CN106862695B - The soldering method for sealing of aluminum oxide ceramic substrate and Ti ring based on artificial retina implant devices - Google Patents
The soldering method for sealing of aluminum oxide ceramic substrate and Ti ring based on artificial retina implant devices Download PDFInfo
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- CN106862695B CN106862695B CN201710253199.2A CN201710253199A CN106862695B CN 106862695 B CN106862695 B CN 106862695B CN 201710253199 A CN201710253199 A CN 201710253199A CN 106862695 B CN106862695 B CN 106862695B
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- 210000001525 retina Anatomy 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007943 implant Substances 0.000 title claims abstract description 29
- 239000000758 substrate Substances 0.000 title claims abstract description 29
- 238000007789 sealing Methods 0.000 title claims abstract description 16
- 238000005476 soldering Methods 0.000 title claims description 16
- 239000011224 oxide ceramic Substances 0.000 title abstract description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 title abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 213
- 229910052751 metal Inorganic materials 0.000 claims abstract description 213
- 238000004140 cleaning Methods 0.000 claims abstract description 122
- 229910000679 solder Inorganic materials 0.000 claims abstract description 85
- 239000000919 ceramic Substances 0.000 claims abstract description 67
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 64
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 64
- 229910015365 Au—Si Inorganic materials 0.000 claims abstract description 56
- 238000003466 welding Methods 0.000 claims abstract description 18
- 238000001465 metallisation Methods 0.000 claims abstract description 16
- 238000005219 brazing Methods 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 223
- 229910052786 argon Inorganic materials 0.000 claims description 145
- 238000000151 deposition Methods 0.000 claims description 95
- 239000007789 gas Substances 0.000 claims description 83
- 230000008021 deposition Effects 0.000 claims description 66
- 239000012300 argon atmosphere Substances 0.000 claims description 39
- 239000010931 gold Substances 0.000 claims description 35
- 238000005477 sputtering target Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000002000 scavenging effect Effects 0.000 claims description 8
- 238000004080 punching Methods 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- 229910010380 TiNi Inorganic materials 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 2
- -1 Argon ion Chemical class 0.000 description 49
- 150000002500 ions Chemical class 0.000 description 39
- 238000005240 physical vapour deposition Methods 0.000 description 10
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 229910004337 Ti-Ni Inorganic materials 0.000 description 4
- 229910011209 Ti—Ni Inorganic materials 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 239000012620 biological material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
Classifications
-
- 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
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
- B23K1/206—Cleaning
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
-
- 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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/16—Composite materials, e.g. fibre reinforced
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Aluminum oxide ceramic substrate and metal Ti ring based on artificial retina implant devices are brazed method for sealing, it belongs to welding technology field, and in particular to the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed method for sealing.Al is realized when the invention aims to solve existing vacuum brazing2O3Ceramics are connect using TiNi solder with metal Ti ring, and damage, and the higher problem of welding temperature can be generated to human body.Method for sealing: one, solder piece is prepared；Two, Al after metal Ti ring, cleaning after being cleaned2O3Au-Si solder after potsherd and cleaning；Three, Al2O3Ceramic surface metallization；Four, metal Ti ring surface metallizes；Five, the Al of artificial retina implant devices is completed in sealing-in2O3Ceramic substrate and metal Ti ring are brazed sealing-in.Present invention is mainly used for the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed sealing-in.
Description
Technical field
The invention belongs to welding technology fields, and in particular to the Al based on artificial retina implant devices2O3Ceramic substrate with
Metal Ti ring is brazed method for sealing.
Background technique
In artificial retina structure, Al2O3Ceramics and the connection of metal Ti ring not only to meet certain bonding strength and
Air-tightness, but also to make entire jointing that there is biocompatibility, i.e., it must not contain in the structure of entire artificial retina
There is the ingredient being harmful to the human body.And the prior art is unable to satisfy Al in artificial retina structure2O3The company of ceramics and metal Ti ring
It connects.
Al2O3Ceramics have excellent bio-compatibility with metal Ti, capture importantly in technical field of biological material
Position.Currently, realizing Al2O3The method that ceramics are connect with metal Ti mainly has diffusion welding (DW), soldering etc., and wherein method for brazing is to study most
Mostly most widely used connection method.Due to Al2O3Ceramic surface is more difficult to be soaked by active metallic soldering material, in order to realize Al2O3Pottery
The connection of porcelain and metal Ti, needs to Al2O3Ceramic surface carries out metalized.Al is realized at present2O3Ceramics are with metal Ti's
Soldering connection mode realizes connection at a higher temperature.
In a kind of Chinese publication " Al in artificial retina2O3Ceramics are brazed method for sealing with Ti ring " (Shen Qing Publication
Number: being disclosed in CN105598542A) using vacuum brazing is to realize Al2O3Ceramics are connect with metal Ti ring, which uses TiNi
Solder, since Ni does not have biocompatibility in TiNi solder, the retina device connected using TiNi solder is in implantation human body
Afterwards, damage can be generated to human body；And the brazing temperature of the patent is 990 DEG C~1450 DEG C, however it remains welding temperature is higher
The problem of.
Summary of the invention
It is to realize Al that the object of the invention, which will solve existing vacuum brazing,2O3Ceramics are connect in the presence of using TiNi with metal Ti ring
Solder can generate damage, and the higher problem of welding temperature to human body, and provide the Al based on artificial retina implant devices2O3
Ceramic substrate and metal Ti ring are brazed method for sealing.
Al based on artificial retina implant devices2O3The soldering method for sealing of ceramic substrate and Ti ring, specifically by following
What step was completed:
One, prepare solder piece: according to metal Ti ring size, by Au-Si solder piece punching at metal Ti ring size phase
The Au-Si solder ring matched；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, in temperature
Degree is cleaned by ultrasonic 7min~12min, Al after metal Ti ring, cleaning after successively being cleaned under conditions of being 25~35 DEG C2O3Ceramics
Au-Si solder after piece and cleaning；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in physical vapour deposition (PVD) and sets
On standby sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, simultaneously will
Vacuum furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, and adjusting its flow is 150sccm~220sccm, while by pulse voltage
Be set as -850V~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow are
Argon ion cleans 10min~15min under the conditions of 150sccm~220sccm and pulse voltage are -850V~-950V, obtain argon from
Al after son cleaning2O3Potsherd；2., after argon ion cleaning, with striking needle in the surface striking of Ti target, and continue temperature be 350~
400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 150sccm~220sccm and pulse voltage be -850V~-
It is cleaned again under the conditions of 950V using Ti ion, scavenging period is 10min~15min, obtains Al after Ti Ion Cleaning2O3Ceramics
Piece；3., after Ti ion, adjust the gas flow of argon gas, pressure made to remain 0.5 × 10-1Pa~1.5 × 10-1Pa, will
Al after Ti Ion Cleaning2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd is 8cm at a distance from sputtering target
~12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV
Under negative high voltage, in 60min~120min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition thickness is 0.1 μm~0.5 μm
Ti layers of metal, obtain depositing Ti layer Al2O3Potsherd；4., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10- 1Pa is 350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV in temperature, in 60min~120min, is depositing
Ti layers of Al2O3Mo layers of metal that a layer thickness is 2 μm~4 μm are deposited on Ti layers of metal of potsherd, obtain Mo layers/Ti of deposition
Layer Al2O3Potsherd；5., convert target again, continue keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa is in temperature
350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3
A layer thickness is deposited on Mo layers of metal of potsherd as 0.1 μm~0.5 μm of Au layer, after deposition, closes power supply and argon
Air cock closes vacuum system when the temperature of vacuum chamber is down to 80~120 DEG C, is filled with filtered pure air and extremely opens the door,
Sampling, Al after being metallized2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in Pvd equipment
On sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum
Furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, and adjusting its flow is 150~220sccm, while setting pulse voltage to-
850~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 150sccm~
Argon ion cleans 10min~15min under the conditions of 220sccm and pulse voltage are -850V~-950V, after obtaining argon ion cleaning
Metal Ti ring；2., argon ion cleaning after, the flow of argon gas is adjusted, so that pressure remains 0.5 × 10-1Pa~1.5 ×
10-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, metal Ti ring is at a distance from sputtering target after argon ion cleaning
8cm~12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, metal Ti ring surface deposition thickness is 2 μm~4 μm of gold after argon ion cleaning
Belong to Mo layers, obtains Mo layers of metal Ti ring of deposition；3., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa,
Temperature is 350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV, in 30min~60min, is depositing Mo layers of metal
The Au layer that a layer thickness is 0.1 μm~0.5 μm is deposited on Mo layers of metal of Ti ring, obtains Au layers/Mo layers metal Ti ring of deposition,
After deposition, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, vacuum system is closed, is filled with
Filtered pure air samples, metal Ti ring after being metallized to opening the door；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3Potsherd and metallization after metal Ti ring it
Between, welding equipment part to be welded is formed, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 1.50 × 10-5Pa~
2.50×10-5After Pa, being heated to temperature in the case where heating speed is 8 DEG C/min~12 DEG C/min is 390~420 DEG C, and in temperature
Degree is keeps the temperature 3min~5min at 390~420 DEG C, then controlling cooling velocity is that 5 DEG C/min~10 DEG C/min is cooled to temperature and is
It 80~120 DEG C, then cools to room temperature with the furnace, that is, completes the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring
It is brazed sealing-in.
The present invention realizes Al using Au-Si solder2O3The connection of ceramics and metal Ti ring, in order to improve the company of jointing
Intensity is connect to reach the requirement of retina device, in Al2O3Ceramics and the side in the surface to be welded of metal Ti ring by magnetron sputtering
Formula depositing metallization, in Al2O3Ceramic surface deposit layer and with its metal Ti with preferable adhesion strength, then
It is further continued on Ti layers of metal and metal Ti ring magnetron sputtering and deposits one layer thicker with Au-Si solder there is preferable wetability
Mo layers of metal, subsequent sealing-in reaction is influenced in order to inhibit Mo layers of metal oxidation occurs before sealing-in, in the metal of deposition
The Au layer of redeposited layer on Mo layers, metal Mo layers of protection prevents its oxidation, in Al2O3Ceramics and metal Ti ring surface
After depositing metallization, with Au-Si solder composition to closure, brazing temperature is controlled between 390~420 DEG C and when heat preservation
Between 3min~5min to guarantee that soldered fitting obtains preferable microstructure and performance be successfully realized Al2O3Ceramics and metal
The sealing-in of Ti, and obtain reliable connector.
Vacuum brazing not only can guarantee that jointing has certain bonding strength and air-tightness, moreover it is possible to prevent external environment
Pollution to component.Therefore carrying out vacuum brazing using biocompatibility solder is to realize Al2O3What ceramics were connect with metal Ti ring
Effective ways.
The invention has the advantages that the one, present invention is using Au-Si solder, compared with TiNi solder used by it, Au-Si
Solder has biocompatibility, will not cause harm to the human body, and since Ni does not have biocompatibility in TiNi solder, it uses
The retina device of TiNi solder connection can generate damage to human body after being implanted into human body；Two, due to the Al of required connection2O3
Ceramic internal and surface is furnished with plain conductor, and the present invention realizes Al in 420 DEG C of temperature below using Au-Si solder2O3Ceramics with
The connection of Ti ring connects, no compared to using Ti-Ni solder to connect in 990 DEG C~1450 DEG C realizations in 400 DEG C of following implemented
It can be to Al2O3Ceramic internal and surface is furnished with plain conductor and generates damage, and the device after guaranteeing connection can work normally.Three, this hair
The connection temperature at bright place is at 420 DEG C hereinafter, 880 DEG C of phase transformation recrystallization temperature of metal Ti are far below, using TiNi solder
It connecting temperature and is higher than 900 DEG C, metal Ti ring undergoes phase transition recrystallization, after connection, and the coarse grains of metal Ti ring, serious shadow
Ring the availability of retina device.Four, the sheet Au-Si solder piece of the present invention for being, relative to using by Ti-Ni powder
Made soldering paste applies connection, and it is uniform for being able to maintain using sheet solder piece in each thickness to connecting portion solder layer,
And the layer of solder paste applied by the way of manual then cannot be guaranteed that the thickness of position to be welded solder layer is uniform.Five, the present invention exists
In Al also by the way of magnetron sputtering before connection2O3Ceramics and Ti ring surface deposited metal layer, in ceramic surface deposited metal
Ti layers can be enhanced the intensity of jointing, and can be enhanced in Mo layers of the Ti of deposition layer and metal Ti ring surface deposited metal
Improve solder in connector surface volume wetability.Six, the present invention is heavy by magnetron sputtering between Au-Si solder and metal Ti ring
Metal Mo layers of product can not only prevent Au-Si solder and metal Ti ring that overreaction occurs, and generating intermetallic compound influences to connect
The intensity of connector, and can guarantee the dimensional stability of metal Ti ring, guarantee the structure of the retina device after connection
Stablize.
Specific embodiment
Specific embodiment 1: Al of the present embodiment based on artificial retina implant devices2O3Ceramic substrate and metal Ti
Ring is brazed method for sealing, is specifically realized by the following steps:
One, solder piece is prepared: according to metal Ti ring size, by Au-Si solder piece punching at matching with metal Ti ring
Au-Si solder ring；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, in temperature
Degree is cleaned by ultrasonic 7min~12min, Al after metal Ti ring, cleaning after successively being cleaned under conditions of being 25~35 DEG C2O3Ceramics
Au-Si solder after piece and cleaning；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in physical vapour deposition (PVD) and sets
On standby sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, simultaneously will
Vacuum furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, and adjusting its flow is 150sccm~220sccm, while by pulse voltage
Be set as -850V~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow are
Argon ion cleans 10min~15min under the conditions of 150sccm~220sccm and pulse voltage are -850V~-950V, obtain argon from
Al after son cleaning2O3Potsherd；2., after argon ion cleaning, with striking needle in the surface striking of Ti target, and continue temperature be 350~
400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 150sccm~220sccm and pulse voltage be -850V~-
It is cleaned again under the conditions of 950V using Ti ion, scavenging period is 10min~15min, obtains Al after Ti Ion Cleaning2O3Ceramics
Piece；3., after Ti ion, adjust the gas flow of argon gas, pressure made to remain 0.5 × 10-1Pa~1.5 × 10-1Pa, will
Al after Ti Ion Cleaning2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd is more at a distance from sputtering target
8cm~12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition thickness is 0.2 μm~1 μm
Ti layers of metal, obtain depositing Ti layer Al2O3Potsherd；4., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10- 1Pa is 350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV in temperature, in 60min~120min, is depositing
Ti layers of Al2O3Mo layers of metal that a layer thickness is 2 μm~4 μm are deposited on Ti layers of metal of potsherd, obtain Mo layers/Ti of deposition
Layer Al2O3Potsherd；5., convert target again, continue keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa is in temperature
350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3
A layer thickness is deposited on Mo layers of metal of potsherd as 0.2 μm~1 μm of Au layer, after deposition, closes power supply and argon gas
Switch closes vacuum system when the temperature of vacuum chamber is down to 80~120 DEG C, is filled with filtered pure air to opening the door, takes
Sample, Al after being metallized2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in Pvd equipment
On sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum
Furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, and adjusting its flow is 150~220sccm, while setting pulse voltage to-
850~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 150sccm~
Argon ion cleans 10min~15min under the conditions of 220sccm and pulse voltage are -850V~-950V, after obtaining argon ion cleaning
Metal Ti ring；2., argon ion cleaning after, the flow of argon gas is adjusted, so that pressure remains 0.5 × 10-1Pa~1.5 ×
10-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, metal Ti ring is at a distance from sputtering target after argon ion cleaning
8cm~12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, metal Ti ring surface deposition thickness is 2 μm~4 μm of gold after argon ion cleaning
Belong to Mo layers, obtains Mo layers of metal Ti ring of deposition；3., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa,
Temperature is 350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV, in 30min~60min, is depositing Mo layers of metal
The Au layer that a layer thickness is 0.2 μm~1 μm is deposited on Mo layers of metal of Ti ring, is obtained Au layers/Mo layers metal Ti ring of deposition, is sunk
After product, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, vacuum system is closed, was filled with
Pure air after filter samples, metal Ti ring after being metallized to opening the door；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3Potsherd and metallization after metal Ti ring it
Between, welding equipment part to be welded is formed, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 1.50 × 10-5Pa~
2.50×10-5After Pa, being heated to temperature in the case where heating speed is 8 DEG C/min~12 DEG C/min is 390~420 DEG C, and in temperature
Degree is keeps the temperature 3min~5min at 390~420 DEG C, then controlling cooling velocity is that 5 DEG C/min~10 DEG C/min is cooled to temperature and is
It 80~120 DEG C, then cools to room temperature with the furnace, that is, completes the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring
It is brazed sealing-in.
With a kind of Chinese publication " Al in artificial retina2O3Ceramics are brazed method for sealing with Ti ring " (Shen Qing Publication
Number: it CN105598542A) compares, the advantage of present embodiment essentially consists in the following aspects
Present embodiment is using Au-Si solder, and compared with TiNi solder used by it, Au-Si solder has life
Object compatibility will not cause harm to the human body, and be connected since Ni does not have biocompatibility using TiNi solder in TiNi solder
The retina device connect can generate damage to human body after being implanted into human body.
Due to the Al of required connection2O3Ceramic internal and surface is furnished with plain conductor, and present embodiment uses Au-Si pricker
Material realizes Al in 420 DEG C of temperature below2O3Ceramics and the connection of Ti ring, compared to use Ti-Ni solder 990 DEG C~1450
It DEG C realizes connection, is connected in 400 DEG C of following implemented, it will not be to Al2O3Ceramic internal and surface is furnished with plain conductor and generates damage,
Device after guaranteeing connection can work normally.
Connection temperature where present embodiment is at 420 DEG C hereinafter, being far below the phase transformation recrystallization temperature 880 of metal Ti
DEG C, it is higher than 900 DEG C using the connection temperature of TiNi solder, metal Ti ring undergoes phase transition recrystallization, after connection, metal Ti ring
Coarse grains, seriously affect the availability of retina device.
The sheet Au-Si solder piece for being used by present embodiment is applied relative to using by the made soldering paste of Ti-Ni powder
Connection is applied, it is uniform for being able to maintain using sheet solder piece in each thickness to connecting portion solder layer, and uses craft
The layer of solder paste that mode applies then cannot be guaranteed that the thickness of position to be welded solder layer is uniform.
Present embodiment is before proceeding in Al also by the way of magnetron sputtering2O3Ceramics and Ti ring surface deposited metal
Layer, the intensity of jointing can be enhanced at Ti layers of ceramic surface deposited metal, and in the Ti of deposition layer and metal Ti ring table
Deposited metal Mo layers of face, which can be enhanced, improves solder in connector surface volume wetability.
Present embodiment between Au-Si solder and metal Ti ring by Mo layers of magnetron sputtering deposited metal, not only can be with
Prevent Au-Si solder and metal Ti ring that overreaction occurs, generating intermetallic compound influences the intensity of jointing, Er Qieke
To guarantee the dimensional stability of metal Ti ring, guarantee the stable structure of the retina device after connection.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: Au-Si described in step 1
Solder piece with a thickness of 30 μm~130 μm, and in the Au-Si solder piece Au element mass fraction be 96%, Si element
Mass fraction be 4%.Other are same as the specific embodiment one.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: in step 2
Temperature is cleaned by ultrasonic 8min under conditions of being 30 DEG C.Other are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: step 3 1. in
Al after cleaning2O3Potsherd is fixedly placed on the sample table of Pvd equipment, closes vacuum furnace chamber, starts vacuum
Vacuum degree is extracted into≤1 × 10 by system-5Under conditions of Pa, while vacuum furnace chamber is preheating to 00 DEG C, is filled with argon gas, adjusts it
Flow is 220sccm, while setting -900V for pulse voltage, temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon gas
Gas flow is 220sccm and pulse voltage is argon ion cleaning 15min under the conditions of -900V, obtains Al after argon ion cleaning2O3
Potsherd.Other are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: step 3 2. in
After argon ion cleaning, with striking needle in the surface striking of Ti target, and continue temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon
Gas gas flow is 220sccm and pulse voltage is cleans again using Ti ion under the conditions of -900V, scavenging period 15min,
Obtain Al after Ti Ion Cleaning2O3Potsherd.Other are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: step 3 3. in
After Ti ion, the gas flow of argon gas is adjusted, pressure is made to remain 1 × 10-1Pa, by Al after Ti Ion Cleaning2O3Ceramics
Before piece is placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd is 8cm at a distance from sputtering target, temperature is 400 DEG C, pressure is
1×10-1Under the negative high voltage of Pa, argon atmosphere and 5kV, in 90min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition
With a thickness of Ti layers of metal of 0.8 μm, depositing Ti layer Al is obtained2O3Potsherd.Other are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: step 3 4. in
Target is converted, keeping pressure is 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, in 90min,
In depositing Ti layer Al2O3It is Mo the layer of metal of 3.5 μm that a layer thickness is deposited on Ti layers of metal of potsherd, obtain depositing Mo layers/
Ti layers of Al2O3Potsherd.Other are identical as specific embodiment one to six.
Specific embodiment 8: one of present embodiment and specific embodiment one to seven difference are: step 3 5. in
Target is converted again, continues to keep pressure to be 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature,
In 45min, Mo layers/Ti layers Al are being deposited2O3The Au layer that a layer thickness is 0.8 μm, deposition are deposited on Mo layers of metal of potsherd
After, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, is filled with filtered
Pure air samples, Al after being metallized to opening the door2O3Potsherd.Other are identical as specific embodiment one to seven.
Specific embodiment 9: one of present embodiment and specific embodiment one to eight difference are: golden in step 4
Belong to the metallization of Ti ring surface: 1., by metal Ti ring after cleaning being fixedly placed on the sample table of Pvd equipment, closes
Vacuum furnace chamber starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while vacuum furnace chamber is preheating to 400
DEG C, it is filled with argon gas, adjusting its flow is 220sccm, while setting -900V for pulse voltage, is 400 DEG C, vacuum in temperature
Degree is≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion cleaning 10min under the conditions of -900V, are obtained
Metal Ti ring after to argon ion cleaning；2., after argon ion cleaning, adjust the flow of argon gas so that pressure remain 1 ×
10-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, metal Ti ring is at a distance from sputtering target after argon ion cleaning
12cm, temperature is 400 DEG C, pressure is 1 × 10-1Under the negative high voltage of Pa, argon atmosphere and 5kV, in 60min, in argon ion
Metal Ti ring surface deposition thickness is Mo layers of metal of 3 μm after cleaning, obtains Mo layers of metal Ti ring of deposition；3., conversion target, protect
Holding pressure is 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, golden at Mo layer of deposition in 60min
Belong to the Au layer that deposition a layer thickness is 0.4 μm on Mo layers of metal of Ti ring, obtains Au layers/Mo layers metal Ti ring of deposition, deposition
After, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, is filled with filtered
Pure air samples, metal Ti ring after being metallized to opening the door.Other are identical as specific embodiment one to eight.
Specific embodiment 10: one of present embodiment and specific embodiment one to nine difference are: in step 5 when
Vacuum degree reaches 2 × 10-5After Pa, being heated to temperature in the case where heating speed is 10 DEG C/min is 400 DEG C, and is 400 in temperature
5min is kept the temperature at DEG C, then controlling cooling velocity is that be cooled to temperature be 100 DEG C to 8 DEG C/min.Other with specific embodiment one to
Nine is identical.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
Using following verification experimental verifications effect of the present invention
Embodiment 1: the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed method for sealing, tool
Body is completed by the following steps:
One, solder piece is prepared: according to metal Ti ring size, by Au-Si solder piece punching at matching with metal Ti ring
Au-Si solder ring；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, in temperature
Degree is cleaned by ultrasonic 8min under conditions of being 30 DEG C, Al after metal Ti ring, cleaning after successively being cleaned2O3After potsherd and cleaning
Au-Si solder；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in physical vapour deposition (PVD) and sets
On standby sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, simultaneously will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -900V for pulse voltage,
Temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon under the conditions of -900V
Ion Cleaning 15min obtains Al after argon ion cleaning2O3Potsherd；2., argon ion cleaning after, drawn with striking needle on Ti target surface
Arc, and continue temperature be 400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be-
It is cleaned again under the conditions of 900V using Ti ion, scavenging period 15min obtains Al after Ti Ion Cleaning2O3Potsherd；③,Ti
After ion, the gas flow of argon gas is adjusted, pressure is made to remain 1 × 10-1Pa, by Al after Ti Ion Cleaning2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd at a distance from sputtering target be 10cm, temperature be 400 DEG C, pressure 1
×10-1Under the negative high voltage of Pa, argon atmosphere and 5kV, in 60min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition of thick
Degree is Ti layers of metal of 0.8 μm, obtains depositing Ti layer Al2O3Potsherd；4., conversion target, keep pressure be 1 × 10-1Pa,
Temperature is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV, in 90min, in depositing Ti layer Al2O3Ti layers of the metal of potsherd
On deposition a layer thickness be Mo the layer of metal of 3 μm, obtain depositing Mo layers/Ti layers Al2O3Potsherd；5., convert target again,
Continue to keep pressure to be 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, in 45min, is depositing
Mo layers/Ti layers Al2O3A layer thickness is deposited on Mo layers of metal of potsherd as 0.6 μm of Au layer, after deposition, closes electricity
Source and argon gas switch close vacuum system when the temperature of vacuum chamber is down to 100 DEG C, are filled with filtered pure air to opening
Door, sampling, Al after being metallized2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in Pvd equipment
On sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum
Furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -850V for pulse voltage, in temperature
It is≤1 × 10 for 400 DEG C, vacuum degree-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
10min is cleaned, metal Ti ring after argon ion cleaning is obtained；2., argon ion cleaning after, adjust the flow of argon gas so that pressure
1 × 10 is remained by force-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti ring with splash
The distance shot at the target is 10cm, temperature is 400 DEG C, pressure is 1 × 10-1Under the negative high voltage of Pa, argon atmosphere and 4kV, in 60min
Interior, metal Ti ring surface deposition thickness is Mo layers of metal of 2 μm after argon ion cleaning, obtains Mo layers of metal Ti ring of deposition；③,
Target is converted, keeping pressure is 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 4kV in temperature, in 50min,
The Au layer that deposition a layer thickness is 0.3 μm on Mo layers of metal of Mo layers of metal Ti ring of deposition obtains Au layers/Mo layers gold of deposition
Belong to Ti ring, after deposition, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
Filtered pure air is filled with to opening the door, is sampled, metal Ti ring after being metallized；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3Potsherd and metallization after metal Ti ring it
Between, welding equipment part to be welded is formed, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 2 × 10-5After Pa,
Heating speed is that temperature is heated under 10 DEG C/min is 400 DEG C, and keeps the temperature 5min at being 400 DEG C in temperature, then control cooling speed
Degree be that be cooled to temperature be 100 DEG C to 8 DEG C/min, then cools to room temperature with the furnace, that is, completes artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring are brazed sealing-in.
Au-Si solder piece described in the present embodiment step 1 with a thickness of 80 μm, and in the Au-Si solder piece Au member
The mass fraction of element is that the mass fraction of 96%, Si element is 4%.
Provided method according to the present invention, the connector connected is finer and close, and has biocompatibility, and even
The shear strength of connector is 25MPa.
Embodiment 2: the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed method for sealing, tool
Body is completed by the following steps:
One, solder piece is prepared: according to metal Ti ring size, by Au-Si solder piece punching at matching with metal Ti ring
Au-Si solder ring；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, in temperature
Degree is cleaned by ultrasonic 8min under conditions of being 30 DEG C, Al after metal Ti ring, cleaning after successively being cleaned2O3After potsherd and cleaning
Au-Si solder；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in physical vapour deposition (PVD) and sets
On standby sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, simultaneously will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -900V for pulse voltage,
Temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon under the conditions of -900V
Ion Cleaning 15min obtains Al after argon ion cleaning2O3Potsherd；2., argon ion cleaning after, drawn with striking needle on Ti target surface
Arc, and continue temperature be 400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be-
It is cleaned again under the conditions of 900V using Ti ion, scavenging period 15min obtains Al after Ti Ion Cleaning2O3Potsherd；③,Ti
After ion, the gas flow of argon gas is adjusted, pressure is made to remain 1 × 10-1Pa, by Al after Ti Ion Cleaning2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd at a distance from sputtering target be 10cm, temperature be 400 DEG C, pressure 1
×10-1Under the negative high voltage of Pa, argon atmosphere and 4.5kV, in 90min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition
With a thickness of Ti layers of metal of 0.8 μm, depositing Ti layer Al is obtained2O3Potsherd；4., conversion target, keep pressure be 1 × 10-1Pa,
It is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, in 90min, in depositing Ti layer Al2O3The metal Ti of potsherd
Deposition a layer thickness is Mo layers of metal of 3.5 μm on layer, obtains Mo layers/Ti layers Al of deposition2O3Potsherd；5., conversion target again
Material continues to keep pressure to be 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, in 45min,
Deposit Mo layers/Ti layers Al2O3A layer thickness is deposited on Mo layers of metal of potsherd as 0.8 μm of Au layer, after deposition, is closed
Power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, is filled with filtered pure air
To enabling, sampling, Al after being metallized2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in Pvd equipment
On sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum
Furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -850V for pulse voltage, in temperature
It is≤1 × 10 for 400 DEG C, vacuum degree-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
10min is cleaned, metal Ti ring after argon ion cleaning is obtained；2., argon ion cleaning after, adjust the flow of argon gas so that pressure
1 × 10 is remained by force-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti ring with splash
The distance shot at the target is 10cm, temperature is 400 DEG C, pressure is 1 × 10-1Under the negative high voltage of Pa, argon atmosphere and 5kV, in 60min
Interior, metal Ti ring surface deposition thickness is Mo layers of metal of 3 μm after argon ion cleaning, obtains Mo layers of metal Ti ring of deposition；③,
Target is converted, keeping pressure is 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 5kV in temperature, in 60min,
The Au layer that deposition a layer thickness is 0.6 μm on Mo layers of metal of Mo layers of metal Ti ring of deposition obtains Au layers/Mo layers gold of deposition
Belong to Ti ring, after deposition, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
Filtered pure air is filled with to opening the door, is sampled, metal Ti ring after being metallized；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3Potsherd and metallization after metal Ti ring it
Between, welding equipment part to be welded is formed, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 2 × 10-5After Pa,
Heating speed is that temperature is heated under 10 DEG C/min is 400 DEG C, and keeps the temperature 5min at being 400 DEG C in temperature, then control cooling speed
Degree be that be cooled to temperature be 100 DEG C to 8 DEG C/min, then cools to room temperature with the furnace, that is, completes artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring are brazed sealing-in.
Au-Si solder piece described in the present embodiment step 1 with a thickness of 100 μm, and Au in the Au-Si solder piece
The mass fraction of element is that the mass fraction of 96.5%, Si element is 3.5%.
Provided method according to the present invention, the connector connected is finer and close, and has biocompatibility, and even
The shear strength of connector is 28MPa.
Embodiment 3: the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed method for sealing, tool
Body is completed by the following steps:
One, solder piece is prepared: according to metal Ti ring size, by Au-Si solder piece punching at matching with metal Ti ring
Au-Si solder ring；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, in temperature
Degree is cleaned by ultrasonic 8min under conditions of being 30 DEG C, Al after metal Ti ring, cleaning after successively being cleaned2O3After potsherd and cleaning
Au-Si solder；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in physical vapour deposition (PVD) and sets
On standby sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, simultaneously will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -900V for pulse voltage,
Temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon under the conditions of -900V
Ion Cleaning 15min obtains Al after argon ion cleaning2O3Potsherd；2., argon ion cleaning after, drawn with striking needle on Ti target surface
Arc, and continue temperature be 400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be-
It is cleaned again under the conditions of 900V using Ti ion, scavenging period 15min obtains Al after Ti Ion Cleaning2O3Potsherd；③,Ti
After ion, the gas flow of argon gas is adjusted, pressure is made to remain 1 × 10-1Pa, by Al after Ti Ion Cleaning2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd at a distance from sputtering target be 8cm, temperature be 400 DEG C, pressure 1
×10-1Under the negative high voltage of Pa, argon atmosphere and 4kV, in 60min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition of thick
Degree is Ti layers of metal of 0.4 μm, obtains depositing Ti layer Al2O3Potsherd；4., conversion target, keep pressure be 1 × 10-1Pa,
Temperature is 400 DEG C, under the negative high voltage of argon atmosphere and 4kV, in 90min, in depositing Ti layer Al2O3Ti layers of the metal of potsherd
On deposition a layer thickness be Mo the layer of metal of 2.8 μm, obtain depositing Mo layers/Ti layers Al2O3Potsherd；5., conversion target again
Material continues to keep pressure to be 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 4.5kV in temperature, in 30min,
Depositing Mo layers/Ti layers Al2O3It is 0.5 μm of Au layer that a layer thickness is deposited on Mo layers of metal of potsherd, after deposition,
Power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, closes vacuum system, is filled with filtered clean empty
Gas samples, Al after being metallized to opening the door2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in Pvd equipment
On sample table, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum
Furnace chamber is preheating to 400 DEG C, is filled with argon gas, and adjusting its flow is 220sccm, while setting -850V for pulse voltage, in temperature
It is≤1 × 10 for 400 DEG C, vacuum degree-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
10min is cleaned, metal Ti ring after argon ion cleaning is obtained；2., argon ion cleaning after, adjust the flow of argon gas so that pressure
1 × 10 is remained by force-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti ring with splash
The distance shot at the target is 10cm, temperature is 400 DEG C, pressure is 1 × 10-1Under the negative high voltage of Pa, argon atmosphere and 4kV, in 90min
Interior, metal Ti ring surface deposition thickness is Mo layers of metal of 3 μm after argon ion cleaning, obtains Mo layers of metal Ti ring of deposition；③,
Target is converted, keeping pressure is 1 × 10-1Pa is 400 DEG C, under the negative high voltage of argon atmosphere and 4kV in temperature, in 30min,
The Au layer that deposition a layer thickness is 0.5 μm on Mo layers of metal of Mo layers of metal Ti ring of deposition obtains Au layers/Mo layers gold of deposition
Belong to Ti ring, after deposition, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
Filtered pure air is filled with to opening the door, is sampled, metal Ti ring after being metallized；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3Potsherd and metallization after metal Ti ring it
Between, welding equipment part to be welded is formed, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 2 × 10-5After Pa,
Heating speed is that temperature is heated under 10 DEG C/min is 400 DEG C, and keeps the temperature 5min at being 400 DEG C in temperature, then control cooling speed
Degree be that be cooled to temperature be 100 DEG C to 8 DEG C/min, then cools to room temperature with the furnace, that is, completes artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring are brazed sealing-in.
Au-Si solder piece described in the present embodiment step 1 with a thickness of 60 μm, and in the Au-Si solder piece Au member
The mass fraction of element is that the mass fraction of 97%, Si element is 3%.
Provided method according to the present invention, the connector connected is finer and close, and has biocompatibility, and even
The shear strength of connector is 23MPa.
Claims (10)
1. the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed method for sealing, it is characterised in that it
It is completed by the following steps:
One, solder piece is prepared: according to metal Ti ring size, by Au-Si solder piece punching at the Au-Si to match with metal Ti ring
Solder ring；
Two, sample cleans: by metal Ti ring, Al2O3Potsherd and Au-Si solder ring are respectively placed in acetone soln, are in temperature
It is cleaned by ultrasonic 7min~12min, Al after metal Ti ring, cleaning after successively being cleaned under conditions of 25~35 DEG C2O3Potsherd and
Au-Si solder after cleaning；
Three, Al2O3Ceramic surface metallization: 1., will cleaning after Al2O3Potsherd is fixedly placed in the examination of Pvd equipment
On sample platform, vacuum chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum furnace chamber
350~400 DEG C are preheating to, argon gas is filled with, adjusting its flow is 150sccm~220sccm, while setting pulse voltage to-
850V~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 150sccm~
Argon ion cleans 10min~15min under the conditions of 220sccm and pulse voltage are -850V~-950V, after obtaining argon ion cleaning
Al2O3Potsherd；2., after argon ion cleaning, with striking needle in the surface striking of Ti target, and continue temperature be 350~400 DEG C, it is true
Reciprocal of duty cycle is≤1 × 10-5Pa, argon gas flow are 150sccm~220sccm and pulse voltage is under the conditions of -850V~-950V
It is cleaned again using Ti ion, scavenging period is 10min~15min, obtains Al after Ti Ion Cleaning2O3Potsherd；3., Ti from
After son cleaning, the gas flow of argon gas is adjusted, pressure is made to remain 0.5 × 10-1Pa~1.5 × 10-1Pa, by Ti ion
Al after cleaning2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd at a distance from sputtering target for 8cm~
12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV it is negative
Under high pressure, in 60min~120min, the Al after Ti Ion Cleaning2O3The gold that potsherd surface deposition thickness is 0.2 μm~1 μm
Belong to Ti layers, obtains depositing Ti layer Al2O3Potsherd；4., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa,
It is 350~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV in temperature, in 60min~120min, in depositing Ti layer
Al2O3Mo layers of metal that a layer thickness is 2 μm~4 μm are deposited on Ti layers of metal of potsherd, obtain Mo layers/Ti layers of deposition
Al2O3Potsherd；5., convert target again, continue keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa is 350 in temperature
~400 DEG C, under the negative high voltage of argon atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3Ceramics
A layer thickness is deposited on Mo layers of metal of piece as 0.1 μm~0.5 μm of Au layer, after deposition, closes power supply and argon gas is opened
It closes, when the temperature of vacuum chamber is down to 80~120 DEG C, closes vacuum system, be filled with filtered pure air to opening the door, take
Sample, Al after being metallized2O3Potsherd；
Four, metal Ti ring surface metallizes: 1., by metal Ti ring after cleaning being fixedly placed in the sample of Pvd equipment
On platform, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum furnace chamber
350~400 DEG C are preheating to, argon gas is filled with, adjusting its flow is 150~220sccm, while setting -850 for pulse voltage
~-950V, temperature be 350~400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow are 150sccm~220sccm
Argon ion cleans 10min~15min under the conditions of being -850V~-950V with pulse voltage, obtains metal Ti after argon ion cleaning
Ring；2., argon ion cleaning after, the flow of argon gas is adjusted, so that pressure remains 0.5 × 10-1Pa~1.5 × 10-1Pa,
Before metal Ti ring is placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti ring at a distance from sputtering target for 8cm~
12cm, temperature is 350~400 DEG C, pressure is 0.5 × 10-1Pa~1.5 × 10-1Pa, argon atmosphere and 4kV~5kV it is negative
Under high pressure, in 60min~120min, metal Ti ring surface deposition thickness is 2 μm~4 μm of metal Mo after argon ion cleaning
Layer obtains Mo layers of metal Ti ring of deposition；3., conversion target, keep pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, in temperature
In 30min~60min, to deposit Mo layers of metal Ti ring under 350~400 DEG C, the negative high voltage of argon atmosphere and 4kV~5kV
Mo layers of metal on deposition a layer thickness be 0.1 μm~0.5 μm of Au layer, obtain Au layers/Mo layers metal Ti ring of deposition, deposit
After, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, vacuum system is closed, is filled with filtering
Pure air afterwards samples, metal Ti ring after being metallized to opening the door；
Five, Au-Si solder after cleaning sealing-in: is placed in Al after metallizing2O3After potsherd and metallization between metal Ti ring, group
At welding equipment part to be welded, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum degree reaches 1.50 × 10-5Pa~2.50 ×
10-5After Pa, being heated to temperature in the case where heating speed is 8 DEG C/min~12 DEG C/min is 390~420 DEG C, and is 390 in temperature
3min~5min is kept the temperature at~420 DEG C, then controlling cooling velocity is that be cooled to temperature be 80~120 to 5 DEG C/min~10 DEG C/min
DEG C, it then cools to room temperature with the furnace, that is, completes the Al of artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
It connects.
2. the Al according to claim 1 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that the piece of Au-Si solder described in step 1 with a thickness of 30 μm~130 μm, and the Au-Si solder
It is 2.75%~5% that the mass fraction of Au element, which is the mass fraction of 95%~97.25%, Si element, in piece.
3. the Al according to claim 1 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that be cleaned by ultrasonic 8min under conditions of temperature is 30 DEG C in step 2.
4. the Al according to claim 1 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that step 3 1. in will cleaning after Al2O3Potsherd is fixedly placed in the sample of Pvd equipment
On platform, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5Under conditions of Pa, while by vacuum furnace chamber
400 DEG C are preheating to, argon gas is filled with, adjusting its flow is 220sccm, while setting -900V for pulse voltage, is in temperature
400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is clear for argon ion under the conditions of -900V
15min is washed, Al after argon ion cleaning is obtained2O3Potsherd.
5. the Al according to claim 4 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that step 3 is 2. after middle argon ion cleaning, and with striking needle in the surface striking of Ti target, and continuation is in temperature
400 DEG C, vacuum degree be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be -900V under the conditions of using Ti from
Son cleans again, and scavenging period 15min obtains Al after Ti Ion Cleaning2O3Potsherd.
6. the Al according to claim 5 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that 3. step 3 after middle Ti ion, adjusts the gas flow of argon gas, pressure is made to remain 1 × 10- 1Pa, by Al after Ti Ion Cleaning2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleaning2O3Potsherd is at a distance from sputtering target
For 10cm, temperature is 400 DEG C, pressure is 1 × 10-1Under the negative high voltage of Pa, argon atmosphere and 4kV~5kV, 60min~
In 90min, the Al after Ti Ion Cleaning2O3Potsherd surface deposition thickness is Ti layers of metal of 0.4 μm~0.8 μm, is deposited
Ti layers of Al2O3Potsherd.
7. the Al according to claim 6 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that step 3 is 4. middle to convert target, and keeping pressure is 1 × 10-1Pa is 400 DEG C, argon atmosphere in temperature
Under the negative high voltage of 4kV~5kV, in 90min, in depositing Ti layer Al2O3A layer thickness is deposited on Ti layers of metal of potsherd
For Mo layers of metal of 2.8 μm~3.5 μm, Mo layers/Ti layers Al of deposition are obtained2O3Potsherd.
8. the Al according to claim 7 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that step 3 5. in convert target again, continue keep pressure be 1 × 10-1Pa, temperature be 400 DEG C,
Under the negative high voltage of argon atmosphere and 4.5kV~5kV, in 30min~45min, Mo layers/Ti layers Al are being deposited2O3The gold of potsherd
Belong to and deposit a layer thickness on Mo layers as 0.1 μm~0.5 μm of Au layer, after deposition, power supply and argon gas switch is closed, to true
When the temperature of cavity is down to 100 DEG C, vacuum system is closed, is filled with filtered pure air to opening the door, sampling is metallized
Al afterwards2O3Potsherd.
9. the Al according to claim 1 based on artificial retina implant devices2O3Ceramic substrate and the soldering of metal Ti ring are sealed
Connect method, it is characterised in that metal Ti ring surface metallizes in step 4: 1., by metal Ti ring after cleaning being fixedly placed in physics
On the sample table of vapor deposition apparatus, vacuum furnace chamber is closed, starts vacuum system, vacuum degree is extracted into≤1 × 10-5The condition of Pa
Under, while vacuum furnace chamber is preheating to 400 DEG C, it is filled with argon gas, adjusting its flow is 220sccm, while pulse voltage being arranged
For -900V, temperature is 400 DEG C, vacuum degree is≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be-
Argon ion cleans 10min under the conditions of 900V, obtains metal Ti ring after argon ion cleaning；2., argon ion cleaning after, adjust argon
The flow of gas, so that pressure remains 1 × 10-1Pa, before metal Ti ring is placed in sputtering target after argon ion is cleaned, argon ion cleaning
Metal Ti ring is 10cm at a distance from sputtering target afterwards, temperature is 400 DEG C, pressure is 1 × 10-1Pa, argon atmosphere and 4kV~
Under the negative high voltage of 5kV, in 60min~90min, metal Ti ring surface deposition thickness is 2 μm~3 μm after argon ion cleaning
Mo layers of metal, obtain Mo layers of metal Ti ring of deposition；3., conversion target, keep pressure be 1 × 10-1Pa is 400 DEG C, argon in temperature
Under the negative high voltage of gas atmosphere and 4kV~5kV, in 30min~60min, on Mo layers of metal of Mo layers of metal Ti ring of deposition
Depositing a layer thickness is 0.5 μm~0.8 μm of Au layer, obtains Au layer/Mo layers metal Ti ring of deposition, and after deposition, closing is electric
Source and argon gas switch close vacuum system when the temperature of vacuum chamber is down to 100 DEG C, are filled with filtered pure air to opening
Door, sampling, metal Ti ring after being metallized.
10. the Al according to claim 1 based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring are brazed
Method for sealing, it is characterised in that when vacuum degree reaches 2 × 10 in step 5-5After Pa, add in the case where heating speed is 10 DEG C/min
Heat to temperature is 400 DEG C, and keeps the temperature 5min at being 400 DEG C in temperature, then controlling cooling velocity is that 8 DEG C/min is cooled to temperature and is
100℃。
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| CN110734296B (en) * | 2019-10-11 | 2021-10-22 | 哈尔滨工业大学 | Connecting joint based on nickel-based superalloy and ceramic and preparation method thereof |
| CN110722234B (en) * | 2019-10-11 | 2020-12-04 | 哈尔滨工业大学 | Nickel titanium base alloy low-temperature connecting joint and preparation method thereof |
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