CN104722955A - High-temperature brazing filler metal for brazing Si3N4 ceramic and stainless steel, preparing method and brazing process - Google Patents
High-temperature brazing filler metal for brazing Si3N4 ceramic and stainless steel, preparing method and brazing process Download PDFInfo
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- CN104722955A CN104722955A CN201510123383.6A CN201510123383A CN104722955A CN 104722955 A CN104722955 A CN 104722955A CN 201510123383 A CN201510123383 A CN 201510123383A CN 104722955 A CN104722955 A CN 104722955A
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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
- B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
- B23K35/325—Ti as the principal constituent
-
- 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
- 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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Abstract
The invention discloses high-temperature brazing filler metal for brazing Si3N4 ceramic and stainless steel. The high-temperature brazing filler metal is characterized in that the brazing filler metal is composed of, by weight, 12-15% of Zr, 14-18% of Cu, 12-14% of Ni, 6.0-10% of V, 2.0-4.0% of Be, 3.0-5.0% of Cr, 0.3-0.7% of Si, and the balance Ti. The invention further discloses a preparing method of the brazing filler metal and a brazing process. According to the brazing process that the brazing filler metal connects the Si3N4 ceramic and the stainless steel, through vacuum brazing connection, samples are in a vacuum atmosphere in the heating process, oxidization, pollution and the like are avoided, the surface wetting spreading of the samples is better, brazing seams are filled beneficially, joint strength is improved, and thus stable and reliable welding joints can be obtained.
Description
Technical field
The present invention relates to the connection of foreign material, specifically, relate to a kind of connection Si3N4 pottery and stainless connecting material and soldering processes, belong to welding technology field.
Background technology
Si3N4 ceramic material has the special performances such as intensity is high, high temperature resistant, corrosion-resistant, it is a kind of up-and-coming engineering structure ceramic material, it is mainly used in the fields such as Aero-Space, national defense and military, the energy, electric power, extensively be applied in heat engine, wear parts and heat exchanger and other component, but the shortcomings such as its fragility is large, intensity dispersion, processing difficulties, limit its mechanism's application in engineering as a whole.Realize pottery to be connected with reliable between pottery with metal or pottery, the application of expansion pottery has important function and meaning.
Connection mainly active soldering and the diffusion welding (DW) of pottery and metal.Because pottery and the physical and chemical performance of metal exist larger difference, comparatively greatly, joint unevenly causes larger residual stress owing to shrinking to the difference of thermal expansion coefficients particularly between bi-material in cooling procedure, and bonding strength is reduced greatly.Serious then ftracture voluntarily, even become the direct or indirect reason of structural failure, due to the change of metallographic structure and newly-generated phase structure or compound, the penalty of welding point can be made, joint mechanical property is poor, and particularly fragility increases, and room temperature strength reduces.Therefore develop a kind of new connecting material to solve the problem and practical implementation problem, so realizing pottery with reliable connection the between metal is important prerequisite and the guarantee that Si3N4 pottery is able to wide range of industrial applications.
The research and development of active solder are important contents of development pottery and metal or intermetallic compound soldering.In the joint of the internal stress problem in jointing, especially pottery and metal.Due to the fragility of pottery, under internal stress effect, therefore very easily cause the cracking of pottery, also can cause the obvious decline of strength of joint even if do not ftracture.The connection of current pottery is mainly using Ag-Cu, Ag-Cu-Ti as connecting material, but its high-temperature behavior is poor, greatly limit its scope of application, and the premium properties of pottery can not be made fully to be played.Effectively can improve the high-temperature behavior of soldered fitting to Si3N4 pottery and stainless soldering, it has most important theories and using value to the research of brazing material.
Summary of the invention
Goal of the invention: there is Si to overcome in prior art
3n
4the problems such as the residual stress existing for pottery is connected with stainless steel is excessive, strength of joint is low, the invention provides a kind of soldering Si
3n
4ceramic and stainless high-temp solder.
Present invention also offers preparation method and the soldering processes of above-mentioned high-temp solder.
Technical scheme: for achieving the above object, a kind of soldering Si provided by the invention
3n
4ceramic and stainless high-temp solder, described solder is made up of the component of following percentage by weight:
Zr 12%～15%，
Cu 14%～18%，
Ni 12%～14%，
V 6.0%～10%，
Be 2.0%～4.0%，
Cr 3.0%～5.0%，
Si 0.3%～0.7%，
Surplus is Ti.
Further, in described fibre material component, the purity of often kind of component is 99.50% ~ 99.90%.
Preferably, described solder is made up of the component of following percentage by weight:
13.5%Zr、
16%Cu、
13%Ni、
8.0%V、
3.0%Be、
4.0%Cr、
0.5%Si，
All the other are Ti.
Further, above-mentioned solder adopts vacuum melting and high vacuum to get rid of band, and solder is prepared into foil-like, and thickness is 20-100 μm.
Present invention also offers above-mentioned soldering Si
3n
4the preparation method of ceramic and stainless high-temp solder,
(1) take sponge zirconium, copper billet, nickel particle, vanadium powder, beryllium powder, chromium particle, sponge silicon and titanium sponge by mass percentage and obtain mixture;
(2) in the container that mixture is housed, add acetone, stir to obtain suspension, then by seal of vessel, wherein mixture and acetone volume ratio are 1:10 ~ 20;
(3) under 20 ~ 40 DEG C of conditions, ultrasonic cleaning is carried out to the container that suspension is housed that step (2) obtains, ultrasonic 180 ~ 300s, wherein, mixture is stirred during ultrasonic cleaning simultaneously;
(4) mixture after step (3) ultrasonic cleaning is dried at the temperature of room temperature to 60 DEG C, obtain the mixture of combination drying;
(5) adopt the method for vacuum melting to be prepared into the foundry alloy of chilling solder mixture Zr, Cu, Ni, V, Be, Cr, Si and Ti, after this foundry alloy is pulverized, load in the quartz glass tube of high vacuum single roller strip machine;
(6) quartz glass tube is installed in the induction heating circle getting rid of band machine, and its nozzle is adjusted to 1-2mm to copper roller surface spacing;
(7) close fire door, adopt mechanical pump to be evacuated to 1.5 × 10
-1pa, then adopt molecular pump pumping high vacuum, condition of high vacuum degree is not less than 3 × 10
-4pa, then cavity is full of high-purity Ar gas to 100-200mbar;
(8) open motor, make copper roller rotating speed u
s=26-32m/s, opens high frequency electric source motor, after the foundry alloy high-frequency induction heating in quartz glass tube to complete molten homogeneous, and its melt-blown temperature T=1450-1550 DEG C, insulation superheated melt 60-90s;
(9) by Ar gas air pressure modulation P=25-65kPa, with high pressure argon gas, the superheated melt continuous spraying in quartz glass is mapped to the cooling copper roller surface of High Rotation Speed, liquid metal is subject to chilling and forms foil shape, thus obtains chilling solder, thickness is 20 ~ 100 μm, thus obtains final solder.
Further, in described step (5), quartz ampoule nozzle is rectangle, and its length is a=8-10mm width is b=0.4-1.0mm.
Further, in described step (8), copper roller diameter is 230mm, and copper roller width is 45mm.
The present invention also provides above-mentioned soldering Si
3n
4the soldering processes of ceramic and stainless high-temp solder, comprise the following steps:
(1) preparatory stage: first Si3N4 to be brazed pottery and stainless steel sample end face are cleared up, impurity, greasy dirt and oxide-film that removing is surperficial, stainless steel abrasive paper for metallograph grinds, Si3N4 pottery stainless steel and diamond paste grind, and Si3N4 pottery, stainless steel and solder foil are placed in pure acetone together and adopt ultrasonic method to clean 10-15min;
(2) installation step: the solder foil after cleaning be placed between pottery and stainless steel welding surface, and be close to and be assemblied in brazing jig, a miniweights is placed in welding, produces the constant pressure of 0.02-0.05MPa;
(3) brazing: the fixture entirety assembled is placed in the brazing equipment that vacuum is not less than 1.5 × 10-3Pa, first with the ramp to 500 DEG C of 5-10 DEG C/min, insulation 30min, continue to be warming up to brazing temperature 850-950 DEG C with the speed of 8-13 DEG C/min again, temperature retention time 15-45min, then be cooled to 300 DEG C with the speed of 5-8 DEG C/min, cool to room temperature with the furnace, take out soldered
Beneficial effect: compared with prior art, the advantage had and beneficial effect are mainly reflected in following several respects in the present invention:
(1) solder of the present invention is adopted to connect Si
3n
4ceramic and stainless soldering processes, are connected by vacuum brazing, and sample is in vacuum atmosphere in heating process, there will not be oxidation, pollution etc., its moistened surface is sprawled better, is conducive to filling brazed seam, improve strength of joint, thus can obtain reliable and stable welding point.
(2) solder paillon foil of the present invention, is conducive to accelerating the atoms permeating in high temperature conjunction process and interfacial reaction, improves the wettability of solder, crystal grain thinning, reduce the residual stress in joint, improves mechanical property and the heat resistance of joint.
(3) preparation method of solder that obtains of the present invention, technique is simple, implements convenient and swift, and the preparation of solder can repetition, easy to utilize.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
embodiment 1:
Si
3n
4pottery and austenitic stainless steel banjo fixing butt jointing vacuum brazing: Si
3n
4ceramic sample is of a size of 20mm × 20mm × 5mm, and austenitic stainless steel is 1Cr18Ni9Ti stainless steel, and size is 20mm × 20mm × 5mm, and to be brazed is 20mm × 5mm cross section.
Composition and the mass percent proportioning of solder are: Zr:12%; Cu:14%; Ni:12%; V:6.0%; Be:2.0%; Cr:3.0%; Si:0.3%; All the other are Ti.Solder thickness is 20 μm.
Soldering Si
3n
4the preparation method of ceramic and stainless high-temp solder:
(1) take sponge zirconium, copper billet, nickel particle, vanadium powder, beryllium powder, chromium particle, sponge silicon and titanium sponge by mass percentage and obtain mixture;
(2) in the container that mixture is housed, add acetone, stir to obtain suspension, then by seal of vessel, wherein mixture and acetone volume ratio are 1:10;
(3) under 20 DEG C of conditions, ultrasonic cleaning is carried out to the container that suspension is housed that step (2) obtains, ultrasonic 180 ~ 300s, wherein, mixture is stirred during ultrasonic cleaning simultaneously;
(4) mixture after step (3) ultrasonic cleaning is dried at the temperature of room temperature to 60 DEG C, obtain the mixture of combination drying;
(5) adopt the method for vacuum melting to be prepared into the foundry alloy of chilling solder mixture Zr, Cu, Ni, V, Be, Cr, Si and Ti, after this foundry alloy is pulverized, load in the quartz glass tube of high vacuum single roller strip machine;
(6) quartz glass tube is installed in the induction heating circle getting rid of band machine, and its nozzle is adjusted to 1-2mm to copper roller surface spacing;
(7) close fire door, adopt mechanical pump to be evacuated to 1.5 × 10
-1pa, then adopt molecular pump pumping high vacuum, condition of high vacuum degree is not less than 3 × 10
-4pa, then cavity is full of high-purity Ar gas to 100mbar;
(8) open motor, make copper roller rotating speed u
s=26-32m/s, opens high frequency electric source motor, after the foundry alloy high-frequency induction heating in quartz glass tube to complete molten homogeneous, and its melt-blown temperature T=1450 DEG C, insulation superheated melt 60s;
(9) by Ar gas air pressure modulation P=25kPa, with high pressure argon gas, the superheated melt continuous spraying in quartz glass is mapped to the cooling copper roller surface of High Rotation Speed, liquid metal is subject to chilling and forms foil shape, thus obtains chilling solder, thickness is 20 μm, thus obtains final solder.
Soldering process step is:
(1) first incite somebody to action: Si
3n
4ceramic and stainless surface to be welded is cleared up, impurity, greasy dirt and oxide-film that removing is surperficial, and 1Cr18Ni9Ti stainless steel abrasive paper for metallograph grinds, Si
3n
4pottery stainless steel and diamond paste grind, by Si
3n
4pottery, 1Cr18Ni9Ti stainless steel and solder paillon foil are placed in pure acetone together and adopt ultrasonic method to clean 15min post-drying;
(2) the solder paillon foil after cleaning is placed in Si
3n
4between pottery and 1Cr18Ni9Ti stainless steel surface to be brazed, and be close to and be assemblied in brazing jig, weldment is placed a miniweights, produce the constant pressure of 0.05MPa;
(3) the fixture entirety assembled is placed in vacuum and is not less than 1.5 × 10
-3in the brazing equipment of Pa, first with the ramp to 500 DEG C of 5 DEG C/min, insulation 30min, continue to be warming up to brazing temperature 850 DEG C, temperature retention time 45min with the speed of 10 DEG C/min again, be then cooled to 300 DEG C with the speed of 5 DEG C/min, cool to room temperature with the furnace, take out soldered.
Result: the Si that soldering obtains
3n
4pottery and 1Cr18Ni9Ti stainless joint are formed well, and metallographic observation finds that brazing area forms fine and close interface cohesion, and room temperature four-point bending intensity is 165MPa.
embodiment 2:
Si
3n
4pottery and austenitic stainless steel banjo fixing butt jointing vacuum brazing: Si
3n
4ceramic sample is of a size of 20mm × 20mm × 5mm, and austenitic stainless steel is 1Cr18Ni9Ti stainless steel, and size is 20mm × 20mm × 5mm, and to be brazed is 20mm × 5mm cross section.
Composition and the mass percent proportioning of solder are: Zr:15%; Cu:18%; Ni:14%; V:10%; Be:4.0%; Cr:5.0%; Si:0.7%; All the other are Ti.Solder thickness is 100 μm.
Soldering Si
3n
4the preparation method of ceramic and stainless high-temp solder:
(1) take sponge zirconium, copper billet, nickel particle, vanadium powder, beryllium powder, chromium particle, sponge silicon and titanium sponge by mass percentage and obtain mixture;
(2) in the container that mixture is housed, add acetone, stir to obtain suspension, then by seal of vessel, wherein mixture and acetone volume ratio are 1:20;
(3) under 20 ~ 40 DEG C of conditions, ultrasonic cleaning is carried out to the container that suspension is housed that step (2) obtains, ultrasonic 180 ~ 300s, wherein, mixture is stirred during ultrasonic cleaning simultaneously;
(4) mixture after step (3) ultrasonic cleaning is dried at the temperature of room temperature to 60 DEG C, obtain the mixture of combination drying;
(5) adopt the method for vacuum melting to be prepared into the foundry alloy of chilling solder mixture Zr, Cu, Ni, V, Be, Cr, Si and Ti, after this foundry alloy is pulverized, load in the quartz glass tube of high vacuum single roller strip machine;
(6) quartz glass tube is installed in the induction heating circle getting rid of band machine, and its nozzle is adjusted to 1-2mm to copper roller surface spacing;
(7) close fire door, adopt mechanical pump to be evacuated to 1.5 × 10
-1pa, then adopt molecular pump pumping high vacuum, condition of high vacuum degree is not less than 3 × 10
-4pa, then cavity is full of high-purity Ar gas to 200mbar;
(8) open motor, make copper roller rotating speed u
s=26-32m/s, opens high frequency electric source motor, after the foundry alloy high-frequency induction heating in quartz glass tube to complete molten homogeneous, and its melt-blown temperature T=1550 DEG C, insulation superheated melt 90s;
(9) by Ar gas air pressure modulation P=65kPa, with high pressure argon gas, the superheated melt continuous spraying in quartz glass is mapped to the cooling copper roller surface of High Rotation Speed, liquid metal is subject to chilling and forms foil shape, thus obtains chilling solder, thickness is 100 μm, thus obtains final solder.
Soldering process step is:
(1) first incite somebody to action: Si
3n
4ceramic and stainless surface to be welded is cleared up, impurity, greasy dirt and oxide-film that removing is surperficial, and 1Cr18Ni9Ti stainless steel abrasive paper for metallograph grinds, Si
3n
4pottery stainless steel and diamond paste grind, by Si
3n
4pottery, 1Cr18Ni9Ti stainless steel and solder paillon foil are placed in pure acetone together and adopt ultrasonic method to clean 15min post-drying;
(2) the solder paillon foil after cleaning is placed in Si
3n
4between pottery and 1Cr18Ni9Ti stainless steel surface to be brazed, and be close to and be assemblied in brazing jig, weldment is placed a miniweights, produce the constant pressure of 0.05MPa;
(3) the fixture entirety assembled is placed in vacuum and is not less than 1.5 × 10
-3in the brazing equipment of Pa, first with the ramp to 500 DEG C of 10 DEG C/min, insulation 30min, continue to be warming up to brazing temperature 950 DEG C, temperature retention time 15min with the speed of 13 DEG C/min again, be then cooled to 300 DEG C with the speed of 8 DEG C/min, cool to room temperature with the furnace, take out soldered.
Result: the Si that soldering obtains
3n
4pottery and 1Cr18Ni9Ti stainless joint are formed well, and metallographic observation finds that brazing area forms fine and close interface cohesion, and room temperature four-point bending intensity is 137MPa.
embodiment 3:
Si
3n
4pottery and austenitic stainless steel banjo fixing butt jointing vacuum brazing: Si
3n
4ceramic sample is of a size of 20mm × 20mm × 5mm, and austenitic stainless steel is 1Cr18Ni9Ti stainless steel, and size is 20mm × 20mm × 5mm, and to be brazed is 20mm × 5mm cross section.
Composition and the mass percent proportioning of solder are: Zr:13.5%; Cu:16%; Ni:13%; V:8.0%; Be:3.0%; Cr:4.0%; Si:0.5%; All the other are Ti.Solder thickness is 60 μm.
Soldering Si
3n
4the preparation method of ceramic and stainless high-temp solder:
(1) take sponge zirconium, copper billet, nickel particle, vanadium powder, beryllium powder, chromium particle, sponge silicon and titanium sponge by mass percentage and obtain mixture;
(2) in the container that mixture is housed, add acetone, stir to obtain suspension, then by seal of vessel, wherein mixture and acetone volume ratio are 1:15;
(3) under 20 ~ 40 DEG C of conditions, ultrasonic cleaning is carried out to the container that suspension is housed that step (2) obtains, ultrasonic 250s, wherein, mixture is stirred during ultrasonic cleaning simultaneously;
(4) mixture after step (3) ultrasonic cleaning is dried at the temperature of room temperature to 60 DEG C, obtain the mixture of combination drying;
(5) adopt the method for vacuum melting to be prepared into the foundry alloy of chilling solder mixture Zr, Cu, Ni, V, Be, Cr, Si and Ti, after this foundry alloy is pulverized, load in the quartz glass tube of high vacuum single roller strip machine;
(6) quartz glass tube is installed in the induction heating circle getting rid of band machine, and its nozzle is adjusted to 1.5mm to copper roller surface spacing;
(7) close fire door, adopt mechanical pump to be evacuated to 1.5 × 10
-1pa, then adopt molecular pump pumping high vacuum, condition of high vacuum degree is not less than 3 × 10
-4pa, then cavity is full of high-purity Ar gas to 150mbar;
(8) open motor, make copper roller rotating speed u
s=26-32m/s, opens high frequency electric source motor, after the foundry alloy high-frequency induction heating in quartz glass tube to complete molten homogeneous, and its melt-blown temperature T=1500 DEG C, insulation superheated melt 80s;
(9) by Ar gas air pressure modulation P=45kPa, with high pressure argon gas, the superheated melt continuous spraying in quartz glass is mapped to the cooling copper roller surface of High Rotation Speed, liquid metal is subject to chilling and forms foil shape, thus obtains chilling solder, thickness is 80 μm, thus obtains final solder.
Soldering process step is:
(1) first incite somebody to action: Si
3n
4ceramic and stainless surface to be welded is cleared up, impurity, greasy dirt and oxide-film that removing is surperficial, and 1Cr18Ni9Ti stainless steel abrasive paper for metallograph grinds, Si
3n
4pottery stainless steel and diamond paste grind, by Si
3n
4pottery, 1Cr18Ni9Ti stainless steel and solder paillon foil are placed in pure acetone together and adopt ultrasonic method to clean 15min post-drying;
(2) the solder paillon foil after cleaning is placed in Si
3n
4between pottery and 1Cr18Ni9Ti stainless steel surface to be brazed, and be close to and be assemblied in brazing jig, weldment is placed a miniweights, produce the constant pressure of 0.05MPa;
(3) the fixture entirety assembled is placed in vacuum and is not less than 1.5 × 10
-3in the brazing equipment of Pa, first with the ramp to 500 DEG C of 8 DEG C/min, insulation 30min, continue to be warming up to brazing temperature 900 DEG C, temperature retention time 30min with the speed of 10 DEG C/min again, be then cooled to 300 DEG C with the speed of 6 DEG C/min, cool to room temperature with the furnace, take out soldered.
Result: the Si that soldering obtains
3n
4pottery and 1Cr18Ni9Ti stainless joint are formed well, and metallographic observation finds that brazing area forms fine and close interface cohesion, and room temperature four-point bending intensity is 192MPa.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a soldering Si
3n
4ceramic and stainless high-temp solder, is characterized in that: described solder is made up of the component of following percentage by weight:
Zr 12%～15%，
Cu 14%～18%，
Ni 12%～14%，
V 6.0%～10%，
Be 2.0%～4.0%，
Cr 3.0%～5.0%，
Si 0.3%～0.7%，
Surplus is Ti.
2. soldering Si according to claim 1
3n
4ceramic and stainless high-temp solder, is characterized in that: in described fibre material component, the purity of often kind of component is 99.50% ~ 99.90%.
3. soldering Si according to claim 1
3n
4ceramic and stainless high-temp solder, is characterized in that: described solder is made up of the component of following percentage by weight:
13.5%Zr、
16%Cu、
13%Ni、
8.0%V、
3.0%Be、
4.0%Cr、
0.5%Si，
All the other are Ti.
4. soldering Si according to claim 1
3n
4ceramic and stainless high-temp solder, is characterized in that: adopt vacuum melting and high vacuum to get rid of band, solder is prepared into foil-like, and thickness is 20-100 μm.
5. a soldering Si as claimed in claim 1
3n
4the preparation method of ceramic and stainless high-temp solder, is characterized in that: (1) takes sponge zirconium, copper billet, nickel particle, vanadium powder, beryllium powder, chromium particle, sponge silicon and titanium sponge by mass percentage and obtains mixture;
(2) in the container that mixture is housed, add acetone, stir to obtain suspension, then by seal of vessel, wherein mixture and acetone volume ratio are 1:10 ~ 20;
(3) under 20 ~ 40 DEG C of conditions, ultrasonic cleaning is carried out to the container that suspension is housed that step (2) obtains, ultrasonic 180 ~ 300s, wherein, mixture is stirred during ultrasonic cleaning simultaneously;
(4) mixture after step (3) ultrasonic cleaning is dried at the temperature of room temperature to 60 DEG C, obtain the mixture of combination drying;
(5) adopt the method for vacuum melting to be prepared into the foundry alloy of chilling solder mixture Zr, Cu, Ni, V, Be, Cr, Si and Ti, after this foundry alloy is pulverized, load in the quartz glass tube of high vacuum single roller strip machine;
(6) quartz glass tube is installed in the induction heating circle getting rid of band machine, and its nozzle is adjusted to 1-2mm to copper roller surface spacing;
(7) close fire door, adopt mechanical pump to be evacuated to 1.5 × 10
-1pa, then adopt molecular pump pumping high vacuum, condition of high vacuum degree is not less than 3 × 10
-4pa, then cavity is full of high-purity Ar gas to 100-200mbar;
(8) open motor, make copper roller rotating speed u
s=26-32m/s, opens high frequency electric source motor, after the foundry alloy high-frequency induction heating in quartz glass tube to complete molten homogeneous, and its melt-blown temperature T=1450-1550 DEG C, insulation superheated melt 60-90s;
(9) by Ar gas air pressure modulation P=25-65kPa, with high pressure argon gas, the superheated melt continuous spraying in quartz glass is mapped to the cooling copper roller surface of High Rotation Speed, liquid metal is subject to chilling and forms foil shape, thus obtains chilling solder, thickness is 20 ~ 100 μm, thus obtains final solder.
6. soldering Si according to claim 5
3n
4the preparation method of ceramic and stainless high-temp solder, is characterized in that: in described step (5), quartz ampoule nozzle is rectangle, and its length is a=8-10mm width is b=0.4-1.0mm.
7. soldering Si3N4 pottery according to claim 5 and the preparation method of stainless high-temp solder, is characterized in that: in described step (8), copper roller diameter is 230mm, and copper roller width is 45mm.
8. a soldering Si according to claim 1
3n
4the soldering processes of ceramic and stainless high-temp solder, is characterized in that comprising the following steps:
(1) preparatory stage: first Si3N4 to be brazed pottery and stainless steel sample end face are cleared up, impurity, greasy dirt and oxide-film that removing is surperficial, stainless steel abrasive paper for metallograph grinds, Si3N4 pottery stainless steel and diamond paste grind, and Si3N4 pottery, stainless steel and solder foil are placed in pure acetone together and adopt ultrasonic method to clean 10-15min;
(2) installation step: the solder foil after cleaning be placed between pottery and stainless steel welding surface, and be close to and be assemblied in brazing jig, a miniweights is placed in welding, produces the constant pressure of 0.02-0.05MPa;
(3) brazing: the fixture entirety assembled is placed in the brazing equipment that vacuum is not less than 1.5 × 10-3Pa, first with the ramp to 500 DEG C of 5-10 DEG C/min, insulation 30min, continue to be warming up to brazing temperature 850-950 DEG C with the speed of 8-13 DEG C/min again, temperature retention time 15-45min, then be cooled to 300 DEG C with the speed of 5-8 DEG C/min, cool to room temperature with the furnace, take out soldered.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510123383.6A CN104722955A (en) | 2015-03-20 | 2015-03-20 | High-temperature brazing filler metal for brazing Si3N4 ceramic and stainless steel, preparing method and brazing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510123383.6A CN104722955A (en) | 2015-03-20 | 2015-03-20 | High-temperature brazing filler metal for brazing Si3N4 ceramic and stainless steel, preparing method and brazing process |
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| CN104722955A true CN104722955A (en) | 2015-06-24 |
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| CN (1) | CN104722955A (en) |
Cited By (8)
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| CN105728981A (en) * | 2016-05-05 | 2016-07-06 | 哈尔滨工业大学（威海） | Brazing filler metal for welding Si3N4 ceramic-stainless steel and brazing method thereof |
| CN106736035A (en) * | 2016-12-30 | 2017-05-31 | 江苏科技大学 | The solder and method for welding of soldering 3D printing stainless steel and silicon nitride ceramics |
| CN106736034A (en) * | 2016-12-30 | 2017-05-31 | 江苏科技大学 | The solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics |
| 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 |
| CN111039692A (en) * | 2019-12-11 | 2020-04-21 | 宁波奇亿金属有限公司 | Diffusion fiber welding method for stainless steel and ceramic sheets |
| CN111732442A (en) * | 2020-05-18 | 2020-10-02 | 株洲天成金属激光高科有限公司 | Seamless welding process for ceramic material and metal material |
| CN113020840A (en) * | 2021-03-02 | 2021-06-25 | 中国工程物理研究院材料研究所 | Brazing method between beryllium material and metal piece |
| CN114178639A (en) * | 2022-02-17 | 2022-03-15 | 太原理工大学 | Pulse laser brazing sealing method for beryllium window and stainless steel base |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105728981A (en) * | 2016-05-05 | 2016-07-06 | 哈尔滨工业大学（威海） | Brazing filler metal for welding Si3N4 ceramic-stainless steel and brazing method thereof |
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| CN111039692A (en) * | 2019-12-11 | 2020-04-21 | 宁波奇亿金属有限公司 | Diffusion fiber welding method for stainless steel and ceramic sheets |
| CN111732442A (en) * | 2020-05-18 | 2020-10-02 | 株洲天成金属激光高科有限公司 | Seamless welding process for ceramic material and metal material |
| CN113020840A (en) * | 2021-03-02 | 2021-06-25 | 中国工程物理研究院材料研究所 | Brazing method between beryllium material and metal piece |
| CN114178639A (en) * | 2022-02-17 | 2022-03-15 | 太原理工大学 | Pulse laser brazing sealing method for beryllium window and stainless steel base |
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