CN111454063A - Ceramic connecting piece with compact connecting layer and connecting method and application thereof - Google Patents

Ceramic connecting piece with compact connecting layer and connecting method and application thereof Download PDF

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CN111454063A
CN111454063A CN202010258895.4A CN202010258895A CN111454063A CN 111454063 A CN111454063 A CN 111454063A CN 202010258895 A CN202010258895 A CN 202010258895A CN 111454063 A CN111454063 A CN 111454063A
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ceramic
powder
dense
layer
connection
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CN111454063B (en
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郭伟明
吴利翔
何盛金
牛文彬
詹创添
朱林林
林华泰
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Guangdong University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
    • C04B35/58014—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON
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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining

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Abstract

The invention belongs to the technical field of ceramic connection, and discloses a ceramic connecting piece with a compact connecting layer, a connecting method and application thereof, wherein the ceramic connecting piece is prepared by adding a solvent and a ball-milling medium into ceramic powder, mixing and drying to obtain ball-milled powder, and carrying out dry pressing and cold isostatic pressing treatment on the powder to obtain a ceramic green body; and then placing the metal connecting material foil or powdery 316 stainless steel between the polished ceramic green bodies, and sintering at 1200-1600 ℃ in a vacuum environment to obtain the ceramic green body. The method can realize compact connection of ceramic materials, and the prepared ceramic connecting piece has good corrosion resistance, the shear strength at room temperature is 150-200 MPa, the shear strength at high temperature of 1200 ℃ is 100-150 MPa, and the residual stress of the joint is 50-100 MPa.

Description

Ceramic connecting piece with compact connecting layer and connecting method and application thereof
Technical Field
The invention belongs to the technical field of ceramic connection, and particularly relates to a ceramic connecting piece with a compact connecting layer, a connecting method and application thereof.
Background
Si3N4Generally, structural ceramics such as SiC, TiC and the like have excellent characteristics of high strength, high hardness, high temperature resistance, wear resistance, corrosion resistance, high temperature resistance and the like, and have wide application in the fields of metallurgy, vehicles, aerospace and the like. However, the above materials have excellent mechanical properties, and the difficult processability thereof also limits the application thereof in the field of complex structural members. Therefore, the components with complex shapes need to be manufactured by the connection technology between ceramics. However, the complex-shaped parts cannot be pressed during the joining process. Therefore, a conventional bonding method under pressure conditions, such as NITE bonding, solid phase diffusion bonding, MAX bonding, cannot be used; for precursor connection, although connection under a non-pressure condition can be realized, the connection strength is low, and the defects of a connection layer are more; the glass ceramic connection can also realize the connection under the non-pressure condition, but the joint has poor high temperature resistance and corrosion resistance; for the existing mature brazing connection, high-strength connection under no pressure can be realized, the high-temperature resistance and the corrosion resistance can be adjusted, but the mismatch of the thermal expansion coefficients of metal and ceramic easily causes the joint to generate larger residual stress, thereby influencing the joint connection quality. Therefore, it is necessary to develop a new connection method based on the advantages of the brazing connection to reduce the residual stress of the joint between the ceramics.
Disclosure of Invention
In order to solve the above-mentioned deficiencies and drawbacks of the prior art, a ceramic connecting member having a dense connecting layer is provided. The ceramic connecting piece is provided with the compact layer, and the connecting layer has better corrosion resistance and can be connected with the ceramic with the complex shape. The shear strength at room temperature is 150-200 MPa, the shear strength at high temperature of 1200 ℃ is 100-150 MPa, and the residual stress of the joint is 50-100 MPa.
Another object of the present invention is to provide a method for connecting ceramic connecting members having a dense connecting layer according to the above method, which can reduce residual stress at joints between ceramics while securing connection performance by connecting ceramics using a fusion infiltration principle using metal 316 stainless steel as a connecting material.
It is a further object of the present invention to provide the use of the above ceramic joining member having a dense joining layer.
The purpose of the invention is realized by the following technical scheme:
a ceramic connecting piece with a compact connecting layer is characterized in that a solvent and a ball milling medium are added into a ceramic powder body, the mixture is mixed and dried to obtain ball-milled powder, and the powder body is subjected to dry pressing and cold isostatic pressing to obtain a ceramic green body; and placing the foil or powdery 316 stainless steel metal connecting material between the polished ceramic green bodies, and sintering at 1200-1600 ℃ in a vacuum environment to obtain the ceramic green body.
Preferably, the shear strength of the ceramic connecting piece at room temperature is 150-200 MPa, the shear strength at high temperature of 1200 ℃ is 100-150 MPa, and the residual stress is 50-100 MPa.
Preferably, the ceramic powder is SiC or Si3N4Or TiC.
More preferably, the purity of the ceramic powder is 99-99.9999%, and the particle size of the ceramic powder is 1-10 μm.
Preferably, the solvent is absolute ethyl alcohol or acetone, and the ball milling medium is Si3N4Balls or SiC balls.
Preferably, the pressure of the dry pressure is 10-30 MPa, and the pressure of the cold isostatic pressing is 100-300 MPa.
Preferably, the metal connecting material is 5-30 vol% of the ceramic powder.
Preferably, the vacuum degree of the vacuum environment is 10-3～10-5Pa；
Preferably, the sintering time is 0.5-4 h.
The connecting method of the ceramic connecting piece with the compact connecting layer comprises the following specific steps:
s1, adding a solvent and a ball milling medium into ceramic powder, mixing and drying to obtain ball-milled powder, and carrying out dry pressing and cold isostatic pressing treatment on the powder to obtain a ceramic green body;
s2, placing foil or powdery 316 stainless steel made of metal connecting materials between the polished ceramic green bodies, and sintering at 1200-1600 ℃ in a vacuum environment to obtain the ceramic connecting piece with the compact connecting layer.
The ceramic connecting piece with the compact connecting layer is applied to the field of ceramic connection of complex structures.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention takes the green ceramic body which is not sintered as the raw material and adopts the metal 316 stainless steel as the connecting material, so that the densification of the ceramic material can be realized while the metal connecting material is connected, and the existing method adopts the dense block as the raw material for connection. The connection method can be carried out under the conditions of low temperature and no pressure, and meets the connection requirement of complex ceramic structural parts.
2. According to the invention, metal 316 stainless steel is used as a connecting material, ceramics are connected by using a melt infiltration principle, the connecting performance is ensured, and the residual stress of a joint between the ceramics is reduced. The prepared ceramic connecting piece has good corrosion resistance, the shear strength at room temperature is 150-200 MPa, the shear strength at high temperature of 1200 ℃ is 100-150 MPa, and the residual stress of the joint is 50-100 MPaa.
3. In the connection process, the metal connection material arranged in the middle of the unsintered ceramic green body permeates to the two sides of the ceramic green body and is diffused in a gradient manner, and because the thermal expansion coefficient of the ceramic is lower than that of the metal, when the metal connection material is diffused into the ceramic green body, the difference of the expansion coefficients between the metal connection material and the ceramic green body is reduced, so that the residual stress at the joint of the ceramic and the metal brazing filler metal is reduced.
4. The invention adopts 316 stainless steel as the metal connecting material, and the formed connecting layer does not reduce the corrosion resistance of the joint.
Drawings
FIG. 1 is a schematic diagram of the present invention for preparing a SiC ceramic having a connecting layer.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. SiC powder is used as raw material powder (the particle size is 10 mu m, and the purity is 99%); using absolute ethyl alcohol as solvent, Si3N4Mixing grinding balls, drying, molding under the pressure of 30MPa, and performing cold isostatic pressing at the pressure of 200MPa to obtain a ceramic green body;
2. polishing the surface of the ceramic green body, connecting with 316 stainless steel foil with thickness of 50 μm as connecting material as shown in FIG. 1, placing the 316 stainless steel foil between SiC green bodies with vacuum degree of 10-4Pa, the connection sintering temperature is 1500 ℃, and the temperature is kept for 2h to prepare the SiC ceramic with the compact connecting layer.
FIG. 1 is a schematic diagram of the present invention for preparing a SiC ceramic having a connecting layer. Wherein (a) shows a state before SiC ceramic is bonded, (b) shows a state during SiC ceramic bonding, and an arrow indicates a diffusion direction of the metal bonding layer, and (c) shows a state after SiC ceramic bonding, and SiC ceramic having a dense bonding layer is obtained. And along with the rise of temperature in the connection process, the metal foil is melted and diffuses towards the two sides of the SiC, and the gaps of the SiC blank are filled in the diffusion process, so that the compact connection of the SiC ceramic material is realized, and the SiC ceramic with the compact connection layer is prepared. The shear strength of the SiC ceramic connecting piece prepared in the embodiment at room temperature is 180MPa, the shear strength at 1200 ℃ is 150MPa, and the joint residual stress is 70 MPa.
Example 2
1. With Si3N4The powder is raw material powder (the particle size is 1 mu m, and the purity is 99.9%); 316 stainless steel powder is used as a connecting material, and the particle size of the powder is 5 mu m; the connection was carried out by the method of example 1, the degree of vacuum during the connection being 10-5Pa, the connection sintering temperature is 1200 ℃, and the heat preservation is carried out for 0.5h, thereby realizing Si3N4Dense connection of ceramic materials to prepare Si with dense connection layer3N4A ceramic.
Si prepared in this example3N4The shear strength of the ceramic connecting piece at room temperature is 150MPa, the shear strength at high temperature of 1200 ℃ is 120MPa, and the residual stress of the joint is 50 MPa.
Example 3
1. TiC powder is used as raw material powder (the particle size is 5 mu m, and the purity is 99.9%); 316 stainless steel foil with the thickness of 100 mu m is taken as connecting material; the connection was carried out by the method of example 1, the degree of vacuum during the connection being 10-3Pa, the connection sintering temperature is 1600 ℃, and the heat preservation is carried out for 4h, so that the compact connection of the TiC ceramic material is realized, and the TiC ceramic with the compact connection layer is prepared.
Si prepared in this example3N4The shear strength of the ceramic connecting piece at room temperature is 170MPa, the shear strength at high temperature of 1200 ℃ is 150MPa, and the residual stress of the joint is 80 MPa.
Example 4
1. TiC powder is used as raw material powder (the particle size is 5 mu m, and the purity is 99.9%); 316 stainless steel powder is used as a connecting material, and the particle size of the powder is 10 mu m; the connection was carried out by the method of example 1, the degree of vacuum during the connection being 10-4Pa, the connection sintering temperature is 1550 ℃, and the temperature is kept for 2h to realize the compact connection of the TiC ceramic material, so as to prepare the TiC ceramic with the compact connection layer.
The TiC ceramic connector prepared in the embodiment has the shear strength of 200MPa at room temperature, the shear strength of 150MPa at the high temperature of 1200 ℃, and the joint residual stress of 60 MPa.
Example 5
1. SiC powder is used as raw material powder (the particle size is 10 mu m, and the purity is 99.9%); 316 stainless steel powder is used as a connecting material, and the particle size of the powder is 10 mu m; the connection was carried out by the method of example 1, the degree of vacuum during the connection being 10-5Pa, the connection temperature is 1200 ℃, the temperature is kept for 0.5h, the compact connection of the SiC ceramic material is realized, and the SiC ceramic with the compact connection layer is prepared.
The shear strength of the SiC ceramic connecting piece prepared by the embodiment at room temperature is 150MPa, the shear strength at the high temperature of 1200 ℃ is 100MPa, and the residual stress of the joint is 90 MPa.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A ceramic connecting piece with a compact connecting layer is characterized in that a solvent and a ball milling medium are added into a ceramic powder body, the mixture is mixed and dried to obtain ball milled powder, and the powder body is subjected to dry pressing and cold isostatic pressing to obtain a ceramic green body; and placing the foil or powdery 316 stainless steel metal connecting material between the polished ceramic green bodies, and sintering at 1200-1600 ℃ in a vacuum environment to obtain the ceramic green body.
2. The ceramic connecting member with the dense connecting layer according to claim 1, wherein the shear strength of the ceramic connecting member at room temperature is 150 to 200MPa, the shear strength at a high temperature of 1200 ℃ is 100 to 150MPa, and the residual stress is 50 to 100 MPa.
3. The ceramic connector with dense joint layer as claimed in claim 1, wherein said ceramic powder is SiC, Si3N4Or TiC.
4. The ceramic connecting piece with the dense connecting layer as recited in claim 3, wherein the purity of the ceramic powder is 99-99.9999%, and the particle size of the ceramic powder is 1-10 μm.
5. The ceramic connection piece with dense connection layer as claimed in claim 1, wherein the solvent is absolute ethanol or acetone, and the ball milling medium is Si3N4Balls or SiC balls.
6. The ceramic connecting member with the dense connecting layer as claimed in claim 1, wherein the dry pressure is 10 to 30MPa, and the cold isostatic pressure is 100 to 300 MPa.
7. The ceramic connecting piece with the dense connecting layer as claimed in claim 1, wherein the metal connecting material is 5-30 vol% of the ceramic powder.
8. The ceramic joint having a dense joint layer according to claim 1, wherein the vacuum environment has a vacuum degree of 10-3～10-5Pa; the sintering time is 0.5-4 h.
9. The method for connecting a ceramic connecting member with a dense connecting layer according to any one of claims 1 to 8, comprising the specific steps of:
s1, adding a solvent and a ball milling medium into ceramic powder, mixing and drying to obtain ball-milled powder, and carrying out dry pressing and cold isostatic pressing treatment on the powder to obtain a ceramic green body;
s2, placing foil or powdery 316 stainless steel made of metal connecting materials between the polished ceramic green bodies, and sintering at 1200-1600 ℃ in a vacuum environment to obtain the ceramic connecting piece with the compact connecting layer.
10. Use of a ceramic joint with a dense joint layer according to any one of claims 1 to 8 in the field of ceramic joints of complex structures.
CN202010258895.4A 2020-04-03 2020-04-03 Ceramic connecting piece with compact connecting layer and connecting method and application thereof Active CN111454063B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111960844A (en) * 2020-07-31 2020-11-20 广东工业大学 Ceramic connecting piece and preparation method and application thereof
CN113860902A (en) * 2021-09-26 2021-12-31 中广核研究院有限公司 Ceramic connection method and ceramic connection member

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GB1223797A (en) * 1968-05-02 1971-03-03 Atomic Energy Commission Diffusion bonding of ceramics
US6348273B1 (en) * 1999-06-25 2002-02-19 Ngk Insulators, Ltd. Method for bonding different members and composite members bonded by the method
US20080274362A1 (en) * 2007-05-01 2008-11-06 Kramer Daniel P Method of joining metals to ceramic matrix composites
CN105130445A (en) * 2015-09-15 2015-12-09 哈尔滨工业大学 Method of co-sintering joined silicon-carbide-based composite ceramic green bodies
CN108546095A (en) * 2018-05-23 2018-09-18 广东工业大学 A kind of method that oxide ceramics is welded to connect with metal
CN109516828A (en) * 2018-10-15 2019-03-26 广东工业大学 The silicon carbide ceramics of a kind of connection method and its preparation of nucleus silicon carbide ceramics and application

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US6348273B1 (en) * 1999-06-25 2002-02-19 Ngk Insulators, Ltd. Method for bonding different members and composite members bonded by the method
US20080274362A1 (en) * 2007-05-01 2008-11-06 Kramer Daniel P Method of joining metals to ceramic matrix composites
CN105130445A (en) * 2015-09-15 2015-12-09 哈尔滨工业大学 Method of co-sintering joined silicon-carbide-based composite ceramic green bodies
CN108546095A (en) * 2018-05-23 2018-09-18 广东工业大学 A kind of method that oxide ceramics is welded to connect with metal
CN109516828A (en) * 2018-10-15 2019-03-26 广东工业大学 The silicon carbide ceramics of a kind of connection method and its preparation of nucleus silicon carbide ceramics and application

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111960844A (en) * 2020-07-31 2020-11-20 广东工业大学 Ceramic connecting piece and preparation method and application thereof
CN113860902A (en) * 2021-09-26 2021-12-31 中广核研究院有限公司 Ceramic connection method and ceramic connection member

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