CN113388751A - Preparation method of superfine metal ceramic - Google Patents
Preparation method of superfine metal ceramic Download PDFInfo
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- CN113388751A CN113388751A CN202110649112.XA CN202110649112A CN113388751A CN 113388751 A CN113388751 A CN 113388751A CN 202110649112 A CN202110649112 A CN 202110649112A CN 113388751 A CN113388751 A CN 113388751A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011195 cermet Substances 0.000 claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 9
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 9
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 8
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011858 nanopowder Substances 0.000 claims abstract 3
- 239000013078 crystal Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 6
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Classifications
-
- 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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
Abstract
The invention belongs to the field of superfine cermet preparation, and relates to a preparation method of superfine cermet. The preparation method comprises the following steps: a. taking nano titanium oxide, nano tungsten oxide, nano cobalt oxide, nano carbon black, nano chromium oxide and nano vanadium oxide powder according to a certain proportion, uniformly mixing, and placing in a drying oven for drying. b. And (b) weighing a certain amount of the nano powder prepared in the step (a), and sintering in discharge plasma sintering equipment to finally prepare the superfine Ti (C, N) -based metal ceramic. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 6-23%, the bending strength is improved by 45-84%, and the fracture toughness is improved by 30-65%. The method has the characteristics of simple process, convenient operation, energy conservation and the like, and the prepared metal ceramic has high comprehensive performance and wide market application prospect.
Description
Technical Field
The invention belongs to the field of superfine cermet preparation, and particularly relates to a method for preparing superfine cermet.
Background
Because of its high toughness and wear resistance, cermet is widely used in metal cutting, PCB (printed circuit board) drilling, and ground mining. Compared with common metal ceramics, the ultra-fine grain metal ceramics greatly improves the bending strength, the hardness and the wear resistance, can meet higher requirements of modern manufacturing industry, and is widely applied to various fields. The ultra-fine grain metal ceramic cutter can effectively overcome the problems of mutual contradiction between hardness and toughness, larger brittleness, processing softening and the like in the traditional hard alloy, has higher hardness, is applied to the field of some high-end hard alloy products, and also shows obvious advantages in the field of high-speed cutting of difficult-to-process materials.
The key to preparing superfine cermet is to obtain homogeneous microstructure, and the size distribution of Ti (C, N) crystal grains is the most important factor. When the superfine cermet is prepared, the superfine and nano Ti (C, N) powder prepared by the traditional method is often coarsened seriously, the coarse crystal particles are easy to cause stress concentration and crack under the action of external force, the coercive force (Hc) value of the alloy is seriously influenced, the mechanical property of the superfine cermet is reduced, and the application of the cermet is further influenced.
The performance of the superfine Ti (C, N) powder in the sintering process has a great relationship with the sintering process. The nano material is used as a raw material, and the multi-element Ti (C, N) -based nano composite powder containing a hard phase, a bonding phase and a composite crystal grain inhibitor is synthesized by adopting a discharge plasma sintering technology, so that the uniform dispersion of all components can be fundamentally realized, and the aims of effectively reducing the sintering temperature, shortening the reaction time and effectively inhibiting the rapid growth of WC crystal grains are fulfilled. The product obtained by the method has fine particles and uniform particle size distribution, and is beneficial to improving the comprehensive performance of the metal ceramic. Meanwhile, the sintering technology has great influence in the process of preparing the superfine cermet, compared with the traditional sintering technology, the spark plasma sintering technology has the characteristic of sintering in the pressurizing process, and the plasma generated by the pulse current and the pressurizing in the sintering process are beneficial to reducing the sintering temperature of the powder. Meanwhile, due to the characteristics of low voltage and high current, the powder can be rapidly sintered and compact, and the method is a novel powder metallurgy sintering technology for preparing high-performance materials. The sintering time can be effectively shortened, the production efficiency is improved, the energy is saved, the environment is protected, and the comprehensive mechanical properties such as the density, the strength and the hardness of the alloy are obviously improved.
Disclosure of Invention
The invention aims to provide a preparation method of superfine cermet, so as to better meet the application of the superfine cermet in the fields of cutter industry, metal cutting, PCB drilling and the like.
The preparation method of the superfine cermet comprises the following steps:
a. respectively taking nano titanium oxide, nano tungsten oxide, nano cobalt oxide, nano carbon black, nano chromium oxide and nano vanadium oxide powder according to different mass percentages, uniformly mixing, and then placing in a drying oven for drying;
b. and (b) weighing a certain amount of the nano composite powder prepared in the step (a), placing the nano composite powder in a discharge plasma sintering device for sintering, and finally preparing the superfine Ti (C, N) -based cermet, wherein the crystal grains of the cermet are uniformly distributed and are fine, and the average size of Ti (C, N) particles is close to the nanometer level.
In the method for preparing the superfine cermet, the superfine Ti (C, N) -based cermet comprises 38-52% of nano titanium oxide, 20-27% of nano carbon black, 26-32% of nano tungsten oxide, 8-15% of nano cobalt oxide, 0.2-1% of nano vanadium oxide and 0.2-1% of nano chromium oxide in percentage by mass respectively.
In the method for preparing the superfine cermet, the sintering process of the superfine Ti (C, N) -based cermet is carried out in the presence of N2The sintering is carried out in the atmosphere, the sintering temperature is 1350-1500 ℃, and the heat preservation time is 5-20 minutes.
In the method for preparing the superfine cermet, the mixing is carried out in any one of a high-energy ball mill, a rolling ball mill or a grinding mill.
In the method for preparing the superfine cermet, the drying temperature is 65-90 ℃ after ball milling, and the drying time is 12-24 h.
The method for preparing the superfine cermetSintering in vacuum or in N2Under the protection condition, the heating rate is 60-250 ℃/min, and the temperature is 1350-.
Compared with the existing preparation method of the superfine metal ceramic, the invention has the advantages that:
(1) the crystal grains of the metal ceramic are distributed uniformly and are fine. The synthesis of multi-element Ti (C, N) based nano composite powder containing hard phase, binding phase and composite crystal grain inhibitor and the synthesis of metal ceramic by using the Ti (C, N) composite powder are all realized in a discharge plasma sintering furnace. Can fundamentally realize the uniform dispersion of each component, effectively inhibit the growth of Ti (C, N) crystal grains, and obtain the hard alloy with uniform crystal grain distribution and fine crystal grains.
(2) Energy-saving and environment-friendly, and improves the production efficiency. The adoption of the spark plasma sintering method is beneficial to reducing the sintering temperature, shortening the reaction time, saving energy, protecting environment, improving the production efficiency, uniformly heating crystal grains, avoiding abnormal growth of the grains, and obviously improving the comprehensive mechanical properties of alloy density, strength, hardness and the like.
Detailed Description
Example 1:
weighing 38% of nano titanium oxide, 13% of nano cobalt oxide, 22% of nano carbon black, 0.2% of nano chromium oxide, 0.8% of nano vanadium oxide and 26% of nano tungsten oxide according to mass percentage. Weighing various original powders according to the proportion, mixing (high-energy ball mill), drying (70 ℃, 20 h), sintering (60-250 ℃/min, 1350 plus 1500 ℃ and nitrogen) by adopting discharge plasma sintering equipment, and finally obtaining the superfine metal ceramic. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 6-23%, the bending strength is improved by 45-84%, and the fracture toughness is improved by 30-65%. The crystal grains of the metal ceramic are uniformly distributed and fine, and the average size of Ti (C, N) particles is close to the nanometer level.
Example 2:
weighing 39% of nano titanium oxide, 13% of nano cobalt oxide, 22% of nano carbon black, 0.5% of nano chromium oxide, 0.5% of nano vanadium oxide and 25% of nano tungsten oxide according to mass percentage. Weighing various original powders according to the proportion, mixing (high-energy ball mill), drying (75 ℃, 18 h), sintering (60-250 ℃/min, 1350 plus 1500 ℃ and nitrogen) by adopting discharge plasma sintering equipment, and finally obtaining the superfine metal ceramic. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 6-23%, the bending strength is improved by 45-84%, and the fracture toughness is improved by 30-65%. The crystal grains of the metal ceramic are uniformly distributed and fine, and the average size of Ti (C, N) particles is close to the nanometer level.
Example 3:
weighing 40% of nano titanium oxide, 10% of nano cobalt oxide, 23% of nano carbon black, 0.4% of nano chromium oxide, 0.6% of nano vanadium oxide and 26% of nano tungsten oxide according to mass percentage. Weighing various original powders according to the proportion, mixing (high-energy ball mill), drying (80 ℃, 16 h), sintering (60-250 ℃/min, 1350-. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 6-23%, the bending strength is improved by 45-84%, and the fracture toughness is improved by 30-65%. The crystal grains of the metal ceramic are uniformly distributed and fine, and the average size of Ti (C, N) particles is close to the nanometer level.
Example 4:
weighing 42% of nano titanium oxide, 8% of nano cobalt oxide, 24% of nano carbon black, 0.3% of nano chromium oxide, 0.7% of nano vanadium oxide and 25% of nano tungsten oxide according to mass percentage. Weighing various original powders according to the proportion, mixing (high-energy ball mill), drying (85 ℃, 14 h), sintering (60-250 ℃/min, 1350 plus 1500 ℃ and nitrogen) by adopting discharge plasma sintering equipment, and finally obtaining the superfine metal ceramic. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 6-23%, the bending strength is improved by 45-84%, and the fracture toughness is improved by 30-65%. The crystal grains of the metal ceramic are uniformly distributed and fine, and the average size of Ti (C, N) particles is close to the nanometer level.
Claims (6)
1. A preparation method of superfine metal ceramic is characterized by comprising the following steps: the preparation method comprises the following steps:
a. taking nano titanium oxide, nano tungsten oxide, nano cobalt oxide, nano carbon black, nano chromium oxide and nano vanadium oxide powder according to a certain proportion, uniformly mixing, and placing in a drying oven for drying;
b. and (b) weighing a certain amount of the nano powder prepared in the step (a), placing the nano powder in a discharge plasma sintering device for sintering, and finally preparing the superfine Ti (C, N) -based cermet, wherein the crystal grains of the cermet are uniformly distributed and are fine, and the average size of Ti (C, N) particles is close to the nanometer level.
2. The method of claim 1, wherein the superfine Ti (C, N) -based cermet comprises about 38-52 wt% of nano-titanium oxide, about 20-27 wt% of nano-carbon black, about 26-32 wt% of nano-tungsten oxide, about 8-15 wt% of nano-cobalt oxide, about 0.2-1 wt% of nano-vanadium oxide, and about 0.2-1 wt% of nano-chromium oxide.
3. The method for preparing ultra fine cermet according to claim 1, characterized in that: the sintering process of the superfine Ti (C, N) -based metal ceramic is carried out in N2The sintering is carried out in the atmosphere, the sintering temperature is 1350-1500 ℃, and the heat preservation time is 5-20 minutes.
4. The method for preparing ultra fine cermet according to claim 1, characterized in that: the mixing is carried out in any one of a high energy ball mill, a roller ball mill or a grinding mill.
5. The method for preparing ultra fine cermet according to claim 1, characterized in that: the drying temperature after ball milling is 65-90 ℃, and the drying time is 12-24 h.
6. The method for preparing ultra fine cermet according to claim 1, characterized in that: the sintering for preparing the superfine cermet is carried out under the condition of nitrogen, the heating rate is 60-250 ℃/min, and the temperature is 1350-1500 ℃.
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| CN202110649112.XA CN113388751A (en) | 2021-06-10 | 2021-06-10 | Preparation method of superfine metal ceramic |
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| CN202110649112.XA CN113388751A (en) | 2021-06-10 | 2021-06-10 | Preparation method of superfine metal ceramic |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834842A (en) * | 2014-03-25 | 2014-06-04 | 龙具硬质合金（苏州）有限公司 | TiCN-based metal ceramic numerical control tool material with nanocrystalline grain size and preparation method thereof |
| CN106756388A (en) * | 2016-12-26 | 2017-05-31 | 苏州新锐合金工具股份有限公司 | Toughness reinforcing Ti（C, N）The preparation technology of based ceramic metal composite |
| CN107099723A (en) * | 2017-05-02 | 2017-08-29 | 四川大学 | Surface self-lubricating Ti (C, N) based ceramic metal preparation method based on metal hydride |
| CN107552802A (en) * | 2017-09-26 | 2018-01-09 | 中南大学 | A kind of cermet titanium carbonitride based solid solution powder and preparation method |
| CN108637268A (en) * | 2018-04-24 | 2018-10-12 | 海南大学 | A kind of method that microwave carbon thermal reduction prepares composite Ti (C, N) cermet powder |
| CN110102752A (en) * | 2019-04-29 | 2019-08-09 | 四川轻化工大学 | A kind of cermet solid solution alloy powder and preparation method |
| CN111378888A (en) * | 2020-01-02 | 2020-07-07 | 四川轻化工大学 | Nano particle interface reinforced Ti (C, N) -based metal ceramic material with high nitrogen content and preparation method thereof |
-
2021
- 2021-06-10 CN CN202110649112.XA patent/CN113388751A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834842A (en) * | 2014-03-25 | 2014-06-04 | 龙具硬质合金（苏州）有限公司 | TiCN-based metal ceramic numerical control tool material with nanocrystalline grain size and preparation method thereof |
| CN106756388A (en) * | 2016-12-26 | 2017-05-31 | 苏州新锐合金工具股份有限公司 | Toughness reinforcing Ti（C, N）The preparation technology of based ceramic metal composite |
| CN107099723A (en) * | 2017-05-02 | 2017-08-29 | 四川大学 | Surface self-lubricating Ti (C, N) based ceramic metal preparation method based on metal hydride |
| CN107552802A (en) * | 2017-09-26 | 2018-01-09 | 中南大学 | A kind of cermet titanium carbonitride based solid solution powder and preparation method |
| CN108637268A (en) * | 2018-04-24 | 2018-10-12 | 海南大学 | A kind of method that microwave carbon thermal reduction prepares composite Ti (C, N) cermet powder |
| CN110102752A (en) * | 2019-04-29 | 2019-08-09 | 四川轻化工大学 | A kind of cermet solid solution alloy powder and preparation method |
| CN111378888A (en) * | 2020-01-02 | 2020-07-07 | 四川轻化工大学 | Nano particle interface reinforced Ti (C, N) -based metal ceramic material with high nitrogen content and preparation method thereof |
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Application publication date: 20210914 |