CN105948778A - Preparation method of active sealing material of alumina ceramic and metal - Google Patents
Preparation method of active sealing material of alumina ceramic and metal Download PDFInfo
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- CN105948778A CN105948778A CN201610259627.8A CN201610259627A CN105948778A CN 105948778 A CN105948778 A CN 105948778A CN 201610259627 A CN201610259627 A CN 201610259627A CN 105948778 A CN105948778 A CN 105948778A
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- metal
- aluminium oxide
- solder
- oxide ceramics
- sealing materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
- C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/125—Metallic interlayers based on noble metals, e.g. silver
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/40—Metallic
- C04B2237/408—Noble metals, e.g. palladium, platina or silver
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a preparation method of active sealing material of alumina ceramic and metal. The method includes performing purification by vacuum electron beam melting of four elementary substances which are Ni, Mo, V, and Au, preparing solder mother alloy by using electric arc melting or induction melting, repeating the melting for 2-3 times, performing oxygen-free copper vacuum packaging of the solder mother alloy, performing hot rolling cogging, removing the sheath, performing cold rolling and annealing to obtain a solder foil, performing assembling according to the form of aluminium oxide, ceramic, solder sheet, and metal from top to bottom in order, and processing the assembled workpieces under a certain conditions to prepare the active sealing material of alumina ceramic and metal. The sealing material has good sealing manufacturability and high joint strength, and is not easy to crack.
Description
Technical field:
The present invention relates to dissimilar materials interconnection technique field, be specifically related to a kind of aluminium oxide ceramics and metal active sealing-in
The preparation method of material.
Background technology:
New Times flies step to the mankind, will bring fundamental change to human society each side, certainly, to pottery-gold
Belonging to this field of sealing technology and also will have new promotion and demand, we both faced new challenges, and there is also and met head on
The opportunity caught up with.
Material is one of three big pillars of modern civilization, and material is all classified as 21 century and preferentially sends out by developed country of the world today
One of key area of exhibition.Along with science and technology development, the most all kinds of relatively independent materials such as metal, pottery,
Macromolecules etc., even to this day, interpenetrate, be combined with each other and multi-crossed disciplines, Ceramic-to-metal seal technology along with
Multi-disciplinary intersection and double to grow up, it is the expression in the eyes of materials application, be a manufacturability and practicality the strongest
Basic technology.
Aluminium oxide ceramics, with Al2O3 as principal crystalline phase, comprises the one pack system pottery of a small amount of glass phase and other crystalline phase, in it
There is substantial amounts of pore in portion, compactness extent is more far short of what is expected than metal, so tensile strength is relatively low.But because pore is at pressurized
Time be not result in cracks can spread, so comprcssive strength still compare the highest, about 10 times of tensile strength, tensile strength
Being about about the 1/2 of rupture strength, its hardness is high, elastic modelling quantity is big.Can not consider to glue under the conditions of general technology
Remain in a standstill dynamic and plastic creep.Al2O3 is typical fragile material, can occur when applied load exceedes its permissible value suddenly
Fracture, the intensity of pottery has the biggest dispersibility simultaneously, and it is distributed Follow Weibull Distribution.95% aluminium oxide ceramics
It is widely used in electronics, machinery, chemical industry and high-tech area, particularly power system and uses 95% aluminium oxide ceramics in a large number
Make the structural material of vacuum switch tube shell.
Aluminium oxide ceramics-metal sealing is the critical process in vacuum electron device, the sealing-in matter of aluminium oxide ceramics-metal
Measure very big on the impact of device and the performance of complete machine and reliability.Along with the development of science and technology, to being applied to various electricity
The performance requirement of the aluminium oxide ceramics in sub-device-metal sealing parts is more and more higher.Usual intact aluminium oxide pottery
Porcelain-metal sealing part must be vacuum tight, meanwhile, has certain mechanical strength, the therefore envelope of closure again
Connect intensity as one of important indicator checking aluminium oxide ceramics-metal sealing quality.
Summary of the invention:
It is an object of the invention to provide the preparation method of a kind of aluminium oxide ceramics and metal active seal, sealing materials, the party's legal system
Standby aluminium oxide ceramics and metal active seal, sealing materials, strength of joint is big, and the most easy to crack, process for sealing is good.
For achieving the above object, the present invention is by the following technical solutions:
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) percentage by weight being respectively Ni 10-22wt%, Mo 0-5.0wt%, V 0.1-10wt%, remaining is Au
Four kinds of simple substance carry out vacuum electron beam melting purification, the metal simple-substance purity after purification reaches 99.999%, gas content
Less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, hot rolling cogging, remove jacket, cold rolling, annealing, system
For obtaining solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 5-10min, is heated to the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again
1100-1200 DEG C, it is incubated 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature,
Obtain aluminium oxide ceramics and metal active closure.
Preferred as technique scheme, in step (1), the percentage by weight of Ni is the weight of 13-22wt%, Mo
Amount percentage ratio be 0.1-5.0wt%, V percentage by weight be 0.5-10wt%, surplus is Au.
Preferred as technique scheme, in step (3), the fusing point of described solder foil is 930-990 DEG C, weldering
Jointing temp is 980-1200 DEG C.
Preferred as technique scheme, in step (3), described solder foil saturated vapor pressure at 1000 DEG C
Less than 1.26 × 10-6Torr。
Preferred as technique scheme, in step (3), the temperature of described annealing is 500 DEG C, and annealing time is
1h。
The method have the advantages that
The aluminium oxide ceramics that the present invention prepares and metal sealing material solder are contained within active component V, it is possible to achieve directly seal
Connect;And high than on market of the fusing point of solder, and high temperature saturated vapor pressure is relatively low;The solder paper tinsel that the present invention prepares
Material composition is uniform, and activity is high, and the strength of joint of the seal, sealing materials prepared is big, the most easy to crack, and process for sealing is good.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, further instruction of the present invention, embodiment are served only for
Explain the present invention, the present invention will not be constituted any restriction.
Embodiment 1
Solder composition and percentage by weight be: Ni 13wt%, Mo 0.1wt%, V 0.5wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance is carried out vacuum electron beam melting purification, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 400 DEG C, is incubated 40min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 5min, is heated to 1100 DEG C with the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again,
Insulation 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain aluminium oxide ceramics
With metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Embodiment 2
Solder composition and percentage by weight be: Ni 22wt%, Mo 5.0wt%, V 10wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance carries out vacuum electric philosophical works melting purify, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 430 DEG C, is incubated 50min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 10min, is heated to the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again
1200 DEG C, it is incubated 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain oxygen
Change aluminum pottery and metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Embodiment 3
Solder composition and percentage by weight be: Ni 14wt%, Mo 1wt%, V 2.5wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance carries out vacuum electric philosophical works melting purify, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 410 DEG C, is incubated 45min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 6min, is heated to 1150 DEG C with the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again,
Insulation 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain aluminium oxide ceramics
With metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Embodiment 4
Solder composition and percentage by weight be: Ni 16wt%, Mo 2wt%, V 4.5wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance carries out vacuum electric philosophical works melting purify, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 415 DEG C, is incubated 45min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 7min, is heated to 1100 DEG C with the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again,
Insulation 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain aluminium oxide ceramics
With metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Embodiment 5
Solder composition and percentage by weight be: Ni 18wt%, Mo 3wt%, V 6.5wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance carries out vacuum electric philosophical works melting purify, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 420 DEG C, is incubated 45min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 8min, is heated to 1150 DEG C with the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again,
Insulation 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain aluminium oxide ceramics
With metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Embodiment 6
Solder composition and percentage by weight be: Ni 20wt%, Mo 4wt%, V 8.5wt%, remaining is Au.
A kind of aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, comprise the following steps:
(1) Au, Ni, Mo, V these four simple substance carries out vacuum electric philosophical works melting purify, the metal simple-substance after purification
Purity reaches 99.999%, and gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy, melt back 2-3
Secondary, obtain solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, now use electron beam welding technology to realize anaerobic copper-clad
The vacuum of set seals, and the foundry alloy of jacket is heated to 425 DEG C, is incubated 50min, takes out and carries out rolling process, removes
Jacket, cold rolling, annealing, prepare solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, the oxygen that surface is clean is obtained
Change aluminum pottery and metal;
(5) solder foil tabletting step (3) obtained, is processed into the solder sheet equal with by weldering surface area,
Then aluminium oxide ceramics and metal after cleaning step (4) obtained are put in acetone, carry out ultrasonic cleaning
15-20min, then after natural air drying, according to being followed successively by aluminium oxide ceramics, solder sheet, the form of metal from top to bottom
Assemble, and ceramic surface apply 3-5MPa pressure be fixed, the workpiece assembled is put into heating in vacuum
In stove;
(6) vacuum drying oven of step (5) is carried out evacuation, starts to be heated to 500 DEG C with the speed of 17 DEG C/min,
Insulation 9min, is heated to 1200 DEG C with the speed of 8 DEG C/min after being then heated to 1000 DEG C with the speed of 12 DEG C/min again,
Insulation 8min, is then cooled to 400 DEG C with the speed of 10 DEG C/min, is then cooled to room temperature, obtain aluminium oxide ceramics
With metal active seal, sealing materials.
This aluminium oxide ceramics is less than 1.0 × 10 with the weld seam helium mass spectrum leak rate of metal active seal, sealing materials-11Pa·m3/s。
Claims (5)
1. an aluminium oxide ceramics and the preparation method of metal active seal, sealing materials, it is characterised in that bag
Include following steps:
(1) percentage by weight is respectively Ni 10-22wt%, Mo 0-5.0wt%, V 0.1-10wt%,
Remaining four kinds of simple substance being Au carries out vacuum electron beam melting purification, and the metal simple-substance purity after purification reaches
To 99.999%, gas content is less than 5ppm;
(2) metal simple-substance after purifying uses electric arc melting or induction melting to prepare solder foundry alloy,
Melt back 2-3 time, obtains solder foundry alloy;
(3) solder foundry alloy is carried out oxygen-free copper vacuum packaging, hot rolling cogging, remove jacket, cold rolling,
Annealing, prepares solder foil;
(4) by aluminium oxide ceramics and the greasy dirt of metal surface, oxide ultrasonic waves for cleaning, table is obtained
Aluminium oxide ceramics that face is clean and metal;
(5) solder foil tabletting step (3) obtained, is processed into equal with by weldering surface area
Solder sheet, aluminium oxide ceramics and metal after the cleaning then step (4) obtained are put in acetone,
Carry out ultrasonic cleaning 15-20min, then after natural air drying, according to being followed successively by aluminium oxide pottery from top to bottom
Porcelain, solder sheet, the form of metal are assembled, and ceramic surface apply 3-5MPa pressure carry out
Fixing, the workpiece assembled is put in vacuum furnace;
(6) vacuum drying oven of step (5) is carried out evacuation, start to heat with the speed of 17 DEG C/min
To 500 DEG C, it is incubated 5-10min, again with 8 DEG C after being then heated to 1000 DEG C with the speed of 12 DEG C/min
The speed of/min is heated to 1100-1200 DEG C, is incubated 8min, then lowers the temperature with the speed of 10 DEG C/min
To 400 DEG C, it is then cooled to room temperature, obtains aluminium oxide ceramics and metal active closure.
A kind of aluminium oxide ceramics the most as claimed in claim 1 and the preparation side of metal active seal, sealing materials
Method, it is characterised in that in step (1), the percentage by weight of Ni is the weight of 13-22wt%, Mo
Percentage ratio be 0.1-5.0wt%, V percentage by weight be 0.5-10wt%, surplus is Au.
A kind of aluminium oxide ceramics the most as claimed in claim 1 and the preparation side of metal active seal, sealing materials
Method, it is characterised in that in step (3), the fusing point of described solder foil is 930-990 DEG C, welding
Temperature is 980-1200 DEG C.
A kind of aluminium oxide ceramics the most as claimed in claim 1 and the preparation side of metal active seal, sealing materials
Method, it is characterised in that in step (3), described solder foil saturated vapor pressure at 1000 DEG C is little
In 1.26 × 10-6Torr。
A kind of aluminium oxide ceramics the most as claimed in claim 1 and the preparation side of metal active seal, sealing materials
Method, it is characterised in that in step (3), the temperature of described annealing is 500 DEG C, and annealing time is 1h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108422058A (en) * | 2018-05-04 | 2018-08-21 | 中国航发北京航空材料研究院 | For Al2O3The auri solder and its welding method of Ceramic and metal joining |
CN108732708A (en) * | 2017-04-15 | 2018-11-02 | 西南技术物理研究所 | The airtight connection of opto-electronic device transparent optical window |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104973879A (en) * | 2015-07-15 | 2015-10-14 | 哈尔滨工业大学(威海) | Method for jointing Al2O3 ceramic and ceramic sealing alloy |
CN105436743A (en) * | 2015-12-28 | 2016-03-30 | 北京有色金属研究总院 | High-melting-point active brazing filler metal with low saturated vapor pressure and preparation method of brazing filler metal |
-
2016
- 2016-04-25 CN CN201610259627.8A patent/CN105948778A/en not_active Withdrawn
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104973879A (en) * | 2015-07-15 | 2015-10-14 | 哈尔滨工业大学(威海) | Method for jointing Al2O3 ceramic and ceramic sealing alloy |
CN105436743A (en) * | 2015-12-28 | 2016-03-30 | 北京有色金属研究总院 | High-melting-point active brazing filler metal with low saturated vapor pressure and preparation method of brazing filler metal |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108732708A (en) * | 2017-04-15 | 2018-11-02 | 西南技术物理研究所 | The airtight connection of opto-electronic device transparent optical window |
CN108422058A (en) * | 2018-05-04 | 2018-08-21 | 中国航发北京航空材料研究院 | For Al2O3The auri solder and its welding method of Ceramic and metal joining |
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Application publication date: 20160921 |