CN107142409B - A kind of self-lubricating hard alloy preparation method - Google Patents

A kind of self-lubricating hard alloy preparation method Download PDF

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CN107142409B
CN107142409B CN201710300221.4A CN201710300221A CN107142409B CN 107142409 B CN107142409 B CN 107142409B CN 201710300221 A CN201710300221 A CN 201710300221A CN 107142409 B CN107142409 B CN 107142409B
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hard alloy
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powder
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CN107142409A (en
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郭智兴
熊计
叶俊镠
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Sichuan University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys 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
    • C22C29/08—Alloys 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 based on tungsten carbide
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys 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
    • C22C29/067—Alloys 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
    • C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
    • C23C8/64—Carburising

Abstract

The invention discloses a kind of self-lubricating hard alloy preparation methods, it is characterized in that first keeping the temperature the hard alloy green body that 2~4h forms the removing forming agent that porosity is 25%~40% at 550~750 DEG C；Then by Al2O3Coat TiH2Core/shell structure powder, thickness be less than 3nm, the number of plies less than 3 layers and specific surface area be greater than 250m2Graphene, the NaHCO of/g3Three kinds of substances in percentage by weight 1:2:1 mixed preparings go out hydrogeneous carburizing medium；Again by green compact be embedded to it is in hydrogeneous carburizing medium and under 5 ~ 15MPa pressure consolidation；Liquid-phase sintering is finally carried out, the preparation of self-lubricating hard alloy is realized based on carbon spread.It grows up the problem of serious, carburizing time is long, low efficiency the present invention overcomes crystal grain existing for prior art, prepares self-lubricating hard alloy during the sintering process.

Description

A kind of self-lubricating hard alloy preparation method
Technical field
The present invention relates to a kind of preparation method of hard alloy, in particular to a kind of self-lubricating hard alloy preparation method, Belong to Hard Materials On Wed.
Background technique
Hard alloy is famous with its high rigidity, high-wearing feature and high intensity, with a long history as tool materials.With Progress, the raising of processing efficiency and the development of CAD/CAM of science and technology, the application field of hard alloy is also growing, It also proposed requirement higher and higher to its comprehensive performance.Solid lubricating phase is introduced wherein, is formed self-lubricating effect, can be dropped Its low abrasion when being used as cutting tool and wear part.
CN105252239A discloses a kind of preparation method of gradient hard alloy cutter, and method described therein includes following Step: (a) the whole poor carbon hard alloy substrate for being free of η phase of preparation；(b) by the poor carbon hard alloy substrate grinding of gained at Cutter；(c) gas carburizing surface treatment carried out to gained cutter, carbon rich atmosphere be methane volumetric percentage concentration be 0.8~ The methane and hydrogen gas mixture of 2.5vol%；(d) hard to get the gradient to the poor Co in surface to gained Carburization Treatment correct grinding of tooth Matter alloy cutter.CN1526847A discloses a kind of Carburization Treatment method of hard metal article, it is characterised in that this method packet Include: A. prepares carburizer: by weight percentage, by Al2O330~50wt% of fine powder, 10~30wt% of granular graphite and carbonate It is stand-by after being uniformly mixed or/and in 30~50wt% of bicarbonate investment blender.B. boat is filled: by prepared carburizing Agent measures be fitted into graphite boat as required, while by the metallographic structure produced according to a conventional method is uniform and mechanical performance is consistent hard Matter alloy sintered compact is embedded in carburizer.C. Carburization Treatment: the above-mentioned graphite boat installed is sent into heat-treatment furnace, 1390 50~120min of Carburization Treatment in~1450 DEG C of temperature ranges；Up to purpose object after cooling.
But the above method is to carry out Carburization Treatment after the completion of sintering cemented carbide again, carburizing time it is long inefficient and Cemented carbide material is easy to appear crystal grain and grows up.Therefore, simple and reliable carburizing tech is found to prepare self-lubricating hard conjunction Gold is very necessary.
Summary of the invention
When the present invention is for self-lubricating hard alloy is prepared at present, crystal grain existing for " sintering+carburizing " technique grow up it is serious, The problem of carburizing time length, low efficiency, proposes that hard alloy green compact, which is first removed forming agent, forms it into porous green compact, then will Al2O3Coat TiH2Core/shell structure powder, graphene, NaHCO3It is uniformly mixed to form when mixing planetary ball mill and is situated between containing hydrogen carbonizing Then porous green compact are put into carburizing medium and carry out consolidation by matter, that self-lubricating is formed in situ is hard when finally carrying out liquid-phase sintering Matter alloy.
Self-lubricating hard alloy preparation method of the invention, it is characterised in that successively comprise the steps of:
(1) it takes off the preparation of forming agent hard alloy green body: weighing various raw material powder ingredients by weight percentage, wherein Co is accounted for 3~20wt%, TiC account for 0~30wt%, and TaC accounts for 0~15wt%, and WC is surplus；Weighed powder is mixed and is passed through ball milling, mistake It filters, is dry, mixing forming agent, compression moulding obtains hard alloy green body；Hard alloy green body is 550~750 in vacuum sintering furnace DEG C heat preservation 2~4h, vacuum degree be 10~25Pa, is formed porosity be 25%~40% remove forming agent hard alloy green body；
(2) hydrogeneous carburizing medium is prepared: first weighing the TiH that granularity is 0.5 ~ 1.5 μm2Powder is added to shape in dehydrated alcohol At TiH2The mixed liquor of 35wt% is accounted for, the ultrasonic disperse processing of 20 ~ 40min is then carried out, and is 10 in 80 ~ 100 DEG C and vacuum degree 1h is dried in vacuo under the conditions of~20Pa；Solution is prepared using deionized water and dehydrated alcohol mixed liquor as solvent again, is 0.1 by concentration Al (NO is added in~0.8mol/L3)3, by Al (NO3)3The TiH for passing through ultrasonic disperse is added in 8 times of concentration2Powder is used in combination CH3COOH adjusts pH value to 3~6, the then stirring 8 at 60~80 DEG C~for 24 hours in magnetic stirring apparatus, and 120 ~ 150
Dry 1~3h, obtains Al at DEG C2O3Coat TiH2Core/shell structure powder；Again by Al2O3Coat TiH2Core shell Structure powder, thickness is less than 3nm, the number of plies less than 3 layers and specific surface area is greater than 250m2The graphene of/g, NaHCO3Three kinds of substances are pressed Weight percent 1:2:1 mixing, and 1 ~ 2h of ball milling in planetary ball mill, are made hydrogeneous carburizing medium；
(3) hydrogeneous carburizing medium: being first fitted into graphite crucible by filling of the green compact in hydrogeneous carburizing medium, then will removing The hard alloy green body of forming agent is embedded to；The weight ratio of hydrogeneous carburizing medium and de- forming agent hard alloy green body is 5:1, and really The hydrogeneous carburizing medium thickness protected around de- forming agent hard alloy green body is greater than 5mm；Then consolidation contains under 5 ~ 15MPa pressure Hydrogen carbonizing medium makes its volume-diminished to the 40 ~ 60% of loose state；With threaded lid sealed graphite crucible, carburizing is prevented Medium evolution；
(4) prepared by self-lubricating hard alloy: 1350~1500 DEG C of 1~3h of heat preservation in vacuum sintering furnace, carbon is by containing Hydrogen carbonizing medium is spread to carbide surface, forms the self-lubricating layer of 450 ~ 750 μ m-thicks, final to realize self-lubricating hard alloy Preparation.
Self-lubricating hard alloy preparation method of the invention, further characterized in that:
(1) Ball-milling Time is 24~72h when prepared by hard alloy green body, and filtering uses 400 mesh screens, it is dry 85~ 100 DEG C of progress mix buna forming agent by the 50~120% of cemented carbide powder weight, under 300~400MPa pressure Compression moulding；When hard alloy green body removes forming agent, heating rate is 1~5 DEG C/min；
(2) when hydrogeneous carburizing medium is prepared, the frequency of ultrasonic wave is 4 × 10 when ultrasonic treatment4Hz, power 100W, matches Deionized water and the volume ratio of dehydrated alcohol are 1:10 in the solvent that solution processed uses, and prepare Al2O3Coat TiH2Core shell knot When structure powder, the speed of magnetic agitation is 20~50r/min, core/shell structure powder, graphene, NaHCO3Mix planetary ball mill When, revolving speed 300r/min;
(3) the graphite material flexural strength of graphite crucible used is greater than 20MPa when green compact load in carburizing medium；
(4) when prepared by self-lubricating hard alloy, 550~750 DEG C first is warming up to 5~10 DEG C/min and keeps the temperature 1~2h；So 1100~1250 DEG C are warming up to 5~10 DEG C/min afterwards and keep the temperature 1~3h；1350~1500 are warming up to again with 5~10 DEG C/min DEG C and keep the temperature 1~3h, sintering vacuum degree be 1~5Pa；Cooling rate after sintering is 1~8 DEG C/min.
The present invention has the advantages that (1), using porous green compact as carburizing body, in-situ accomplishes surface is seeped during the sintering process Carbon, this technique compared with traditional first sintering recarburization is more succinct, and there is no crystal grain secondary the problem of growing up；(2) carburizing Metal hydride TiH is introduced in agent2, H is decomposited during the sintering process2And C+2H occurs with graphene2=CH4, CH4=[C]+H2, The active atoms of carbon of formation, which enters, realizes carburizing in metal；Al2O3It is coated on TiH2Surface can control H2Rate of release avoids fast Speed exhausts；(3) the porous green compact formed after green compact removing forming agent have huge surface area, are conducive to the suction of active atoms of carbon Echo the raising of carburizing efficiency；(4) propose the degree of packing by controlling carburizing medium ensure carburizing medium and hard alloy it Between contact, improve carburizing efficiency；(5) use graphene for carbon source, the small reactivity of granularity is bigger, and carburizing is high-efficient.
Detailed description of the invention
The process schematic representation of self-lubricating hard alloy preparation method Fig. 1 of the invention.
Specific embodiment
Example 1: self-lubricating hard alloy is prepared according to the following steps:
(1) it takes off the preparation of forming agent hard alloy green body: weighing various raw material powder ingredients by weight percentage, wherein Co is accounted for 6wt%, TaC account for 2wt%, and WC is surplus；Weighed powder mixes to and passed through 32h ball milling, 400 mesh net filtrations, 89 DEG C of dryings, Buna forming agent is mixed by the 62% of cemented carbide powder weight, compression moulding obtains hard alloy under 340MPa pressure Green compact；Hard alloy green body 650 DEG C of heat preservation 2h in vacuum sintering furnace, heating rate are 2 DEG C/min, vacuum degree 14Pa, shape At the hard alloy green body for the removing forming agent that porosity is 27%；
(2) hydrogeneous carburizing medium is prepared: first weighing the TiH that granularity is 0.5 μm2Powder is added in dehydrated alcohol and is formed TiH2The mixed liquor of 35wt% is accounted for, the ultrasonic disperse processing of 22min is then carried out, the frequency of ultrasonic wave is 4 × 104Hz, power are 100W；And 1h is dried in vacuo under the conditions of 85 DEG C and vacuum degree are 12Pa；Again with volume ratio for the deionized water of 1:10 and anhydrous Alcohol mixeding liquid is that solvent prepares solution, is that Al (NO is added in 0.8mol/L by concentration3)3, it is added by 6.4mol/L by ultrasound point Scattered TiH2Powder, and use CH3COOH adjusts pH value to 3, then stirs 8h, magnetic agitation at 70 DEG C in magnetic stirring apparatus Speed be 30r/min, and the dry 1h at 128 DEG C obtains Al2O3Coat TiH2Core/shell structure powder；Again by Al2O3Packet Cover TiH2Core/shell structure powder, thickness be less than 3nm, the number of plies less than 3 layers and specific surface area be greater than 250m2The graphene of/g, NaHCO3Three kinds of substances in percentage by weight 1:2:1 mixing, and the ball milling 1h in planetary ball mill, rotational speed of ball-mill 300r/ Hydrogeneous carburizing medium is made in min；
(3) filling of the green compact in hydrogeneous carburizing medium: first hydrogeneous carburizing medium is fitted into graphite crucible, graphite crucible Graphite material flexural strength be greater than 20MPa, then will remove forming agent hard alloy green body embedment；Hydrogeneous carburizing medium and de- The weight ratio of forming agent hard alloy green body is 5:1, and ensures the hydrogeneous carburizing medium around de- forming agent hard alloy green body Thickness is greater than 5mm；Then the hydrogeneous carburizing medium of consolidation under 13MPa pressure, makes its volume-diminished to the 45% of loose state；With Threaded lid sealed graphite crucible, prevents carburizing medium from escaping；
(4) prepared by self-lubricating hard alloy: being first warming up to 650 DEG C with 7 DEG C/min and keeps the temperature 1h；Then with 9 DEG C/min liter Temperature is to 1190 DEG C and keeps the temperature 1h；1440 DEG C are warming up to 8 DEG C/min again and keeps the temperature 2h, and sintering vacuum degree is 3Pa；After sintering Cooling rate be 6 DEG C/min, carbon from hydrogeneous carburizing medium to carbide surface spread, formed 600 μ m-thicks from moisten Slip layer, it is final to realize the preparation of self-lubricating hard alloy.
Example 2: self-lubricating hard alloy is prepared according to the following steps:
(1) it takes off the preparation of forming agent hard alloy green body: weighing various raw material powder ingredients by weight percentage, wherein Co is accounted for 15wt%, TiC account for 15wt%, and WC is surplus；Weighed powder is mixed to and is passed through 42h ball milling, 400 mesh net filtrations, 97 DEG C dry It is dry, buna forming agent is mixed by the 70% of cemented carbide powder weight, compression moulding obtains hard conjunction under 360MPa pressure Golden green compact；Hard alloy green body 580 DEG C of heat preservation 2h in vacuum sintering furnace, heating rate be 3 DEG C/min, vacuum degree 17Pa, Form the hard alloy green body for the removing forming agent that porosity is 32%；
(2) hydrogeneous carburizing medium is prepared: first weighing the TiH that granularity is 0.9 μm2Powder is added in dehydrated alcohol and is formed TiH2The mixed liquor of 35wt% is accounted for, the ultrasonic disperse processing of 32min is then carried out, the frequency of ultrasonic wave is 4 × 104Hz, power are 100W；And 1h is dried in vacuo under the conditions of 88 DEG C and vacuum degree are 10Pa；Again with volume ratio for the deionized water of 1:10 and anhydrous Alcohol mixeding liquid is that solvent prepares solution, is that Al (NO is added in 0.2mol/L by concentration3)3, it is added by 1.6mol/L by ultrasound point Scattered TiH2Powder, and use CH3COOH adjusts pH value to 5, then stirs 20h, magnetic agitation at 70 DEG C in magnetic stirring apparatus Speed be 27r/min, and the dry 2h at 120 ~ 150 DEG C obtains Al2O3Coat TiH2Core/shell structure powder；Again will Al2O3Coat TiH2Core/shell structure powder, thickness be less than 3nm, the number of plies less than 3 layers and specific surface area be greater than 250m2The stone of/g Black alkene, NaHCO3Three kinds of substances in percentage by weight 1:2:1 mixing, and the ball milling 2h in planetary ball mill, rotational speed of ball-mill are Hydrogeneous carburizing medium is made in 300r/min；
(3) filling of the green compact in hydrogeneous carburizing medium: first hydrogeneous carburizing medium is fitted into graphite crucible, graphite crucible Graphite material flexural strength be greater than 20MPa, then will remove forming agent hard alloy green body embedment；Hydrogeneous carburizing medium and de- The weight ratio of forming agent hard alloy green body is 5:1, and ensures the hydrogeneous carburizing medium around de- forming agent hard alloy green body Thickness is greater than 5mm；Then the hydrogeneous carburizing medium of consolidation under 11MPa pressure, makes its volume-diminished to the 50% of loose state；With Threaded lid sealed graphite crucible, prevents carburizing medium from escaping；
(4) prepared by self-lubricating hard alloy: being first warming up to 620 DEG C with 8 DEG C/min and keeps the temperature 1h；Then with 7 DEG C/min liter Temperature is to 1220 DEG C and keeps the temperature 2h；1410 DEG C are warming up to 9 DEG C/min again and keeps the temperature 2h, and sintering vacuum degree is 3Pa；After sintering Cooling rate be 4 DEG C/min, carbon from hydrogeneous carburizing medium to carbide surface spread, formed 500 μ m-thicks from moisten Slip layer, it is final to realize the preparation of self-lubricating hard alloy.

Claims (2)

1. a kind of self-lubricating hard alloy preparation method, it is characterised in that successively comprise the steps of:
(1) take off the preparation of forming agent hard alloy green body: weighing various raw material powder ingredients by weight percentage, wherein Co account for 3~ 20wt%, TiC account for 0~30wt%, and TaC accounts for 0~15wt%, and WC is surplus；Weighed powder is mixed and passed through ball milling, filtering, is done It is dry, mix forming agent, compression moulding obtains hard alloy green body；Hard alloy green body 550~750 DEG C of heat preservations in vacuum sintering furnace 2~4h, vacuum degree are 10~25Pa, form the hard alloy green body for the removing forming agent that porosity is 25%~40%；
(2) hydrogeneous carburizing medium is prepared: first weighing the TiH that granularity is 0.5 ~ 1.5 μm2Powder is added in dehydrated alcohol and is formed TiH2Account for the mixed liquor of 35wt%, then carry out the ultrasonic disperse processing of 20 ~ 40min, and 80 ~ 100 DEG C and vacuum degree be 10~ 1h is dried in vacuo under the conditions of 20Pa；Prepare solution by solvent of deionized water and dehydrated alcohol mixed liquor again, by concentration for 0.1~ Al (NO is added in 0.8mol/L3)3, by Al (NO3)3The TiH for passing through ultrasonic disperse is added in 8 times of concentration2Powder, and use CH3COOH PH value is adjusted to 3~6, the then stirring 8 at 60~80 DEG C~for 24 hours in magnetic stirring apparatus, and 120 ~ 150
Dry 1~3h, obtains Al at DEG C2O3Coat TiH2Core/shell structure powder；Again by Al2O3Coat TiH2Core/shell structure Powder, thickness is less than 3nm, the number of plies less than 3 layers and specific surface area is greater than 250m2The graphene of/g, NaHCO3Three kinds of substances are by weight Percentage 1:2:1 mixing, and 1 ~ 2h of ball milling in planetary ball mill, are made hydrogeneous carburizing medium；
(3) hydrogeneous carburizing medium: being first fitted into graphite crucible by filling of the green compact in hydrogeneous carburizing medium, then removing is formed The hard alloy green body of agent is embedded to；The weight ratio of hydrogeneous carburizing medium and de- forming agent hard alloy green body is 5:1, and ensures to take off Hydrogeneous carburizing medium thickness around forming agent hard alloy green body is greater than 5mm；Then the hydrogeneous infiltration of consolidation under 5 ~ 15MPa pressure Carbon medium makes its volume-diminished to the 40 ~ 60% of loose state；With threaded lid sealed graphite crucible, carburizing medium is prevented Evolution；
(4) prepared by self-lubricating hard alloy: 1350~1500 DEG C of 1~3h of heat preservation in vacuum sintering furnace, carbon is by hydrogeneous infiltration Carbon medium is spread to carbide surface, forms the self-lubricating layer of 450 ~ 750 μ m-thicks, final to realize self-lubricating hard alloy system It is standby.
2. self-lubricating hard alloy preparation method according to claim 1, further characterized in that:
(1) Ball-milling Time is 24~72h when prepared by hard alloy green body, and filtering uses 400 mesh screens, dry at 85~100 DEG C It carries out, mixes buna forming agent by the 50~120% of cemented carbide powder weight, be pressed under 300~400MPa pressure Type；When hard alloy green body removes forming agent, heating rate is 1~5 DEG C/min；
(2) when hydrogeneous carburizing medium is prepared, the frequency of ultrasonic wave is 4 × 10 when ultrasonic treatment4Hz, power 100W prepare solution Deionized water and the volume ratio of dehydrated alcohol are 1:10 in the solvent used, prepare Al2O3Coat TiH2Core/shell structure powder When, the speed of magnetic agitation is 20~50r/min, core/shell structure powder, graphene, NaHCO3When mixing planetary ball mill, revolving speed For 300r/min;
(3) the graphite material flexural strength of graphite crucible used is greater than 20MPa when green compact load in carburizing medium；
(4) when prepared by self-lubricating hard alloy, 550~750 DEG C first is warming up to 5~10 DEG C/min and keeps the temperature 1~2h；Then with 5~10 DEG C/min is warming up to 1100~1250 DEG C and keeps the temperature 1~3h；1350~1500 DEG C are warming up to simultaneously again with 5~10 DEG C/min 1~3h is kept the temperature, sintering vacuum degree is 1~5Pa；Cooling rate after sintering is 1~8 DEG C/min.
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