阅读说明：本技术 一种TiCx增强Ti3AlC2-Fe基耐高温自润滑复合材料的制备方法 (Preparation method of TiCx-enhanced Ti3AlC 2-Fe-based high-temperature-resistant self-lubricating composite material ) 是由 邹芹 李艳国 王明智 袁东方 于 2020-07-09 设计创作，主要内容包括：本发明提供一种TiCx增强Ti<Sub>3</Sub>AlC<Sub>2</Sub>-Fe基耐高温自润滑复合材料的制备方法,包括如下步骤：S1、氩气氛围中将Fe合金粉、TiC<Sub>x</Sub>粉和Ti<Sub>3</Sub>AlC<Sub>2</Sub>颗粒进行球磨,制得混合粉末；S2、将所述混合粉末在氩气氛围内烘干,并装入模具中预压成型,得到预压原料块；S3、将所述预压原料块进行真空热压烧结,得到毛坯试件；S4、将所述毛坯试件进行表面抛光处理得到以Ti<Sub>3</Sub>AlC<Sub>2</Sub>为润滑相和TiC<Sub>x</Sub>为润滑结合相的Fe基耐高温自润滑复合材料。采用真空热压烧结的制备方式使材料拥有良好的力学性能,材料的致密度等大大提升。(The invention provides a TiCx enhanced Ti 3 AlC 2 The preparation method of the Fe-based high-temperature resistant self-lubricating composite material comprises the following steps: s1, mixing Fe alloy powder and TiC in argon atmosphere x Powder and Ti 3 AlC 2 Ball milling the particles to obtain mixed powder; s2, drying the mixed powder in an argon atmosphere, and putting the dried mixed powder into a mold for prepressing and forming to obtain a prepressed raw material block; s3, carrying out vacuum hot-pressing sintering on the pre-pressed raw material block to obtain a blank test piece; s4, carrying out surface polishing treatment on the blank test piece to obtain Ti 3 AlC 2 To a lubricating phase and TiC x Is Fe-based high-temperature resistant self-lubricating composite material for lubricating binding phase. The preparation method of vacuum hot-pressing sintering is adopted, so that the material has good mechanical properties, and the density and the like of the material are greatly improved.)

1. TiCx enhanced Ti₃AlC₂The preparation method of the Fe-based high-temperature-resistant self-lubricating composite material is characterized by comprising the following steps of:

s1, mixing Fe alloy powder and TiC in argon atmosphere_xPowder and Ti₃AlC₂Ball milling the particles to obtain mixed powder;

s2, drying the mixed powder in an argon atmosphere, and putting the dried mixed powder into a mold for prepressing and forming to obtain a prepressed raw material block;

s3, carrying out vacuum hot-pressing sintering on the pre-pressed raw material block to obtain a blank test piece;

s4, carrying out surface polishing treatment on the blank test piece to obtain Ti₃AlC₂To a lubricating phase and TiC_xIs Fe-based high-temperature resistant self-lubricating composite material for lubricating binding phase.

2. A TiCx enhanced Ti of claim 1₃AlC₂The preparation method of the Fe-based high-temperature resistant self-lubricating composite material is characterized in that in the step S1, the Fe alloy powder is formed by ball milling of Cu powder, Ni powder, Cr powder and Fe powder.

3. A TiCx enhanced Ti of claim 2₃AlC₂The preparation method of the Fe-based high-temperature-resistant self-lubricating composite material is characterized in that Fe alloy powder and TiC are added in the argon atmosphere in the step S1_xPowder and Ti₃AlC₂Ball milling the particles to obtain a mixed powder comprising: uniformly ball-milling and mixing Cu powder, Ni powder, Cr powder and Fe by using a planetary ball mill in an argon atmosphere, taking alcohol as a dispersing agent, and preparing the Fe alloy powder by using hard alloy balls as milling balls of the planetary ball mill at a ball-to-material ratio of 4:1, a rotation speed of 200 plus materials of 350r/min and a ball-milling time of 0.5-4 h; adding TiCx powder and Ti₃AlC₂And (4) performing ball milling on the particles for 0.5 to 2 hours at the same rotating speed to obtain the mixed powder.

4. A TiCx enhanced Ti according to claim 2 or 3₃AlC₂-Fe-based high temperature resistant self-lubricating composite material, characterized in that in step S1, the TiC is_xThe volume percentage of the powder is 5-20 vol.%, and the Ti is₃AlC₂Volume percent of 10-40 vol.%, volume percent of Cu of 1-7 vol.%, volume percent of Ni of 0.1-3 vol.%, volume percent of Cr of 0.1-3 vol.%。

5. A TiCx enhanced Ti of claim 1₃AlC₂The preparation method of the Fe-based high-temperature resistant self-lubricating composite material is characterized in that the prepressing forming process in the step S2 is as follows: the pressure is 15-100MPa, and the dwell time is 10-30 s.

6. A TiCx enhanced Ti of claim 1₃AlC₂The preparation method of the Fe-based high temperature resistant self-lubricating composite material is characterized in that the vacuum hot-pressing sintering process in the step S3 is as follows: and (3) carrying out vacuum hot-pressing sintering on the pre-pressed raw material block in an argon atmosphere, wherein the vacuum degree is 15-200Pa, the sintering pressure is 20-100MPa, the temperature is increased to 850-1300 ℃ at the heating rate of 10-50 ℃/min, and then the temperature is kept for 10-120min, so as to obtain the blank test piece.

7. A TiCx enhanced Ti of claim 1₃AlC₂A preparation method of Fe-based high-temperature resistant self-lubricating composite material, which is characterized in that TiC is prepared_xX is more than or equal to 0.4 and less than or equal to 1.1.

8. A TiCx enhanced Ti of claim 2₃AlC₂The preparation method of the Fe-based high-temperature resistant self-lubricating composite material is characterized in that the granularity of the TiCx powder is 2-45 mu m; the Ti₃AlC₂The particle size of the particles is 20-200 meshes; the particle size of the Fe powder is 10-30 mu m; the granularity of the Cu powder is 10-30 mu m; the particle size of the Ni powder is 1-20 mu m, and the particle size of the Cr powder is 10-60 mu m.

Technical Field

The invention relates to the technical field of material compounding, in particular to TiCx enhanced Ti₃AlC₂Fe-based high temperature resistant self-lubricatingA method for preparing a slip composite.

Background

With the continuous research and development of Fe alloy, the performance is continuously improved, and the application of Fe-based self-lubricating composite materials is attempted in the field of rotational friction of aerospace bearings, aerospace landing gears and the like at present. Manmen Liu et al utilized Ti after much of the previous research₃AlC₂Replacing graphite with Ag/Ti₃AlC₂Combined with alternative Ag/graphite, in which Ti₃AlC₂To form an Ag (Al) solid solution in the interface region, greatly enhancing the Ag/Ti ratio₃AlC₂The mechanical property of the composite material improves the friction property and the strength.

[Manmen Liu，Jialin Chen，Hao Cui，Xudong Sun，S hao hong Liu，mingXie.Ag/Ti₃AlC₂Composites with High Hardness，High Strength and HighConductivity[J].Materials Letters，2017](ii) a Study on Ti content in Chenglin group₃AlC₂The Ti is prepared under the hot pressing condition of 1300 ℃, 30MPa and 30min heat preservation in the presence of the Fe-based material₃AlC₂a/Fe composite material, the composite material being subjected to thermal shock at 800 ℃ except 30 vol.% Ti₃AlC₂The strength of other samples except Fe is basically unchanged or slightly increased, the fracture mode of the material before and after thermal shock is basically unchanged, and the good thermal shock resistance is shown. Demonstrating its good impact resistance. ' Chenglin, Zhai Xiang, Huang Ying, Zhai Ti₃AlC₂Preparation and mechanical properties of/Fe composite material [ J]Artificial crystal bulletin, 2015, 4(11):3288-](ii) a The study at this time noted Ti₃AlC₂Although having good lubricating properties, Ti is made good if sintering is not performed₃AlC₂If the lubricant is preserved, the lubricant effect is not achieved, and the aging and the like are examined for Ti₃AlC₂The mutual reaction with Fe at high temperature shows that Ti reacts with Fe at the sintering temperature of 760-1045 DEG C₃AlC₂The reaction with Fe is weak and TiC begins to form_0.6Phase, and theoretical analysis found Ti₃AlC₂The precipitation of Al in the alloy is caused by Ti₃AlC₂Reacting with Fe at a temperature far below its decomposition temperatureThe main factor of the response. [ Chenxinhua, Zhai Xiang, Song Peng Fei, yellow Ying, Ti₃AlC₂Reaction behavior with Fe at high temperatures (English) [ J]Rare Metal materials and engineering, 2011, 40(S1):499-](ii) a Ti in the previous study₃AlC₂Too low a dissolution temperature of the mixed metal material will result in Ti₃AlC₂So that the proper sintering temperature will make the material successfully prepared, and the material is Ti₃AlC₂Ti is prepared by using an electroless copper plating method₃AlC₂Cu material followed by copper powder, Ti₃AlC₂Material Ti prepared by sintering material at 850 DEG C₃AlC₂Uniformly distributed, 15 vol.% Ti content under higher friction pressure₃AlC₂The friction coefficient of the alloy can reach 0.15 at the lowest, and the wear performance is improved by nearly 20 percent after electroless copper plating. [ Wang Xiujuan. Ti₃AlC₂Preparation of/Cu composite and Performance study thereof [ D]Combined fertilizer industry university, 2014](ii) a Study on Chenlu et al Ti₃AlC₂The temperature effect of the material and the Fe-based material suggests that the raw material Ti is at 1400 DEG C₃AlC₂When the content by volume of (A) is changed from 10 vol.% to 40 vol.%, Al is changed from Ti₃AlC₂Escape out of the reaction kettle to form TiCx, and then the TiCx-Fe-based composite material is prepared in situ. Influence of Telu-TiCx content on hot pressing preparation of TiCx-Fe base composite material]China Special ceramic conference of silicate society, nineteenth national high-tech ceramic academic annual meeting summary collection [ C)]The China society for silicate society Special ceramics: 2016:1](ii) a Lijing and the like adopt a mechanical alloying combined annealing treatment process to prepare Fe3Al powder with different Al contents, and the Fe3Al intermetallic compound bulk material is obtained by vacuum hot-pressing sintering. The room temperature mechanical property of the Fe3Al sintered block material is obviously improved compared with that of an as-cast state, the room temperature bending strength is 1000-1400 MPa, the compressive yield strength and the compressive strain are 1200-1800 MPa and 10-15% respectively, and the Rockwell hardness is 55-60 HRC; the change of Al content has certain influence on the microstructure and the mechanical property of the alloy. [ microstructure and mechanical properties of Lijing, Yi derived Sheng, Liu Ying, et al. hot pressing sintering FeAl intermetallic compound [ J]Material heat treatment journal(04).]. The above studies have demonstrated Ti₃AlC₂Has good lubricating properties, but Ti₃AlC₂Is easy to fall off from the matrix, so that the overall performance, especially the lubricating performance, of the composite material is influenced.

This patent is at Ti₃AlC₂The improvement on the preparation technology of the Fe composite material is promoted, the traditional preparation technology is not suitable for preparing the novel composite material, the powder metallurgy technology is started, a good preparation environment is provided for the novel composite material, and the powder metallurgy technology can be used for completing good preparation at a lower sintering temperature. The SPS sintering technology is high in sintering speed and applied to numerous researches, but certain defects can be generated when the sintering speed is too high, the bonding performance of the metal ceramic material can be particularly influenced, and meanwhile, the sintering reaction decomposition of the composite material can be promoted to a certain extent by the spark plasma heating method, so that Ti is more inhibited₃AlC₂-applicability of Fe composite materials. The processing technology for ensuring the good performance of the material is very important.

Disclosure of Invention

In accordance with the above technical problems, there is provided a TiCx-enhanced Ti₃AlC₂A preparation method of Fe-based high-temperature resistant self-lubricating composite material.

The technical means adopted by the invention are as follows:

TiCx enhanced Ti₃AlC₂The preparation method of the Fe-based high-temperature resistant self-lubricating composite material comprises the following steps:

s1, mixing Fe alloy powder, TiCx powder and Ti in argon atmosphere₃AlC₂Ball milling the particles to obtain mixed powder;

s2, drying the mixed powder in an argon atmosphere, and putting the dried mixed powder into a mold for prepressing and forming to obtain a prepressed raw material block; the pre-pressing forming can improve the sintering density of the material;

s3, carrying out vacuum hot-pressing sintering on the pre-pressed raw material block to obtain a blank test piece;

s4, carrying out surface polishing treatment on the blank test piece to obtain Ti₃AlC₂For lubricating phase and TiCx for lubricating bondThe Fe-based high-temperature resistant self-lubricating composite material of the phase.

Further, in step S1, the Fe alloy powder is formed by ball milling Cu powder, Ni powder, Cr powder, and Fe powder.

Further, Fe alloy powder, TiCx powder and Ti are mixed in the argon atmosphere in the step S1₃AlC₂Ball milling the particles to obtain a mixed powder comprising: uniformly ball-milling and mixing Cu powder, Ni powder, Cr powder and Fe by using a planetary ball mill in an argon atmosphere, taking alcohol as a dispersing agent (other dispersing agents which have strong volatility and do not react with the mixed powder can be used for mixing, so that the dispersing agent can influence the final sintering material during sintering), and preparing the Fe alloy powder by using hard alloy balls as milling balls of the planetary ball mill at a ball-to-material ratio of 4:1, a rotation speed of 200 and 350r/min and ball-milling time of 0.5-4 h; adding TiCx powder and Ti₃AlC₂And (4) performing ball milling on the particles for 0.5 to 2 hours at the same rotating speed to obtain the mixed powder.

Further, in the step S1, the volume percentage of the TiCx powder is 5-20 vol.%, and the Ti content is₃AlC₂The volume percent is 10-40 vol.%, the volume percent of Cu is 1-7 vol.%, the volume percent of Ni is 0.1-3 vol.%, and the volume percent of Cr is 0.1-3 vol.%.

Further, the pre-press molding process in the step S2 is: the pressure is 15-100MPa, and the dwell time is 10-30 s.

Further, the vacuum hot-pressing sintering process in the step S3 is as follows: and (3) carrying out vacuum hot-pressing sintering on the pre-pressed raw material block in an argon atmosphere, wherein the vacuum degree is 15-200Pa, the sintering pressure is 20-100MPa, the temperature is increased to 850-1300 ℃ at the heating rate of 10-50 ℃/min, and then the temperature is kept for 10-120min, so as to obtain the blank test piece.

Further, the TiC_xX is more than or equal to 0.4 and less than or equal to 1.1.

Further, the granularity of the TiCx powder is 2-45 μm; the Ti₃AlC₂The particle size of the particles is 20-200 meshes; the particle size of the Fe powder is 10-30 mu m; the granularity of the Cu powder is 10-30 mu m; the particle size of the Ni powder is 1-20 mu m, and the particle size of the Cr powder is10-60μm。

Compared with the prior art, the invention has the following advantages:

1. the Fe alloy is adopted as the matrix, so that the composite material with high density and high hardness can be obtained at the temperature of 850-1300 ℃; and Ti₃AlC₂The Fe-based self-lubricating composite material belongs to a ternary-layer ceramic compound, integrates excellent performances of ceramics and metals, can strengthen the Fe-based self-lubricating composite material, can be used as a lubricating mechanism with rich lubricating phases, and overcomes the defects of high dry friction coefficient and high wear rate of Fe alloy materials.

2. The prepared Fe-based high-temperature self-lubricating composite material not only has high bearing, high strength and high temperature resistance, but also can effectively improve the self-lubricating property under the action of a multi-component lubricating phase, and is more suitable for manufacturing friction materials such as self-lubricating bearings under severe working conditions.

3. The preparation method of vacuum hot-pressing sintering is adopted, so that the material has good mechanical properties, and the density and the like of the material are greatly improved. Meanwhile, the vacuum hot-pressing sintering preparation adopts an induction heating method, the sintering speed is slightly slowed down, but the stability of the sintered material is greatly improved, and meanwhile, the sintering pressure can be greatly improved, so that the material performance is improved.

Based on the reasons, the invention can be widely popularized in the fields of friction plates, bearings, high-temperature wear-resistant structural parts and the like.

Detailed Description

It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The described embodiments are only some embodiments of the invention, not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The relative arrangement of the steps set forth in these embodiments does not limit the scope of the invention unless specifically stated otherwise. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any particular value, in all examples shown and discussed herein, should be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values.

TiCx enhanced Ti₃AlC₂The preparation method of the Fe-based high-temperature resistant self-lubricating composite material comprises the following steps:

s1, mixing Fe alloy powder, TiCx powder and Ti in argon atmosphere₃AlC₂Ball milling the particles to obtain mixed powder;

s2, drying the mixed powder in an argon atmosphere, and putting the dried mixed powder into a mold for prepressing and forming to obtain a prepressed raw material block; the pre-pressing forming can improve the sintering density of the material;

s3, carrying out vacuum hot-pressing sintering on the pre-pressed raw material block to obtain a blank test piece;

s4, carrying out surface polishing treatment on the blank test piece to obtain Ti₃AlC₂Is a Fe-based high-temperature resistant self-lubricating composite material with a lubricating phase and TiCx as a lubricating binding phase.

Further, in step S1, the Fe alloy powder is formed by ball milling Cu powder, Ni powder, Cr powder, and Fe powder.

Further, Fe alloy powder, TiCx powder and Ti are mixed in the argon atmosphere in the step S1₃AlC₂Ball milling the particles to obtain a mixed powder comprising: uniformly ball-milling and mixing Cu powder, Ni powder, Cr powder and Fe by using a planetary ball mill in an argon atmosphere, taking alcohol as a dispersing agent (other dispersing agents which have strong volatility and do not react with the mixed powder can be used for mixing, so that the dispersing agent can influence the final sintering material during sintering), and preparing the Fe alloy powder by using hard alloy balls as milling balls of the planetary ball mill at a ball-to-material ratio of 4:1, a rotation speed of 200 and 350r/min and ball-milling time of 0.5-4 h; adding TiCx powder and Ti₃AlC₂And (4) performing ball milling on the particles for 0.5 to 2 hours at the same rotating speed to obtain the mixed powder.

Further, in the step S1, the volume percentage of the TiCx powder is 5-20 vol.%, and the Ti content is₃AlC₂The volume percent is 10-40 vol.%, the volume percent of Cu is 1-7 vol.%, the volume percent of Ni is 0.1-3 vol.%, and the volume percent of Cr is 0.1-3 vol.%.

Further, the pre-press molding process in the step S2 is: the pressure is 15-100MPa, and the dwell time is 10-30 s.

Further, the vacuum hot-pressing sintering process in the step S3 is as follows: and (3) carrying out vacuum hot-pressing sintering on the pre-pressed raw material block in an argon atmosphere, wherein the vacuum degree is 15-200Pa, the sintering pressure is 20-100MPa, the temperature is increased to 850-1300 ℃ at the heating rate of 10-50 ℃/min, and then the temperature is kept for 10-120min, so as to obtain the blank test piece.

Further, the TiC_xX is more than or equal to 0.4 and less than or equal to 1.1.

Further, the granularity of the TiCx powder is 2-45 μm; the Ti₃AlC₂The particle size of the particles is 20-200 meshes; the particle size of the Fe powder is 10-30 mu m; the granularity of the Cu powder is 10-30 mu m; the particle size of the Ni powder is 1-20 mu m, and the particle size of the Cr powder is 10-60 mu m.