CN106736034A - The solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics - Google Patents

The solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics Download PDF

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Publication number
CN106736034A
CN106736034A CN201611252454.3A CN201611252454A CN106736034A CN 106736034 A CN106736034 A CN 106736034A CN 201611252454 A CN201611252454 A CN 201611252454A CN 106736034 A CN106736034 A CN 106736034A
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solder
stainless steel
soldering
aluminium oxide
oxide ceramics
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CN201611252454.3A
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Inventor
许祥平
康昊杰
何力
夏春智
邹家生
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Jiangsu University of Science and Technology
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Jiangsu University of Science and Technology
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Priority to CN201611252454.3A priority Critical patent/CN106736034A/en
Publication of CN106736034A publication Critical patent/CN106736034A/en
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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
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/30Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3006Ag as the principal constituent
    • 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
    • B23K1/19Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • 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
    • B23K35/02Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0233Sheets, foils
    • 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
    • B23K2103/02Iron or ferrous alloys
    • B23K2103/04Steel or steel alloys
    • B23K2103/05Stainless steel
    • 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
    • B23K2103/08Non-ferrous metals or alloys
    • B23K2103/10Aluminium or alloys thereof
    • 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

Abstract

The invention discloses a kind of soldering 3D printing stainless steel and the solder of aluminium oxide ceramics, solder elemental composition by weight percentage includes:Cu20.0%~25.0%, In13.0%~16.0%, Ti2.0%~5.0%, Sm0.02%~0.2%, Er0.01%~0.1%, balance of Ag.Soldering 3D printing stainless steel of the invention and aluminium oxide ceramics, the good fluidity of the solder are good to mother metal wetability, and good with the binding ability of 3D printing stainless steel and aluminium oxide ceramics, and shear strength is high, can effectively reduce the residual stress produced during soldering;At 760 DEG C or so, brazing filler metal melts temperature declines many to the brazing temperature of solder of the present invention than the fusion temperature of conventional ceramic soldering and common stainless steel, and brazing filler metal melts are uniform;Particularly with the addition of mixed rare-earth elements Sm, Er, the wetability of solder is significantly improved, the thickness of control interface compound significantly improves joint mechanical property.

Description

The solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics
Technical field
The present invention relates to the solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics, belong to soldering Field.
Background technology
Aluminium oxide ceramics has unique intensity, wearability, corrosion resistance and insulating properties, has been widely used industry Many fields.But aluminium oxide ceramics fragility is big, and machinability is poor, also it is difficult to make big or complicated component, consequently, it is desirable to Using solder technology by size is small, ceramet of simple shape is welded, the big and component of complexity is formed, to meet engineering reality The need for.
Both at home and abroad to aluminium oxide ceramics and the soldering processes of 304 stainless steels, the welding point of formation can meet engineering Need, but the soldering to 3D printing stainless steel and aluminium oxide ceramics there is no research, in order to weld oxygen under relatively low brazing temperature Change aluminium ceramics and 3D printing stainless steel, it is necessary to make major technological breakthrough in conventional technology.
Since 3D printing technique is born, each state all conducts a research, and especially its Laser Study, has been achieved for very More more satisfactory achievement.Its principle is to make part drawing first with CAD software, then using the special-purpose software pair of slicing delamination CAD diagram is processed, and 3 dimensional drawing is changed into 2 d plane picture in layer, thus can be according to size, shape Determine scanning pattern, be then incorporated into scanning imaging system, then synchronous powder feeding system, laser scanning.Because after laser scanning, powder it is molten It is substantially to complete moment to change with solidification, Gu without waiting for can immediately carry out next step.Work is highly lowered according to scan line Platform, it is ensured that the hot spot of laser is in same focus state, then powdering, laser scanning, repeats the above steps, and layer upon layer is until complete Into 3 d part.3D printing stainless steel is the hot topic in 3D printing technique, and it greatly shortens life cycle of the product, produces some phases The fine tissue more less common than other production technologies, and the similar casting process of process of setting, part are fine and close, process it To part have good mechanical property and mechanical performance, with casting and forging quite it is even better, at the same time also have stronger Corrosion resistance.Powder used in process, can collect, and be reused after being processed through sieving, save material. 3D printing can produce the product of complex contour.
But, 3D printing stainless steel consistency is extremely difficult to absolutely, and material surface can produce hole, and influence is fine and close Property, joint quality can be influenceed in welding process, it is serious to reduce the mechanics and mechanical performance of welding point, and then influence it practical Property.So, soldering 3D printing stainless steel and aluminium oxide ceramics just have it is more difficult, it is necessary to solder have splendid wetting and spreading energy Power, it is desirable to which the uniform cross after soldering is smooth.Conventional stainless steel and Ceramic brazing temperature all reaches 850 DEG C, and 3D printing Stainless steel and aluminium oxide ceramics brazing temperature are unsuitable too high, and too high meeting causes that 3D printing stainless steel produces pressure distortion, serious shadow Ring the performance of welding point.
There is no the solder of special soldering 3D printing stainless steel and aluminium oxide ceramics, a kind of external existing pricker both at home and abroad at present The solder of weldering ceramics and 304 stainless steels, its trade mark is IncusilABA, and the solder has relatively low liquidus temperature, soldering temperature Degree can be controlled at 750 DEG C~800 DEG C, and brazing temperature is at 800 DEG C or so, but wherein Ti, In content is relatively low, and wetability is not It is ideal;Beijing Institute of Aeronautical Materials, China Aviation Industry Group Corporation have developed on this basis a kind of silver-copper-indium- Titanium middle temperature brazing material, its number of patent application is 201510920495.4, and this solder is used for the gold such as SiO 2-ceramic and tungsten, molybdenum The soldering of category, this intermediate temperature solder is not alleviated in ceramics and metal heterogenous material joint due to two kinds of material thermal expansion coefficients not With the thermal stress for causing, but 3D printing stainless steel and ceramic soldering cannot be applied to, its wetability is not obviously improved, nothing Method is filled up completely with the hole of 3D printing stainless steel, and quality of weld joint cannot ensure.
The content of the invention
Goal of the invention:In order to overcome the deficiencies in the prior art, the present invention to provide a kind of soldering 3D printing stainless steel With the solder of aluminium oxide ceramics and preparation and method for welding, mixed rare-earth elements Sm, Er are added, significantly improve the wetting of solder Property, the thickness of control interface compound significantly improves joint mechanical property.
Technical scheme:In order to solve the above technical problems, a kind of soldering 3D printing stainless steel of the invention and aluminium oxide ceramics Solder, solder elemental composition by weight percentage includes:Cu20.0%~25.0%, In13.0%~ 16.0%, Ti2.0%~5.0%, Sm0.02%~0.2%, Er0.01%~0.1%, balance of Ag.
Preferably, solder elemental composition by weight percentage includes:Cu21.5%~23.5%, In13.5%~15.0%, Ti2.5%~4.0%, Sm0.05%~0.1%, Er0.01%~0.05%, balance of Ag.
Preferably, solder elemental composition by weight percentage includes:Cu22.7%, In14.5%, Ti3.6%, Sm0.05%, Er0.05%, balance of Ag.
Preferably, the solder is paillon foil banding, thickness is 50~100 μm.
The solder preparation method of a kind of above-mentioned soldering 3D printing stainless steel and aluminium oxide ceramics, comprises the following steps:
1) Ti particles, In particles, Er particles, Sm particles, the prepared mixture of Cu pieces of high-purity are weighed by mass percentage, It is put into the container added with acetone, 15~20min of ultrasonic cleaning is carried out at a temperature of 15-25 DEG C;
2) mixture after step 1 is cleaned by ultrasonic is dried at a temperature of 30~50 DEG C, obtains dry mixture;
3) mixture and Ag will be prepared using the uniform solder foundry alloy of method prepared composition of vacuum induction melting Foundry alloy pulverize after, load high vacuum single roller strip machine quartz glass tube in;
4) quartz glass tube is installed in getting rid of the electrical induction circle with machine, and its nozzle to copper roller surface spacing is adjusted Whole is 150~200 μm;
5) fire door is closed, 1.5 × 10 is evacuated to using mechanical pump-3Pa, then using molecular pump pumping high vacuum, high vacuum Degree is not less than 9 × 10-5Pa, then cavity is full of high-purity Ar gas to 200~230mbar;
6) motor is opened, is made in the range of 28~33m/s of copper roller rotating speed, high frequency electric source is then turned on, by quartz glass tube Foundry alloy high-frequency induction heating to substantially uniformity melting after, insulation superheated melt 60s~80s;
7) Ar gas air pressure is modulated into P=50KPa, the superheated melt in quartz glass is continuously ejected into height with high pressure argon gas The cooling copper roller surface of speed rotation, liquid metal formed foil shape by chilling, and so as to obtain solder foil strip, thickness is 50~ 100μm。
Preferably, the step 4) in nozzle be rectangle, its length be 8~10mm, width be 0.8~1.2mm.
Preferably, the step 6) in copper roller diameter be 250mm, copper roller width be 50mm.
The method for welding of a kind of above-mentioned soldering 3D printing stainless steel and aluminium oxide ceramics, comprises the following steps:
1) preparatory stage:Aluminium oxide ceramics to be brazed and the stainless steel curved beam end face of 3D printing are cleared up, table is removed The impurity in face, greasy dirt and oxide-film, be ground with abrasive paper for metallograph it is smooth, by aluminium oxide ceramics and 3D printing stainless steel and pricker Material paillon foil is placed in acetone together, and 15~20min is cleaned using ultrasonic wave, and carries out drying and processing, and period is paid special attention to prevent The oxidation of solder element;
2) assembling stage:By the solder paillon foil after cleaning be placed in aluminium oxide ceramics and 3D printing stainless steel welding surface it Between, and be close to be assemblied in special brazing jig, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce The constant perpendicular pressure of 0.04~0.06MPa;
3) the soldering connection stage:The fixture that will be assembled is integrally placed at vacuum and is not less than 1.5 × 10-5The soldering oven of Pa In, 500 DEG C are warming up to the speed of 15 DEG C/min, 30min is incubated, then 760 DEG C, insulation are warming up to the speed of 10 DEG C/min 20min, then 300 DEG C are cooled to the speed of 5 DEG C/min, cooling to room temperature with the furnace again afterwards, blow-on is taken out and is by weldering connector Can.
Present invention addition element Cu in brazing material, can improve the microstructure of solder, and the fusion temperature of solder is omited Edge down low, improve the wetability on alumina ceramic face, significantly improve strength of joint.
Addition element Ti is obviously improved the high-temperature heat-resistance and corrosion resistance of joint, and solder is improved while strengthening its high-temperature behavior Wetability.
Addition element In, can significantly reduce the fusing point of solder, reduce surface tension during solder liquid, be conducive to improving Wetability.
In order to solve the pore problem of 3D printing surface of stainless steel:
Addition rare earth element Sm, can improve the deficiency of solder:Solder fusing point is reduced, rare earth is surface active element, fitted The surface tension that the rare earth of amount can improve liquid solder improves wetability so that interface compound even uniform, while providing Strength of joint.
Addition element Er, can be engaged with rare earth element Sm, reduce solder fusing point, prevent element segregation, reduce interface The gross thickness growth rate of compound, improves the shear strength of joint.
Beneficial effect:Compared with prior art, the present invention has advantages below:
(1) remarkable advantage of the invention is the good fluidity of the solder, good to mother metal wetability, and with 3D printing stainless steel Binding ability with aluminium oxide ceramics is good, and shear strength is high, can effectively reduce the residual stress produced during soldering;Pricker of the present invention The brazing temperature of material at 760 DEG C or so, under fusion temperature of the brazing filler metal melts temperature than conventional ceramic soldering and common stainless steel Drop is many, and brazing filler metal melts are uniform;Particularly with the addition of mixed rare-earth elements Sm, Er, the wetability of solder is significantly improved, control boundary The thickness of face compound, significantly improves joint mechanical property.
(2) it is reliable and stable using solder Joining Technology of the invention, connected using vacuum brazing, component is in heating process In vacuum state, whole component without microfissure, stomata and the defect such as is mingled with without deformation, and its moistened surface is sprawled preferably, pricker Material is sufficiently formed solid solution metallurgical reaction with matrix mother metal, and tissue particle is sufficient filling with brazed seam, improves the bulk strength of joint, And possess good plastic deformation ability, thus more reliable and stable jointing can be obtained;
(3) the solder preparation method and soldering processes that the present invention is obtained are simple, easy to implement quick, the preparation of solder and Soldering processes are repeatable to be reproduced, and Process of Vacuum Brazing need not add brazing flux and safeguard measure, is easy to extensive popularization and application.
Specific embodiment
Embodiment 1
The composition and mass percent of solder are matched:Cu:21.0%, In13.5%, Ti2.0%, Sm0.02%, Er0.01%, balance of Ag.
The solder preparation method of a kind of above-mentioned soldering 3D printing stainless steel and aluminium oxide ceramics is comprised the following steps:
1) Ti particles, In particles, Er particles, Sm particles, the prepared mixture of Cu pieces of high-purity are weighed by mass percentage, It is put into the container added with acetone, 15~20min of ultrasonic cleaning is carried out at a temperature of 20 DEG C or so;
2) mixture after step 1 is cleaned by ultrasonic is dried at a temperature of 30~50 DEG C, obtains dry mixture;
3) mixture and Ag will be prepared using the uniform solder foundry alloy of method prepared composition of vacuum induction melting Foundry alloy pulverize after, load high vacuum single roller strip machine quartz glass tube in;
4) quartz glass tube is installed in getting rid of the electrical induction circle with machine, and its nozzle to copper roller surface spacing is adjusted Whole is 150~200 μm;
5) fire door is closed, 1.5 × 10 is evacuated to using mechanical pump-3Pa, then using molecular pump pumping high vacuum, high vacuum Degree is not less than 9 × 10-5Pa, then cavity is full of high-purity Ar gas to 200~230mbar;
6) motor is opened, is made in the range of 28~33m/s of copper roller rotating speed, high frequency electric source is then turned on, by quartz glass tube Foundry alloy high-frequency induction heating to substantially uniformity melting after, insulation superheated melt 60s~80s;
7) Ar gas air pressure is modulated into P=50KPa, the superheated melt in quartz glass is continuously ejected into height with high pressure argon gas The cooling copper roller surface of speed rotation, liquid metal formed foil shape by chilling, and so as to obtain solder foil strip, thickness is 50~ 100μm。
The soldering processes of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics, comprise the following steps:
1) preparatory stage:Aluminium oxide ceramics to be brazed and the stainless steel curved beam end face of 3D printing are cleared up, table is removed The impurity in face, greasy dirt and oxide-film, be ground with abrasive paper for metallograph it is smooth, by aluminium oxide ceramics and 3D printing stainless steel and pricker Material paillon foil is placed in acetone together, and 15~20min is cleaned using ultrasonic wave, and carries out drying and processing, and period is paid special attention to prevent The oxidation of solder element;
2) assembling stage:By the solder paillon foil after cleaning be placed in aluminium oxide ceramics and 3D printing stainless steel welding surface it Between, and be close to be assemblied in special brazing jig, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce The constant perpendicular pressure of 0.04~0.06MPa;
3) the soldering connection stage:The fixture that will be assembled is integrally placed at vacuum and is not less than 1.5 × 10-5The soldering oven of Pa In, 500 DEG C are warming up to the speed of 15 DEG C/min, 30min is incubated, then 760 DEG C, insulation are warming up to the speed of 10 DEG C/min 20min, then 300 DEG C are cooled to the speed of 5 DEG C/min, cooling to room temperature with the furnace again afterwards, blow-on is taken out and is by weldering connector Can.
As a result:The jointing that soldering is obtained is formed well, and metallographic observation finds that brazing area forms the interface cohesion of densification, Alloying component is evenly distributed, and room temperature shear strength is 161MPa.
Embodiment 2
The composition and mass percent of solder are matched:Cu:23.0%, In15.0%, Ti4.0%, Sm0.1%, Er0.05%, balance of Ag.
The solder preparation method of a kind of above-mentioned soldering 3D printing stainless steel and aluminium oxide ceramics, comprises the following steps:
1) Ti particles, In particles, Er particles, Sm particles, the prepared mixture of Cu pieces of high-purity are weighed by mass percentage, It is put into the container added with acetone, 15~20min of ultrasonic cleaning is carried out at a temperature of 20 DEG C or so;
2) mixture after step 1 is cleaned by ultrasonic is dried at a temperature of 30~50 DEG C, obtains dry mixture;
3) mixture and Ag will be prepared using the uniform solder foundry alloy of method prepared composition of vacuum induction melting Foundry alloy pulverize after, load high vacuum single roller strip machine quartz glass tube in;
4) quartz glass tube is installed in getting rid of the electrical induction circle with machine, and its nozzle to copper roller surface spacing is adjusted Whole is 150~200 μm;
5) fire door is closed, 1.5 × 10 is evacuated to using mechanical pump-3Pa, then using molecular pump pumping high vacuum, high vacuum Degree is not less than 9 × 10-5Pa, then cavity is full of high-purity Ar gas to 200~230mbar;
6) motor is opened, is made in the range of 28~33m/s of copper roller rotating speed, high frequency electric source is then turned on, by quartz glass tube Foundry alloy high-frequency induction heating to substantially uniformity melting after, insulation superheated melt 60s~80s;
7) Ar gas air pressure is modulated into P=50KPa, the superheated melt in quartz glass is continuously ejected into height with high pressure argon gas The cooling copper roller surface of speed rotation, liquid metal formed foil shape by chilling, and so as to obtain solder foil strip, thickness is 50~ 100μm。
The soldering processes of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics, comprise the following steps:
1) preparatory stage:Aluminium oxide ceramics to be brazed and the stainless steel curved beam end face of 3D printing are cleared up, table is removed The impurity in face, greasy dirt and oxide-film, be ground with abrasive paper for metallograph it is smooth, by aluminium oxide ceramics and 3D printing stainless steel and pricker Material paillon foil is placed in acetone together, and 15~20min is cleaned using ultrasonic wave, and carries out drying and processing, and period is paid special attention to prevent The oxidation of solder element;
2) assembling stage:By the solder paillon foil after cleaning be placed in aluminium oxide ceramics and 3D printing stainless steel welding surface it Between, and be close to be assemblied in special brazing jig, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce The constant perpendicular pressure of 0.04~0.06MPa;
3) the soldering connection stage:The fixture that will be assembled is integrally placed at vacuum and is not less than 1.5 × 10-5The soldering oven of Pa In, 500 DEG C are warming up to the speed of 15 DEG C/min, 30min is incubated, then 760 DEG C, insulation are warming up to the speed of 10 DEG C/min 20min, then 300 DEG C are cooled to the speed of 5 DEG C/min, cooling to room temperature with the furnace again afterwards, blow-on is taken out and is by weldering connector Can.
As a result:The jointing that soldering is obtained is formed well, and metallographic observation finds that brazing area forms the interface cohesion of densification, Alloying component is evenly distributed, and room temperature shear strength is 166MPa.
Embodiment 3
The composition and mass percent of solder are matched:Cu:22.7%, In14.5%, Ti3.6%, Sm0.05%, Er0.05%, balance of Ag.
The solder preparation method of a kind of above-mentioned soldering 3D printing stainless steel and aluminium oxide ceramics, comprises the following steps:
1) Ti particles, In particles, Er particles, Sm particles, the prepared mixture of Cu pieces of high-purity are weighed by mass percentage, It is put into the container added with acetone, 15~20min of ultrasonic cleaning is carried out at a temperature of 20 DEG C or so;
2) mixture after step 1 is cleaned by ultrasonic is dried at a temperature of 30~50 DEG C, obtains dry mixture;
3) mixture and Ag will be prepared using the uniform solder foundry alloy of method prepared composition of vacuum induction melting Foundry alloy pulverize after, load high vacuum single roller strip machine quartz glass tube in;
4) quartz glass tube is installed in getting rid of the electrical induction circle with machine, and its nozzle to copper roller surface spacing is adjusted Whole is 150~200 μm;
5) fire door is closed, 1.5 × 10 is evacuated to using mechanical pump-3Pa, then using molecular pump pumping high vacuum, high vacuum Degree is not less than 9 × 10-5Pa, then cavity is full of high-purity Ar gas to 200~230mbar;
6) motor is opened, is made in the range of 28~33m/s of copper roller rotating speed, high frequency electric source is then turned on, by quartz glass tube Foundry alloy high-frequency induction heating to substantially uniformity melting after, insulation superheated melt 60s~80s;
7) by Ar gas air pressure modulation P=50KPa or so, the superheated melt in quartz glass is continuously sprayed with high pressure argon gas To the cooling copper roller surface of high speed rotation, liquid metal formed foil shape by chilling, and so as to obtain solder foil strip, thickness is 50~100 μm.
The soldering processes of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics, comprise the following steps:
1) preparatory stage:Aluminium oxide ceramics to be brazed and the stainless steel curved beam end face of 3D printing are cleared up, table is removed The impurity in face, greasy dirt and oxide-film, be ground with abrasive paper for metallograph it is smooth, by aluminium oxide ceramics and 3D printing stainless steel and pricker Material paillon foil is placed in acetone together, and 15~20min is cleaned using ultrasonic wave, and carries out drying and processing, and period is paid special attention to prevent The oxidation of solder element;
2) assembling stage:By the solder paillon foil after cleaning be placed in aluminium oxide ceramics and 3D printing stainless steel welding surface it Between, and be close to be assemblied in special brazing jig, it is ensured that the precision of connection, the pressure head of nominal-mass is placed on fixture, produce The constant perpendicular pressure of 0.04~0.06MPa;
3) the soldering connection stage:The fixture that will be assembled is integrally placed at vacuum and is not less than 1.5 × 10-5The soldering oven of Pa In, 500 DEG C are warming up to the speed of 15 DEG C/min, 30min is incubated, then 760 DEG C, insulation are warming up to the speed of 10 DEG C/min 20min, then 300 DEG C are cooled to the speed of 5 DEG C/min, cooling to room temperature with the furnace again afterwards, blow-on is taken out and is by weldering connector Can.
As a result:The jointing that soldering is obtained is formed well, and metallographic observation finds that brazing area forms the interface cohesion of densification, Alloying component is evenly distributed, and room temperature shear strength is 178MPa.
Embodiment 4
5 groups of comparative examples are designed, basic step is same as Example 3, difference is different material content, specially:
The constituent content of comparative example 1:Cu22.5%, In17.0%, Ti3.5%, Sm0.05%, Er0.05%, it is balance of Ag。
The constituent content of comparative example 2:Cu22.7%, In14.5%, Ti3.6%, Sm0.1%, Er0.1%, balance of Ag.
The constituent content of comparative example 3:Cu22.7%, In14.5%, Ti3.6%, Sm0.2%, Er0.1%, balance of Ag.
The constituent content of comparative example 4:Cu22.5%, In17.0%, Ti3.5%, Er0.05%, balance of Ag.
The constituent content of comparative example 5:Cu22.5%, In17.0%, Ti3.5%, Sm0.05%, balance of Ag.
Welding point obtained in embodiment 1-4 is carried out into performance detection, the result of the test of acquisition is as shown in table 1.
Table 1
As shown in Table 1, soldered fitting dense micro-structure obtained in embodiment 1-3, is uniformly distributed, and linkage interface is obvious, Shear strength is between 161~178MPa, it can thus be appreciated that the solder tool of soldering 3D printing stainless steel of the present invention and aluminium oxide ceramics Standby good adhesive force and wettability, and soldered fitting bond strength is high.
Contrast test 1 shows that although element In advantageously reduces brazing filler metal melts temperature, but excessive In can produce catalysis Shearing strength of joint is mutually caused to decline.Contrast test 2 shows, after rare earth element Sm reaches certain value, is further added by Er and contains well Amount can cause the wetability of solder to decline, and excessive rare earth can aoxidize slagging, hinder the wetting of solder.Contrast test 3 shows, dilute Earth elements can not be added excessively, and Sm contents may not exceed 0.1%, and excessive rare earth can increase the viscosity of solder, and wetability is serious Decline, joint performance is also remarkably decreased;Contrast test 4 shows:Rare earth element er is only added, without rare earth element Sm, joint Performance is decreased obviously compared with embodiment 3, and rare-earth Sm plays the role of stronger improvement solder wetting, lacks the wetting action of Sm, boundary Face compound growth is uneven, causes joint performance to decline;Contrast test 5 shows:Rare earth element Sm is only added, without rare earth Element Er, joint performance is decreased obviously compared with embodiment 3, and rare earth Er atomic radius is larger, can prevent the segregation of element, and other Rare earth element is combined together the fusing point that can further reduce solder, while improve the wetability of solder, so lacking rare earth Element Er, the segregation of solder is difficult to control to, and joint performance declines.
The above is only the preferred embodiment of the present invention, it should be pointed out that:For the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (8)

1. the solder of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics, it is characterised in that:The solder is with percentage by weight The elemental composition of meter includes:Cu20.0%~25.0%, In13.0%~16.0%, Ti2.0%~5.0%, Sm0.02%~ 0.2%, Er0.01%~0.1%, balance of Ag.
2. the solder of soldering 3D printing stainless steel according to claim 1 and aluminium oxide ceramics, it is characterised in that:The pricker Material elemental composition by weight percentage includes:Cu21.5%~23.5%, In13.5%~15.0%, Ti2.5%~ 4.0%, Sm0.05%~0.1%, Er0.01%~0.05%, balance of Ag.
3. the solder of soldering 3D printing stainless steel according to claim 2 and aluminium oxide ceramics, it is characterised in that:The pricker Material elemental composition by weight percentage includes:Cu22.7%, In14.5%, Ti3.6%, Sm0.05%, Er0.05%, it is remaining It is Ag to measure.
4. the solder of soldering 3D printing stainless steel according to claim 1 and aluminium oxide ceramics, it is characterised in that:The pricker Expect to be paillon foil banding, thickness is 50~100 μm.
5. the solder preparation side of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics as described in any one of Claims 1-4 Method, it is characterised in that comprise the following steps:
1) Ti particles, In particles, Er particles, Sm particles, the prepared mixture of Cu pieces of high-purity are weighed by mass percentage, are put into In container added with acetone, 15~20min of ultrasonic cleaning is carried out at a temperature of 15-25 DEG C;
2) mixture after step 1 is cleaned by ultrasonic is dried at a temperature of 30~50 DEG C, obtains dry mixture;
3) mixture and Ag are used the uniform solder foundry alloy of method prepared composition of vacuum induction melting, the mother that will be prepared After alloy pulverizes, load in the quartz glass tube of high vacuum single roller strip machine;
4) quartz glass tube is installed in getting rid of the electrical induction circle with machine, and its nozzle to copper roller surface spacing is adjusted to 150~200 μm;
5) fire door is closed, 1.5 × 10 is evacuated to using mechanical pump-3Pa, then using molecular pump pumping high vacuum, condition of high vacuum degree is not Less than 9 × 10-5Pa, then cavity is full of high-purity Ar gas to 200~230mbar;
6) motor is opened, is made in the range of 28~33m/s of copper roller rotating speed, high frequency electric source is then turned on, by the mother in quartz glass tube After alloy high-frequency induction heating is melted to substantially uniformity, insulation superheated melt 60s~80s;
7) Ar gas air pressure is modulated into P=50KPa, the superheated melt in quartz glass is continuously ejected into rotation at a high speed with high pressure argon gas The cooling copper roller surface for turning, liquid metal is formed foil shape by chilling, and so as to obtain solder foil strip, thickness is 50~100 μ m。
6. the solder preparation method of soldering 3D printing stainless steel according to claim 5 and aluminium oxide ceramics, its feature exists In:The step 4) in nozzle be rectangle, its length be 8~10mm, width be 0.8~1.2mm.
7. the solder preparation method of soldering 3D printing stainless steel according to claim 5 and aluminium oxide ceramics, its feature exists In:The step 6) in copper roller diameter be 250mm, copper roller width be 50mm.
8. the method for welding of a kind of soldering 3D printing stainless steel and aluminium oxide ceramics as described in claim any one of 1-4, its It is characterised by, comprises the following steps:
1) preparatory stage:Aluminium oxide ceramics to be brazed and the stainless steel curved beam end face of 3D printing are cleared up, surface is removed Impurity, greasy dirt and oxide-film, be ground with abrasive paper for metallograph it is smooth, by aluminium oxide ceramics and 3D printing stainless steel and solder paper tinsel Piece is placed in acetone together, and 15~20min is cleaned using ultrasonic wave, and carries out drying and processing, and period is paid special attention to prevent solder The oxidation of element;
2) assembling stage:Solder paillon foil after cleaning is placed between aluminium oxide ceramics and 3D printing stainless steel welding surface, and It is close to be assemblied in special brazing jig, it is ensured that the precision of connection, the pressure head of placement nominal-mass on fixture, generation 0.04~ The constant perpendicular pressure of 0.06MPa;
3) the soldering connection stage:The fixture that will be assembled is integrally placed at vacuum and is not less than 1.5 × 10-5In the soldering oven of Pa, with The speed of 15 DEG C/min is warming up to 500 DEG C, is incubated 30min, then is warming up to 760 DEG C with the speed of 10 DEG C/min, is incubated 20min, 300 DEG C are cooled to the speed of 5 DEG C/min again, room temperature is cooled to the furnace again afterwards, blow-on is taken out by weldering connector.
CN201611252454.3A 2016-12-30 2016-12-30 The solder and preparation and method for welding of soldering 3D printing stainless steel and aluminium oxide ceramics Pending CN106736034A (en)

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CN108161274A (en) * 2017-11-24 2018-06-15 北京有色金属与稀土应用研究所 It is a kind of for sealing-in solder of electron tube and preparation method thereof
CN112372179A (en) * 2020-10-29 2021-02-19 西北工业大学 Alloy solder for connecting stainless steel and carbon/carbon composite material and preparation and use method thereof
CN114749750A (en) * 2021-12-31 2022-07-15 上海工程技术大学 Forming control method for brazing joint of 3D printed product

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CN114749750A (en) * 2021-12-31 2022-07-15 上海工程技术大学 Forming control method for brazing joint of 3D printed product

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