CN104711457A - High temperature solder and application thereof - Google Patents

High temperature solder and application thereof Download PDF

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Publication number
CN104711457A
CN104711457A CN201310676658.XA CN201310676658A CN104711457A CN 104711457 A CN104711457 A CN 104711457A CN 201310676658 A CN201310676658 A CN 201310676658A CN 104711457 A CN104711457 A CN 104711457A
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solder
temperature
silicon carbide
high temperature
temperature solder
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CN201310676658.XA
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CN104711457B (en
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张辉
闫永杰
刘岩
陈忠明
刘学建
黄政仁
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention discloses a high temperature solder and an application thereof. The high temperature solder is a nickel based alloy formed by nickel and at least one of molybdenum and chromium. The high temperature solder can be used for high temperature welding of silicon carbide ceramic materials. Experiments prove that the high temperature solder provided by the invention has good wetability, good high temperature thermodynamics, oxidation resistance and corrosion resistance, can reduce the influences of welded points on the integral performances of silicon carbide ceramic parts, can reduce the residual thermal stress in the welded points, improves the high temperature and corrosion resistance of welded silicon carbide ceramic connectors, and is in favor of popularizing the application of the silicon carbide ceramic materials.

Description

A kind of high-temperature solder and application thereof
Technical field
The present invention relates to a kind of high-temperature solder and application thereof, belong to stupalith welding technology field.
Background technology
Silicon carbide ceramics has the corrosion-resistant and chemical resistance of concrete ability etc. of low density, high strength, high-modulus, high rigidity, high thermal conductance, low thermal coefficient of expansion, good high-temperature mechanics and antioxidant property and excellence, thus is widely used in the every field of the national products such as metallurgy, machinery, chemical industry, electronics.
In actual applications, by the restriction preparing technology and device condition, be difficult to the ceramic component directly manufacturing large size, complicated shape; Simultaneously not only consuming time, expensive by later stage mechanical workout for the ceramic component that some structures are special, and technique also faces huge challenge.Then easily addressed this problem by ceramic joining.
At present, the main method that thyrite connects has active metal brazing method, reaction forming method, diffusion welding connection method and oxide glass connection method etc.Mainly there is following problem in aforesaid method: (1) activated solder has lower fusing point usually, and welding temperature is general≤and 1000 DEG C, the resistance to elevated temperatures of welding ceramics joint is poor; (2) weld product (or its fractions) and there is poor corrosion-resistant erosion performance.These problems limit the application of thyrite in the extreme environment such as high temperature, corrosion, thus hinder the widespread use of this material.
Summary of the invention
The object of the present invention is to provide a kind of high-temperature solder and application thereof, to solve that welding temperature existing for existing solder is lower and corrosion resistance nature is poor to limit the problem that silicon carbide ceramics welding material uses in the extreme environments such as high temperature corrosion, promote the widespread use of thyrite.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of high-temperature solder is the nickel-base alloy formed with at least one component in molybdenum (Mo), chromium (Cr) by nickel (Ni).
As a kind of preferred version, simultaneously also containing at least one component in tungsten (W), cobalt (Co) and iron (Fe) in described high-temperature solder.
As a kind of preferred version, the nickel content in described high-temperature solder is 40 ~ 75wt.%.
As further preferred version, the compositing formula of described high-temperature solder is as follows: 8 ~ 30wt.%Mo, 1 ~ 30wt.%Cr, 0 ~ 5wt.%W, 0 ~ 5wt.%Co, 0 ~ 5wt.%Fe, and remainder is Ni.
High-temperature solder of the present invention can be used for the welding between thyrite.
Described welding process, comprises the steps:
A) solder uniform spreading is placed on the surface to be welded of the pretreated silicon carbide ceramics matrix of surface cleaning, makes formation pottery-solder-ceramic three-layer structure;
B) put into High Temperature Furnaces Heating Apparatus and carry out high-temperature soldering.
As a kind of preferred version, the solder layer of lay is 10 ~ 1000 μm.
As a kind of preferred version, described silicon carbide ceramics matrix selects compact silicon carbide ceramic.
As a kind of preferred version, graphite carbon pipe furnace selected by described High Temperature Furnaces Heating Apparatus.
As a kind of preferred version, the technique of high-temperature soldering is as follows: in a vacuum or inert atmosphere, first with the ramp to 1200 of 5 ~ 20 DEG C/min DEG C ~ 1600 DEG C, is incubated 0.5 ~ 2 hour; Then 500 DEG C are cooled to the speed of 10 DEG C/min; Finally be cooled to room temperature with stove.
Experiment proves: high-temperature solder provided by the present invention not only has good wettability, and to silicon carbide ceramics matrix, there is similar heat physical properties (good high-temperature thermodynamics, antioxidant property and corrosion resistance nature), thus reduce the impact of welding joint on silicon carbide ceramic components overall performance; Reduce the residual thermal stress in welding joint simultaneously, improve the high temperature resistant and corrosion resistance of the silicon carbide ceramics linker of welding, be conducive to the application promoting thyrite.
Accompanying drawing explanation
Fig. 1 is the wetting angle contrast of pure Ni and Ni base alloy on SiC ceramic matrix;
Fig. 2 is the silicon carbide welding joint interfacial microstructure photo that the embodiment of the present invention 1 obtains;
Fig. 3 is the silicon carbide welding joint interfacial microstructure photo that the embodiment of the present invention 2 obtains.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1
One, by each to nano level Ni, Mo, Cr, Fe powder, be respectively 67%, 30%, 1%, 2% according to the mass percent of 67Ni-30Mo-1Cr-2Fe(and Ni, Mo, Cr, Fe) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1450 DEG C of 5 DEG C/min, be incubated 1 hour, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Formed welding joint interfacial microstructure photo as shown in Figure 2, as seen from Figure 2: joint interface in conjunction with respond well, intact weldering phenomenon.
Embodiment 2
One, by each to nano level Ni, Mo, Cr, W, Co, Fe powder, be respectively 57%, 16%, 16%, 4%, 2%, 5% according to the mass percent of 57Ni-16Mo-16Cr-4W-2Co-5Fe(and Ni, Mo, Cr, W, Co, Fe) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1400 DEG C of 10 DEG C/min, be incubated 0.5 hour, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Formed welding joint interfacial microstructure photo as shown in Figure 3, as seen from Figure 3: obvious Elements Diffusion occurs joint interface, and bonding is good.
Embodiment 3
One, by each to nano level Ni, Mo, Cr, W, Co, Fe powder, be respectively 40%, 15%, 30%, 5%, 5%, 5% according to the mass percent of 40Ni-15Mo-30Cr-5W-5Co-5Fe(and Ni, Mo, Cr, W, Co, Fe) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1450 DEG C of 5 DEG C/min, be incubated 1 hour, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Analyze and show that the interface cohesion of formed welding joint is respond well, intact weldering phenomenon.
Embodiment 4
One, by each to nano level Ni, Mo, Cr, Fe powder, be respectively 75%, 15%, 6%, 4% according to the mass percent of 75Ni-15Mo-6Cr-4Fe(and Ni, Mo, Cr, Fe) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1450 DEG C of 5 DEG C/min, be incubated 2 hours, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Analyze and show that the interface cohesion of formed welding joint is respond well, intact weldering phenomenon.
Embodiment 5
One, by each to nano level Ni, Mo, Cr, Fe powder, be respectively 60%, 8%, 30%, 2% according to the mass percent of 60Ni-8Mo-30Cr-2Fe(and Ni, Mo, Cr, Fe) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1400 DEG C of 5 DEG C/min, be incubated 1 hour, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Analyze and show that the interface cohesion of formed welding joint is respond well, intact weldering phenomenon.
Embodiment 6
One, by each to nano level Ni, Mo, Cr powder, be respectively 61%, 16%, 23% according to the mass percent of 61Ni-16Mo-23Cr(and Ni, Mo, Cr) stoichiometric ratio mixing, add polyvinyl butyral acetal (PVB), ball mill mixing 24 hours in planetary ball mill, obtain the cream solder of distributed components, for subsequent use;
Two, the surface to be welded of silicon carbide ceramics matrix is first used the liquid honing of No. 600, then to put in acetone and alcohol ultrasonic cleaning successively 15 ~ 30 minutes, dry for standby;
Three, be evenly coated in by solder on the welding surface of the pretreated silicon carbide ceramics matrix of surface cleaning, make formation pottery-solder-ceramic three-layer structure, fix with fixture, the gauge control of intermediate solder layer is between 10 ~ 1000 microns;
Four, the three-decker sample that above-mentioned fixture is fixing is put into graphite carbon pipe furnace, under an argon atmosphere, about furnace pressure maintains a standard atmospheric pressure, first with the ramp to 1400 DEG C of 5 DEG C/min, be incubated 2 hours, cool to 500 DEG C with the speed of 10 DEG C/min again after insulation terminates, be then cooled to stove the welding that room temperature can complete silicon carbide ceramics joint.
Analyze and show that the interface cohesion of formed welding joint is respond well, intact weldering phenomenon.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.

Claims (10)

1. a high-temperature solder, is characterized in that: be the nickel-base alloy formed by least one component in nickel and molybdenum, chromium.
2. high-temperature solder as claimed in claim 1, is characterized in that: simultaneously also containing at least one component in tungsten, cobalt and iron in described high-temperature solder.
3. high-temperature solder as claimed in claim 1 or 2, is characterized in that: the nickel content in described high-temperature solder is 40 ~ 75wt.%.
4. high-temperature solder as claimed in claim 3, it is characterized in that, the compositing formula of described high-temperature solder is as follows: 8 ~ 30wt.%Mo, 1 ~ 30wt.%Cr, 0 ~ 5wt.%W, 0 ~ 5wt.%Co, 0 ~ 5wt.%Fe, and remainder is Ni.
5. an application for the high-temperature solder described in claim 1 or 2, is characterized in that: for the high-temperature soldering between thyrite.
6. apply as claimed in claim 5, it is characterized in that, described high-temperature soldering comprises the steps:
A) solder uniform spreading is placed on the surface to be welded of the pretreated silicon carbide ceramics matrix of surface cleaning, makes formation pottery-solder-ceramic three-layer structure;
B) put into High Temperature Furnaces Heating Apparatus and carry out high-temperature soldering.
7. apply as claimed in claim 6, it is characterized in that: the solder layer of lay is 10 ~ 1000 μm.
8. apply as claimed in claim 6, it is characterized in that: described silicon carbide ceramics matrix selects compact silicon carbide ceramic.
9. apply as claimed in claim 6, it is characterized in that: graphite carbon pipe furnace selected by described High Temperature Furnaces Heating Apparatus.
10. apply as claimed in claim 6, it is characterized in that, the technique of high-temperature soldering is as follows: in a vacuum or inert atmosphere, first with the ramp to 1200 of 5 ~ 20 DEG C/min DEG C ~ 1600 DEG C, is incubated 0.5 ~ 2 hour; Then 500 DEG C are cooled to the speed of 10 DEG C/min; Finally be cooled to room temperature with stove.
CN201310676658.XA 2013-12-11 2013-12-11 High temperature solder and application thereof Active CN104711457B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106927848A (en) * 2015-12-29 2017-07-07 中国科学院上海硅酸盐研究所 A kind of Zirconium Diboride-based Ultra-high Temperature Ceramics welding point and preparation method thereof
CN109909643A (en) * 2019-04-30 2019-06-21 上海交通大学 A kind of medium entropy alloy material and welding method for welding
CN112453755A (en) * 2020-10-30 2021-03-09 中国航发北京航空材料研究院 Welding flux for casting defect of K477 high-temperature alloy guider and repair welding method
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
CN113857715A (en) * 2021-09-13 2021-12-31 中国科学院上海硅酸盐研究所 Preformed solder block for repairing service defects of Hastelloy X high-temperature alloy component and preparation method thereof
CN114310028A (en) * 2022-01-27 2022-04-12 厦门虹鹭钨钼工业有限公司 Brazing filler metal for magnetron cathode assembly, preparation method of brazing filler metal, molybdenum end cap and magnetron

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CN102272342A (en) * 2008-11-04 2011-12-07 西门子公司 Welding filler material, use of the welding filler material and component
CN103079752A (en) * 2010-09-13 2013-05-01 福田金属箔粉工业株式会社 Nickel-based hydrochloric acid corrosion resistant alloy for soldering
CN103372731A (en) * 2012-04-25 2013-10-30 乔治洛德方法研究和开发液化空气有限公司 Flux containing a nickel-chromium (Ni-Cr) alloy for electroslag over-lay welding (esw)

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JPH02108493A (en) * 1988-10-14 1990-04-20 Sumitomo Metal Ind Ltd Ceramics joining material
US20060249231A1 (en) * 2005-04-28 2006-11-09 Patricia Bezerra Solder comprising elemental powder
CN101182230A (en) * 2007-11-28 2008-05-21 哈尔滨工业大学 Method for vacuum diffusion connecting ceramic
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106927848A (en) * 2015-12-29 2017-07-07 中国科学院上海硅酸盐研究所 A kind of Zirconium Diboride-based Ultra-high Temperature Ceramics welding point and preparation method thereof
CN109909643A (en) * 2019-04-30 2019-06-21 上海交通大学 A kind of medium entropy alloy material and welding method for welding
CN109909643B (en) * 2019-04-30 2020-11-10 上海交通大学 Medium-entropy alloy material for welding and welding method
CN112453755A (en) * 2020-10-30 2021-03-09 中国航发北京航空材料研究院 Welding flux for casting defect of K477 high-temperature alloy guider and repair welding method
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
CN113857715A (en) * 2021-09-13 2021-12-31 中国科学院上海硅酸盐研究所 Preformed solder block for repairing service defects of Hastelloy X high-temperature alloy component and preparation method thereof
CN114310028A (en) * 2022-01-27 2022-04-12 厦门虹鹭钨钼工业有限公司 Brazing filler metal for magnetron cathode assembly, preparation method of brazing filler metal, molybdenum end cap and magnetron
CN114310028B (en) * 2022-01-27 2023-08-04 厦门虹鹭钨钼工业有限公司 Solder for magnetron cathode assembly, preparation method of solder, molybdenum end cap and magnetron

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