CN115991609A - Ceramic-metal discharge plasma connection method - Google Patents
Ceramic-metal discharge plasma connection method Download PDFInfo
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Abstract
The invention discloses a ceramic-metal discharge plasma connection method, which relates to the technical field of ceramic material connection and comprises the following steps: (1) Grinding and polishing the ceramic and metal connection surfaces respectively, and grinding the metal foil; (2) Carrying out ultrasonic cleaning on the treated ceramics, metal and metal foil; (3) And placing the ceramic, metal and metal foil in a graphite die, and performing spark plasma sintering. Compared with brazing and diffusion welding, the ceramic-metal discharge plasma connecting method improves the heating rate and the cooling rate by 5-10 times, and the obtained ceramic-metal connecting interface has high strength.
Description
Technical Field
The invention relates to the technical field of ceramic material connection, in particular to a ceramic-metal discharge plasma connection method.
Background
The ceramic material has good high-temperature mechanical property, excellent oxidation resistance and corrosion resistance, high hardness, good wear resistance and high specific strength, has wide application prospect in the fields of aerospace, automobiles, engineering machinery and the like, and becomes one of the materials with the highest potential and competitiveness. However, ceramics are brittle and difficult to make into large-sized or complex components, which makes them limited in practical applications. Therefore, the ceramic and the metal are connected to realize performance complementation, and the composite component with the excellent performances of the ceramic and the metal is obtained.
The current methods for connecting ceramics and metals include brazing, diffusion welding, liquid phase connection and the like. Li C (Microstructure and mechanical properties of the AlON/Ti6Al4V active element brazing joint [ J)]Materials Science and Engineering A,2020, 793:139859.) AlON was joined to Ti6Al4V by brazing with an Ag-28Cu eutectic solder with a joint maximum shear strength of 78.3MPa. Lan L (Microstructure and mechanical properties of partial transient liquid phase bonded Si) 3 N 4 –DZ483 superalloy joints[J]Materials Letters,2014, 121:223-226.) Si is joined by liquid phase joining 3 N 4 And the bending strength of the joint can reach 170MPa at most compared with DZ 483. In view of the chemical inertness of ceramics, the most mature method at present is to use brazing for joining. K. Nagatsuka (Nagatsuka K et al Effect of Ti content in Ag-Cu-Ti activated filler metal on dissimilar joint formation of SiAlON and WC-Co alloy by laser brazing [ J)]Science and Technology of Welding and Joining,2014,19 (6): 521-526.) the SiAlON ceramic and cemented carbide are joined by brazing using laser heating as a heat source, the joint obtained having a shear strength of at most 106MPa. The joint brazed and connected by using the silver-based brazing filler metal has poor high-temperature performance and lower strength, and is difficult to meet the requirements of actual production.
Disclosure of Invention
The invention aims to provide a ceramic-metal discharge plasma connection method which solves the problems of the prior art, and the invention is based on the dual advantages of plasma activation and pressurization, so that the ceramic and the metal are connected with high strength.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a ceramic-metal discharge plasma connection method, which comprises the following steps:
(1) Grinding and polishing the ceramic and metal connection surfaces respectively, and grinding the metal foil;
(2) Carrying out ultrasonic cleaning on the treated ceramics, metal and metal foil;
(3) And stacking and assembling ceramic, metal and metal foil, and placing the stacked and assembled ceramic, metal and metal foil in a graphite die to perform spark plasma sintering.
Preferably, in the step (1), the ceramic and metal connection surface is sequentially provided with B having the specifications of W14 and W5 4 Grinding the grinding powder C for 5-10 minutes respectively, and then polishing the grinding powder C on a metallographic specimen polishing machine by using a diamond polishing agent with the specification of W1.5-W0.5 for 5-15 minutes at the rotating speed of 900r/min; after grinding and polishing treatment, greasy dirt, grease, oxide skin and rust on the surface of the ceramic and metal connecting surface are removed, and meanwhile, high friction between the ceramic and metal connecting surface is caused, so that the roughness of the surface is reduced.
The metal foil is sequentially polished by 400# sand paper, 800# sand paper, 1200# sand paper and 1500# sand paper, and pollutants, rust and other substances on the surface of the metal foil can be removed after polishing treatment, so that the roughness is reduced.
Preferably, the ceramic is SiAlON, al 2 O 3 、ZrO 2 、Si 3 N 4 One of SiC, BN, alN and cermet;
the metal is one of hard alloy, high-temperature alloy, titanium alloy and stainless steel.
The metal foil is one or more than two of Ti foil, cu foil, ni foil, nb foil, mo foil, W foil, ag foil and Ta foil, and the metal foil can realize the connection of ceramic and metal through diffusion or chemical reaction.
Preferably, the thickness of the metal foil is 10-500 μm, and in the thickness range, the metal foil can slow down residual stress caused by the difference of thermal expansion coefficients in the process of connecting the ceramic and the metal through certain plastic deformation, and the excessive thinness of the metal foil can lead to insufficient interface reaction, so that the residual stress relieving capability is weakened instead.
Preferably, in the step (2), ultrasonic cleaning is performed in absolute ethyl alcohol for 15min, so that impurities and grease on the surface are further removed. .
Preferably, in the step (3), the ceramic-metal foil-metal laminated structure is sequentially placed in a graphite mold. In this step, the inner wall of the graphite mold is covered with a graphite gasket having a thickness of 0.2mm, and more preferably, is sequentially installed in the graphite mold in accordance with a stack structure of a graphite ram-graphite gasket-ceramic-metal foil-metal-graphite gasket-graphite ram. When the metal foil is not placed, the ceramic and metal connection typically fails or the strength of the connection is low.
Preferably, when the metal foil is a combination of two or more of Ti foil, cu foil, ni foil, nb foil, mo foil, W foil, ag foil and Ta foil, the ceramic-Ti foil-X foil-metal configuration is followed, wherein the X foil is at least one metal foil other than Ti foil. Ti can react with ceramics with strong chemical inertia as an active element, so Ti foil is selected to be placed on the side of the ceramics, and the chemical property of metal is more active than that of the ceramics, so the key for realizing the connection between the ceramics and the metal is that the existence of the active element such as Ti foil and the like, and the combination of the Ti foil and the X foil can improve the interface connection strength by relieving the residual stress or controlling the generation of metal compounds.
Preferably, in the step (3), the spark plasma sintering process is as follows: the temperature rising rate is 10-100 ℃/min, the temperature is 800-1300 ℃, the pressure is 10-100MPa, and the constant pressure is kept for 0-120min. Before the spark plasma sintering process, the spark plasma sintering furnace is washed with gas once, vacuumized to 40Pa and then flushed with argon protective atmosphere to 0.05MPa. Too low a heating rate results in low production efficiency, and too high a heating rate results in difficulty in soaking to generate larger thermal stress; incomplete reaction or diffusion of the metal foil with ceramic or metal at a lower connection temperature, and adverse effects on the performance of the base metal may occur at an excessively high temperature; the influence of the heat preservation time is equal to the connection temperature; the connection strength increases with increasing connection pressure, but too high a connection pressure results in greater residual stress. So that under a certain connection pressure, the metal foil is raised to the connection temperature at a certain heating rate, and then is kept for a period of time, so that the chemical reaction or diffusion of the metal foil and the ceramic/metal is promoted to fully occur, and the good connection is realized. Spark plasma sintering (Spark Plasma Sintering, SPS for short) is a novel material sintering technology, has the distinct advantages of high heating speed, short sintering time, controllable tissue structure, energy conservation, environmental protection and the like, and has no report on a spark plasma connection method of ceramics and metals at the present stage. The invention uses SPS for the connection of ceramics and metal by utilizing the characteristics of rapid plasma activation and temperature rise and reduction of spark plasma sintering, can effectively promote the phase change reaction, reduce the thermal damage and connection deformation of a matrix, is beneficial to improving the uniformity of tissues, obtains high connection strength, shortens the connection time and improves the production efficiency. The ceramic and metal discharge plasma connection method has high practical value.
The invention discloses the following technical effects:
(1) Compared with brazing and diffusion welding, the ceramic-metal discharge plasma connecting method improves the heating rate and the cooling rate by 5-10 times. The invention greatly reduces the energy consumption, improves the production efficiency and has popularization value.
(2) The invention adopts the metal foil as the connecting material, the obtained ceramic-metal connecting interface has high strength, expands the application occasions of the ceramic and has high practical value.
(3) The ceramic and metal connecting interface has no defects such as cracks and holes, good chemical combination is realized on the ceramic side, the base metal grains do not grow up under the action of plasma, the matrix is less damaged, and excessive brittle intermetallic compounds are not generated at the interface.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a shear schematic of a shear test of the present invention;
FIG. 2 is a diagram of a SiAlON ceramic-cemented carbide joint according to example 1 of the present invention;
FIG. 3 is an SEM image of the SiAlON ceramic-cemented carbide interface prepared in example 1, where 1 is SiAlON ceramic, 2 is cemented carbide, and 3 is metal foil;
FIG. 4 is an SEM enlarged view of the SiAlON ceramic side connection interface obtained in example 1, wherein 1 is SiAlON ceramic and 2 is metal foil;
FIG. 5 is an SEM magnified view of a cemented carbide side joint interface prepared in example 1, where 1 is a metal foil and 2 is cemented carbide;
FIG. 6 is an SEM image of the SiAlON ceramic-cemented carbide joint interface prepared in example 2, where 1 is SiAlON ceramic, 2 is cemented carbide, and 3 is metal foil;
FIG. 7 is an SEM enlarged view of a SiAlON ceramic side connection interface obtained in example 2, wherein 1 is SiAlON ceramic and 2 is metal foil;
FIG. 8 is an SEM magnified view of a cemented carbide side joint interface prepared in example 2, where 1 is a metal foil and 2 is cemented carbide;
FIG. 9 is an SEM image of the SiAlON ceramic-cemented carbide joint interface prepared in example 3, where 1 is SiAlON ceramic, 2 is cemented carbide, and 3 is metal foil;
FIG. 10 is an SEM enlarged view of a SiAlON ceramic side connection interface obtained in example 3, wherein 1 is SiAlON ceramic and 2 is metal foil;
fig. 11 is an SEM enlarged view of the cemented carbide side connection interface prepared in example 3, wherein 1 is a metal foil and 2 is cemented carbide.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
(1) Grinding SiAlON ceramic to Φ13×4mm, and cutting cemented carbide (YG 8) to Φ13×4mm by wire electric discharge machining; polishing the surfaces to be connected of the SiAlON ceramic and the hard alloy by using an angle grinder, sequentially grinding the surfaces for 5 minutes by using B4C grinding powder with the specification of W14 and W5 respectively, and then polishing the surfaces on a metallographic specimen polishing machine by using a diamond polishing agent with the specification of W1.5 for 10 minutes at the rotating speed of 900r/min; cutting a Ti foil with the thickness of 10 mu m and a Cu foil with the thickness of 100 mu m into wafers with the diameter of 13mm, and polishing the Ti foil and the Cu foil with 400# sand paper, 800# sand paper, 1200# sand paper and 1500# sand paper in sequence; placing the treated SiAlON ceramic, hard alloy, ti foil and Cu foil in absolute ethyl alcohol for ultrasonic cleaning for 15min; covering a graphite gasket with the thickness of 0.2mm on the inner wall of a graphite mould with the inner diameter of 13.6mm and the height of 40 mm; sequentially loading SiAlON ceramic, hard alloy and metal foil into a graphite mold according to a laminated structure of graphite press head-0.2 mm graphite gasket-SiAlON ceramic-metal foil-hard alloy-0.2 mm graphite gasket-graphite press head;
(2) And placing the graphite mold in a discharge plasma sintering furnace, vacuumizing the discharge plasma sintering furnace for one time, and then vacuumizing to 40Pa, and then flushing argon protective atmosphere to 0.05MPa. The sintering process is that the heating rate is 50 ℃/min, and the constant pressure heat preservation is carried out for 60min at the temperature of 900 ℃ and the pressure of 30MPa, so that the SiAlON ceramic-hard alloy is connected. And after the heat preservation is finished, naturally cooling along with the furnace. The SiAlON ceramic-cemented carbide joint was then ground to 8mm x 6mm dimensions and installed into a shear die, the shear schematic being shown in fig. 1, and a shear test was performed using a universal tester at a speed of 0.1 mm/min.
The SiAlON ceramic-hard alloy connecting physical diagram obtained in the embodiment is shown in fig. 2, and the shear strength of the SiAlON ceramic-hard alloy connecting joint is 194MPa; the SEM image of the SiAlON ceramic-hard alloy connecting interface is shown in fig. 3, wherein 1 is SiAlON ceramic, 2 is hard alloy, 3 is metal foil, and the SEM image shows that the SiAlON ceramic and YG8 realize good connection under the action of Ti foil/Cu foil, and have no defects of micro cracks, non-welding and the like; an SEM enlarged view of a SiAlON ceramic side connection interface is shown in fig. 4, wherein 1 is SiAlON ceramic, 2 is metal foil, and it is known that a reaction layer with a certain thickness is generated by chemical reaction between the intermediate layer metal foil and the SiAlON ceramic, and the distribution of reaction products is relatively uniform; the SEM enlarged view of the cemented carbide side connection interface is shown in fig. 5, wherein 1 is a metal foil, 2 is cemented carbide, and it is known that YG8 and Cu foil generate certain diffusion and chemical reaction, and generate better bonding.
Example 2
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at a temperature of 900 ℃ for 30min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shear strength of 189MPa. An SEM (SEM) diagram of a SiAlON ceramic-hard alloy connecting interface is shown in fig. 6, wherein 1 is SiAlON ceramic, 2 is hard alloy, and 3 is metal foil; an SEM enlarged view of a SiAlON ceramic side connection interface is shown in FIG. 7, wherein 1 is SiAlON ceramic and 2 is metal foil; the SEM enlarged view of the cemented carbide side connection interface is shown in fig. 8, wherein 1 is a metal foil and 2 is cemented carbide, and it is seen from the SEM image that the thickness of the reaction layer formed between the intermediate metal foil and the base materials on both sides is reduced under the condition of reduced heat preservation time compared with example 1.
Example 3
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at a temperature of 950 ℃ for 60min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shearing strength of 144MPa. The SEM diagram of the SiAlON ceramic-hard alloy connecting interface is shown in fig. 9, wherein 1 is SiAlON ceramic, 2 is hard alloy, and 3 is metal foil; an SEM enlarged view of a SiAlON ceramic side connection interface is shown in FIG. 10, wherein 1 is SiAlON ceramic and 2 is metal foil; an SEM enlarged view of the cemented carbide side connection interface is shown in fig. 11, wherein 1 is a metal foil, 2 is a cemented carbide, and it is seen from the SEM image that the element diffusion distance is significantly increased under the condition of increasing the connection temperature compared with example 1, but the intermetallic compound generated at high temperature is pushed out of the interface more along with the eutectic liquid phase generated during the connection process, resulting in a slight decrease in strength.
Example 4
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure at 1000 ℃ and a pressure of 30MPa for 30min.
The shear strength of the SiAlON ceramic-hard alloy connecting joint prepared in the embodiment is 145MPa.
Example 5
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at 1000 ℃ for 60min.
The SiAlON ceramic/hard alloy connecting joint prepared in the embodiment has the shearing strength of 142MPa.
Example 6
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at 800 ℃.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shearing strength of 116MPa.
Example 7
The difference from example 1 is that the sintering process in step (2) is performed at a heating rate of 100 ℃/min and a constant pressure of 30MPa at 900 ℃.
The shear strength of the SiAlON ceramic-hard alloy connecting joint prepared in the embodiment is 165MPa.
Example 8
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 10 ℃/min and a constant pressure of 30MPa at a temperature of 900 ℃ for 30min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shear strength of 198MPa.
Example 9
The difference from example 1 is that the sintering process in step (2) is carried out at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at 900 ℃ for 120min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shearing strength of 175MPa.
Example 10
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 10MPa at 900 ℃ for 30min.
The shear strength of the SiAlON ceramic-hard alloy connecting joint prepared in the embodiment is 137MPa.
Example 11
The difference from example 1 is that the sintering process in step (2) is performed at a temperature rising rate of 50 ℃/min and a constant pressure of 100MPa at 900 ℃ for 30min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shearing strength of 103MPa.
Example 12
(1) Al is added with 2 O 3 Grinding the ceramic to phi 13X 4mm, and cutting stainless steel (1 Cr18Ni9 Ti) to phi 13X 4mm by using a wire electric discharge machine; polishing the Al by an angle grinder 2 O 3 After the ceramic and stainless steel are connected, grinding for 10 minutes respectively by using B4C grinding powder with the specification of W14 and W5 in sequence, and then polishing on a metallographic specimen polishing machine by using a diamond polishing agent with the specification of W1.515 minutes, the rotating speed is 900r/min; cutting a Ti foil with the thickness of 10 mu m, a W foil with the thickness of 300 mu m and a Ni foil with the thickness of 200 mu m into wafers with the diameter of 13mm, and polishing the Ti foil, the Ni foil and the Nb foil with 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 1500# abrasive paper in sequence; treating the treated Al 2 O 3 Placing ceramic, stainless steel, ti foil, ni foil and Nb foil in absolute ethyl alcohol, and ultrasonically cleaning for 15min; covering a graphite gasket with the thickness of 0.2mm on the inner wall of a graphite mould with the inner diameter of 13.6mm and the height of 40 mm; al is added with 2 O 3 Ceramic, stainless steel and metal foil are processed according to graphite pressing head-0.2 mm graphite gasket-Al 2 O 3 The laminated structure of ceramic-metal foil-stainless steel-0.2 mm graphite gasket-graphite press head is sequentially arranged in a graphite die;
(2) And placing the graphite mold in a discharge plasma sintering furnace, vacuumizing the discharge plasma sintering furnace for one time, and then vacuumizing to 40Pa, and then flushing argon protective atmosphere to 0.05MPa. The sintering process is that the temperature rising rate is 80 ℃/min, and the constant pressure heat preservation is carried out for 60min at the temperature of 1000 ℃ and the pressure of 50MPa, so that Al is obtained 2 O 3 Ceramic-stainless steel is joined. And after the heat preservation is finished, naturally cooling along with the furnace. Subsequently Al is added 2 O 3 The ceramic-stainless steel joint was ground to 8mm by 6mm in size for shear testing.
Al prepared in this example 2 O 3 The shear strength of the ceramic-steel connection joint is 170MPa.
Example 13
(1) ZrO (ZrO) 2 Grinding ceramic to phi 13 x 4mm, and cutting high-temperature alloy (GH 4169) to phi 13 x 4mm by utilizing a wire electric discharge machine; polishing the ZrO with an angle grinder 2 After the ceramic and the high-temperature alloy are subjected to surface connection, grinding for 5 minutes respectively by using B4C grinding powder with the specification of W14 and W5 in sequence, and then polishing for 10 minutes by using a diamond polishing agent with the specification of W0.5 on a metallographic specimen polishing machine, wherein the rotating speed is 900r/min; cutting 50 μm thick Ti foil and 500 μm thick Ta foil into round pieces with diameter of 13mm, and polishing the Ti foil and the Ta foil with 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 1500# abrasive paper in sequence; the treated ZrO 2 Placing the ceramic, the superalloy, the Ti foil and the Ta foil in absolute ethyl alcohol for ultrasonic cleaning for 15min; in a graphite mold with an inner diameter of 13.6mm and a height of 40mmA graphite gasket with a wall covering thickness of 0.2 mm; zrO (ZrO) 2 Ceramic, superalloy, and metal foil according to graphite indenter-0.2 mm graphite gasket-ZrO 2 The laminated structure of ceramic-metal foil-superalloy-0.2 mm graphite gasket-graphite press head is sequentially arranged in a graphite die;
(2) And placing the graphite mold in a discharge plasma sintering furnace, vacuumizing the discharge plasma sintering furnace for one time, and then vacuumizing to 40Pa, and then flushing argon protective atmosphere to 0.05MPa. The sintering process is that the heating rate is 60 ℃/min, and the constant pressure heat preservation is carried out for 80min at the temperature of 1200 ℃ and the pressure of 30MPa, so that the ZrO 2 The ceramic-superalloy is joined. And after the heat preservation is finished, naturally cooling along with the furnace. Subsequently, zrO is taken up 2 The ceramic-superalloy joint was ground to 8mm by 6mm in size for shear testing.
ZrO obtained by the preparation of this example 2 The shear strength of the ceramic-superalloy joint is 160MPa.
Example 14
(1) Si is mixed with 3 N 4 Grinding the ceramic to phi 13 multiplied by 4mm, and cutting the titanium alloy (TC 4) to phi 13 multiplied by 4mm by utilizing a wire electric discharge machine; polishing the Si with an angle grinder 3 N 4 After the ceramic and the high-temperature alloy are subjected to surface connection, grinding for 5 minutes respectively by using B4C grinding powder with the specification of W14 and W5 in sequence, and then polishing for 10 minutes by using a diamond polishing agent with the specification of W0.5 on a metallographic specimen polishing machine, wherein the rotating speed is 900r/min; cutting 200 mu m thick Ag foil into a wafer with the diameter of 13mm, and polishing the Ag foil by using 400# abrasive paper, 800# abrasive paper, 1200# abrasive paper and 1500# abrasive paper in sequence; will treat the Si 3 N 4 Placing the ceramic, titanium alloy and Ag foil in absolute ethyl alcohol, and ultrasonically cleaning for 15min; covering a graphite gasket with the thickness of 0.2mm on the inner wall of a graphite mould with the inner diameter of 13.6mm and the height of 40 mm; si is mixed with 3 N 4 Ceramic, titanium alloy and metal foil are processed according to graphite pressing head-0.2 mm graphite gasket-Si 3 N 4 The laminated structure of ceramic-metal foil-titanium alloy-0.2 mm graphite gasket-graphite pressure head is sequentially arranged in a graphite die;
(2) Placing the graphite mold in a discharge plasma sintering furnace, and vacuumizing the discharge plasma sintering furnace for washingAnd (3) carrying out gas once, vacuumizing to 40Pa, and then flushing an argon protective atmosphere to 0.05MPa. The sintering process is that the heating rate is 50 ℃/min, and the constant pressure heat preservation is carried out for 50min at the temperature of 1000 ℃ and the pressure of 50MPa, so that Si is obtained 3 N 4 The ceramic-titanium alloy is joined. And after the heat preservation is finished, naturally cooling along with the furnace. Subsequently Si is added 3 N 4 The ceramic-titanium alloy joint was ground to 8mm by 6mm in size for shear testing.
Si prepared in this example 3 N 4 The shear strength of the ceramic-titanium alloy connecting joint is 122MPa.
Example 15
The only difference from example 1 is that the ceramic is BN ceramic, the metal is titanium alloy (TC 4), and the metal foil is 250 μm Nb foil.
The BN ceramic-titanium alloy connecting joint prepared in the embodiment has the shearing strength of 91MPa.
Example 16
The only difference from example 1 is that the ceramic is AlN ceramic, the metal is tool steel (T10A), and the metal foil is a 500 μm Cu foil.
The AlN ceramic-steel joint prepared in this example had a shear strength of 137MPa.
Example 17
The only difference from example 1 is that the ceramic is a cermet (Ti (C, N)), the metal is a superalloy (GH 4169), and the metal foil is a Ti foil of 200 μm.
The shear strength of the metal ceramic-superalloy connecting joint prepared in the embodiment is 149MPa.
Example 18
The difference from example 1 was that the ceramic was SiC ceramic, the metal was titanium alloy TC4, and the metal foil was 100 μm Mo foil.
The shear strength of the SiC ceramic-titanium alloy connecting joint prepared in the embodiment is 73MPa.
Comparative example 1
The difference from example 1 is that the sintering process in step (2) is carried out at a temperature rising rate of 50 ℃/min and a constant pressure of 30MPa at 750 ℃ for 60min. And after the heat preservation is finished, keeping pressure circulation water cooling for natural cooling to obtain the SiAlON ceramic-hard alloy connecting joint.
The SiAlON ceramic-hard alloy connecting joint prepared by the embodiment is separated in the subsequent grinding process, namely, the connecting strength is lower. The reason for the lower joint connection strength is that the connection temperature is set to be lower, and at the connection temperature, the diffusion or the reaction of the middle layer metal foil and the base metal to be connected is insufficient, and macroscopic gaps appear at the interface, so that the connection strength is lower.
Comparative example 2
The difference from example 1 is that in step (2), the SiAlON ceramic-cemented carbide is connected by constant pressure heat preservation at 1400 ℃ and 30MPa for 60min.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the advantages that a large amount of metal is extruded at the interface because the melting point of the metal in the middle layer is exceeded, a small amount of cracks exist at the interface, and the shearing strength is 19MPa.
Comparative example 3
The difference is that the SiAlON ceramics and the hard alloy in the step (1) are not polished after being ground as in the embodiment 1.
The SiAlON ceramic-hard alloy connecting joint prepared in the embodiment has the shearing strength of 43MPa. Because SiAlON ceramic and hard alloy are not polished after being ground, the surface to be connected is rough, and the surface to be connected and the metal foil are not tightly attached in the connecting process, small holes can possibly appear, and the strength is reduced more.
Comparative example 4
The difference from example 1 is that no metal foil is added between the SiAlON ceramic and the cemented carbide in step (1).
The SiAlON ceramic-cemented carbide prepared in this example failed to achieve the connection. When no metal foil is added, the chemical properties of SiAlON ceramic and hard alloy are stable, and chemical reaction is difficult to occur between the SiAlON ceramic and the hard alloy, so that connection cannot be realized.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. A ceramic-metal discharge plasma connection method, comprising the steps of:
(1) Grinding and polishing the ceramic and metal connection surfaces respectively, and grinding the metal foil;
(2) Carrying out ultrasonic cleaning on the treated ceramics, metal and metal foil;
(3) And stacking and assembling ceramic, metal and metal foil, and placing the stacked and assembled ceramic, metal and metal foil in a graphite die to perform spark plasma sintering.
2. The method of plasma joining of ceramic and metal according to claim 1, wherein in step (1), the ceramic and metal joining surfaces are sequentially joined by B having the specifications W14 and W5 4 Grinding the grinding powder C for 5-10 minutes respectively, and then polishing the grinding powder C on a metallographic specimen polishing machine by using a diamond polishing agent with the specification of W1.5-W0.5 for 5-15 minutes at the rotating speed of 900r/min;
the metal foil was sanded sequentially with 400#, 800#, 1200#, 1500# sandpaper.
3. The method for plasma-based ceramic-metal discharge connection according to claim 2, wherein the ceramic is SiAlON, al 2 O 3 、ZrO 2 、Si 3 N 4 One of SiC, BN, alN and cermet;
the metal is one of hard alloy, high-temperature alloy, titanium alloy and stainless steel;
the metal foil is one or more than two of Ti foil, cu foil, ni foil, nb foil, mo foil, W foil, ag foil and Ta foil.
4. A ceramic-metal discharge plasma connection method according to claim 3, characterized in that the thickness of the metal foil is 10-500 μm.
5. The ceramic-metal discharge plasma bonding method according to claim 1, wherein in step (2), ultrasonic cleaning is performed in absolute ethanol for 15min.
6. The ceramic-metal discharge plasma bonding method according to claim 1, wherein in step (3), the ceramic-metal foil-metal laminate structure is sequentially placed in a graphite mold.
7. The method of claim 6, wherein when the metal foil is a combination of two or more of Ti foil, cu foil, ni foil, nb foil, mo foil, W foil, ag foil, and Ta foil, the ceramic-Ti foil-X foil-metal configuration is followed, wherein the X foil is at least one metal foil other than Ti foil.
8. The ceramic-metal discharge plasma joining method according to claim 1, wherein in the step (3), the spark plasma sintering process is as follows: the temperature rising rate is 10-100 ℃/min, the temperature is 800-1300 ℃, the pressure is 10-100MPa, and the constant pressure is kept for 0-120min.
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