Soldering processes
The soldering processes for being used for the high-temp solder of silicon carbide ceramics and its composite in the present embodiment are as follows:
The 1st, silicon carbide ceramics and its composite are cut into 15mm × 10mm × 4mm material to be welded with inside diameter slicer, The face to be connected that wlding material is treated with 3 μm and 1 μm of diamond suspension liquid is polished, then they are placed in absolute ethyl alcohol It is cleaned by ultrasonic, is then cleaned with cotton and hair-dryer dries up;Weigh the composite soldering 24Ti-76Si+1wt.%SiC of preparation 0.3g (corresponding 150 μm of weld thickness), adds absolute ethyl alcohol and prepares the suspension that solder mass fraction is 80%.
2nd, by material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, then each part for assembling completion is put into vacuum tungsten coil furnace.
3rd, vacuum tungsten coil furnace is warming up to 1400 DEG C, and heating rate is 10 DEG C/min, 1400 DEG C be incubated 10min, after with 10 DEG C/min rate of temperature fall is down to 500 DEG C, furnace cooling afterwards.
The soldering joint strength that the present embodiment obtains can reach 84MPa.
Embodiment 7:Soldering processes
The soldering processes for being used for the high-temp solder of silicon carbide ceramics and its composite in the present embodiment are as follows:
The 1st, silicon carbide ceramics and its composite are cut into 15mm × 10mm × 4mm material to be welded with inside diameter slicer, The face to be connected that wlding material is treated with 3 μm of diamond suspension liquid is polished 1h, then they are placed in absolute ethyl alcohol Row is cleaned by ultrasonic, and is then cleaned with cotton and hair-dryer dries up;Weigh the composite soldering 22Ti-78Si+1wt.%B of preparation4C 0.12g (corresponding 60 μm of weld thickness), adds absolute ethyl alcohol and prepares the suspension that solder mass fraction is 80%.
2nd, by material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, then each part for assembling completion is put into vacuum tungsten coil furnace.
3rd, vacuum tungsten coil furnace is warming up to 1360 DEG C, and heating rate is 10 DEG C/min, brazing temperature be incubated 30min, after with 5 DEG C/min rate of temperature fall is down to 500 DEG C, furnace cooling afterwards.
The soldering joint strength that the present embodiment obtains can reach 94MPa.
Embodiment 8:Soldering processes
The soldering processes for being used for the high-temp solder of silicon carbide ceramics and its composite in the present embodiment are as follows:
The 1st, silicon carbide ceramics and its composite are cut into 15mm × 10mm × 4mm material to be welded with inside diameter slicer, The face to be connected that wlding material is treated with 3 μm of diamond suspension liquid is polished 1h, then they are placed in absolute ethyl alcohol Row is cleaned by ultrasonic, and is then cleaned with cotton and hair-dryer dries up;Weigh the composite soldering 24Ti-76Si+0.5wt.%SiC of preparation 0.02g (corresponding 10 μm of weld thickness), adds absolute ethyl alcohol and prepares the suspension that solder mass fraction is 80%.
2nd, by material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, then each part for assembling completion is put into vacuum tungsten coil furnace.
3rd, vacuum tungsten coil furnace is warming up to 1400 DEG C, and heating rate is 10 DEG C/min, 1400 DEG C be incubated 15min, after with 10 DEG C/min rate of temperature fall is down to 500 DEG C, furnace cooling afterwards.
The soldering joint strength that the present embodiment obtains can reach 78MPa.
Embodiment 9:Soldering processes
The soldering processes for being used for the high-temp solder of silicon carbide ceramics and its composite in the present embodiment are as follows:
The 1st, silicon carbide ceramics and its composite are cut into 15mm × 10mm × 4mm material to be welded with inside diameter slicer, The face to be connected that wlding material is treated with 3 μm of diamond suspension liquid is polished 1h, then they are placed in absolute ethyl alcohol Row is cleaned by ultrasonic, and is then cleaned with cotton and hair-dryer dries up;Weigh the composite soldering 24Ti-76Si+0.5wt.%SiC of preparation 0.02g (corresponding 10 μm of weld thickness), adds absolute ethyl alcohol and prepares the suspension that solder mass fraction is 80%.
2nd, by material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, then each part for assembling completion is put into vacuum tungsten coil furnace.
3rd, vacuum tungsten coil furnace is warming up to 1420 DEG C, and heating rate is 10 DEG C/min, 1420 DEG C be incubated 15min, after with 10 DEG C/min rate of temperature fall is down to 500 DEG C, furnace cooling afterwards.
The soldering joint strength that the present embodiment obtains can reach 71MPa.
Embodiment result is summarized:
Titanium silicon and its composite high-temp solder soldering carborundum and its composite can obtain obtained by the present invention To the joint of excellent in mechanical performance.Composite soldering is prepared using SiC particulate dispersion-strengtherning, to silicon carbide ceramics and its composite It is attached, SiC particulate Dispersed precipitate has reached the effect of enhancing joint in brazing seam structure.Utilize B4C reaction in-situs strengthen Composite soldering is prepared, silicon carbide ceramics and its composite are attached, B4C forms resistance to titanium silicon generation reaction in-situ The TiB of high-temperature oxidation resistant2Strengthen phase with SiC, be evenly distributed in brazing seam structure, reach the effect of activeness and quietness joint.

Claims (10)

1. a kind of high-temp solder preparation method for silicon carbide ceramics and its composite, it is characterised in that its raw material and proportioning For:
High purity titanium 20-30wt%,
HIGH-PURITY SILICON 70-80wt%,
Boron carbide or carborundum addition quality are high purity titanium and the 0-10wt% of HIGH-PURITY SILICON gross mass.
2. the preparation method described in a kind of claim 1, it is characterised in that comprise the following steps:
Step 1:By the high purity titanium of proportional quantity and HIGH-PURITY SILICON mixed smelting, furnace cooling, brazing filler metal alloy block is solidified as;
Step 2:Step 1 gained brazing filler metal alloy block is processed into powder, average grain is then broken into by ball mill or pulverizer The solder powder in 5-20 μm of footpath;
Step 3:The solder powder that step 2 is obtained mixes with boron carbide powder or silicon carbide powder, obtains composite soldering.
3. preparation method according to claim 2, it is characterised in that:
In step 1, the melting is non-consumable electric arc melting or vacuum induction melting.
4. preparation method according to claim 3, it is characterised in that:
The non-consumable electric arc melting is melting 4-6 time in argon gas atmosphere;The vacuum induction melting is in vacuum≤10- 220-120min is incubated under the conditions of Pa, 1500-1700 DEG C of smelting temperature.
5. preparation method according to claim 2, it is characterised in that:
In step 3, the mode for being combined by ball milling or mixed by way of mechanical agitation adds ultrasonic disperse.
6. preparation method according to claim 2, it is characterised in that:
In step 3, the particle diameter of boron carbide powder or silicon carbide powder is 0.5-10 μm.
7. a kind of soldering processes of the high-temp solder for being used for silicon carbide ceramics and its composite described in claim 1, it is special Sign is to comprise the following steps:
Step 1:Pretreatment
Silicon carbide ceramics and its composite are cut into the material to be welded of definite shape with slicer, treated with diamond suspension The surface to be connected of wlding material is polished, and is subsequently placed in absolute ethyl alcohol and is cleaned by ultrasonic, and is then cleaned and is dried up with cotton, obtained The material to be welded that must be pre-processed;Required composite soldering is weighed, the amount of weighing is to ensure weld thickness as 10~200 μm, to compound Absolute ethyl alcohol is added in solder and forms the solder suspension that solder mass concentration is 80%;
Step 2:By material and the solder suspension to be welded of pretreatment according to material to be welded/solder suspension/material to be welded Order is assembled, and is subsequently placed into vacuum drying oven and is welded;
Step 3:Soldering
In vacuum 10-2Below Pa, it is warming up to 1350~1430 DEG C of brazing temperature and is incubated 5~45min, then cooling.
8. soldering processes according to claim 7, it is characterised in that:
In step 3, heating rate is 5-30 DEG C/min.
9. soldering processes according to claim 7, it is characterised in that:
In step 3, the mode of the cooling is furnace cooling, or is down to 500 DEG C with 5-15 DEG C/min rate of temperature fall, after with Stove cools down.
10. soldering processes according to claim 9, it is characterised in that:
In step 3, the mode of the cooling is to be down to 500 DEG C with 5 DEG C/min rate of temperature fall, rear furnace cooling.
CN201710674127.5A 2017-08-09 2017-08-09 High-temperature solder preparation and brazing process for silicon carbide ceramic and composite material thereof Active CN107457499B (en)

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CN108274086A (en) * 2018-01-24 2018-07-13 哈尔滨工业大学 A kind of method of two-step method high temperature soldering carbon fiber reinforced carbon matrix composite material
CN109354504A (en) * 2018-11-27 2019-02-19 合肥工业大学 A kind of boron carbide base composite ceramic sintering aid and sintering process
CN110041090A (en) * 2019-05-23 2019-07-23 合肥工业大学 A kind of plasma discharging diffusion connection method of silicon carbide ceramics
CN110407600A (en) * 2019-07-29 2019-11-05 浙江工业大学 A method of SiC ceramic is connected using Au base high-temp solder
CN110734298A (en) * 2018-12-31 2020-01-31 深圳硅基仿生科技有限公司 Brazing structure of ceramic and metal
CN111958145A (en) * 2020-08-24 2020-11-20 合肥工业大学 Brazing material for MAX phase composite ceramic and brazing process
CN113385851A (en) * 2021-05-28 2021-09-14 中国科学院上海硅酸盐研究所苏州研究院 High-temperature-resistant corrosion-resistant solder for silicon carbide ceramic connection and preparation method and application thereof
CN114315402A (en) * 2022-01-11 2022-04-12 成都成维精密机械制造有限公司 Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic
CN115322005A (en) * 2022-07-15 2022-11-11 西北工业大学 Coating raw material for SiCf/SiC composite material connection and reaction diffusion connection method
CN115360463A (en) * 2022-08-05 2022-11-18 新化柏盛陶瓷科技有限公司 Ceramic sealer for lithium battery and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827809A (en) * 2006-03-24 2006-09-06 哈尔滨工业大学 Method and apparatus for preparing composite solder for welding particle enhanced aluminium-based composite material
CN101890590A (en) * 2010-07-01 2010-11-24 哈尔滨工业大学 Composite soldering material for soldering titanium alloy and ceramic or ceramic matrix composition material and method for soldering by using same
CN105149717A (en) * 2015-10-19 2015-12-16 哈尔滨工业大学 Silicon-based ceramic surface metallization method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827809A (en) * 2006-03-24 2006-09-06 哈尔滨工业大学 Method and apparatus for preparing composite solder for welding particle enhanced aluminium-based composite material
CN101890590A (en) * 2010-07-01 2010-11-24 哈尔滨工业大学 Composite soldering material for soldering titanium alloy and ceramic or ceramic matrix composition material and method for soldering by using same
CN105149717A (en) * 2015-10-19 2015-12-16 哈尔滨工业大学 Silicon-based ceramic surface metallization method

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
B. RICCARDI等: "Low activation brazing materials and techniques for SiCf/SiC composites", 《JOURNAL OF NUCLEAR MATERIALS》 *
宋雪: "(Cf-SiCf)/SiBCN高温钎焊连接工艺及其机理研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *
李家科等: "22Ti-78Si 高温共晶钎料对SiC陶瓷的钎焊连接", 《无机材料学报》 *
李家科等: "Ti-Si共晶钎料的制备及其对SiC陶瓷可焊性", 《无机材料学报》 *
赵静: "薄膜复合钎料的制备及其在碳化硅陶瓷连接上的应用", 《上海应用技术大学专业学位硕士学位论文》 *

Cited By (14)

* Cited by examiner, † Cited by third party
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CN108213771B (en) * 2018-01-15 2020-05-22 合肥工业大学 Composite brazing filler metal for brazing silicon carbide ceramic in vacuum and brazing process thereof
CN108213771A (en) * 2018-01-15 2018-06-29 合肥工业大学 A kind of composite soldering and its soldering processes for soldering silicon carbide ceramics in vacuum
CN108274086A (en) * 2018-01-24 2018-07-13 哈尔滨工业大学 A kind of method of two-step method high temperature soldering carbon fiber reinforced carbon matrix composite material
CN109354504A (en) * 2018-11-27 2019-02-19 合肥工业大学 A kind of boron carbide base composite ceramic sintering aid and sintering process
CN109354504B (en) * 2018-11-27 2021-09-14 合肥工业大学 Boron carbide-based composite ceramic sintering aid and sintering process
CN110734298A (en) * 2018-12-31 2020-01-31 深圳硅基仿生科技有限公司 Brazing structure of ceramic and metal
CN110041090A (en) * 2019-05-23 2019-07-23 合肥工业大学 A kind of plasma discharging diffusion connection method of silicon carbide ceramics
CN110407600A (en) * 2019-07-29 2019-11-05 浙江工业大学 A method of SiC ceramic is connected using Au base high-temp solder
CN111958145A (en) * 2020-08-24 2020-11-20 合肥工业大学 Brazing material for MAX phase composite ceramic and brazing process
CN113385851A (en) * 2021-05-28 2021-09-14 中国科学院上海硅酸盐研究所苏州研究院 High-temperature-resistant corrosion-resistant solder for silicon carbide ceramic connection and preparation method and application thereof
CN114315402A (en) * 2022-01-11 2022-04-12 成都成维精密机械制造有限公司 Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic
CN115322005A (en) * 2022-07-15 2022-11-11 西北工业大学 Coating raw material for SiCf/SiC composite material connection and reaction diffusion connection method
CN115360463A (en) * 2022-08-05 2022-11-18 新化柏盛陶瓷科技有限公司 Ceramic sealer for lithium battery and preparation method thereof
CN115360463B (en) * 2022-08-05 2024-04-16 新化柏盛陶瓷科技有限公司 Ceramic sealer for lithium battery and preparation method thereof

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