CN106862695A - The soldering method for sealing of aluminum oxide ceramic substrate and Ti rings based on artificial retina implant devices - Google Patents
The soldering method for sealing of aluminum oxide ceramic substrate and Ti rings based on artificial retina implant devices Download PDFInfo
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- CN106862695A CN106862695A CN201710253199.2A CN201710253199A CN106862695A CN 106862695 A CN106862695 A CN 106862695A CN 201710253199 A CN201710253199 A CN 201710253199A CN 106862695 A CN106862695 A CN 106862695A
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- 210000001525 retina Anatomy 0.000 title claims abstract description 40
- 238000005476 soldering Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 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
- 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
- 229910052751 metal Inorganic materials 0.000 claims abstract description 204
- 239000002184 metal Substances 0.000 claims abstract description 204
- 238000004140 cleaning Methods 0.000 claims abstract description 139
- 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 55
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 55
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 55
- 238000001465 metallisation Methods 0.000 claims abstract description 26
- 238000003466 welding Methods 0.000 claims abstract description 18
- 238000005219 brazing Methods 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 301
- 229910052786 argon Inorganic materials 0.000 claims description 184
- 239000007789 gas Substances 0.000 claims description 122
- 238000000151 deposition Methods 0.000 claims description 90
- -1 argon ion Chemical class 0.000 claims description 66
- 229910015365 Au—Si Inorganic materials 0.000 claims description 55
- 150000002500 ions Chemical class 0.000 claims description 49
- 230000008021 deposition Effects 0.000 claims description 38
- 239000010931 gold Substances 0.000 claims description 33
- 238000005477 sputtering target Methods 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 230000002000 scavenging effect Effects 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 238000004080 punching Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 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 3
- 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
- 238000001953 recrystallisation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 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
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization 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 soldering method for sealing based on artificial retina implant devices, it belongs to welding technology field, and in particular to the Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering method for sealing.The invention aims to solve to realize Al during existing vacuum brazing2O3Ceramics are connected by TiNi solders with metal Ti rings, and damage, and welding temperature problem higher can be produced to human body.Method for sealing：First, solder piece is prepared；2nd, Al after metal Ti rings, cleaning after being cleaned2O3Au Si solders after potsherd and cleaning；3rd, Al2O3Ceramic surface metallization；4th, metal Ti ring surfaces metallization；5th, sealing-in, that is, complete the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering sealing-ins.Present invention is mainly used for the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering sealing-ins.
Description
Technical field
The invention belongs to welding technology field, and in particular to the Al based on artificial retina implant devices2O3Ceramic substrate with
Metal Ti ring soldering method for sealing.
Background technology
In artificial retina structure, Al2O3Ceramics and the connection of metal Ti rings not only to meet certain bonding strength and
Air-tightness, but also to cause that whole jointing has biocompatibility, i.e., must not contain in the structure of whole artificial retina
There is harmful composition.And prior art cannot meet Al in artificial retina structure2O3The company of ceramics and metal Ti rings
Connect.
Al2O3Ceramics have excellent bio-compatibility with metal Ti, are captured importantly in technical field of biological material
Position.At present, Al is realized2O3The method that ceramics are connected with metal Ti mainly has diffusion welding (DW), soldering etc., and wherein method for brazing is to study most
More 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 is, it is necessary to Al2O3Ceramic surface carries out metalized.Realize Al 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 and Ti ring solderings method for sealing " (Shen Qing Publication
Number：CN105598542A using vacuum brazing it is to realize Al disclosed in)2O3Ceramics are connected with metal Ti rings, and the patent uses TiNi
Solder, because Ni does not have biocompatibility in TiNi solders, the retina device connected using TiNi solders is being implanted into human body
Afterwards, damage can be produced to human body；And the brazing temperature of the patent is 990 DEG C~1450 DEG C, however it remains welding temperature is higher
Problem.
The content of the invention
It is to realize Al that the object of the invention will solve existing vacuum brazing2O3Ceramics are connected to exist with metal Ti rings and use TiNi
Solder, can produce damage, and welding temperature problem higher to human body, and provide the Al based on artificial retina implant devices2O3
Ceramic substrate and metal Ti ring soldering method for sealing.
Al based on artificial retina implant devices2O3The soldering method for sealing of ceramic substrate and Ti rings, specifically by following
What step was completed：
First, solder piece is prepared：According to metal Ti ring sizes, by Au-Si solder piece punching into metal Ti ring size phases
The Au-Si solder rings matched somebody with somebody；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, in temperature
Spend to be cleaned by ultrasonic 7min~12min under conditions of 25~35 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3Ceramics
Au-Si solders after piece and cleaning；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement sets in physical vapour deposition (PVD)
On standby sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5Under conditions of Pa, while will
Vacuum furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, adjusts its flow for 150sccm~220sccm, while by pulse voltage
Be set to -850V~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow are
150sccm~220sccm and pulse voltage are argon ion cleaning 10min~15min under the conditions of -850V~-950V, obtain argon from
Al after son cleaning2O3Potsherd；2., after argon ion cleaning, with striking pin in the surface striking of Ti targets, and continue temperature be 350~
400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 150sccm~220sccm and pulse voltage be -850V~-
Cleaned again using Ti ions under the conditions of 950V, scavenging period is 10min~15min, obtains Al after Ti Ion Cleanings2O3Ceramics
Piece；3. after, Ti ions terminate, the gas flow of argon gas is adjusted, pressure is remained 0.5 × 10-1Pa~1.5 × 10-1Pa, will
Al after Ti Ion Cleanings2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleanings2O3Potsherd is 8cm with the distance of sputtering target
~12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV's
Under negative high voltage, in 60min~120min, the Al after Ti Ion Cleanings2O3Potsherd surface deposit thickness is 0.1 μm~0.5 μm
Metal Ti layers, obtain depositing Ti layer Al2O3Potsherd；4. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10- 1Pa, temperature be 350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 60min~120min, in deposition
Ti layers of Al2O3Deposition a layer thickness is metal Mo layer of 2 μm~4 μm on metal Ti layers of potsherd, obtains depositing Mo layers/Ti
Layer Al2O3Potsherd；5. target, is changed again, and it is 0.5 × 10 to continue to keep pressure-1Pa~1.5 × 10-1Pa, be in temperature
350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3
Deposition a layer thickness is Au layer of 0.1 μm~0.5 μm on metal Mo layers of potsherd, after deposition terminates, closes power supply and argon
Air cock, when the temperature of vacuum chamber is down to 80~120 DEG C, closes vacuum system, is filled with the pure air after filtering to enabling,
Sampling, Al after being metallized2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti ring fixed placements after cleaning in Pvd equipment
On sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum 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, adjusts its flow for 150~220sccm, while pulse voltage is set to-
850~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 150sccm~
220sccm and pulse voltage are argon ion cleaning 10min~15min under the conditions of -850V~-950V, after obtaining argon ion cleaning
Metal Ti rings；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure remains 0.5 × 10-1Pa~1.5 ×
10-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, metal Ti rings are with the distance of sputtering target after argon ion cleaning
8cm~12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, metal Ti ring surface deposit thickness is 2 μm~4 μm of gold after argon ion cleaning
Mo layers of category, obtains depositing Mo layers of metal Ti ring；3. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10-1Pa,
Temperature is 350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers of metal
Deposition a layer thickness is Au layer of 0.1 μm~0.5 μm on metal Mo layers of Ti rings, obtains depositing Au layers/Mo layers metal Ti ring,
After deposition terminates, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, close vacuum system, be filled with
Pure air after filtering is sampled, metal Ti rings after being metallized to opening the door；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3Potsherd and metallization after metal Ti rings it
Between, welding equipment part to be welded is constituted, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 1.50 × 10-5Pa~
2.50×10-5After Pa, temperature is heated in the case where firing rate is 8 DEG C/min~12 DEG C/min for 390~420 DEG C, and in temperature
Spend for 390~420 DEG C is lower insulation 3min~5min, then control cooling velocity to be cooled to temperature for 5 DEG C/min~10 DEG C/min
It is 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 soldering sealing-in.
The present invention realizes Al using Au-Si solders2O3The connection of ceramics and metal Ti rings, in order to improve the company of jointing
Intensity is connect to reach the requirement of retina device, in Al2O3By the side of magnetron sputtering in the junction to be welded of ceramics and metal Ti rings
Formula depositing metallization, in Al2O3Ceramic surface deposition layer and there is the metal Ti of preferable adhesion with it, then
Be further continued for one layer of the magnetron sputtering deposition on metal Ti layers and metal Ti rings it is thicker there is preferable wetability with Au-Si solders
Metal Mo layers, there is the follow-up sealing-in reaction of oxidation influence before sealing-in to suppress metal Mo layers, in the metal of deposition
Au layers of redeposited layer on Mo layers, Mo layers of metal of protection prevents it from aoxidizing, in Al2O3Ceramics and metal Ti ring surfaces
After depositing metallization, closure is treated with Au-Si solders composition, control brazing temperature is between 390~420 DEG C and when being incubated
Between 3min~5min, to ensure that soldered fitting obtains preferable microstructure and performance, be successfully realized Al2O3Ceramics and metal
The sealing-in of Ti, and obtain reliable joint.
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 it is to realize Al to carry out vacuum brazing using biocompatibility solder2O3What ceramics were connected with metal Ti rings
Effective ways.
Advantage of the present invention：First, the present invention uses Au-Si solders, compared with its TiNi for being used solder, Au-Si
Solder has biocompatibility, and human body will not be damaged, and is used because Ni does not have biocompatibility in TiNi solders
The retina device of TiNi solders connection can produce damage after human body is implanted into human body；2nd, due to the Al of required connection2O3
Ceramic internal and surface is furnished with plain conductor, and temperature of the present invention using Au-Si solders below 420 DEG C realizes Al2O3Ceramics with
The connection of Ti rings, connection is realized compared to using Ti-Ni solders at 990 DEG C~1450 DEG C, is connected in 400 DEG C of implemented below, no
Can be to Al2O3Ceramic internal and surface is furnished with plain conductor and produces damage, it is ensured that the device energy normal work after connection.3rd, this hair
The connection temperature at bright place below 420 DEG C, 880 DEG C of the phase transformation recrystallization temperature far below metal Ti, using TiNi solders
Connection temperature is higher than 900 DEG C, and metal Ti rings undergo phase transition recrystallization, after connection, the coarse grains of metal Ti rings, serious shadow
Ring the availability of retina device.4th, the sheet Au-Si solder pieces for being of the present invention, relative to using by Ti-Ni powder
Made soldering paste coating connection, the thickness that can be maintained at each position solder layer to be connected using sheet solder piece be it is homogeneous,
And the layer of solder paste applied by the way of craft is then it cannot be guaranteed that the thickness of position to be welded solder layer is homogeneous.5th, the present invention exists
In Al also by the way of magnetron sputtering before connection2O3Ceramics and Ti ring surfaces deposited metal layer, in ceramic surface deposited metal
The Ti layers of intensity that can strengthen jointing, and can strengthen in Ti layers of deposition and Mo layers of metal Ti ring surface deposited metals
Improve solder in connector surface volume wetability.6th, the present invention is heavy by magnetron sputtering between Au-Si solders and metal Ti rings
Mo layers of metal of product, can not only prevent Au-Si solders that overreaction occurs with metal Ti rings, and generation intermetallic compound influence connects
The intensity of joint, and the dimensional stability of metal Ti rings can be ensured, it is ensured that the structure of the retina device after connection
Stabilization.
Specific embodiment
Specific embodiment one：Present embodiment is based on the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti
Ring soldering method for sealing, is specifically realized by the following steps：
First, solder piece is prepared：According to metal Ti ring sizes, Au-Si solder piece punching is matched into metal Ti rings
Au-Si solder rings；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, in temperature
Spend to be cleaned by ultrasonic 7min~12min under conditions of 25~35 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3Ceramics
Au-Si solders after piece and cleaning；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement sets in physical vapour deposition (PVD)
On standby sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5Under conditions of Pa, while will
Vacuum furnace chamber is preheating to 350~400 DEG C, is filled with argon gas, adjusts its flow for 150sccm~220sccm, while by pulse voltage
Be set to -850V~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow are
150sccm~220sccm and pulse voltage are argon ion cleaning 10min~15min under the conditions of -850V~-950V, obtain argon from
Al after son cleaning2O3Potsherd；2., after argon ion cleaning, with striking pin in the surface striking of Ti targets, and continue temperature be 350~
400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 150sccm~220sccm and pulse voltage be -850V~-
Cleaned again using Ti ions under the conditions of 950V, scavenging period is 10min~15min, obtains Al after Ti Ion Cleanings2O3Ceramics
Piece；3. after, Ti ions terminate, the gas flow of argon gas is adjusted, pressure is remained 0.5 × 10-1Pa~1.5 × 10-1Pa, will
Al after Ti Ion Cleanings2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleanings2O3Potsherd is many with the distance of sputtering target
8cm~12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, the Al after Ti Ion Cleanings2O3Potsherd surface deposit thickness is 0.2 μm~1 μm
Metal Ti layers, obtain depositing Ti layer Al2O3Potsherd；4. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10- 1Pa, temperature be 350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 60min~120min, in deposition
Ti layers of Al2O3Deposition a layer thickness is metal Mo layer of 2 μm~4 μm on metal Ti layers of potsherd, obtains depositing Mo layers/Ti
Layer Al2O3Potsherd；5. target, is changed again, and it is 0.5 × 10 to continue to keep pressure-1Pa~1.5 × 10-1Pa, be in temperature
350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3
Deposition a layer thickness is Au layer of 0.2 μm~1 μm on metal Mo layers of potsherd, after deposition terminates, closes power supply and argon gas
Switch, when the temperature of vacuum chamber is down to 80~120 DEG C, closes vacuum system, is filled with the pure air after filtering to opening the door, and takes
Sample, Al after being metallized2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti ring fixed placements after cleaning in Pvd equipment
On sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum 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, adjusts its flow for 150~220sccm, while pulse voltage is set to-
850~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 150sccm~
220sccm and pulse voltage are argon ion cleaning 10min~15min under the conditions of -850V~-950V, after obtaining argon ion cleaning
Metal Ti rings；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure remains 0.5 × 10-1Pa~1.5 ×
10-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, metal Ti rings are with the distance of sputtering target after argon ion cleaning
8cm~12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV
Negative high voltage under, in 60min~120min, metal Ti ring surface deposit thickness is 2 μm~4 μm of gold after argon ion cleaning
Mo layers of category, obtains depositing Mo layers of metal Ti ring；3. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10-1Pa,
Temperature is 350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers of metal
Deposition a layer thickness is Au layer of 0.2 μm~1 μm on metal Mo layers of Ti rings, obtains depositing Au layers/Mo layers metal Ti ring, is sunk
After product terminates, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, close vacuum system, be filled with
Pure air after filter is sampled, metal Ti rings after being metallized to opening the door；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3Potsherd and metallization after metal Ti rings it
Between, welding equipment part to be welded is constituted, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 1.50 × 10-5Pa~
2.50×10-5After Pa, temperature is heated in the case where firing rate is 8 DEG C/min~12 DEG C/min for 390~420 DEG C, and in temperature
Spend for 390~420 DEG C is lower insulation 3min~5min, then control cooling velocity to be cooled to temperature for 5 DEG C/min~10 DEG C/min
It is 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 soldering sealing-in.
With a kind of Chinese publication " Al in artificial retina2O3Ceramics and Ti ring solderings method for sealing " (Shen Qing Publication
Number：CN105598542A) compare, the advantage of present embodiment essentially consists in the following aspects
Present embodiment uses Au-Si solders, and compared with its TiNi for being used solder, Au-Si solders have life
Thing compatibility, will not damage to human body, and be connected using TiNi solders because Ni does not have biocompatibility in TiNi solders
The retina device for connecing can produce damage after human body is 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 prickers
Expect that the temperature below 420 DEG C realizes Al2O3The connection of ceramics and Ti rings, compared to use Ti-Ni solders 990 DEG C~1450
DEG C connection is realized, in the connection of 400 DEG C of implemented below, will not be to Al2O3Ceramic internal and surface is furnished with plain conductor and produces damage,
Ensure the device energy normal work after connection.
Connection temperature where present embodiment below 420 DEG C, the phase transformation recrystallization temperature 880 far below metal Ti
DEG C, it is higher than 900 DEG C using the connection temperature of TiNi solders, metal Ti rings undergo phase transition recrystallization, after connection, metal Ti rings
Coarse grains, have a strong impact on the availability of retina device.
The sheet Au-Si solder pieces that present embodiment is used, apply relative to using by the made soldering paste of Ti-Ni powder
Connection is applied, it is homogeneous that the thickness of each position solder layer to be connected can be maintained at using sheet solder piece, and use craft
The layer of solder paste that mode is applied is then it cannot be guaranteed that the thickness of position to be welded solder layer is homogeneous.
Present embodiment is before proceeding in Al also by the way of magnetron sputtering2O3Ceramics and Ti ring surface deposited metals
Layer, the intensity of jointing can be strengthened in Ti layer of ceramic surface deposited metal, and in Ti layers and metal Ti ring tables of deposition
Mo layers of face deposited metal can strengthen improvement solder in connector surface volume wetability.
Present embodiment can be with by Mo layers of magnetron sputtering deposition metal, not only between Au-Si solders and metal Ti rings
Prevent Au-Si solders that overreaction occurs with metal Ti rings, generation intermetallic compound influences the intensity of jointing, Er Qieke
To ensure the dimensional stability of metal Ti rings, it is ensured that the Stability Analysis of Structures of the retina device after connection.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：Au-Si described in step one
The thickness of solder piece is that the mass fraction of Au elements in 30 μm~130 μm, and described Au-Si solder pieces is 96%, Si elements
Mass fraction be 4%.Other are identical with specific embodiment one.
Specific embodiment three：One of present embodiment and specific embodiment one or two difference is：In step 2
Temperature be 30 DEG C under conditions of be cleaned by ultrasonic 8min.Other are identical with specific embodiment one or two.
Specific embodiment four：One of present embodiment and specific embodiment one to three difference is：Step 3 1. in
Al after cleaning2O3Potsherd fixed placement closes vacuum furnace chamber on the sample bench of Pvd equipment, starts vacuum
System ,≤1 × 10 is extracted into by vacuum-5Under conditions of Pa, while vacuum furnace chamber is preheating into 00 DEG C, argon gas is filled with, adjusts it
Flow is 220sccm, while pulse voltage is set into -900V, temperature be 400 DEG C, vacuum be≤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 with specific embodiment one to three.
Specific embodiment five：One of present embodiment and specific embodiment one to four difference is：Step 3 2. in
After argon ion cleaning, with striking pin in the surface striking of Ti targets, and continue temperature be 400 DEG C, vacuum be≤1 × 10-5Pa, argon
Gas gas flow is that 220sccm and pulse voltage are to be cleaned again using Ti ions under the conditions of -900V, and scavenging period is 15min,
Obtain Al after Ti Ion Cleanings2O3Potsherd.Other are identical with specific embodiment one to four.
Specific embodiment six：One of present embodiment and specific embodiment one to five difference is：Step 3 3. in
After Ti ions terminate, the gas flow of argon gas is adjusted, pressure is remained 1 × 10-1Pa, by Al after Ti Ion Cleanings2O3Ceramics
Before piece is placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target is 8cm, temperature be 400 DEG C, pressure be
1×10-1Under the negative high voltage of Pa, argon gas atmosphere and 5kV, in 90min, the Al after Ti Ion Cleanings2O3Potsherd surface deposits
Thickness is metal Ti layers of 0.8 μm, obtains depositing Ti layer Al2O3Potsherd.Other are identical with specific embodiment one to five.
Specific embodiment seven：One of present embodiment and specific embodiment one to six difference is：Step 3 4. in
Conversion target, it is 1 × 10 to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 90min,
In depositing Ti layer Al2O3It is metal Mo layer of 3.5 μm that a layer thickness is deposited on metal Ti layers of potsherd, obtain depositing Mo layers/
Ti layers of Al2O3Potsherd.Other are identical with specific embodiment one to six.
Specific embodiment eight：One of present embodiment and specific embodiment one to seven difference is：Step 3 5. in
Target is changed again, and it is 1 × 10 to continue to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV,
In 45min, Mo layers/Ti layers Al is being deposited2O3Deposition a layer thickness is Au layers of 0.8 μm, deposition on metal Mo layers of potsherd
After end, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, after being filled with filtering
Pure air is sampled, Al after being metallized to opening the door2O3Potsherd.Other are identical with specific embodiment one to seven.
Specific embodiment nine：One of present embodiment and specific embodiment one to eight difference is：Gold in step 4
Category Ti ring surface metallization：1., metal Ti rings fixed placement after cleaning is closed on the sample bench of Pvd equipment
Vacuum furnace chamber, starts vacuum system, and vacuum is extracted into≤1 × 10-5Under conditions of Pa, while vacuum furnace chamber is preheating into 400
DEG C, argon gas is filled with, its flow is adjusted for 220sccm, it is 400 DEG C, vacuum in temperature while pulse voltage is set into -900V
Spend 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 rings after to argon ion cleaning；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure remains 1 ×
10-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, metal Ti rings are with the distance of sputtering target after argon ion cleaning
12cm, temperature be 400 DEG C, pressure be 1 × 10-1Under the negative high voltage of Pa, argon gas atmosphere and 5kV, in 60min, in argon ion
Metal Ti ring surface deposit thickness is metal Mo layer of 3 μm after cleaning, obtains depositing Mo layers of metal Ti ring；3. target, is changed, is protected
It is 1 × 10 to hold pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, it is golden in Mo layer of deposition in 60min
Deposition a layer thickness is Au layer of 0.4 μm on metal Mo layers of category Ti rings, obtains depositing Au layers/Mo layers metal Ti ring, deposition
After end, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, after being filled with filtering
Pure air is sampled, metal Ti rings after being metallized to opening the door.Other are identical with specific embodiment one to eight.
Specific embodiment ten：One of present embodiment and specific embodiment one to nine difference is：In step 5 when
Vacuum reaches 2 × 10-5After Pa, temperature is heated in the case where firing rate is 10 DEG C/min for 400 DEG C, and is 400 in temperature
DEG C be lower insulation 5min, then control cooling velocity for 8 DEG C/min be cooled to temperature be 100 DEG C.Other and specific embodiment one
It is identical to nine.
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
Contract sample can also realize the purpose of invention.
Using following verification experimental verifications effect of the present invention
Embodiment 1：Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering method for sealing, tool
Body is completed according to the following steps：
First, solder piece is prepared：According to metal Ti ring sizes, Au-Si solder piece punching is matched into metal Ti rings
Au-Si solder rings；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, in temperature
Spend to be cleaned by ultrasonic 8min under conditions of 30 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3After potsherd and cleaning
Au-Si solders；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement sets in physical vapour deposition (PVD)
On standby sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5Under conditions of Pa, while will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, adjusts its flow for 220sccm, while pulse voltage is set to -900V,
Temperature is 400 DEG C, vacuum 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., after argon ion cleaning, drawn on Ti targets surface with striking pin
Arc, and continue temperature be 400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage for-
Cleaned again using Ti ions under the conditions of 900V, scavenging period is 15min, obtain Al after Ti Ion Cleanings2O3Potsherd；③、Ti
After ion terminates, the gas flow of argon gas is adjusted, pressure is remained 1 × 10-1Pa, by Al after Ti Ion Cleanings2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target is 10cm, temperature be 400 DEG C, pressure be 1
×10-1Under the negative high voltage of Pa, argon gas atmosphere and 5kV, in 60min, the Al after Ti Ion Cleanings2O3Potsherd surface deposition of thick
Metal Ti layers for 0.8 μm is spent, depositing Ti layer Al is obtained2O3Potsherd；4. target, is changed, it is 1 × 10 to keep pressure-1Pa,
Temperature is 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 90min, in depositing Ti layer Al2O3Metal Ti layers of potsherd
On to deposit a layer thickness be metal Mo layer of 3 μm, obtain Mo layers/Ti layers Al of deposition2O3Potsherd；5. target, is changed again,
It is 1 × 10 to continue to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 45min, in deposition
Mo layers/Ti layers Al2O3Deposition a layer thickness is Au layer of 0.6 μm on metal Mo layers of potsherd, after deposition terminates, closes electricity
Source and argon gas are switched, and when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system, are filled with the pure air after filtering to opening
Door, sampling, Al after being metallized2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti ring fixed placements after cleaning in Pvd equipment
On sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum 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, adjusts its flow for 220sccm, while pulse voltage is set to -850V, in temperature
For 400 DEG C, vacuum are≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
Cleaning 10min, obtains metal Ti rings after argon ion cleaning；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure
Remain 1 × 10 by force-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti rings with splash
The distance shot at the target be 10cm, temperature be 400 DEG C, pressure be 1 × 10-1Under the negative high voltage of Pa, argon gas atmosphere and 4kV, in 60min
Interior, metal Ti ring surface deposit thickness is metal Mo layer of 2 μm after argon ion cleaning, obtains depositing Mo layers of metal Ti ring；③、
Conversion target, it is 1 × 10 to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV, in 50min,
It is Au layers of 0.3 μm to deposit a layer thickness on Mo layer metal Mo layer of metal Ti rings of deposition, obtain depositing Au layers/Mo layers it is golden
Category Ti rings, after deposition terminates, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
The pure air after filtering is filled with to opening the door, is sampled, metal Ti rings after being metallized；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3Potsherd and metallization after metal Ti rings it
Between, welding equipment part to be welded is constituted, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 2 × 10-5After Pa,
Firing rate is to be heated to temperature for 400 DEG C under 10 DEG C/min, and it is lower insulation 5min to be 400 DEG C in temperature, then controls cooling
Speed is cooled to temperature for 100 DEG C for 8 DEG C/min, then cools to room temperature with the furnace, that is, complete artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring soldering sealing-ins.
The thickness of Au-Si solders piece described in the present embodiment step one is Au units in 80 μm, and described Au-Si solder pieces
The mass fraction of element is 4% for the mass fraction of 96%, Si elements.
According to method provided by the present invention, it is dense to connect the joint for obtaining, and with biocompatibility, and even
The shear strength of joint is 25MPa.
Embodiment 2：Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering method for sealing, tool
Body is completed according to the following steps：
First, solder piece is prepared：According to metal Ti ring sizes, Au-Si solder piece punching is matched into metal Ti rings
Au-Si solder rings；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, in temperature
Spend to be cleaned by ultrasonic 8min under conditions of 30 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3After potsherd and cleaning
Au-Si solders；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement sets in physical vapour deposition (PVD)
On standby sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5Under conditions of Pa, while will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, adjusts its flow for 220sccm, while pulse voltage is set to -900V,
Temperature is 400 DEG C, vacuum 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., after argon ion cleaning, drawn on Ti targets surface with striking pin
Arc, and continue temperature be 400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage for-
Cleaned again using Ti ions under the conditions of 900V, scavenging period is 15min, obtain Al after Ti Ion Cleanings2O3Potsherd；③、Ti
After ion terminates, the gas flow of argon gas is adjusted, pressure is remained 1 × 10-1Pa, by Al after Ti Ion Cleanings2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target is 10cm, temperature be 400 DEG C, pressure be 1
×10-1Under the negative high voltage of Pa, argon gas atmosphere and 4.5kV, in 90min, the Al after Ti Ion Cleanings2O3Potsherd surface deposits
Thickness is metal Ti layers of 0.8 μm, obtains depositing Ti layer Al2O3Potsherd；4. target, is changed, it is 1 × 10 to keep pressure-1Pa,
Temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 90min, in depositing Ti layer Al2O3The metal Ti of potsherd
Deposition a layer thickness is metal Mo layer of 3.5 μm on layer, obtains depositing Mo layers/Ti layers Al2O3Potsherd；5., conversion target again
Material, it is 1 × 10 to continue to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 45min,
Mo layers/Ti layers Al of deposition2O3Deposition a layer thickness is Au layer of 0.8 μm on metal Mo layers of potsherd, after deposition terminates, 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, the pure air after filtering is filled with
To opening the door, sample, Al after being metallized2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti ring fixed placements after cleaning in Pvd equipment
On sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum 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, adjusts its flow for 220sccm, while pulse voltage is set to -850V, in temperature
For 400 DEG C, vacuum are≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
Cleaning 10min, obtains metal Ti rings after argon ion cleaning；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure
Remain 1 × 10 by force-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti rings with splash
The distance shot at the target be 10cm, temperature be 400 DEG C, pressure be 1 × 10-1Under the negative high voltage of Pa, argon gas atmosphere and 5kV, in 60min
Interior, metal Ti ring surface deposit thickness is metal Mo layer of 3 μm after argon ion cleaning, obtains depositing Mo layers of metal Ti ring；③、
Conversion target, it is 1 × 10 to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 5kV, in 60min,
It is Au layers of 0.6 μm to deposit a layer thickness on Mo layer metal Mo layer of metal Ti rings of deposition, obtain depositing Au layers/Mo layers it is golden
Category Ti rings, after deposition terminates, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
The pure air after filtering is filled with to opening the door, is sampled, metal Ti rings after being metallized；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3Potsherd and metallization after metal Ti rings it
Between, welding equipment part to be welded is constituted, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 2 × 10-5After Pa,
Firing rate is to be heated to temperature for 400 DEG C under 10 DEG C/min, and it is lower insulation 5min to be 400 DEG C in temperature, then controls cooling
Speed is cooled to temperature for 100 DEG C for 8 DEG C/min, then cools to room temperature with the furnace, that is, complete artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring soldering sealing-ins.
The thickness of Au-Si solders piece described in the present embodiment step one is Au in 100 μm, and described Au-Si solder pieces
The mass fraction of element is 3.5% for the mass fraction of 96.5%, Si elements.
According to method provided by the present invention, it is dense to connect the joint for obtaining, and with biocompatibility, and even
The shear strength of joint is 28MPa.
Embodiment 3：Al based on artificial retina implant devices2O3Ceramic substrate and metal Ti ring soldering method for sealing, tool
Body is completed according to the following steps：
First, solder piece is prepared：According to metal Ti ring sizes, Au-Si solder piece punching is matched into metal Ti rings
Au-Si solder rings；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, in temperature
Spend to be cleaned by ultrasonic 8min under conditions of 30 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3After potsherd and cleaning
Au-Si solders；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement sets in physical vapour deposition (PVD)
On standby sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5Under conditions of Pa, while will
Vacuum furnace chamber is preheating to 400 DEG C, is filled with argon gas, adjusts its flow for 220sccm, while pulse voltage is set to -900V,
Temperature is 400 DEG C, vacuum 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., after argon ion cleaning, drawn on Ti targets surface with striking pin
Arc, and continue temperature be 400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage for-
Cleaned again using Ti ions under the conditions of 900V, scavenging period is 15min, obtain Al after Ti Ion Cleanings2O3Potsherd；③、Ti
After ion terminates, the gas flow of argon gas is adjusted, pressure is remained 1 × 10-1Pa, by Al after Ti Ion Cleanings2O3Potsherd
Before being placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target is 8cm, temperature be 400 DEG C, pressure be 1
×10-1Under the negative high voltage of Pa, argon gas atmosphere and 4kV, in 60min, the Al after Ti Ion Cleanings2O3Potsherd surface deposition of thick
Metal Ti layers for 0.4 μm is spent, depositing Ti layer Al is obtained2O3Potsherd；4. target, is changed, it is 1 × 10 to keep pressure-1Pa,
Temperature is 400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV, in 90min, in depositing Ti layer Al2O3Metal Ti layers of potsherd
On to deposit a layer thickness be metal Mo layer of 2.8 μm, obtain Mo layers/Ti layers Al of deposition2O3Potsherd；5., conversion target again
Material, it is 1 × 10 to continue to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 4.5kV, in 30min,
Depositing Mo layers/Ti layers Al2O3Deposition a layer thickness is Au layer of 0.5 μm on metal Mo layers of potsherd, after deposition terminates,
Power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 100 DEG C, vacuum system is closed, the cleaning after filtering is filled with empty
Gas is sampled, Al after being metallized to opening the door2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti ring fixed placements after cleaning in Pvd equipment
On sample bench, vacuum furnace chamber is closed, start vacuum system, vacuum 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, adjusts its flow for 220sccm, while pulse voltage is set to -850V, in temperature
For 400 DEG C, vacuum are≤1 × 10-5Pa, argon gas flow are 220sccm and pulse voltage is argon ion under the conditions of -850V
Cleaning 10min, obtains metal Ti rings after argon ion cleaning；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure
Remain 1 × 10 by force-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, argon ion cleaning after metal Ti rings with splash
The distance shot at the target be 10cm, temperature be 400 DEG C, pressure be 1 × 10-1Under the negative high voltage of Pa, argon gas atmosphere and 4kV, in 90min
Interior, metal Ti ring surface deposit thickness is metal Mo layer of 3 μm after argon ion cleaning, obtains depositing Mo layers of metal Ti ring；③、
Conversion target, it is 1 × 10 to keep pressure-1Pa, temperature be 400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV, in 30min,
It is Au layers of 0.5 μm to deposit a layer thickness on Mo layer metal Mo layer of metal Ti rings of deposition, obtain depositing Au layers/Mo layers it is golden
Category Ti rings, after deposition terminates, close power supply and argon gas switch, when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system,
The pure air after filtering is filled with to opening the door, is sampled, metal Ti rings after being metallized；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3Potsherd and metallization after metal Ti rings it
Between, welding equipment part to be welded is constituted, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 2 × 10-5After Pa,
Firing rate is to be heated to temperature for 400 DEG C under 10 DEG C/min, and it is lower insulation 5min to be 400 DEG C in temperature, then controls cooling
Speed is cooled to temperature for 100 DEG C for 8 DEG C/min, then cools to room temperature with the furnace, that is, complete artificial retina implant devices
Al2O3Ceramic substrate and metal Ti ring soldering sealing-ins.
The thickness of Au-Si solders piece described in the present embodiment step one is Au units in 60 μm, and described Au-Si solder pieces
The mass fraction of element is 3% for the mass fraction of 97%, Si elements.
According to method provided by the present invention, it is dense to connect the joint for obtaining, and with biocompatibility, and even
The shear strength of joint is 23MPa.
Claims (10)
1. the Al of artificial retina implant devices is based on2O3Ceramic substrate and metal Ti ring soldering method for sealing, it is characterised in that it
Complete according to the following steps：
First, solder piece is prepared：According to metal Ti ring sizes, by Au-Si solder piece punching into the Au-Si matched with metal Ti rings
Solder ring；
2nd, sample cleaning：By metal Ti rings, Al2O3Potsherd and Au-Si solder rings are respectively placed in acetone soln, are in temperature
It is cleaned by ultrasonic 7min~12min under conditions of 25~35 DEG C, Al after metal Ti rings, cleaning after being cleaned successively2O3Potsherd and
Au-Si solders after cleaning；
3rd, Al2O3Ceramic surface metallization：1. Al after, cleaning2O3Potsherd fixed placement is in the examination of Pvd equipment
On sample platform, vacuum chamber is closed, start vacuum system, vacuum 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, its flow is adjusted for 150sccm~220sccm, while pulse voltage is set to-
850V~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 150sccm~
220sccm and pulse voltage are argon ion cleaning 10min~15min under the conditions of -850V~-950V, after obtaining argon ion cleaning
Al2O3Potsherd；2., after argon ion cleaning, with striking pin in the surface striking of Ti targets, 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 under the conditions of -850V~-950V
Cleaned again using Ti ions, scavenging period is 10min~15min, obtains Al after Ti Ion Cleanings2O3Potsherd；3., Ti from
After son cleaning terminates, the gas flow of argon gas is adjusted, pressure is remained 0.5 × 10-1Pa~1.5 × 10-1Pa, by Ti ions
Al after cleaning2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target for 8cm~
12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV's is negative
Under high pressure, in 60min~120min, the Al after Ti Ion Cleanings2O3Potsherd surface deposit thickness is 0.2 μm~1 μm of gold
Ti layers of category, obtains depositing Ti layer Al2O3Potsherd；4. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10-1Pa,
Temperature be 350~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 60min~120min, in depositing Ti layer
Al2O3Deposition a layer thickness is metal Mo layer of 2 μm~4 μm on metal Ti layers of potsherd, obtains Mo layers/Ti layers of deposition
Al2O3Potsherd；5. target, is changed again, and it is 0.5 × 10 to continue to keep pressure-1Pa~1.5 × 10-1Pa, is 350 in temperature
~400 DEG C, under the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, depositing Mo layers/Ti layers Al2O3Ceramics
Deposition a layer thickness is Au layer of 0.1 μm~0.5 μm on metal Mo layers of piece, after deposition terminates, closes power supply and argon gas is opened
Close, when the temperature of vacuum chamber is down to 80~120 DEG C, close vacuum system, be filled with the pure air after filtering to opening the door, take
Sample, Al after being metallized2O3Potsherd；
4th, metal Ti ring surfaces metallization：1., by metal Ti rings fixed placement after cleaning in the sample of Pvd equipment
On platform, vacuum furnace chamber is closed, start vacuum system, vacuum 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, its flow are adjusted for 150~220sccm, while pulse voltage is set into -850
~-950V, temperature be 350~400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow are 150sccm~220sccm
It is argon ion cleaning 10min~15min under the conditions of -850V~-950V with pulse voltage, obtains metal Ti after argon ion cleaning
Ring；2. after, argon ion cleaning terminates, the flow of argon gas is adjusted so that pressure remains 0.5 × 10-1Pa~1.5 × 10-1Pa,
Before metal Ti rings are placed in sputtering target after argon ion is cleaned, after argon ion cleaning the distance of metal Ti rings and sputtering target for 8cm~
12cm, temperature be 350~400 DEG C, pressure be 0.5 × 10-1Pa~1.5 × 10-1Pa, argon gas atmosphere and 4kV~5kV's is negative
Under high pressure, in 60min~120min, metal Ti ring surface deposit thickness is 2 μm~4 μm of metal Mo after argon ion cleaning
Layer, obtains depositing Mo layers of metal Ti ring；3. target, is changed, it is 0.5 × 10 to keep pressure-1Pa~1.5 × 10-1Pa, in temperature
Under for 350~400 DEG C, the negative high voltage of argon gas atmosphere and 4kV~5kV, in 30min~60min, Mo layers of metal Ti ring is being deposited
Metal Mo layers on to deposit a layer thickness be Au layer of 0.1 μm~0.5 μm, obtain depositing Au layers/Mo layers metal Ti ring, deposit
After end, power supply and argon gas switch are closed, when the temperature of vacuum chamber is down to 80~120 DEG C, close vacuum system, be filled with filtering
Pure air afterwards is sampled, metal Ti rings after being metallized to opening the door；
5th, sealing-in：Au-Si solders after cleaning are placed in Al after metallizing2O3After potsherd and metallization between metal Ti rings, group
Into welding equipment part to be welded, welding equipment part to be welded is placed in vacuum brazing furnace, when vacuum reaches 1.50 × 10-5Pa~2.50 ×
10-5After Pa, temperature is heated in the case where firing rate is 8 DEG C/min~12 DEG C/min for 390~420 DEG C, and is 390 in temperature
~420 DEG C be lower insulation 3min~5min, then control cooling velocity for 5 DEG C/min~10 DEG C/min be cooled to temperature be 80~
120 DEG C, then cool to room temperature with the furnace, that is, complete the Al of artificial retina implant devices2O3Ceramic substrate and metal Ti ring solderings
Sealing-in.
2. the Al based on artificial retina implant devices according to claim 12O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that the thickness of the pieces of Au-Si solders described in step one is 30 μm~130 μm, and described Au-Si solders
The mass fraction of Au elements is that the mass fraction of 95%~97.25%, Si elements is 2.75%~5% in piece.
3. the Al based on artificial retina implant devices according to claim 12O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that be cleaned by ultrasonic 8min under conditions of being 30 DEG C in temperature in step 2.
4. the Al based on artificial retina implant devices according to claim 12O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that step 3 is 1. middle by Al after cleaning2O3Potsherd fixed placement is in the sample of Pvd equipment
On platform, vacuum furnace chamber is closed, start vacuum system, vacuum 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, its flow is adjusted for 220sccm, while pulse voltage is set into -900V, are in temperature
400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow are that 220sccm and pulse voltage are that argon ion is clear under the conditions of -900V
15min is washed, Al after argon ion cleaning is obtained2O3Potsherd.
5. the Al based on artificial retina implant devices according to claim 42O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that 2. step 3 after the cleaning of middle argon ion, be in temperature in the surface striking of Ti targets, and continuation with striking pin
400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage be under the conditions of -900V using Ti from
Son is cleaned again, and scavenging period is 15min, obtains Al after Ti Ion Cleanings2O3Potsherd.
6. the Al based on artificial retina implant devices according to claim 52O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that step 3 adjusts the gas flow of argon gas after 3. middle Ti ions terminate, and pressure is remained 1 × 10- 1Pa, by Al after Ti Ion Cleanings2O3Before potsherd is placed in sputtering target, Al after Ti Ion Cleanings2O3The distance of potsherd and sputtering target
Be 10cm, temperature be 400 DEG C, pressure be 1 × 10-1Under the negative high voltage of Pa, argon gas atmosphere and 4kV~5kV, 60min~
In 90min, the Al after Ti Ion Cleanings2O3Potsherd surface deposit thickness is metal Ti layer of 0.4 μm~0.8 μm, is deposited
Ti layers of Al2O3Potsherd.
7. the Al based on artificial retina implant devices according to claim 62O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that step 3 4. middle conversion target, it is 1 × 10 to keep pressure-1Pa, is 400 DEG C, argon gas atmosphere in temperature
Under the negative high voltage of 4kV~5kV, in 90min, in depositing Ti layer Al2O3A layer thickness is deposited on metal Ti layers of potsherd
It is metal Mo layers of 2.8 μm~3.5 μm, obtains depositing Mo layers/Ti layers Al2O3Potsherd.
8. the Al based on artificial retina implant devices according to claim 72O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that step 3 5. in change target again, it is 1 × 10 to continue to keep pressure-1Pa, temperature be 400 DEG C,
Under the negative high voltage of argon gas atmosphere and 4.5kV~5kV, in 30min~45min, Mo layers/Ti layers Al is being deposited2O3The gold of potsherd
Deposition a layer thickness is Au layer of 0.1 μm~0.5 μm on Mo layers of category, after deposition terminates, closes power supply and argon gas switch, treats true
When the temperature of cavity is down to 100 DEG C, vacuum system is closed, be filled with the pure air after filtering to opening the door, sampling is metallized
Al afterwards2O3Potsherd.
9. the Al based on artificial retina implant devices according to claim 12O3Ceramic substrate is sealed with the soldering of metal Ti rings
Connect method, it is characterised in that metal Ti ring surfaces metallization in step 4：1. metal Ti ring fixed placements are in physics after, cleaning
On the sample bench of vapor deposition apparatus, vacuum furnace chamber is closed, start vacuum system, vacuum is extracted into≤1 × 10-5The condition of Pa
Under, while vacuum furnace chamber is preheating into 400 DEG C, argon gas is filled with, its flow is adjusted for 220sccm, while pulse voltage is set
Be -900V, temperature be 400 DEG C, vacuum be≤1 × 10-5Pa, argon gas flow be 220sccm and pulse voltage for-
Argon ion cleaning 10min under the conditions of 900V, obtains metal Ti rings after argon ion cleaning；2. after, argon ion cleaning terminates, argon is adjusted
The flow of gas so that pressure remains 1 × 10-1Pa, before metal Ti rings are placed in sputtering target after argon ion is cleaned, argon ion cleaning
The distance of metal Ti rings and sputtering target is 10cm afterwards, temperature be 400 DEG C, pressure be 1 × 10-1Pa, argon gas atmosphere and 4kV~
Under the negative high voltage of 5kV, in 60min~90min, metal Ti ring surface deposit thickness is 2 μm~3 μm after argon ion cleaning
Metal Mo layers, obtain depositing Mo layers of metal Ti ring；3. target, is changed, it is 1 × 10 to keep pressure-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 metal Mo layers of metal Ti rings of deposition
Deposition a layer thickness is Au layer of 0.5 μm~0.8 μm, obtains depositing Au layers/Mo layers metal Ti ring, after deposition terminates, closes electricity
Source and argon gas are switched, and when the temperature of vacuum chamber is down to 100 DEG C, close vacuum system, are filled with the pure air after filtering to opening
Door, sampling, metal Ti rings after being metallized.
10. the Al based on artificial retina implant devices according to claim 12O3Ceramic substrate and metal Ti ring solderings
Method for sealing, it is characterised in that when vacuum reaches 2 × 10 in step 5-5After Pa, add in the case where firing rate is 10 DEG C/min
Heat to temperature is 400 DEG C, and it is lower insulation 5min to be 400 DEG C in temperature, then controls cooling velocity to be cooled to temperature for 8 DEG C/min
It is 100 DEG C.
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| CN110683855A (en) * | 2018-07-05 | 2020-01-14 | 哈尔滨工业大学 | Biocompatible Al2O3Method for diffusion bonding of Ti |
| CN110722234A (en) * | 2019-10-11 | 2020-01-24 | 哈尔滨工业大学 | Nickel titanium base alloy low-temperature connecting joint and preparation method thereof |
| CN110734296A (en) * | 2019-10-11 | 2020-01-31 | 哈尔滨工业大学 | connection joint based on nickel-based superalloy and ceramic and preparation method thereof |
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