CN109694969A - A kind of pre-alloyed powder and the TiCN based ceramic metal composite material and preparation method for adding pre-alloyed powder - Google Patents
A kind of pre-alloyed powder and the TiCN based ceramic metal composite material and preparation method for adding pre-alloyed powder Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 62
- 239000002905 metal composite material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000009689 gas atomisation Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 49
- 239000012071 phase Substances 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 18
- 229910004337 Ti-Ni Inorganic materials 0.000 claims description 17
- 229910011209 Ti—Ni Inorganic materials 0.000 claims description 17
- 229910003178 Mo2C Inorganic materials 0.000 claims description 16
- 229910003470 tongbaite Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
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- 238000000227 grinding Methods 0.000 claims description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000011195 cermet Substances 0.000 abstract description 7
- 150000002739 metals Chemical class 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 38
- 229910052786 argon Inorganic materials 0.000 description 19
- 229910052757 nitrogen Inorganic materials 0.000 description 17
- 238000000889 atomisation Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 229910052761 rare earth metal Inorganic materials 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 238000012545 processing Methods 0.000 description 9
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- 238000005275 alloying Methods 0.000 description 8
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- 238000001816 cooling Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
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- 230000009471 action Effects 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
- C22C29/04—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 carbonitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses the TiCN based ceramic metal composite material and preparation methods of a kind of pre-alloyed powder and addition pre-alloyed powder.The pre-alloyed powder, consists of the following components in percentage by weight: it be 17 ~ 30%, Ni is 50 ~ 78% that Ru, which is 5 ~ 20%, Ti,；The average grain diameter of the pre-alloyed powder is 2.1 ~ 4.5 μm.Pre-alloyed powder of the invention is using Ru, Ti, Ni elemental metals as raw material, prealloy melt is first prepared using arc melting method, then prealloy melt is obtained using high pressure gas atomization method, the ratio of scientific and reasonable design Ru, Ti, Ni, the technological parameter of strict control melting and high pressure gas atomization process, the pre-alloyed powder being had excellent performance；Crystal grain can be refined by being applied in cermet, strengthened Binder Phase, improved and improve the mechanical property of cermet.
Description
Technical field
The invention belongs to powder metallurgical technologies, more particularly, to a kind of pre-alloyed powder and addition prealloy powder
The TiCN based ceramic metal composite material and preparation method at end.
Background technique
Ti (C, N) based ceramic metal due to hardness is high, density is low, chemical stability, can polishability be good, inoxidizability
The features such as good and creep-resistant property is excellent, thus by common concern both domestic and external.But traditional Ti (C, N) based ceramic metal is still
Old the disadvantages of there are intensity and insufficient toughness, seriously limit its service life and use scope.Therefore, Ti (C, N) how is improved
The obdurability of based ceramic metal just becomes investigation of materials scholar problem of interest.
A small amount of rare earth element is added in Ti (C, N) based ceramic metal can refine hard phase organization, improve metal phase to pottery
The wetability of porcelain phase improves interface impurity distribution situation, purification crystal boundary, strengthens Binder Phase, to effectively improve cermet
Mechanical property.But it since most of rare earth element activity is high, is extremely oxidized easily, and the additive amount of rare earth element belongs to micro-
Amount necessarily causes uniform distribution of the rare earth element in Ti (C, N) based ceramic metal to be difficult to control, leads to rare earth Ti (C, N)
The stability of base metal-ceramic material is poor, to greatly affected the further development of this technology.
Pre-alloyed powder is several elemental metals to be reached molten condition by smelting process, then use hydraulic atomized or gas
Body atomization technique produces.Its major advantage is: the uniform multicomponent alloy of a variety of alloying element forming properties, can be more effective
Ground utilizes alloying element；Alloying elements distribution and uniform microstructure in powder particle composition, with high intensity and good resistance to
Mill property.The material produced with pre-alloyed powder is than the material microstructure with diffusible alloy powder or the production of segregation-free mixed powder
More evenly, there is higher hardness and dimensional stability.Currently, there is not yet prepared by the pre-alloyed powder using the u containing rare-earth element R
The report of TiCN based ceramic metal composite material.
Summary of the invention
For deficiency existing for TiCN based ceramic metal composite material in the prior art, the purpose of the present invention is to provide one
Kind pre-alloyed powder.Contain rare-earth element R u in the pre-alloyed powder, the inclined of the alloying elements such as W, Ta, Mo, Cr can be reduced
Analysis, refining eutectic carbide improve Interface adhesive strength, improve metallic binding phase to the wetability of hard phase and improve sintering
Performance.
Another technical problem to be solved by the present invention is that providing the preparation method of the pre-alloyed powder.
It is multiple in preparation TiCN based ceramic metal that a present invention also technical problems to be solved are to provide the pre-alloyed powder
Application in condensation material.
The purpose of the present invention is achieved through the following technical solutions:
A kind of pre-alloyed powder, consists of the following components in percentage by weight: Ru is that 5~20%, Ti is 17~30%, Ni
It is 50~78%；The average grain diameter of the pre-alloyed powder is 2.1~4.5 μm.
It is further preferred that the pre-alloyed powder consists of the following components in percentage by weight: Ru is 12~17%, Ti
It is 52~68% for 18~24%, Ni.
The pre-alloyed powder is prepared as a raw material with Ru, Ti, Ni elemental metals, and rare-earth element R u itself can be reduced
W, the segregation of the alloying elements such as Ta, Mo, Cr, refining eutectic carbide, raising Interface adhesive strength, improvement metallic binding phase are to hard
The wetability and raising sintering character of matter phase.The present invention passes through long term test, according to reasonable dosage by the prealloy powder
Raw material of the end as ceramic-metal composite, and it is applied to TiCN based ceramic metal composite material, it will be effectively improved
The performance of TiCN based ceramic metal composite material.
The pre-alloyed powder can be prepared using the existing achievable technological means in this field.
Present invention simultaneously provides the preferred preparation method of the pre-alloyed powder, be by Ru, Ti, Ni be raw material, using electricity
Prealloy melt is prepared in arc smelting process, and the prealloy melt is made of high pressure gas atomization.
Further, specific step is as follows for the preparation method of the pre-alloyed powder: the mixture of Ru, Ti, Ni are placed in
In the cold-crucible of arc-melting furnace, melting is carried out under the protection of argon gas using non-consumable arc melting method, is vacuumized first
To 10-2Pa, then applying argon gas to air pressure is 0.04~0.06MPa, and melting current density is 185~200A/cm2, heating temperature
After 1800~2000 DEG C melt, it is kept molten by 10~60min, obtains prealloy melt, followed by aeroponics gas
Prealloy melt is smashed into fine drop, effect of the fine drop in surface tension by atomization system, high pressure inert argon gas
Under, settling cooling forming in atomisation tower is ball shape particulate powders material, separates and collects through filter, prepares high-purity
Spherical fine particles dusty material；During atomization, high energy dielectric gas air pressure: 28~45bar, air-flow: 25~30m3/
Min, gas temperature: 0 DEG C~30 DEG C, atomization rates: 0.5~1.2kg/min.
Present invention simultaneously provides the applications of the pre-alloyed powder, are applied to preparation TiCN based ceramic metal composite wood
Material.
Preferably, the TiCN based ceramic metal composite material includes hard phase, Binder Phase and pre-alloyed powder, described hard
Matter is mutually by TiCN, TaC, TiC, NbC, WC, Mo2C and Cr3C2Composition, the Binder Phase are Co powder, and the composite material is by following
The raw material of weight percent is made:
TiCN:42~64%,
TaC:0.5~9%,
TiC:1~12%,
NbC:1~8%,
WC:12~22%,
Mo2C:1.5~10%,
Cr3C2: 0.2~0.9%,
Co:6~12%,
Ru-Ti-Ni:4~12%；
The average grain diameter of the Co powder is 0.5~1.5 μm, and the average grain diameter of other powders is less than 4 μm.
It is further preferred that the TiCN based ceramic metal composite material is made of the raw material of following weight percent:
TiCN:42~53%,
TaC:0.5~3%,
TiC:1~4%,
NbC:1~6%,
WC:12~18.5%,
Mo2C:8~10%,
Cr3C2: 0.2~0.5%,
Co:6~8%,
Ru-Ti-Ni:7~8%.
The present invention provides a kind of preparation method of preferred TiCN based ceramic metal composite material, comprising the following steps:
S1. pre-alloyed powder, hard phase and bonding phase component are subjected to ingredient by above-mentioned weight percent, molding is added
After agent, ball milling mixing is uniform, and spray-drying process, obtains mixture particle；
S2. the mixture particle that the S1 is obtained is pressed and molded, obtains TiCN based ceramic metal green compact；
S3. the TiCN based ceramic metal green compact S2 obtained carries out atmosphere sintering in more atmosphere sintering furnaces, cooling
To room temperature to get TiCN based ceramic metal composite material.
The present invention in traditional Ti (C, N) based ceramic metal by being added rare earth existing for pre-alloyed powder processing form
Element Ru, and it is successively simple by processing steps, technical process such as ball milling, granulation, compression molding and sintering；Due to prealloy powder
Elemental redistribution is uniform, is introduced into cermet, can be avoided component segregation, and powder even tissue, performance is made to reach unanimity.
Further, since prealloy powder each element ingredient is fixed, moreover it is possible to avoid the generation of various problems in blending process, be product quality
Offer condition is provided.
Preferably, in step S1, the forming agent is paraffin or PEG.
It is further preferred that the paraffin additive amount is the 2.8~4.5% of raw material total amount, the PEG additive amount is raw material
The 3.2~4.5% of total amount.
It is further preferred that the technological parameter of the ball milling are as follows: use diameter for the WC-8%Co hard alloy of 7~10mm
Ball carries out ball milling, uses dehydrated alcohol for ball-milling medium, and ratio of grinding media to material is 7~10:1, and revolving speed is 45~70rpm, and Ball-milling Time is
56~72h.
Preferably, in step S3, the atmosphere sintering is five stage atmosphere sinterings, successively includes negative pressure dewaxing stage, true
Empty solid-phase sintering stage, for the first time partial pressure sintering stage, vacuum liquid-phase sintering stage and second of partial pressure sintering stage.
It is further preferred that the technological parameter of the negative pressure dewaxing stage are as follows: temperature range is 20~550 DEG C, protects gas
Atmosphere is nitrogen, and partial pressure pressure is 2~4mbar；
The technological parameter in the vacuum solid-phase sintering stage are as follows: temperature range is 550~1255 DEG C, and vacuum degree is lower than
10Pa；
The technological parameter of the first time partial pressure sintering stage are as follows: temperature range is 1255~1450 DEG C, keeps the temperature 1h, protection
Atmosphere is nitrogen and argon gas, and partial pressure pressure is 12~180mbar, and heating rate is 4~7.5 DEG C/min；
The technological parameter in the vacuum liquid-phase sintering stage: temperature range is 1450~1520 DEG C, and vacuum degree is lower than 10pa；
The technological parameter of second of partial pressure sintering stage are as follows: temperature is 1520 DEG C, and constant temperature keeps the temperature 1h, protective atmosphere argon
Gas, partial pressure pressure are 8~250mbar.
The present invention use multistage sintering atmosphere sintering method, wherein vacuum solid-phase sintering stage diffusion rate increase,
Grain Plastic Flow is reinforced, and green compact is obviously shunk, and releases the gas in green body gap, and fixed oxygen is also reduced in this stage, this
These exhaust gas can be guided and be excluded by stage nitrogen and partial pressure of ar gas sintering, and be converted to argon for the nitrogen of partial pressure sintering next time
Gas is excessive.In addition, the partial pressure sintering of solid-phase sintering is able to suppress the volatilization of cobalt phase, reduces cobalt and be lost, mentioned in the liquid-phase sintering stage
Wetability of the high Binder Phase to hard phase.
Compared with prior art, the beneficial effects of the present invention are:
The present invention mixes in specific proportions using Ru, Ti, Ni as raw material, and prealloy first is prepared using arc melting method
Then prealloy melt is obtained pre-alloyed powder, strict control melting and high pressure gas using high pressure gas atomization method by melt
The technological parameter of body atomization process, the pre-alloyed powder being had excellent performance；Conjunction can be refined by being applied in cermet
Jin Jing's grain, strengthens Binder Phase, improves and improve the mechanical property of cermet.
Compared with traditional mechanical mixture powder, pre-alloyed powder Elemental redistribution of the invention is uniform, effectively avoids composition
Segregation, makes carcass even tissue, performance reach unanimity；Prealloy powder alloying of the invention is abundant, and carcass is made to have high rigidity
And high impact, it is greatly improved resistance to compression, the bending strength of sintered article, improves metal ceramic material as high temperature stability, increases gold
Belong to the toughness of ceramics, further extends the service life of cermet.
Rare-earth element R u is added the present invention in the form of pre-alloyed powder processing technique, using the characteristic of Ru itself, is subtracted
The segregation of the alloying elements such as few W, Ta, Mo, Cr, refining eutectic carbide improve Interface adhesive strength, improve metallic binding phase pair
The wetability and raising sintering character of hard phase；In addition, metallic atom in sintering process can also be reduced using preparatory alloying
Diffusion needed for activation energy, improve metal ceramic material as high temperature stability, be convenient for control of product quality.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with embodiment, but this hair
Bright protection scope is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, it is no intended to limit of the invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
The present embodiment provides a kind of pre-alloyed powder, pre-alloyed powder consists of the following components in percentage by weight: Ru and is
17%, Ti 18%, Ni 65%；The average grain diameter of pre-alloyed powder is 3 μm；
Specific step is as follows for the preparation method of above-mentioned pre-alloyed powder: the mixture of Ru, Ti, Ni are placed in arc-melting furnace
Cold-crucible in, melting is carried out under the protection of argon gas using non-consumable arc melting method, is evacuated to 10 first-2Pa, so
Applying argon gas to air pressure is 0.04MPa afterwards, and melting current density is 185A/cm2, after 1900 DEG C of heating temperature melt, keep melting
State 30min obtains Ru-Ti-Ni prealloy melt；Followed by aeroponics gas atomization system, high pressure inert argon gas gas
Body Ru-Ti-Ni prealloy melt smashes into fine droplets, and fine droplets settle in atomisation tower under the action of surface tension
Cooling forming is ball shape ultra-fine powder materials, separates and collects through filter, prepares the ball shaped nano eutectic powder of high-purity
Material；During atomization, high energy dielectric gas air pressure is 35bar, air-flow 28m3/ min, gas temperature are 18 DEG C, atomization
Rate is 0.6kg/min.
Embodiment 2
The present embodiment provides a kind of pre-alloyed powders, difference from example 1 is that, the prealloy powder of the present embodiment
End consists of the following components in percentage by weight: Ru 12%, Ti 24%, Ni 64%；The average grain diameter of pre-alloyed powder
It is 2.1 μm；
The preparation method of above-mentioned pre-alloyed powder, referring to the processing step of embodiment 1, the main distinction is, smelting process
Technological parameter are as follows: applying argon gas to air pressure is 0.05MPa, and melting current density is 200A/cm2, heating temperature is 1800 DEG C, is kept
Molten condition 10min；The technological parameter of high pressure gas atomization are as follows: high energy dielectric gas air pressure is 28bar, air-flow 25m3/
Min, gas temperature are 30 DEG C, atomization rates 1.2kg/min.
Embodiment 3
The present embodiment provides a kind of pre-alloyed powders, difference from example 1 is that, pre-alloyed powder is by following heavy
The group of amount percentage is grouped as: Ru 5%, Ti 17%, Ni 78%；The average grain diameter of pre-alloyed powder is 3.5 μm；
The preparation method of above-mentioned pre-alloyed powder, referring to the processing step of embodiment 1, the main distinction is, smelting process
Technological parameter are as follows: applying argon gas to air pressure is 0.05MPa, and melting current density is 195A/cm2, heating temperature is 2000 DEG C, is kept
Molten condition 60min；The technological parameter of high pressure gas atomization are as follows: high energy dielectric gas air pressure is 45bar, air-flow 30m3/
Min, gas temperature are 0 DEG C, atomization rates 0.5kg/min.
Embodiment 4
The present embodiment provides a kind of pre-alloyed powders, difference from example 1 is that, pre-alloyed powder is by following heavy
The group of amount percentage is grouped as: Ru 20%, Ti 30%, Ni 50%；The average grain diameter of pre-alloyed powder is 4.5 μm；On
The preparation method of pre-alloyed powder is stated, referring to the processing step of embodiment 1.
Embodiment 5
The present embodiment provides a kind of TiCN based ceramic metal composite material for adding pre-alloyed powder, TiCN based ceramic metals
Composite material includes hard phase, Binder Phase and pre-alloyed powder, wherein hard phase is by TiCN, TaC, TiC, NbC, WC, Mo2C and
Cr3C2Composition, Binder Phase are the Co powder that average grain diameter is 1.2 μm, and TiCN based ceramic metal composite material is by following weight percent
Raw material be made: TiCN 53%, TaC 2%, TiC 2%, NbC 2%, WC 16.5%, Mo2C is 8%, Cr3C2For
0.5%, Co 9%, Ru-Ti-Ni 7%；
The preparation method of above-mentioned TiCN based ceramic metal composite material, comprising the following steps:
S1. pre-alloyed powder, other hard phase components and the bonding phase component by weight hundred embodiment 1 being prepared
Dividing than carrying out ingredient, addition PEG, PEG additive amount is the 3.6% of raw material total amount, then using dehydrated alcohol as ball-milling medium, use
The WC-8%Co sintered carbide ball progress ball milling that diameter is 10mm, ratio of grinding media to material 9:1, revolving speed 60rpm, Ball-milling Time 60h,
Ball milling mixing is uniform, and spray-drying process, obtains mixture particle；
S2. the mixture particle that S1 is obtained is pressed and molded, pressing pressure 350MPa, obtains TiCN Base Metal pottery
Porcelain green compact；
S3. the TiCN based ceramic metal green compact that the S2 is obtained five stage atmosphere are carried out to burn in more atmosphere sintering furnaces
Knot, is cooled to room temperature to get TiCN based ceramic metal composite material；
Above-mentioned five stages atmosphere sintering successively includes negative pressure dewaxing stage, the vacuum solid-phase sintering stage, partial pressure is burnt for the first time
Knot stage, vacuum liquid-phase sintering stage and second of partial pressure sintering stage；Wherein, the technological parameter of negative pressure dewaxing stage are as follows: temperature
Spending section is 20~550 DEG C, and protective atmosphere is nitrogen, and partial pressure pressure is 2mbar；The technological parameter in vacuum solid-phase sintering stage
Are as follows: temperature range is 550~1255 DEG C, vacuum degree 8Pa；The technological parameter of sintering stage is divided for the first time are as follows: temperature range
Be 1255~1450 DEG C, keep the temperature 1h, protective atmosphere be nitrogen and argon gas, partial pressure pressure be 12mbar, heating rate for 4 DEG C/
min；The technological parameter in vacuum liquid-phase sintering stage: temperature range is 1450~1520 DEG C, vacuum degree 8pa；Second of partial pressure
The technological parameter of sintering stage are as follows: temperature is 1520 DEG C, and constant temperature keeps the temperature 1h, protective atmosphere argon gas, and partial pressure pressure is 8mbar.
Embodiment 6
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
52%, TaC 2%, TiC 2%, NbC 2%, WC 17.5%, Mo2C is 8%, Cr3C2For 0.5%, Co 8%, Ru-
Ti-Ni is 8%.
The preparation method of above-mentioned TiCN based ceramic metal composite material, referring to the processing step of embodiment 5, the main distinction exists
In: in step S1, pre-alloyed powder is that embodiment 2 is prepared, and forming agent is paraffin, and paraffin additive amount is raw material total amount
2.8%, ratio of grinding media to material is 10:1, revolving speed 45rpm, Ball-milling Time 72h in mechanical milling process.
Embodiment 7
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
42%, TaC 0.5%, TiC 12%, NbC 8%, WC 17.3%, Mo2C is 4%, Cr3C2For 0.2%, Co 12%,
Ru-Ti-Ni is 4%.
The preparation method of above-mentioned TiCN based ceramic metal composite material, referring to the processing step of embodiment 5, the main distinction exists
In: in step S1, pre-alloyed powder is that embodiment 3 is prepared, and forming agent selects PEG, and PEG additive amount is raw material total amount
4.4%, during ball-milling treatment, ratio of grinding media to material 7:1, revolving speed 70rpm, Ball-milling Time 56h.
Embodiment 8
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
63.8%, TaC 7%, TiC 1%, NbC 2%, WC 12%, Mo2C is 2%, Cr3C2For 0.2%, Co 6%, Ru-
Ti-Ni is 6%.
The preparation method of above-mentioned TiCN based ceramic metal composite material, referring to the processing step of embodiment 5, the main distinction exists
In: the technological parameter of negative pressure dewaxing stage are as follows: temperature range is 20~550 DEG C, and protective atmosphere is nitrogen, and partial pressure pressure is
4mbar；The technological parameter in vacuum solid-phase sintering stage are as follows: temperature range is 550~1255 DEG C, vacuum degree 9Pa；Divide for the first time
Press the technological parameter of sintering stage are as follows: temperature range is 1255~1450 DEG C, keeps the temperature 1h, and protective atmosphere is nitrogen and argon gas, is divided
Pressure pressure is 120mbar, and heating rate is 7.5 DEG C/min；The technological parameter in vacuum liquid-phase sintering stage: temperature range 1450
~1520 DEG C, vacuum degree 7pa；The technological parameter of second of partial pressure sintering stage are as follows: temperature is 1520 DEG C, and constant temperature keeps the temperature 1h,
Protective atmosphere argon gas, partial pressure pressure are 240mbar.
Embodiment 9
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
49%, TaC 3%, TiC 4%, NbC 2%, WC 16.5%, Mo2C is 9%, Cr3C2For 0.5%, Co 7%, Ru-
Ti-Ni is 9%.
The preparation method of above-mentioned TiCN based ceramic metal composite material, referring to the processing step of embodiment 5, the main distinction exists
In: the technological parameter of negative pressure dewaxing stage are as follows: temperature range is 20~550 DEG C, and protective atmosphere is nitrogen, and partial pressure pressure is
3mbar；The technological parameter in vacuum solid-phase sintering stage are as follows: temperature range is 550~1255 DEG C, vacuum degree 4Pa；Divide for the first time
Press the technological parameter of sintering stage are as follows: temperature range is 1255~1450 DEG C, keeps the temperature 1h, and protective atmosphere is nitrogen and argon gas, is divided
Pressure pressure is 50mbar, and heating rate is 6 DEG C/min；The technological parameter in vacuum liquid-phase sintering stage: temperature range be 1450~
1520 DEG C, vacuum degree 6pa；The technological parameter of second of partial pressure sintering stage are as follows: temperature is 1520 DEG C, and constant temperature keeps the temperature 1h, is protected
Atmosphere argon gas is protected, partial pressure pressure is 150mbar.
Embodiment 10
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
51%, TaC 2%, TiC 3%, NbC 2%, WC 18.5%, Mo2C is 7%, Cr3C2For 0.5%, Co 8%, Ru-
Ti-Ni is 8%.
Embodiment 11
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
52%, TaC 2%, TiC 2%, NbC 2%, WC 17.5%, Mo2C is 8%, Cr3C2For 0.5%, Co 8%, Ru-
Ti-Ni is 8%.
Embodiment 12
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
50%, TaC 3%, TiC 3%, NbC 2%, WC 18.5%, Mo2C is 8%, Cr3C2For 0.5%, Co 7%, Ru-
Ti-Ni is 8%.
Embodiment 13
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the TiCN based ceramic metal composite material of the present embodiment is made: TiCN by the raw material of following weight percent and is
58%, TaC 5%, TiC 1%, NbC 2%, WC 12%, Mo2C is 8%, Cr3C2For 0.8%, Co 9.2%, Ru-
Ti-Ni is 4%.
Comparative example 1
The present embodiment provides a kind of TiCN based ceramic metal composite materials, referring to the processing step of embodiment 5, with embodiment
5 the difference is that, the rare-earth element R u of the present embodiment is added with simple substance form, and wherein Ru is 1%, Ti 4%, and Ni is
2%.
Comparative example 2
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the pre-alloyed powder of the present embodiment consists of the following components in percentage by weight: Ru 4%, Ti 16%, Ni
It is 80%.
Comparative example 3
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, the pre-alloyed powder of the present embodiment consists of the following components in percentage by weight: Ru 21%, Ti 31%,
Ni is 48%.
Comparative example 4
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, in the pre-alloyed powder preparation process of the present embodiment, the technological parameter of smelting process are as follows: applying argon gas to air pressure is
0.02MPa, melting current density are 170A/cm2, heating temperature is 1600 DEG C, is kept molten by 8min；High pressure gas atomization
The technological parameter of method are as follows: high energy dielectric gas air pressure is 50bar, air-flow 28m3/ min, gas temperature are 0 DEG C, atomization rates
For 0.2kg/min.
Comparative example 5
The present embodiment provides a kind of TiCN based ceramic metal composite materials for adding pre-alloyed powder, not with embodiment 5
It is with place, in the pre-alloyed powder preparation process of the present embodiment, the technological parameter of smelting process are as follows: applying argon gas to air pressure is
0.08MPa, melting current density are 220A/cm2, heating temperature is 2100 DEG C, is kept molten by 65min；High pressure gas mist
The technological parameter of change method are as follows: high energy dielectric gas air pressure is 25bar, air-flow 28m3/ min, gas temperature are 0 DEG C, atomization speed
Rate is 1.5kg/min.
The TiCN based ceramic metal composite material prepared to embodiment 5~13 and comparative example 1~5 carries out properties inspection
It surveys, including density, consistency, hardness and bending strength, specific testing result are shown in Table 1.
Table 1
Obviously, above-described embodiment is only intended to clearly illustrate technical solution of the present invention example, and is not
Restriction to embodiments of the present invention.For those of ordinary skill in the art, on the basis of the above description also
It can make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all
Made any modifications, equivalent replacements, and improvements etc. within the spirit and principles in the present invention should be included in right of the present invention and want
Within the protection scope asked.
Claims (10)
1. a kind of pre-alloyed powder, which is characterized in that consist of the following components in percentage by weight: Ru be 5 ~ 20%, Ti be 17 ~
30%, Ni are 50 ~ 78%；The average grain diameter of the pre-alloyed powder is 2.1 ~ 4.5 μm.
2. pre-alloyed powder according to claim 1, which is characterized in that consist of the following components in percentage by weight: Ru is
12 ~ 17%, Ti are that 18 ~ 24%, Ni is 52 ~ 65%.
3. the preparation method of pre-alloyed powder according to claim 1 or claim 2, which is characterized in that be by Ru, Ti, Ni elemental gold
Belonging to is raw material, and Ru-Ti-Ni prealloy melt is prepared using arc melting method, the Ru-Ti-Ni prealloy melt is adopted
It is made of high pressure gas atomization.
4. the application of any one pre-alloyed powder according to claim 1 ~ 3, which is characterized in that be applied to preparation TiCN
Based ceramic metal composite material.
5. application according to claim 4, which is characterized in that the TiCN based ceramic metal composite material includes hard
Phase, Binder Phase and pre-alloyed powder, the hard phase is by TiCN, TaC, TiC, NbC, WC, Mo2C and Cr3C2Composition, the bonding
Mutually it is Co powder, the composite material is made of the raw material of following weight percent:
TiCN:42 ~ 64%,
TaC:0.5 ~ 9%,
TiC:1 ~ 12%,
NbC:1 ~ 8%,
WC:12 ~ 22%,
Mo2C:1.5 ~ 10%,
Cr3C2: 0.2 ~ 0.9%,
Co:6 ~ 12%,
Ru-Ti-Ni:4 ~ 12%；
The average grain diameter of the Co powder is 0.5 ~ 1.5 μm, and the average grain diameter of other powders is less than 4 μm.
6. application according to claim 5, which is characterized in that the TiCN based ceramic metal composite material is by following weight
The raw material of percentage is made:
TiCN:42 ~ 53%,
TaC:0.5 ~ 3%,
TiC:1 ~ 4%,
NbC:1 ~ 6%,
WC:12 ~ 18.5%,
Mo2C:8 ~ 10%,
Cr3C2: 0.2 ~ 0.5%,
Co:6 ~ 8%,
Ru-Ti-Ni:7 ~ 8%.
7. application according to claim 5 or 6, which is characterized in that the preparation of the TiCN based ceramic metal composite material
Method the following steps are included:
S1. pre-alloyed powder, hard phase and bonding phase component are subjected to ingredient by above-mentioned weight percent, forming agent is added
Afterwards, ball milling mixing is uniform, and spray-drying process, obtains mixture particle；
S2. the mixture particle that the S1 is obtained is pressed and molded, obtains TiCN based ceramic metal green compact；
S3. the TiCN based ceramic metal green compact S2 obtained carries out atmosphere sintering in more atmosphere sintering furnaces, is cooled to room
Temperature is to get TiCN based ceramic metal composite material.
8. application according to claim 7, which is characterized in that in step S1, the forming agent is paraffin or PEG；It is described
Paraffin additive amount is the 2.8 ~ 4.5% of raw material total amount, and the PEG additive amount is the 3.2 ~ 4.5% of raw material total amount.
9. application according to claim 8, which is characterized in that the technological parameter of the ball milling are as follows: use diameter for 7 ~ 10
The WC-8%Co sintered carbide ball of mm carries out ball milling, uses dehydrated alcohol for ball-milling medium, and ratio of grinding media to material is 7 ~ 10:1, revolving speed for 45 ~
70 rpm, Ball-milling Time are 56 ~ 72 h.
10. application according to claim 7, which is characterized in that in step S3, the atmosphere sintering is five stage atmosphere burning
Knot successively includes negative pressure dewaxing stage, vacuum solid-phase sintering stage, for the first time partial pressure sintering stage, vacuum liquid-phase sintering stage
With second of partial pressure sintering stage.
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