CN110257680A - A kind of Fe based high-temp-resistant composite material and preparation method containing polynary lubrication phase - Google Patents

A kind of Fe based high-temp-resistant composite material and preparation method containing polynary lubrication phase Download PDF

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CN110257680A
CN110257680A CN201910724405.2A CN201910724405A CN110257680A CN 110257680 A CN110257680 A CN 110257680A CN 201910724405 A CN201910724405 A CN 201910724405A CN 110257680 A CN110257680 A CN 110257680A
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composite material
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李艳国
邹芹
袁东方
王明智
关勇
成照楠
赵玉成
陈伟东
党赏
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Yanshan University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/067Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • C22C33/0257Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0292Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with more than 5% preformed carbides, nitrides or borides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of Fe based high-temp-resistant composite material containing polynary lubrication phase, the percents by volume of chemical component are as follows: TiCx5-20vol.% (0.4≤x≤1.1), Ti3AlC210-40vol.%, Cu 1-7vol.%, Ni 0.1-3vol.%, Cr 0.1-3vol.%, remaining is Fe powder;The preparation method of above-mentioned composite material is mainly by TiCxPowder, Ti3AlC2Particle, Fe powder, Cu powder, Ni powder, Cr powder pass through mixing, precompressed drying and discharge plasma sintering, are made with Ti3AlC2And TiCxFor the Fe based high-temp-resistant composite material for lubricating phase.Operation of the present invention is simple, short preparation period, and Fe based high-temp-resistant composite material obtained not only has lower coefficient of friction and wear rate, but also has the performances such as high-mechanic, high intensity, is suitable for the antifriction materials such as self-lubricating bearing under mass production bad working environments.

Description

A kind of Fe based high-temp-resistant composite material and preparation method containing polynary lubrication phase
Technical field
The present invention relates to technical field of composite materials, specifically a kind of Fe based high-temp-resistant composite material containing polynary lubrication phase And preparation method thereof.
Background technique
With the continuous research and development of Fe alloy, performance constantly improves, at present the fields such as aerospace bearing, space flight undercarriage Attempting using Fe based self lubricated composite material.Manmen Liu et al. people utilizes Ti in many studies3AlC2It is found instead of graphite Ti3AlC2Ag (Al) solid solution is formed in interface area after decomposition, greatly strengthens Ag/Ti3AlC2The mechanical property of composite material, Improve friction and wear behavior and intensity [Manmen Liu, Jialin Chen, hao Cui, et al.Ag/Ti3AlC2 Composites withhighhardness, highstrength andhigh conductivity.Materials Letters, 2017].The research Ti such as Huang vibration warbler3AlC2When performance, Ti is had found by steel disk opposite grinding3AlC2High-speed friction performance [Huang vibration warbler .Ti very well3AlC2The coefficient of sliding friction and friction surface the national high-performance ceramics of oxidation behavior the 13rd Art annual meeting abstract collection .2004].The obtained Ti such as Chen Lin3AlC2/ Fe composite material, composite material remove after 800 DEG C of thermal shocks 30vol.%Ti3AlC2Except/Fe, other probe intensities are basically unchanged or slightly increase, and show good anti-thermal shock characteristic [Chen Lin, Zhai Hongxiang, Huang vibration warbler, Xu Hao .Ti3AlC2The preparation of/Fe composite material and mechanical characteristic artificial lens journal, 2015, 44(11):3288-3291].CHEN XINHUAs etc. pass through research Ti3AlC2Ti is found with Fe reacting to each other at high temperature3AlC2With Fe Reaction generates TiC0.6Phase, analysis find Ti3AlC2The precipitation of middle Al is to lead to Ti3AlC2Just in the case where being far below its decomposition temperature Principal element [CHEN XINHUA, Zhai Hongxiang, Song Pengfei, the Huang vibration warbler .Ti to react with Fe3AlC2With Fe at high temperature react row For Rare Metals Materials and engineering, 2011,40:499-502].Ti is made using the method for electroless copper in Wang Xiujuan etc.3AlC2- After Cu material and copper powder, Ti3AlC2Material is sintered at 850 DEG C is made Ti3AlC2The composite material being evenly distributed, larger Under friction pressure, contain 15vol.%Ti3AlC2Composite material coefficient of friction it is minimum up to 0.15, and polishing machine mentions Nearly 20% [Wang Xiujuan .Ti is risen3AlC2The preparation of/Cu composite material and its performance study HeFei University of Technology, 2014].It is old Road road etc. has studied Ti3AlC2With the temperature effect of Fe sill, the Ti at 1400 DEG C is proposed3AlC2Content is 10- Al is from Ti when 40vol.%3AlC2In escape to form TiCxAnd then TiC is formed in situx- Fe based composites, TiCxIt improves The overall performance of composite material [Chen Lulu .TiCxContent is to hot pressing for TiCxThe influence of-Fe based composites the 19th National high-performance ceramics Annual Conference abstract collection, 2016:1].Although the studies above demonstrates Ti3AlC2With good lubricating properties Can, but Ti3AlC2It easily falls off from matrix, the overall performance of composite material, especially greasy property is caused to be affected.Therefore, The application for researching and proposing TiCx is to solve Ti3AlC2It is also easy to produce good one of the solution that friction falls off.
Summary of the invention
The purpose of the present invention is to provide it is a kind of containing it is polynary lubrication phase Fe based high-temp-resistant composite material and preparation method, To solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of Fe based high-temp-resistant composite material containing polynary lubrication phase, the percent by volume of chemical component are as follows: TiCx 5- 20vol.%, Ti3AlC210-40vol.%, Cu 1-7vol.%, Ni 0.1-3vol.%, Cr 0.1-3vol.%, remaining is Fe powder.
As a further solution of the present invention: the TiCxIn, 0.4≤x≤1.1.
As a further solution of the present invention: the TiCxThe granularity of powder is 2-45 μm.
As a further solution of the present invention: the Ti3AlC2The granularity of particle is 20-200 mesh.
As a further solution of the present invention: the Fe powder, Cu powder granularity be 10-30 μm.
As a further solution of the present invention: the granularity of the Ni powder is 1-20 μm.
As a further solution of the present invention: the granularity of the Cr powder is 10-60 μm.
The preparation method of the Fe based high-temp-resistant composite material containing polynary lubrication phase, comprising the following steps:
Step 1): first carrying out uniform ball to Cu powder, Ni powder, Cr powder, Fe powder using planetary ball mill in argon atmosphere and mix, Alcohol is as dispersing agent, ratio of grinding media to material 6:1, revolving speed 200-350r/min, Ball-milling Time 0.5-2h;TiC is then addedx、Ti3AlC2 Particle, then with same rotational speed ball milling 1h;
Step 2): the mixed-powder of step 1) is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure Power 15-30MPa, dwell time 10-30s, mould diameter 30mm;
Step 3): sintering temperature is 850-1250 DEG C, and heating rate is 40-100 DEG C/min, sintering pressure 20- 100MPa, vacuum degree 15-40Pa keep the temperature 5-30min, carry out discharge plasma sintering in argon atmosphere, obtain blank test specimen;
Step 4): the blank test specimen of step 3) preparation is subjected to surface polishing treatment and is obtained with Ti3AlC2And TiCxFor collaboration Lubricate the Fe based high-temp-resistant composite material of phase.
As a further solution of the present invention: in step 1), abrading-ball uses WC sintered carbide ball.
The Fe based high-temp-resistant composite material containing polynary lubrication phase is in production self-lubricating bearing and antifriction material Purposes.
Compared with prior art, the beneficial effects of the present invention are:
1) using Fe alloy as matrix, the compound of high-compactness and high rigidity can be obtained under the conditions of 850-1250 DEG C Material;Ti3AlC2Belong to ternary layered ceramic compound, has gathered the excellent properties of ceramics and metal, Fe base can not only be strengthened Self-lubricating composite, moreover it is possible to mutually enrich lubrication mechanism as lubrication, improve the higher dry friction coefficient of Fe alloy material and abrasion The defect of rate;
2) the Fe base high temperature self lubricating composite material prepared not only has high-mechanic, high intensity, a high temperature resistance, and Its self-lubricating property can be effectively improved under the action of multicomponent lubrication phase, the self-lubricating axis being more suitable under production bad working environments Hold equal friction materials.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
In the embodiment of the present invention, one kind is provided with Ti3AlC2And TiCxPhase is lubricated for collaboration, and there is high-mechanic, high-strength The good a kind of Fe based high-temp-resistant composite material and preparation method containing polynary lubrication phase of degree, wearability.
The percent by volume of the chemical component of Fe based high-temp-resistant composite material of the invention are as follows: TiCx5-20vol.%, Ti3AlC210-40vol.%, Cu 1-7vol.%, Ni 0.1-3vol.%, Cr 0.1-3vol.%, remaining is iron powder.It is described TiCxThe granularity of powder is 2-45 μm;Ti3AlC2The granularity of particle is 20-200 mesh;Fe powder, Cu powder granularity be 10-30 μm, Ni powder Granularity be 1-20 μm, the granularity of Cr powder is 10-60 μm.
Containing it is polynary lubrication phase Fe based high-temp-resistant composite material preparation method the following steps are included:
Step 1), the preparation of mixed-powder
It first carries out uniform ball to Cu powder, Ni powder, Cr powder, Fe powder using planetary ball mill in argon atmosphere to mix, alcohol is made For dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200-350r/min, Ball-milling Time 0.5-2h;Then TiC is addedx、Ti3AlC2Particle, then with same rotational speed ball milling 1h;
Step 2), pre-molding
The mixed-powder of step 1) is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 15- 30MPa, dwell time 10-30s, mould diameter 30mm;
Step 3), discharge plasma sintering process
Sintering temperature is 850-1250 DEG C, and heating rate is 40-100 DEG C/min, sintering pressure 20-100MPa, vacuum 15-40Pa is spent, 5-30min is kept the temperature, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;
The blank test specimen of step 3) preparation is carried out surface polishing treatment and obtained with Ti by step 4)3AlC2And TiCxFor collaboration Lubricate the Fe based high-temp-resistant composite material of phase.
Embodiment 1
By percent by volume TiC0.45vol.%, Ti3AlC215vol.%, Cu 2.6vol.%, Ni 0.1vol.%, Cr 0.1vol.%, remaining is Fe powder, weighs raw material;By granularity be 10 μm Cu, the Fe powder that granularity is 20 μm, granularity be 1 μm Ni powder, that granularity is that 40 μm of Cr powder carries out uniform ball to it using planetary ball mill in argon atmosphere is mixed, alcohol is added As dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 350r/min, Ball-milling Time 0.5h;Then it is added The Ti of 160-200 mesh3AlC2Particle, 45 μm of TiC0.4, then with same rotational speed ball milling 1h, mixed-powder is made;By mixed powder End is dried in argon atmosphere, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 15MPa, dwell time 10s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1000 DEG C of sintering temperature, 80 DEG C of heating rate/ Min, sintering pressure 30MPa, vacuum degree 40Pa keep the temperature 20min, obtain blank test specimen;The blank test specimen of above-mentioned preparation is carried out Surface polishing treatment is obtained with Ti3AlC2And TiC0.4For the Fe base high temperature self lubricating composite material of collaboration lubrication phase.
Embodiment 2
By percent by volume TiC0.4For 10vol.%, Ti3AlC2It is for 15vol.%, Cu 2.6vol.%, Ni 1.2vol.%, Cr 2.4vol.%, remaining is Fe powder, weighs raw material;By granularity be 20 μm Cu powder, the Fe that granularity is 20 μm Ni powder that powder, granularity are 20 μm, the Cr powder that granularity is 20 μm carry out it uniformly in argon atmosphere using planetary ball mill Ball is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200r/min, Ball-milling Time 0.6h;The Ti of 120-160 mesh is then added3AlC2Particle, 2 μm of TiC0.4, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 30MPa, Dwell time 10s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1000 DEG C of sintering temperature, heating Rate 60 DEG C/min, sintering pressure 40MPa, vacuum degree 40Pa keep the temperature 20min, carry out discharge plasma sintering in argon atmosphere, Obtain blank test specimen;By the blank test specimen of above-mentioned preparation carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.4For The Fe base high temperature self lubricating composite material of collaboration lubrication phase.
Embodiment 3
By percent by volume TiC0.4For 15vol.%, Ti3AlC2It is for 15vol.%, Cu 2.6vol.%, Ni 1.2vol.%, Cr 3vol.%, remaining is Fe powder, weighs raw material;By granularity be 10 μm Cu, Fe powder, Ni powder, Cr powder is in argon Atmosphere enclose it is middle using planetary ball mill to carry out uniform ball to it mixed, alcohol is added and is used as dispersing agent, abrading-ball is using the conjunction of WC hard Gold goal, ratio of grinding media to material 6:1, revolving speed 350r/min, Ball-milling Time 0.7h;The Ti of 80-120 mesh is then added3AlC2Particle, 30 μm TiC0.4, then with same rotational speed ball milling 1h, mixed-powder is made;Mixed-powder is dried in argon atmosphere, and is packed into diameter and is Pre-molding in the graphite jig of 30mm, pressure 20MPa, dwell time 30s;Then it puts it into furnace and is carried out in argon atmosphere Discharge plasma sintering, 900 DEG C of sintering temperature, heating rate 60 DEG C/min, sintering pressure 35MPa, vacuum degree 30Pa, heat preservation 5min, argon atmosphere is interior to carry out discharge plasma sintering, obtains blank test specimen;The blank test specimen of above-mentioned preparation is subjected to surface throwing Light processing obtains described with Ti3AlC2And TiC0.4For the Fe based high-temp-resistant composite material of collaboration lubrication phase.
Embodiment 4
By percent by volume TiC0.4For 20vol.%, Ti3AlC2It is for 15vol.%, Cu 2.6vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;By granularity be 10 μm Cu powder, the Fe that granularity is 30 μm Ni powder that powder, granularity are 20 μm, the Cr powder that granularity is 30 μm carry out it uniformly in argon atmosphere using planetary ball mill Ball is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 350r/min, Ball-milling Time 0.8h;The Ti of 120-160 mesh is then added3AlC2Particle, 25 μm of TiC0.4, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 50MPa, Dwell time 30s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1000 DEG C of sintering temperature, heating Rate 40 DEG C/min, sintering pressure 100MPa, vacuum degree 30Pa keep the temperature 30min, obtain blank test specimen;By the hair of above-mentioned preparation Base test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.4For the Fe based high-temp-resistant composite wood of collaboration lubrication phase Material.
Embodiment 5
By percent by volume TiC0.4For 15vol.%, Ti3AlC2It is for 25vol.%, Cu 2.6vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 10 μm for being 10 μm by granularity Ni powder that powder, granularity are 1 μm, the Cr powder that granularity is 60 μm carry out uniform ball to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 250r/min, Ball-milling Time 0.9h;The Ti of 160-200 mesh is then added3AlC2Particle, 20 μm of TiC0.4, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 15MPa, Dwell time 20s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1250 DEG C of sintering temperature, heating Rate 80 DEG C/min, sintering pressure 34MPa, vacuum degree 40Pa keep the temperature 25min, obtain blank test specimen;By the blank of above-mentioned preparation Test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.4Fe based high-temperature self-lubricating for collaboration lubrication phase is compound Material.
Embodiment 6
By percent by volume TiC0.4For 15vol.%, Ti3AlC2It is for 30vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 10 μm for being 20 μm by granularity Ni powder that powder, granularity are 20 μm, the Cr powder that granularity is 10 μm carry out it uniformly in argon atmosphere using planetary ball mill Ball is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 340r/min, Ball-milling Time 0.5h;The Ti of 160-200 mesh is then added3AlC2Particle, 20 μm of TiC0.4Particle, then with same rotational speed ball milling 1h, it is made mixed Close powder;Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 20MPa, dwell time 20s;Then it puts it into and carries out discharge plasma sintering, sintering temperature 1250 in furnace in argon atmosphere DEG C, heating rate 85 DEG C/min, sintering pressure 32MPa, vacuum degree 40Pa keep the temperature 19min, obtain blank test specimen;By above-mentioned system Standby blank test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.4For the Fe based high-temp-resistant of collaboration lubrication phase Composite material.
Embodiment 7
By quality percentage TiC0.4For 15vol.%, Ti3AlC2It is for 40vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 30 μm for being 10 μm by granularity Ni powder that powder, granularity are 20 μm, the Cr powder that granularity is 40 μm carry out it uniformly in argon atmosphere using planetary ball mill Ball is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 320r/min, Ball-milling Time 0.6h;The Ti of 160-200 mesh is then added3AlC2Particle, 20 μm of TiC0.4, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 20MPa, Dwell time 30s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 850 DEG C of sintering temperature, heating speed Rate 100 DEG C/min, sintering pressure 100MPa, vacuum degree 15Pa keep the temperature 18min, obtain blank test specimen;By the blank of above-mentioned preparation Test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.4For the Fe based high-temp-resistant composite wood of collaboration lubrication phase Material.
Embodiment 8
By percent by volume TiC0.6For 9vol.%, Ti3AlC2It is for 18vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;By granularity be 10 μm Fe powder, the Cu that granularity is 20 μm Ni powder that powder, granularity are 3 μm, the Cr powder that granularity is 10 μm carry out uniform ball to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 220r/min, Ball-milling Time 0.7h;The Ti of 160-200 mesh is then added3AlC2Particle, 45 μm of TiC0.6, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 30MPa, Dwell time 30s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1050 DEG C of sintering temperature, heating Rate 90 DEG C/min, sintering pressure 44MPa, vacuum degree 15Pa keep the temperature 10min, obtain blank test specimen;By the blank of above-mentioned preparation Test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.6Fe based high-temperature self-lubricating for collaboration lubrication phase is compound Material.
Embodiment 9
By percent by volume TiC0.6For 13vol.%, Ti3AlC2It is for 18vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 10 μm for being 10 μm by granularity Ni powder that powder, granularity are 10 μm, the Cr powder that granularity is 10 μm carry out it uniformly in argon atmosphere using planetary ball mill Ball mixes, and alcohol is added and is used as dispersing agent, and abrading-ball is using WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 280r/min, when ball milling Between 0.8h;The Ti of 120-160 mesh is then added3AlC2Particle, 2 μm of TiC0.6, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 25MPa, Dwell time 10s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1150 DEG C of sintering temperature, heating Rate 90 DEG C/min, sintering pressure 41MPa, vacuum degree 30Pa keep the temperature 12min, obtain blank test specimen;By the blank of above-mentioned preparation Test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.6For the Fe based high-temp-resistant composite wood of collaboration lubrication phase Material.
Embodiment 10
By percent by volume TiC0.6For 13vol.%, Ti3AlC2It is for 23vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 30 μm for being 30 μm by granularity Ni powder that powder, granularity are 5 μm, the Cr powder that granularity is 40 μm carry out uniform ball to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 280r/min, Ball-milling Time 0.9h;The Ti of 120-160 mesh is then added3AlC2Particle, 2 μm of TiC0.6, then with same rotational speed ball milling 1h, mixed powder is made End;Mixed-powder is dried in argon atmosphere, and be fitted into diameter be 30mm graphite jig in pre-molding, pressure 30MPa, Dwell time 10s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1250 DEG C of sintering temperature, heating Rate 90 DEG C/min, sintering pressure 100MPa, vacuum degree 30Pa keep the temperature 12min, obtain blank test specimen;By the hair of above-mentioned preparation Base test specimen carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.6For the Fe based high-temp-resistant composite wood of collaboration lubrication phase Material.
Embodiment 11
By percent by volume TiC0.6For 18vol.%, Ti3AlC2It is for 23vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 30 μm for being 30 μm by granularity Ni powder that powder, granularity are 3 μm, the Cr powder that granularity is 60 μm carry out uniform ball to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 250r/min, Ball-milling Time 2h; The Ti of 120-160 mesh is then added3AlC2Particle, 45 μm of TiC0.6, then with same rotational speed ball milling 1h, mixed-powder is made;It will Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 20MPa, pressure maintaining Time 30s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 975 DEG C of sintering temperature, heating rate 100 DEG C/min, sintering pressure 39MPa, vacuum degree 15Pa, 21min is kept the temperature, blank test specimen is obtained;The blank of above-mentioned preparation is tried Part carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC0.6For the Fe based high-temp-resistant composite material of collaboration lubrication phase.
Embodiment 12
By percent by volume TiC1.1For 15vol.%, Ti3AlC2It is for 32vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 2.4vol.%, remaining is Fe powder, weighs raw material;Cu, the Fe that granularity is 10 μm for being 10 μm by granularity Ni powder that powder, granularity are 1 μm, the Cr powder that granularity is 10 μm carry out uniform ball to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200r/min, Ball-milling Time 2h; The Ti of 120-160 mesh is then added3AlC2Particle, 45 μm of TiC1.1, then with same rotational speed ball milling 1h, mixed-powder is made;It will Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 20MPa, pressure maintaining Time 30s;Then it puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, 1050 DEG C of sintering temperature, heating rate 80 DEG C/min, sintering pressure 30MPa, vacuum degree 40Pa, 20min is kept the temperature, blank test specimen is obtained;By the blank test specimen of above-mentioned preparation Carry out surface polishing treatment obtain it is described with Ti3AlC2And TiC1.1For the Fe based high-temp-resistant composite material of collaboration lubrication phase.
Embodiment 13
By percent by volume TiC0.4For 15vol.%, Ti3AlC2It is for 35vol.%, Cu 2.6vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, and the Cu that granularity is 10 μm, the Fe powder that granularity is 10 μm, granularity are 10 μm Ni powder, granularity be 10 μm of Cr powder, 20 μm of TiC0.4Uniform ball is carried out to it using planetary ball mill in argon atmosphere It is mixed, alcohol is added as dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 250r/min, Ball-milling Time 0.9h;The Ti of 160-200 mesh is then added3AlC2Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;By mixed powder End is dried in argon atmosphere, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 30MPa, dwell time Then 20s puts it into and carries out discharge plasma sintering in furnace in argon atmosphere, sintering temperature is 1200 DEG C, and heating rate is 80 DEG C/min, sintering pressure 34MPa, vacuum degree 40Pa, 25min is kept the temperature, discharge plasma sintering is carried out in argon atmosphere, obtains To blank test specimen;By the blank test specimen of above-mentioned preparation carry out surface polishing treatment obtain it is described with TiC0.4、Ti3AlC2For lubrication The Fe based high-temp-resistant self-lubricating composite of phase.
Embodiment 14
By percent by volume TiC0.6For 20vol.%, Ti3AlC2It is for 20vol.%, Cu 3.2vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, Cu that granularity is 10 μm, the Fe powder that granularity is 10 μm, 10 μm of Ni Powder, 10 μm of Cr powder, 35 μm of TiC0.6Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and wine is added Essence is used as dispersing agent, and abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 350r/min, Ball-milling Time 1.8h;Then add Enter the Ti of 120-160 mesh3AlC2Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;By mixed-powder in argon atmospher Interior drying is enclosed, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 25MPa, dwell time 20s;Then by it It is put into furnace and carries out discharge plasma sintering in argon atmosphere, sintering temperature is 1000 DEG C, and heating rate is 85 DEG C/min, sintering Pressure is 40MPa, vacuum degree 15Pa, keeps the temperature 14min, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;It will The blank test specimen of above-mentioned preparation carry out surface polishing treatment obtain it is described with TiC0.6、Ti3AlC2For the Fe Ji Naigao for lubricating phase Warm self-lubricating composite.
Embodiment 15
By percent by volume TiC0.8For 5vol.%, Ti3AlC2It is for 26vol.%, Cu 4.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, Cu that granularity is 10 μm, the Fe powder that granularity is 30 μm, 20 μm of Ni Powder, 20 μm of Cr powder, 20 μm of TiC0.8Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and wine is added Essence is used as dispersing agent, and abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 220r/min, Ball-milling Time 1.2h;Then add Enter the Ti of 120-160 mesh3AlC2Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;By mixed-powder in argon atmospher Interior drying is enclosed, and is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 25MPa, dwell time 10s;Then by it It is put into furnace and carries out discharge plasma sintering in argon atmosphere, sintering temperature is 1050 DEG C, and heating rate is 80 DEG C/min, sintering Pressure is 48MPa, vacuum degree 40Pa, keeps the temperature 13min, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;It will The blank test specimen of above-mentioned preparation carry out surface polishing treatment obtain it is described with TiC0.8、Ti3AlC2For the Fe Ji Naigao for lubricating phase Warm self-lubricating composite.
Embodiment 16
By percent by volume TiC0.8For 12vol.%, Ti3AlC2It is for 23vol.%, Cu 2.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining be Fe powder, the Cu that granularity is 20 μm, the Fe powder that granularity is 20 μm, Ni powder, Cr powder, 25 μm of TiC0.8Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and alcohol is added as dispersing agent, mill Ball uses WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 250r/min, Ball-milling Time 1.5h;80-120 purpose is then added Ti3AlC2Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;Mixed-powder is dried in argon atmosphere, and is filled Enter pre-molding in the graphite jig that diameter is 30mm, pressure 25MPa, dwell time 10s;Then argon atmospher in furnace is put it into Enclose interior carry out discharge plasma sintering, sintering temperature is 1150 DEG C, and heating rate is 70 DEG C/min, sintering pressure 50MPa, very Reciprocal of duty cycle 40Pa keeps the temperature 28min, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;By the blank of above-mentioned preparation Test specimen carry out surface polishing treatment obtain it is described with TiC0.8、Ti3AlC2For the Fe based high-temp-resistant self-lubricating composite wood for lubricating phase Material.
Embodiment 17
By percent by volume TiC0.8For 7vol.%, Ti3AlC2It is for 35vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is Fe powder, Cu that granularity is 10 μm, the Fe powder that granularity is 30 μm, 10 μm of Ni Powder, 10 μm of Cr powder, 5 μm of TiC0.8Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and alcohol is added As dispersing agent, abrading-ball uses WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 240r/min, Ball-milling Time 1.8h;Then it is added The Ti of 80-120 mesh3AlC2Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;By mixed-powder in argon atmosphere Drying, and it is fitted into pre-molding in the graphite jig that diameter is 30mm, pressure 30MPa, dwell time 30s;Then it puts it into Discharge plasma sintering is carried out in furnace in argon atmosphere, sintering temperature is 900 DEG C, and heating rate is 70 DEG C/min, sintering pressure For 50MPa, vacuum degree 15Pa, 25min is kept the temperature, discharge plasma sintering is carried out in argon atmosphere, obtains blank test specimen;It will be above-mentioned The blank test specimen of preparation carry out surface polishing treatment obtain it is described with TiC0.8、Ti3AlC2To lubricate the Fe based high-temp-resistant of phase certainly Lubricating composite.
Embodiment 18
By percent by volume TiC1.1For 15vol.%, Ti3AlC2It is for 25vol.%, Cu 3.8vol.%, Ni 1.2vol.%, Cr 0.6vol.%, remaining is the Cu that Fe Powder Particle Size is 20 μm, granularity is 20 μm Fe powder, Ni powder, Cr powder, 2 μm TiC1.1Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and alcohol is added as dispersing agent, abrading-ball Using WC sintered carbide ball, ratio of grinding media to material 4:1, revolving speed 320r/min, Ball-milling Time 1.4h;160-200 mesh Ti is then added3AlC2 Particle, then with same rotational speed ball milling 0.5h, mixed-powder is made;Mixed-powder is dried in argon atmosphere, and is packed into diameter For pre-molding in the graphite jig of 30mm, pressure 30MPa, dwell time 20s;Then put it into furnace in argon atmosphere into Row discharge plasma sintering, sintering temperature are 1050 DEG C, and heating rate is 100 DEG C/min, sintering pressure 49MPa, vacuum degree 30Pa keeps the temperature 30min, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;By the blank test specimen of above-mentioned preparation Carry out surface polishing treatment obtain it is described with TiC1.1、Ti3AlC2For the Fe based high-temp-resistant self-lubricating composite for lubricating phase.
The performance of Fe based high-temp-resistant composite material made from above-described embodiment 1-18 is as shown in table 1.
The performance of composite material made from 1 the various embodiments described above of table
The invention has the following advantages that
1) using Fe alloy as matrix, the compound of high-compactness and high rigidity can be obtained under the conditions of 850-1250 DEG C Material;Ti3AlC2Belong to ternary layered ceramic compound, has gathered the excellent properties of ceramics and metal, Fe base can not only be strengthened Self-lubricating composite, moreover it is possible to mutually enrich lubrication mechanism as lubrication, improve the higher dry friction coefficient of Fe alloy material and abrasion The defect of rate;
2) the Fe base high temperature self lubricating composite material prepared not only has high-mechanic, high intensity, a high temperature resistance, and Its self-lubricating property can be effectively improved under the action of multicomponent lubrication phase, the self-lubricating axis being more suitable under production bad working environments Hold equal friction materials.
The above are merely the preferred embodiment of the present invention, it is noted that for those skilled in the art, not Under the premise of being detached from present inventive concept, several modifications and improvements can also be made, these also should be considered as protection model of the invention It encloses, these all will not influence the effect and patent practicability that the present invention is implemented.

Claims (10)

1. a kind of Fe based high-temp-resistant composite material containing polynary lubrication phase, which is characterized in that the percent by volume of its chemical component Are as follows: TiCx5-20vol.%, Ti3AlC210-40vol.%, Cu 1-7vol.%, Ni 0.1-3vol.%, Cr 0.1- 3vol.%, remaining is Fe powder.
2. the Fe based high-temp-resistant composite material according to claim 1 containing polynary lubrication phase, which is characterized in that the TiCx In, 0.4≤x≤1.1.
3. the Fe based high-temp-resistant composite material according to claim 2 containing polynary lubrication phase, which is characterized in that the TiCx The granularity of powder is 2-45 μm.
4. the Fe based high-temp-resistant composite material according to claim 1 containing polynary lubrication phase, which is characterized in that described Ti3AlC2The granularity of particle is 20-200 mesh.
5. the Fe based high-temp-resistant composite material according to claim 4 containing polynary lubrication phase, which is characterized in that the Fe Powder, Cu powder granularity be 10-30 μm.
6. the Fe based high-temp-resistant composite material according to claim 5 containing polynary lubrication phase, which is characterized in that the Ni powder Granularity be 1-20 μm.
7. the Fe based high-temp-resistant composite material according to claim 6 containing polynary lubrication phase, which is characterized in that the Cr powder Granularity be 10-60 μm.
8. a kind of such as the described in any item preparation sides containing the polynary Fe based high-temp-resistant composite materials for lubricating phase claim 1-7 Method, which comprises the following steps:
Step 1): first carrying out uniform ball to Cu powder, Ni powder, Cr powder, Fe powder using planetary ball mill in argon atmosphere and mix, alcohol As dispersing agent, ratio of grinding media to material 6:1, revolving speed 200-350r/min, Ball-milling Time 0.5-2h;TiC is then addedx、Ti3AlC2Particle, Again with same rotational speed ball milling 1h;
Step 2): the mixed-powder of step 1) is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 15-30MPa, dwell time 10-30s, mould diameter 30mm;
Step 3): sintering temperature be 850-1250 DEG C, heating rate be 40-100 DEG C/min, sintering pressure 20-100MPa, very Reciprocal of duty cycle 15-40Pa keeps the temperature 5-30min, carries out discharge plasma sintering in argon atmosphere, obtain blank test specimen;
Step 4): the blank test specimen of step 3) preparation is subjected to surface polishing treatment and is obtained with Ti3AlC2And TiCxFor collaboration lubrication The Fe based high-temp-resistant composite material of phase.
9. the preparation method of the Fe based high-temp-resistant composite material according to claim 8 containing polynary lubrication phase, feature exist In in step 1), abrading-ball uses WC sintered carbide ball.
10. if the described in any item Fe based high-temp-resistant composite materials containing polynary lubrication phase of claim 1-7 are in production self-lubricating Purposes in bearing and antifriction material.
CN201910724405.2A 2018-08-17 2019-08-07 A kind of Fe based high-temp-resistant composite material and preparation method containing polynary lubrication phase Pending CN110257680A (en)

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