CN105272369B - A kind of porous ceramics connection method - Google Patents
A kind of porous ceramics connection method Download PDFInfo
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- CN105272369B CN105272369B CN201510830337.XA CN201510830337A CN105272369B CN 105272369 B CN105272369 B CN 105272369B CN 201510830337 A CN201510830337 A CN 201510830337A CN 105272369 B CN105272369 B CN 105272369B
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Abstract
A kind of porous ceramics connection method, it is related to a kind of ceramic joining method.It is to solve in existing porous ceramics and metal connection procedure, while when realizing that wetability improves and thermal stress alleviates, the problem of process complexity.Method：First, formulated phenolic resin organic solution；2nd, porous ceramics is heat-treated；3rd, porous ceramics connects.The present invention utilizes the top layer pore structure of porous ceramics, solder infiltration is entered intrinsic silicon and form the attachment structure that mechanical snap is combined with chemical combination key, it not only can effectively alleviate joint residual thermal stress, and add interfacial reaction calmodulin binding domain CaM, be advantageous to the raising of strength of joint.The present invention is used for ceramics and metal material connection area.
Description
Technical field
The present invention relates to a kind of ceramic joining method.
Background technology
Due to there is thermophysical property mismatch problem in ceramics and metal material so that ceramics and metal exist in this connection
The problem of residual stress is big, and strength of joint is low or even can not effectively connect.How to reduce Ceramic and metal joining stress is to obtain
The key of highly reliable ceramic/metal composite article.Substantial amounts of document report is by using joint gradient powder method, composite soldering
Method, soft or rigid cushion method, porous material or metal web padded coaming method are portalled in ceramic surface processing, rectangle
The structures such as ripple, triangular wave or sine wave can alleviate postwelding thermal stress to a certain extent, improve strength of joint.Again by
The lamination layer structure of one layer of ceramics of ceramic post sintering and metal so that ceramic surface metallization, be then connected and obtain with other metals again
The effect of obvious reduction Ceramic and metal joining joint thermal stress was obtained, it is in actual applications to have embodiment more.Porous pottery
For porcelain due to low intensity, the thermal stress of Welded Joints is more sensitive, and at the same time its loose structure to use traditional
Method for metallising alleviates the connection stress with metal.According to traditional metallization, ceramic and intermetallic profit can be improved
It is moist, but the follow-up alleviation for also needing to carry out thermal stress using other a series of complex methods, process are more complicated.
Therefore exploitation is adapted with porous ceramics method for metallising and realize its with metal material be reliably connected for
Its application in Practical Project is most important.
The content of the invention
The present invention is to solve in existing porous ceramics and metal connection procedure, while realize that wetability improves and thermal stress
During alleviation, the problem of process complexity, there is provided a kind of porous ceramics connection method.
Porous ceramics connection method of the present invention, is carried out according to the following steps：
First, formulated phenolic resin organic solution
Water soluble phenol resin and solvent are weighed, dose volume concentration is 30%~70% organic solution；
2nd, porous ceramics is heat-treated
Porous ceramics is placed in organic solution after vacuum infiltration, is put into precuring in baking oven, wherein vacuum infiltration time
For 30~60min, oven temperature is 120~170 DEG C, and hardening time is 1~24h；
The porous ceramics infiltrated after solidifying is placed in vacuum sintering furnace, treats that vacuum reaches 7.0 × 10-2Pa~1.5 ×
10-2During Pa, 900~1200 DEG C are heated to 15~30 DEG C/min of heating rate, and is incubated 10~30min, is then turned off power supply
Room temperature is naturally cooled to, that is, the porous ceramics being heat-treated；
3rd, porous ceramics connects
To contain Si inactive metal solders be placed in porous ceramics with connector pre-connection face prepare combine exemplar, wherein pricker
It is 10~400 μm to expect thickness；
Combination exemplar is put into vacuum brazing stove and vacuumized, treats that vacuum reaches 7.0 × 10-2Pa~1.5 × 10-2Pa
When, 900~1400 DEG C are heated to 10~30 DEG C/min of heating rate, and 10~30min is incubated, then with 5~20 DEG C/min
Cooldown rate be cooled to 300~500 DEG C, power off and naturally cool to room temperature, that is, the porous ceramics exemplar after being connected.
Solvent is acetone or methanol in step 1.
Contain carbon simple substance in porous ceramics hole in step 2 after heat treatment.
Solder modes of emplacement can be that simple substance multilayer is laid, mixed-powder single or multiple lift is laid in step 3.
The principle of the present invention：
This method improves its wetability to brazing filler metal alloy by carrying out inner surface treatment to the hole in porous ceramics
Energy.Infiltrated through to a certain extent inside porous ceramics by the brazing filler metal alloy of fusing, realize that porous ceramics is connected one with metal
Side cermet Composite, the method can make porous ceramic material, be then connected again with metal material, can also be porous
While ceramic metallization, while realize the connection with metal material.This method utilizes porous ceramics hole characteristic, on the one hand connects
Solder cladding fills and leads up top layer hole and penetrates into intrinsic silicon when connecing, the company being combined with forming mechanical snap between matrix with chemical combination key
Binding structure, increase the adhesion of metal and porous ceramics, on the other hand because the formation of cermet Composite layer adds boundary
Face reaction bonded region, the gradual transition from porous ceramics to metal side is realized, therefore it is residual effectively to alleviate joint
Waste heat stress, improve strength of joint.
The preparation method of the present invention has the following advantages that：
1st, the present invention utilizes porous ceramics hole feature, is raw material at ceramic surface carburizing using phenolic resin organic solution
Reason, the species by porous ceramics, the shape of internal porosity, dimension constraint, can not prepared in porous ceramic surface and hole
It is uniformly distributed, the graphite carbon film that form is consistent；In brazing process, the free silica in liquid solder reacts with carbon film, more
Hole ceramic surface and pore surface generation SiC, make ceramic surface form the composite construction of metal/ceramic, realize porous pottery
The surface metalation of porcelain, so as to improve wetability of the solder to ceramics.
2nd, the present invention utilizes the top layer pore structure of porous ceramics, solder infiltration is entered intrinsic silicon and forms mechanical snap
With the attachment structure that chemical combination key is combined, it not only can effectively alleviate joint residual thermal stress, and add interfacial reaction
Calmodulin binding domain CaM, be advantageous to the raising of strength of joint.
3rd, present invention process is simple, and repeatability is high, and carbon content is controllable, and large scale, complex-shaped sample can be carried out
Case-carbonizing is handled, and connects porous ceramics in this way, joint design is simple, and interface binding power is strong, and can be synchronous
The problem of improving wetability difference and big residual stress, it is adapted to industrialization production, there is fabulous industrial applications prospect.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
Embodiment one：Present embodiment porous ceramics connection method, is carried out according to the following steps：
First, formulated phenolic resin organic solution
Water soluble phenol resin and solvent are weighed, dose volume concentration is 30%~70% organic solution；
2nd, porous ceramics is heat-treated
Porous ceramics is placed in organic solution after vacuum infiltration, is put into precuring in baking oven, wherein vacuum infiltration time
For 30~60min, oven temperature is 120~170 DEG C, and hardening time is 1~24h；
The porous ceramics infiltrated after solidifying is placed in vacuum sintering furnace, treats that vacuum reaches 7.0 × 10-2Pa~1.5 ×
10-2During Pa, 900~1200 DEG C are heated to 15~30 DEG C/min of heating rate, and is incubated 10~30min, is then turned off power supply
Room temperature is naturally cooled to, that is, the porous ceramics being heat-treated；
3rd, porous ceramics connects
To contain Si inactive metal solders be placed in porous ceramics with connector pre-connection face prepare combine exemplar, wherein pricker
It is 10~400 μm to expect thickness；
Combination exemplar is put into vacuum brazing stove and vacuumized, treats that vacuum reaches 7.0 × 10-2Pa~1.5 × 10-2Pa
When, 900~1400 DEG C are heated to 10~30 DEG C/min of heating rate, and 10~30min is incubated, then with 5~20 DEG C/min
Cooldown rate be cooled to 300~500 DEG C, power off and naturally cool to room temperature, that is, the porous ceramics exemplar after being connected.
Present embodiment utilizes porous ceramics hole characteristic, when on the one hand connecting solder cladding fill and lead up top layer hole and penetrate into
The knot of intrinsic silicon, the attachment structure being combined with forming mechanical snap between matrix with chemical combination key, increase metal and porous ceramics
With joint efforts, on the other hand realized because the formation of cermet Composite layer adds interfacial reaction calmodulin binding domain CaM from porous pottery
Gradual transition of the porcelain to metal side, therefore can effectively alleviate joint residual thermal stress, improve strength of joint.
Embodiment two：Present embodiment is unlike embodiment one：Solvent is acetone in step 1
Or methanol.It is other identical with embodiment one.
Embodiment three：Present embodiment is unlike embodiment one or two：It is organic molten in step 1
The volumetric concentration of liquid is 40%~60%.It is other identical with embodiment one or two.
Embodiment four：Present embodiment is unlike embodiment one or two：It is organic molten in step 1
The volumetric concentration of liquid is 50%.It is other identical with embodiment one or two.
Embodiment five：Unlike one of present embodiment and embodiment one to four：It is true in step 2
The sky infiltration time is 40~50min.It is other identical with one of embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：It is solid in step 2
The change time is 5~20h.It is other identical with one of embodiment one to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to five：It is solid in step 2
The change time is 10~15h.It is other identical with one of embodiment one to five.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Will in step 2
Porous ceramics after infiltration solidification is placed in vacuum sintering furnace, and vacuum reaches 9.0 × 10-2Pa~1.3 × 10-2Pa.It is other with
One of embodiment one to seven is identical.
Embodiment nine：Unlike one of present embodiment and embodiment one to seven：Will in step 2
Porous ceramics after infiltration solidification is placed in vacuum sintering furnace, and vacuum reaches 1 × 10-2Pa~1.2 × 10-2Pa.Other and tool
One of body embodiment one to seven is identical.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：In step 2 with
20~26 DEG C/min of heating rate is heated to 1000~1100 DEG C.It is other identical with one of embodiment one to nine.
Embodiment 11：Unlike one of present embodiment and embodiment one to ten：In step 2
Porous ceramics is the composite ceramic material of composite ceramics or activeness and quietness, and the composite ceramics is Si3N4Ceramic, SiAlON ceramics,
Si2N2O ceramics, AlN ceramic, TiN ceramics, SiC ceramic, SiBCN ceramics, BN ceramics, ZrO2Ceramics, Al2O3Ceramics, TiB2Pottery
Porcelain, B4C ceramics, ZrB2Ceramics, TaB2Ceramics, ZrC ceramics, MoSi2Two kinds in ceramics, MAX phase ceramics, fused quartz ceramicses or
Two or more to be mutually combined, the composite ceramic material of the activeness and quietness is that the long fiber, short cut is added in composite ceramics
Cut the composite ceramic material that fiber, whisker, nanotube, nano wire, graphene or particle preparation form.Other and specific embodiment party
One of formula one to ten is identical.
Particle described in present embodiment is the particulate matter for ceramic activeness and quietness.
Embodiment 12：Present embodiment is unlike embodiment one to one of 11：Step 2
Middle porous ceramics hole rate is 5%~90%.It is other identical with embodiment one to one of 11.
Embodiment 13：Present embodiment is unlike embodiment one to one of 12：Step 3
In in the solder of inactive metal containing Si inactive metal be Co, Cu, Ni, Sn, Fe, Pr, Pd, Ag or Au, the shape of inactive metal
State is powder, eutectic alloy or paillon foil.It is other identical with embodiment one to one of 12.
The solder of inactive metal containing Si described in present embodiment is to be prepared by inactive metal according to this area conventional method
The solder formed.The solder of inactive metal containing Si is also commercially available.
Embodiment 14：Present embodiment is unlike embodiment one to one of 13：Step 3
Middle solder modes of emplacement can be that simple substance multilayer is laid, mixed-powder single or multiple lift is laid.It is other with embodiment one to
One of 13 is identical.
Embodiment 15：Present embodiment is unlike embodiment one to one of 14：Step 3
Middle solder thickness is 50~300 μm.It is other identical with embodiment one to one of 14.
Embodiment 16：Present embodiment is unlike embodiment one to one of 14：Step 3
Middle solder thickness is 100~200 μm.It is other identical with embodiment one to one of 14.
Tests below is carried out for checking beneficial effects of the present invention：
Embodiment 1：
The present embodiment is used as porous Si carbon containing after being heat-treated3N4Ceramics itself connection, is specifically realized by the following method.
First, it is medium to porous Si using acetone3N4Ceramics carry out 3 times and are cleaned by ultrasonic, 5min/ times；
2nd, 20ml phenolic resin and 20ml acetone are weighed, is configured to 50% phenolic resin organic solution；
3rd, by porous Si3N4Ceramics, which are placed in phenolic resin organic solution after vacuum infiltration 30min, to be put into 120 DEG C of baking ovens
Precuring 2h；
4th, by the porous Si after solidification3N4Ceramics are placed in sintering furnace and are heat-treated, and treat that vacuum reaches 1.5 × 10- 21000 DEG C of insulation 20min are heated to 20 DEG C/min speed after Pa, room temperature is naturally cooled to, that is, obtains the porous Si of carburizing3N4
Ceramic sample.
5th, Co-Si alloy sheets are placed in two pieces of carbon containing porous Si3N4Among ceramic, two groups of samples are put into soldering furnace
In, treat that vacuum reaches 1.5 × 10-21260 DEG C of insulation 10min are risen to 20 DEG C/min programming rate after Pa, with 10 DEG C/min
Speed is cooled to 400 DEG C, then naturally cools to room temperature, that is, obtains porous Si3N4Ceramic joining test specimen.
Co-Si alloy sheets brazing filler metal compositions useful (at%) is 22.5Co-77.5Si in step 5.
Embodiment 2：
The present embodiment is used as porous Si carbon containing after being heat-treated3N4Ceramics itself connection, is specifically realized by the following method.
First, it is medium to porous Si using acetone3N4Ceramics carry out 3 times and are cleaned by ultrasonic, 5min/ times；
2nd, 20ml phenolic resin and 20ml acetone are weighed, is configured to 50% phenolic resin organic solution；
3rd, by porous Si3N4Ceramics, which are placed in phenolic resin organic solution after vacuum infiltration 30min, to be put into 120 DEG C of baking ovens
Precuring 2h；
4th, by the porous Si after solidification3N4Ceramics are placed in sintering furnace and are heat-treated, and treat that vacuum reaches 1.5 × 10- 21000 DEG C of insulation 20min are heated to 20 DEG C/min speed after Pa, room temperature is naturally cooled to, that is, obtains the porous Si of carburizing3N4
Ceramic sample.
5th, Co-Si-B alloy sheets are placed in two pieces of carbon containing porous Si3N4Among ceramic, two groups of samples are put into soldering furnace
In, treat that vacuum reaches 1.5 × 10-21080 DEG C of insulation 10min are risen to 20 DEG C/min programming rate after Pa, with 10 DEG C/min
Speed is cooled to 400 DEG C, then naturally cools to room temperature, that is, obtains porous Si3N4Ceramic joining test specimen.
Co-Si-B alloy sheets brazing filler metal compositions useful (at%) is 73.5Co-11.5Si-15B in step 5.
Embodiment 3：
The present embodiment is used as porous Si carbon containing after being heat-treated3N4Ceramics are connected with metal niobium, specifically real by the following method
It is existing.
First, it is medium to porous Si using acetone3N4Ceramics and niobium block carry out 3 times and are cleaned by ultrasonic, 5min/ times；
2nd, 20ml phenolic resin and 20ml acetone are weighed, is configured to 50% phenolic resin organic solution；
3rd, by porous Si3N4Ceramics, which are placed in phenolic resin organic solution after vacuum infiltration 30min, to be put into 120 DEG C of baking ovens
Precuring 2h；
4th, by the porous Si after solidification3N4Ceramics are placed in sintering furnace and are heat-treated, and treat that vacuum reaches 1.5 × 10- 21000 DEG C of insulation 20min are heated to 20 DEG C/min speed after Pa, room temperature is naturally cooled to, that is, obtains the porous Si of carburizing3N4
Ceramic sample.
The 5th, Co-Si-Nb alloy sheets are placed in carbon containing porous Si3N4Ceramics are among niobium, welding is put into by two groups of samples
In stove, treat that vacuum reaches 1.5 × 10-2After Pa with 20 DEG C/min programming rate rise to 1200 DEG C insulation 10min, with 10 DEG C/
Min speed is cooled to 400 DEG C, then naturally cools to room temperature, that is, obtains porous Si3N4Ceramics are connected test specimen with niobium.
Co-Si-Nb alloy sheets brazing filler metal compositions useful (at%) is 96Co-2.5Si-1.5Nb in step 5.
Solder and mother metal angle of wetting and soldering rear joint shear strength are shown in Table 1 after carburizing in embodiment 1,2 and 3：
Table 1：
| Connect temperature (DEG C) | Connection Time (min) | Brazing filler metal compositions useful (at%) | Angle of wetting (°) | Shear strength (MPa) |
| 1260 | 10 | 22.5Co-77.5Si | 5 | 108, break on ceramic mother metal |
| 1080 | 10 | 73.5Co-11.5Si-15B | 5 | 116, break on ceramic mother metal |
| 1200 | 10 | 96Co-2.5Si-1.5Nb | 10 | 130, break on ceramic mother metal |
Claims (8)
1. a kind of porous ceramics connection method, it is characterised in that this method is carried out according to the following steps：
First, formulated phenolic resin organic solution
Water soluble phenol resin and solvent are weighed, dose volume concentration is 30%~70% organic solution；
2nd, porous ceramics is heat-treated
Porous ceramics is placed in organic solution after vacuum infiltration, is put into precuring in baking oven, the wherein vacuum infiltration time is 30
~60min, oven temperature are 120~170 DEG C, and hardening time is 1~24h；
The porous ceramics infiltrated after solidifying is placed in vacuum sintering furnace, treats that vacuum reaches 7.0 × 10-2Pa~1.5 × 10-2Pa
When, 900~1200 DEG C are heated to 15~30 DEG C/min of heating rate, and 10~30min is incubated, it is naturally cold to be then turned off power supply
But to room temperature, that is, the porous ceramics being heat-treated；
3rd, porous ceramics connects
Si inactive metal solders will be contained it is placed in porous ceramics and combine exemplar with being prepared on connector pre-connection face, wherein solder thickness
Spend for 10~400 μm；
Combination exemplar is put into vacuum brazing stove and vacuumized, treats that vacuum reaches 7.0 × 10-2Pa~1.5 × 10-2During Pa, with
10~30 DEG C/min of heating rate is heated to 900~1400 DEG C, and is incubated 10~30min, then with 5~20 DEG C/min cooling
Speed is cooled to 300~500 DEG C, powers off and naturally cools to room temperature, that is, the porous ceramics exemplar after being connected；
Inactive metal is Co, Cu, Ni, Sn, Pd, Ag or Au in the solder of inactive metal containing Si in step 3, inactive metal
State be powder or paillon foil.
A kind of 2. porous ceramics connection method according to claim 1, it is characterised in that in step 1 solvent be acetone or
Methanol.
A kind of 3. porous ceramics connection method according to claim 1, it is characterised in that the body of organic solution in step 1
Product concentration is 40%~60%.
A kind of 4. porous ceramics connection method according to claim 1, it is characterised in that in step 2 hardening time be 5~
20h。
5. a kind of porous ceramics connection method according to claim 1, it is characterised in that porous ceramics is multiple in step 2
Ceramics are closed, the composite ceramics is Si3N4Ceramics, SiAlON ceramics, Si2N2O ceramics, AlN ceramic, TiN ceramics, SiC ceramic,
SiBCN ceramics, BN ceramics, ZrO2Ceramics, Al2O3Ceramics, TiB2Ceramics, B4C ceramics, ZrB2Ceramics, TaB2Ceramic, ZrC ceramics,
MoSi2Two or more in ceramics, MAX phase ceramics, fused quartz ceramicses is mutually combined.
6. a kind of porous ceramics connection method according to claim 5, it is characterised in that porous ceramics is increasing in step 2
The composite ceramic material of strong toughness reinforcing, the composite ceramic material of the activeness and quietness are that the long fiber, short cut is added in composite ceramics
Cut the composite ceramic material that fiber, whisker, nanotube, nano wire, graphene or particle preparation form.
7. a kind of porous ceramics connection method according to claim 1, it is characterised in that solder thickness is 50 in step 3
~300 μm.
8. a kind of porous ceramics connection method according to claim 1, it is characterised in that solder thickness is 100 in step 3
~200 μm.
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| CN107182139B (en) * | 2016-03-11 | 2020-06-09 | 周宏明 | Metal film porous ceramic heating body and application thereof |
| CN105796211B (en) * | 2016-05-19 | 2018-09-18 | 北京爱康宜诚医疗器材有限公司 | Prosthetic component and its manufacturing method |
| CN105877876B (en) * | 2016-05-19 | 2018-07-03 | 北京爱康宜诚医疗器材有限公司 | Hip prosthesis component |
| CN105919698A (en) * | 2016-05-19 | 2016-09-07 | 北京爱康宜诚医疗器材有限公司 | Prosthesis assembly and manufacturing method thereof |
| CN108218462A (en) * | 2016-12-22 | 2018-06-29 | 中国科学院上海硅酸盐研究所 | Resin based sizing and SiC ceramic reaction forming method |
| CN109369209B (en) * | 2018-12-06 | 2021-03-30 | 哈尔滨工业大学 | Method for auxiliary brazing of porous negative expansion ceramic interlayer |
| CN110407600A (en) * | 2019-07-29 | 2019-11-05 | 浙江工业大学 | A method of SiC ceramic is connected using Au base high-temp solder |
| CN110370748B (en) * | 2019-07-31 | 2021-03-16 | 成都工业学院 | Metal-ceramic composite material with high interface bonding strength and preparation method thereof |
| CN110723979B (en) * | 2019-11-12 | 2022-02-08 | 中国工程物理研究院核物理与化学研究所 | MAX phase ceramic connection method |
| CN114043026B (en) * | 2021-11-12 | 2023-08-29 | 哈尔滨工业大学 | Stress relieving method in ceramic-metal |
| CN115991609A (en) * | 2023-01-09 | 2023-04-21 | 南京理工大学 | Ceramic-metal discharge plasma connection method |
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| CN105016762B (en) * | 2015-07-22 | 2017-06-20 | 哈尔滨工业大学 | One kind reinforcing porous ceramics connector connecting method |
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