CN116024476A - Composite ceramic and preparation method and application thereof - Google Patents
Composite ceramic and preparation method and application thereof Download PDFInfo
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- CN116024476A CN116024476A CN202310043282.2A CN202310043282A CN116024476A CN 116024476 A CN116024476 A CN 116024476A CN 202310043282 A CN202310043282 A CN 202310043282A CN 116024476 A CN116024476 A CN 116024476A
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Abstract
The invention provides composite ceramic, a preparation method and application thereof, and belongs to the field of metal ceramic composite material manufacture, wherein the composite ceramic comprises a first ceramic phase, a second ceramic phase and a sintering aid; wherein the first ceramic phase is Ti (C, N)/Ti (C, N) +TiC; the second ceramic phase is TiB 2 The method comprises the steps of carrying out a first treatment on the surface of the The sintering aid is Cr 3 C 2 And/or VC. The invention adopts the sintering modes of vacuum sintering, argon and nitrogen atmosphere sintering, argon and nitrogen air pressure sintering, hot-pressing sintering and hot isostatic pressing sintering, and introduces Cr into the raw materials 3 C 2 And/or VC sintering aid, which plays a role in inhibiting grain growth while reducing the highest sintering temperature of the matrix; at the same time, the red hardness, oxidation resistance and wear resistance of the titanium carbonitride can be improved by directly adding the titanium carbonitride, thereby obtaining good dimensional stability and comprehensive mechanical propertyExcellent composite ceramic matrix, and thus the service life of the material is prolonged.
Description
Technical Field
The invention relates to the field of metal ceramic composite material manufacturing, in particular to composite ceramic, and a preparation method and application thereof.
Background
Titanium carbonitride is used for manufacturing sintered bodies of cutting tools and wear-resistant parts because of higher red hardness, better oxidation resistance and stronger wear resistance than titanium carbide. And is often used in semi-finishing and finishing due to its excellent surface finishing quality. Thus, titanium carbonitride has a greater potential than titanium carbide in the preparation of tool materials. Existing titanium carbonitride based and titanium carbide cermets for tool materials are commonly prepared by adding WC, nbC, taC, mo 2 Carbide of elements of subgroup IV, V and VI such as C and metal phase such as cobalt and nickel improve wettability, and fracture toughness is improved, but the existence of metal binding phase reduces hardness, red hardness, oxidation resistance and wear resistance, so that the carbide is difficult to be suitable for high-speed and high-finish machining requirements.
TiB 2 The TiC composite ceramic has excellent red hardness, oxidation resistance, wear resistance and thermal stability. TiB is directly used in the prior art 2 The material is directly mixed with TiC raw material powder mechanically and then sintered and formed, so that the material has higher sintering temperature, large grain size and poor mechanical property although the process is simpler and the dimensional stability of the material is better; tiO with fine particles is also used 2 B powder or B 4 The C powder and the C powder are sintered and molded in situ after mechanical mixing, and although the process method can obtain a matrix with finer grains and higher density, the reaction degree is difficult to control due to too severe in-situ reaction, so that the molded matrix has poor dimensional stability, and the application of the matrix on high-precision wear-resistant parts and cutting tools is difficult to ensure. Therefore, on the premise of ensuring the dimensional stability, the effective improvement of the comprehensive mechanical properties of the material and the reduction of the process cost become technical problems to be solved urgently by the technicians in the field.
Disclosure of Invention
In order to solve the technical problems, the invention provides composite ceramic and a preparation method and application thereof. By introducing Cr into the raw material 3 C 2 And/or VC sintering aid, which plays a role in inhibiting grain growth while reducing the highest sintering temperature of the matrix;meanwhile, ti (C, N) is introduced in a direct adding mode, so that the red hardness, oxidation resistance and wear resistance of the composite ceramic matrix can be improved, and the composite ceramic matrix with good dimensional stability and excellent comprehensive mechanical property is obtained, so that the service life of the material is prolonged.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a composite ceramic, which comprises a first ceramic phase, a second ceramic phase and a sintering aid;
wherein the first ceramic phase is Ti (C, N)/Ti (C, N) +TiC; the second ceramic phase is TiB 2 The method comprises the steps of carrying out a first treatment on the surface of the The sintering aid is Cr 3 C 2 And/or VC.
Further, the raw materials comprise, in terms of mass fraction: tiB (TiB) 2 5％～45％，Ti(C,N)+TiC40％～80％，Cr 3 C 2 And/or VC 1-15%.
Further, ti (C, N) +Ti (C, N) in TiC accounts for 10% -80%, and the balance is TiC.
The preparation method of the composite ceramic comprises the steps of uniformly mixing powder raw materials, wet grinding, drying, pressing into a green body, and then sintering at high temperature to obtain the composite ceramic.
Further, the particle size of the powder raw material powder is 0.5-2 mu m, and the oxygen element content is less than or equal to 0.5% in terms of mass fraction.
Further, the wet grinding specifically includes: water or ethanol is adopted as a wet grinding solvent, the mass ratio of the solvent to the powder raw material is=2:1-3:1, the hard alloy balls or steel balls are ball milling media, the mass ratio of the ball milling media to the raw material is=5:1-7:1, the ball milling time is 20-100 h, and the temperature of the ball milling slurry is 5-25 ℃; the drying is selected from spray drying and oven drying.
Further, the pressing can be any mode in the ceramic preparation process, preferably one of unidirectional pressing, bidirectional pressing or isostatic pressing, and the pressing pressure is 150-300 MPa.
Further, the high-temperature sintering condition includes: vacuum sintering, argon or nitrogen atmosphere sintering, argon or nitrogen pressure sintering, hot press sintering or hot isostatic pressing sintering.
The invention adopts the sintering modes of vacuum sintering, argon and nitrogen atmosphere sintering, argon and nitrogen air pressure sintering, hot-pressing sintering and hot isostatic pressing sintering, and introduces Cr into the raw materials 3 C 2 And/or VC sintering aid, which plays a role in inhibiting grain growth while reducing the highest sintering temperature of the matrix; meanwhile, the red hardness, oxidation resistance and wear resistance of the titanium carbonitride can be improved by introducing the titanium carbonitride in a direct adding mode, so that a composite ceramic matrix with good dimensional stability and excellent comprehensive mechanical property is obtained, and the service life of the material is prolonged.
Further, the specific sintering process of high-temperature sintering is as follows:
vacuum sintering: heating to 650-750 ℃ in vacuum with the pressure lower than 100Pa for 0.5-2 h, then continuously heating to 1000-1100 ℃ for 0.5-2 h, finally heating to 1300-1900 ℃ for 0.5-2 h, and cooling to room temperature along with the sintering;
sintering under argon or nitrogen atmosphere: heating to 750-800 ℃ in argon or nitrogen atmosphere of 0.6-5 kPa, and preserving heat for 0.5-2 h; then continuously heating to 1100-1250 ℃ and preserving heat for 0.5-2 h, finally heating to 1400-2000 ℃ and preserving heat for 0.5-2 h, and cooling to room temperature along with the furnace after sintering;
argon or nitrogen gas pressure sintering: heating to 800-850 ℃ in argon or nitrogen atmosphere with the pressure of 1-10 MPa, and preserving heat for 0.5-2 h; then continuously heating to 1250-1350 ℃ and preserving heat for 0.5-2 h, finally heating to 1500-2000 ℃ and preserving heat for 0.5-2 h, and cooling to room temperature along with the furnace after sintering;
hot pressing and sintering: under the protection of 0.3 kPa-2 kPa argon atmosphere, the hot pressing temperature is 1500-2000 ℃, the pressure is 10-45 MPa, and the pressure maintaining time is 10-60 min;
and (3) hot isostatic pressing sintering, namely heating to 650-750 ℃ in vacuum of less than 100Pa, preserving heat for 0.5-2 h, then continuously heating to 1000-1100 ℃ and preserving heat for 0.5-2 h, finally introducing 100-220 MPa nitrogen or argon, heating to 1500-1800 ℃ and preserving heat for 20-80 min, and cooling to room temperature along with a furnace after sintering.
The composite ceramic is applied to cutting tools and sintered bodies of wear-resistant parts.
The technical principle of the invention is as follows:
at TiB 2 Cr is added into TiC composite ceramic 3 C 2 And/or VC is used as a sintering aid, can be dispersed and distributed at a ceramic grain boundary in the sintering process, and can inhibit the growth of crystal grains in the sintering process, thereby achieving the effect of fine grains. And Cr 3 C 2 The VC has a low melting point, and can play a role in reducing the highest sintering temperature of the system after being added, so that the density of a matrix is improved. By adding Ti (C, N) to replace TiC partially or completely, the oxidation resistance and the wear resistance of the Ti (C, N) are better than those of TiC in red hardness, and the Ti B formed by adding the Ti (C, N) is added 2 The TiC+Ti (C, N)/Ti (C, N) ceramic system has more excellent comprehensive mechanical property.
Directly adopts an in-situ synthesis method, on one hand, the target product such as TiB after sintering the phase 2 The TiC content error is larger, on the other hand, the in-situ reaction is too severe, the reaction degree is difficult to control, and the dimensional stability after molding is poor. In the technical scheme of the invention, tiB is selected for realizing the technical purpose 2 ，TiC，Ti(C,N)，Cr 3 C 2 And/or VC finished product raw materials, ball milling raw material powder and sintering auxiliary agent at the same time, wherein the sintering auxiliary agent is uniformly distributed in a ball milling solvent, and the sintering auxiliary agent is coated on the surface of the raw material powder along with evaporation of the ball milling solvent in a subsequent drying process. When the addition amount of the sintering additive is lower than the limit content of the invention, the powder surface can not be completely coated, and the effect of grain refinement can not be achieved; above the limit content of the invention, an inclusion phase is formed after sintering, and the mechanical property of the ceramic is deteriorated. In the sintering process, the sintering aid is dispersed on the surface of the ceramic crystal grains, the highest sintering temperature is reduced, and Ti (C, N) is added, so that the ceramic matrix with high density, good dimensional stability and fine crystal grains is realized, the comprehensive mechanical property of the ceramic matrix is greatly improved, and the service life of the cutter is further prolonged.
The invention discloses the following technical effects:
the invention provides a method for directly synthesizing TiB by adding sintering auxiliary agent 2 Process method of-TiC/Ti (C, N)/Ti (C, N) +TiC composite ceramicOn the premise of ensuring the compactness and the dimensional stability of the matrix, the red hardness, the oxidation resistance and the wear resistance of the alloy are improved. The method has greater potential in the field of machining, and simultaneously, the application prospect of the method serving as a high-precision structural member is expected to be expanded.
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 an SEM image of the composite ceramic of example 1.
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.
In the embodiment of the invention, ti (C, N), tiC and TiB 2 、Cr 3 C 2 And VC were purchased from beijing taixin long limited.
Example 1
(1) Weighing the following raw materials in percentage by mass: cr (Cr) 3 C 2 15%, ti (C, N) 40%, the balance TiB 2 The sum of the mass fractions of the raw materials is 100%; the average grain diameter of the raw material powder is 0.5-2 um;
(2) Weighing powder raw materials, uniformly mixing, placing in a ball mill, wet-grinding, drying, and pressing into a green body by a press;
wherein wet milling conditions: ethanol is adopted as a wet grinding solvent, the mass of the solvent/the mass of the raw material=2:1, the hard alloy balls are adopted as grinding media, the mass of the grinding media/the mass of the raw material=5:1, the ball milling time is 20h, and the temperature of ball milling slurry is 5 ℃; drying is spray drying;
and one-way mould pressing with the pressing pressure of 150MPa.
(3) The obtained green body is sintered in vacuum: heating to 650 ℃ and preserving heat for 0.5h, then continuously heating to 1000 ℃ and preserving heat for 0.5h, finally heating to 1800 ℃ and preserving heat for 1h, cooling to room temperature along with the furnace after sintering to obtain the composite ceramic, wherein an SEM image of the composite ceramic in the embodiment 1 is shown in figure 1.
Example 2
The difference from example 1 is that the raw materials consist of: cr (Cr) 3 C 2 10%, ti (C, N) 55%, the balance TiB 2 。
Wherein wet milling conditions: water is adopted as a wet grinding solvent, the mass of the solvent/the mass of the raw material=3:1, the steel balls are used as grinding media, the mass of the grinding media/the mass of the raw material=7:1, the ball milling time is 30 hours, and the temperature of ball milling slurry is 25 ℃; the drying is oven drying at 80deg.C.
Example 3
The difference from example 1 is that the raw materials consist of: cr (Cr) 3 C 2 1%, 50% of Ti (C, N), 20% of TiC and the balance of TiB 2 。
Example 4
The difference from example 1 is that the raw materials consist of: cr (Cr) 3 C 2 8%, tiC48%, ti (C, N) 12%, and TiB the rest 2 。
Example 5
The difference from example 1 is that the raw materials consist of: cr (Cr) 3 C 2 5%, ti (C, N) 80%, the balance TiB 2 。
Example 6
As in example 1, cr is added 3 C 2 And is replaced by VC of equal quality.
Example 7
The difference from example 1 is that the raw materials consist of: cr (Cr) 3 C 2 5%, VC10%, the balance TiB 2 。
Example 8
The difference from example 1 is that the wet milling drying process is omitted; the results show that omitting this step does not make it possible to obtain the target substance.
Example 9
The difference from example 1 is that wet milling is replaced by dry milling.
Example 10
The difference from example 1 is that the obtained green body is sintered in an argon atmosphere: heating to 750 ℃ in 3kPa argon atmosphere, and preserving heat for 0.5h; then continuously heating to 1250 ℃ and preserving heat for 0.5h, finally heating to 1900 ℃ and preserving heat for 1.5h, and cooling to room temperature along with the furnace after sintering.
Example 11
The difference from example 1 is that the green body obtained was sintered with nitrogen gas pressure: heating to 850 ℃ in a nitrogen atmosphere of 5MPa, and preserving heat for 0.5h; then continuously heating to 1250 ℃ and preserving heat for 0.5h, finally heating to 2000 ℃ and preserving heat for 1h, and cooling to room temperature along with the furnace after sintering.
Example 12
The difference from example 1 is that the green body obtained was sintered by hot pressing: under the protection of 0.5kPa argon atmosphere, the hot pressing temperature is 1700 ℃, the pressure is 30MPa, and the pressure maintaining time is 30min.
Example 13
The difference from example 1 is that the green body obtained was sintered by hot isostatic pressing: heating to 700 ℃ in vacuum, preserving heat for 0.5h, then continuously heating to 1000 ℃ and preserving heat for 0.5h, finally introducing 100MPa argon, heating to 1650 ℃ and preserving heat for 70min, and cooling to room temperature along with the sintering.
Example 14
The difference from example 1 is that the molding was conducted in both directions, and the pressing pressure was 200MPa.
Example 15
The difference is that the average particle diameter of the raw material powder is 5 μm to 10. Mu.m, as in example 1.
Effect verification
For the mechanical property verification of the composite ceramics prepared in examples 1 to 15, the hardness was measured by using an LM700AT microhardness tester manufactured by LECO company, the flexural strength was measured according to GBT 4741, the fracture toughness was measured by using a CMT5105 microcomputer controlled universal material tester, and the results are shown in Table 1.
TABLE 1
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 (10)
1. A composite ceramic is characterized by comprising a first ceramic phase, a second ceramic phase and a sintering aid;
wherein the first ceramic phase is Ti (C, N)/Ti (C, N) +TiC; the second ceramic phase is TiB 2 The method comprises the steps of carrying out a first treatment on the surface of the The sintering aid is Cr 3 C 2 And/or VC.
2. The composite ceramic according to claim 1, wherein the raw materials include, in terms of mass fraction: tiB (TiB) 2 5％～45％，Ti(C,N)+TiC40％～80％，Cr 3 C 2 And/or VC 1-15%.
3. The composite ceramic of claim 2, wherein Ti (C, N) +tic comprises 10% -80% Ti (C, N) and the balance TiC.
4. A method for preparing a composite ceramic according to any one of claims 1 to 3, wherein the composite ceramic is obtained by uniformly mixing powder raw materials, wet-milling, drying, pressing into a green body, and then sintering at a high temperature.
5. The method for producing a composite ceramic according to claim 4, wherein the powder raw material has a powder particle size of 0.5 to 2. Mu.m, and the oxygen content thereof is 0.5% or less in mass fraction.
6. The method for producing a composite ceramic according to claim 4, wherein the wet milling specifically comprises: water or ethanol is adopted as a wet grinding solvent, the mass ratio of the solvent to the powder raw material is=2:1-3:1, the hard alloy balls or steel balls are ball milling media, the mass ratio of the ball milling media to the raw material is=5:1-7:1, the ball milling time is 20-100 h, and the temperature of the ball milling slurry is 5-25 ℃.
7. The method for producing a composite ceramic according to claim 4, wherein the pressing pressure is 150 to 300MPa.
8. The method of producing a composite ceramic according to claim 4, wherein the high-temperature sintering conditions include: vacuum sintering, argon or nitrogen atmosphere sintering, argon or nitrogen pressure sintering, hot press sintering or hot isostatic pressing sintering.
9. The method for preparing composite ceramic according to claim 8, wherein the specific sintering process of high-temperature sintering is as follows:
vacuum sintering: heating to 650-750 ℃ in vacuum with the pressure lower than 100Pa for 0.5-2 h, then continuously heating to 1000-1100 ℃ for 0.5-2 h, finally heating to 1300-1900 ℃ for 0.5-2 h, and cooling to room temperature along with the sintering;
sintering under argon or nitrogen atmosphere: heating to 750-800 ℃ in argon or nitrogen atmosphere of 0.6-5 kPa, and preserving heat for 0.5-2 h; then continuously heating to 1100-1250 ℃ and preserving heat for 0.5-2 h, finally heating to 1400-2000 ℃ and preserving heat for 0.5-2 h, and cooling to room temperature along with the furnace after sintering;
argon or nitrogen gas pressure sintering: heating to 800-850 ℃ in argon or nitrogen atmosphere with the pressure of 1-10 MPa, and preserving heat for 0.5-2 h; then continuously heating to 1250-1350 ℃ and preserving heat for 0.5-2 h, finally heating to 1500-2000 ℃ and preserving heat for 0.5-2 h, and cooling to room temperature along with the furnace after sintering;
hot pressing and sintering: under the protection of 0.3 kPa-2 kPa argon atmosphere, the hot pressing temperature is 1500-2000 ℃, the pressure is 10-45 MPa, and the pressure maintaining time is 10-60 min;
and (3) hot isostatic pressing sintering, namely heating to 650-750 ℃ in vacuum of less than 100Pa, preserving heat for 0.5-2 h, then continuously heating to 1000-1100 ℃ and preserving heat for 0.5-2 h, finally introducing 100-220 MPa nitrogen or argon, heating to 1500-1800 ℃ and preserving heat for 20-80 min, and cooling to room temperature along with a furnace after sintering.
10. Use of the composite ceramic according to any one of claims 1 to 3 in a sintered body of a cutting tool, a wear part.
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