CN113430410A - Novel preparation method of Ti (C, N) -based metal ceramic - Google Patents
Novel preparation method of Ti (C, N) -based metal ceramic Download PDFInfo
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- CN113430410A CN113430410A CN202110648963.2A CN202110648963A CN113430410A CN 113430410 A CN113430410 A CN 113430410A CN 202110648963 A CN202110648963 A CN 202110648963A CN 113430410 A CN113430410 A CN 113430410A
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- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 63
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 61
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 47
- 239000002184 metal Substances 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010936 titanium Substances 0.000 claims abstract description 69
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002114 nanocomposite Substances 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005452 bending Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 7
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 7
- 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 7
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 7
- 229910009043 WC-Co Inorganic materials 0.000 claims abstract description 6
- 238000009768 microwave sintering Methods 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 230000015572 biosynthetic process Effects 0.000 claims abstract 2
- 238000003786 synthesis reaction Methods 0.000 claims abstract 2
- 239000011195 cermet Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 238000002490 spark plasma sintering Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
-
- 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
- C22C29/005—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
- 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
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Abstract
The invention belongs to the field of metal ceramic preparation, and relates to a novel preparation method of Ti (C, N) -based metal ceramic. The preparation method comprises the following steps: a. taking nano titanium oxide, nano carbon black, nano tungsten oxide and nano cobalt oxide according to a certain proportion, uniformly mixing them, placing them into microwave sintering furnace to make microwave in-situ synthesis so as to obtain Ti (C)0.5,N0.5) -WC-Co nanocomposite powder. b. Weighing the Ti (C) prepared in the step a0.5,N0.5) And (3) sintering the WC-Co nano composite powder by adopting a discharge plasma sintering device to finally prepare the superfine or nano Ti (C, N) -based metal ceramic. Compared with Ti (C, N) -based metal ceramics prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramics is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, and the bending strength is improved by 35-83%. The method usesThe material is uniformly mixed, dried and then placed in discharge plasma equipment for sintering, and the method has the characteristics of low reaction temperature, short time, simple operation process and the like, the obtained Ti (C, N) -based metal ceramic has uniform tissue and no obvious holes, the comprehensive performance of the Ti (C, N) -based metal ceramic is obviously improved, important reference is provided for the preparation and production of high-performance Ti (C, N) -based metal ceramic, and the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of metal ceramic preparation, and particularly relates to a novel preparation method of Ti (C, N) -based metal ceramic.
Background
Ti (C, N) -based cermet has high melting point, high strength, high hardness, and high wear resistance, and is widely used in metal cutting tools, wear-resistant parts, and the like. Transition metals such as Co and Ni are often used as binder phases for Ti (C, N) -based cermets, in which Co has good wettability to carbides, and thus are often used as binder phases for Ti (C, N) -based cermets. With the development of modern industry, the requirements on the service life and the cutting efficiency of the cutter are higher and higher, and the traditional Ti (C, N) -based metal ceramic cannot meet the use requirements.
The grain size, porosity and pore uniformity of titanium carbonitride in Ti (C, N) -based cermet all affect the structure and processability of the alloy. The Ti (C, N) is easy to grow abnormally at high temperature, so that the porosity inside the metal ceramic is increased, the pore distribution is wider, and the like, which influence the organization structure and the processing performance of the alloy. Therefore, the key to the preparation of Ti (C, N) -based cermets is the inhibition of Ti (C, N) grain growth during sintering, thereby increasing their hardness and bending strength.
The application of the inhibitor prevents the excessive growth of crystal grains, thereby improving the compactness of the alloy. By adding the composite grain growth inhibitor, the metal ceramic with finer Ti (C, N) grains and outstanding comprehensive mechanical properties can be obtained. Meanwhile, the sintering technology has the same important influence on the preparation of Ti (C, N) -based metal ceramics. Common sintering methods for cermet include microwave sintering, hot isostatic pressing sintering, hot pressing sintering, and spark plasma sintering. The spark plasma sintering has the advantages of uniform heating, high temperature rise speed, low sintering temperature, short sintering time, high production efficiency, fine and uniform product tissue, capability of keeping the natural state of raw materials, capability of obtaining high-density materials and the like, and is widely applied to the sintering technology of metal ceramics. The spark plasma sintering technology has the advantages of simple operation, high reproducibility, safety, reliability, space saving, energy saving and low cost, shows great superiority in the preparation of nano materials, composite materials and the like, and is a new sintering technology with important use value and wide prospect. The rapid pressurizing and heating sintering technology of the discharge plasma can more effectively inhibit abnormal growth of Ti (C, N) crystal grains, shorten the sintering time, improve the production efficiency and the comprehensive performance of the metal ceramic and provide convenience for industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of novel Ti (C, N) -based metal ceramic, so as to better meet the application of the Ti (C, N) -based metal ceramic in the fields of metal cutting tools and wear-resistant parts.
The novel preparation method of the Ti (C, N) -based metal ceramic comprises the following steps:
a. mixing nanometer titanium oxide, nanometer carbon black, nanometer tungsten oxide and nanometer cobalt oxide, drying, and performing carbothermic reduction in a microwave sintering furnace to obtain Ti (C)0.5,N0.5) -WC-Co nanocomposite powder;
b. and (b) sintering the nano composite powder prepared in the step a by adopting discharge plasma sintering equipment to finally prepare the superfine or nano Ti (C, N) -based metal ceramic. Compared with the Ti (C, N) -based metal ceramic prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramic is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, the bending strength is improved by 35-83%, and the Ti (C, N) -based metal ceramic has uniform structure and no obvious holes.
In the novel preparation method of the Ti (C, N) -based metal ceramic, nano Ti (C)0.5,N0.5) The mass percentages of the-WC-Co composite powder are that the nano titanium carbonitride accounts for 55-67%, the nano cobalt accounts for 8-15%, and the nano tungsten carbide accounts for 25-35%.
In the novel preparation method of the Ti (C, N) -based cermet, mixing is carried out in any one of a high-energy ball mill, a roller ball mill or a grinding mill.
In the novel preparation method of the Ti (C, N) -based metal ceramic, the drying temperature is 70-90 ℃ after ball milling, and the drying time is 12-24 h.
The sintering for preparing the Ti (C, N) -based metal ceramic is carried out under the condition of nitrogen, the heating rate is 100-minus-one ℃/min, and the sintering temperature is 1300-minus-one 1450 ℃.
Compared with the existing preparation method of Ti (C, N) -based metal ceramic, the invention has the advantages that:
(1) the Ti (C, N) -based metal ceramic has uniform structure and high comprehensive performance. Firstly, nano composite powder is synthesized in situ by adopting a microwave method, and then sintering is carried out by adopting a discharge plasma sintering furnace, so that the growth of Ti (C, N) crystal grains is fully inhibited, the structure of the Ti (C, N) -based metal ceramic is uniform, the densification is realized, and the comprehensive performance of the metal ceramic is obviously improved.
(2) Simple operation, energy saving and cost reduction. The sintering technology of rapid pressurization and rapid temperature rise of the discharge plasma is adopted, so that the production efficiency can be obviously improved, the production cost is reduced, and the energy is saved.
Detailed Description
Example 1:
the nano titanium oxide, nano tungsten oxide, nano cobalt oxide and nano carbon black powder are taken according to the mass percentage, so that the mass percentage of each substance in the generated nano composite powder is 67 percent of titanium carbonitride, 8 percent of nano cobalt powder and 25 percent of nano tungsten carbide. Mixing the powders, drying at 70 deg.C for 24 hr, and sintering at 1450 deg.C and N at a temperature of 100 deg.C and 250 deg.C/min and 1300 deg.C by spark plasma sintering equipment2) Finally, the Ti (C, N) -based cermet is prepared. Compared with Ti (C, N) -based metal ceramics prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramics is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, and the bending strength is improved by 35-83%.
Example 2:
the nano titanium oxide, nano tungsten oxide, nano cobalt oxide and nano carbon black powder are taken according to the mass percentage, so that the mass percentage of each substance in the generated nano composite powder is 55 percent of titanium carbonitride, 10 percent of nano cobalt powder and 35 percent of nano tungsten carbide. Mixing the powders, drying (90 deg.C, 12 hr), and discharging plasmaSintering equipment is used for sintering (the heating rate is 100-250 ℃/min, the sintering temperature is 1300-1450 ℃, and N is2) Finally, the Ti (C, N) -based cermet is prepared. Compared with Ti (C, N) -based metal ceramics prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramics is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, and the bending strength is improved by 35-83%.
Example 3:
the nano titanium oxide, nano tungsten oxide, nano cobalt oxide and nano carbon black powder are taken according to the mass percentage, so that the mass percentage of each substance in the generated nano composite powder is that titanium carbonitride accounts for 50%, nano cobalt powder accounts for 12% and nano tungsten carbide accounts for 38%. Mixing the powders, drying at 80 deg.C for 18h, and sintering at 1450 deg.C and N at a temperature of 100 deg.C and 250 deg.C/min and 1300 deg.C by spark plasma sintering equipment2) Finally, the Ti (C, N) -based cermet is prepared. Compared with Ti (C, N) -based metal ceramics prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramics is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, and the bending strength is improved by 35-83%.
Example 4:
the nano titanium oxide, nano tungsten oxide, nano cobalt oxide and nano carbon black powder are taken according to the mass percentage, so that the mass percentage of each substance in the generated nano composite powder is that titanium carbonitride accounts for 60%, nano cobalt powder accounts for 15%, and nano tungsten carbide accounts for 25%. Mixing the powders, drying at 85 deg.C for 16h, and sintering at 1450 deg.C and N at a temperature of 100 deg.C and 250 deg.C/min and 1300 deg.C by using spark plasma sintering equipment2) Finally, the Ti (C, N) -based cermet is prepared. Compared with Ti (C, N) -based metal ceramics prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramics is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, and the bending strength is improved by 35-83%.
Claims (5)
1. A novel preparation method of Ti (C, N) -based cermet is characterized in that: the preparation method comprises the following steps:
a. taking nano titanium oxide and nano titanium oxide with different mass percentages according to the proportionCarbon black, nano tungsten oxide and nano cobalt oxide are evenly mixed and then placed in a microwave sintering furnace for microwave in-situ synthesis to prepare Ti (C)0.5,N0.5) -WC-Co nanocomposite powder;
b. b, proportionally taking the nano composite powder prepared in the step a, and sintering by adopting discharge plasma sintering equipment to finally prepare superfine or nano Ti (C, N) -based metal ceramic; compared with the Ti (C, N) -based metal ceramic prepared by the traditional sintering method, the fracture toughness of the Ti (C, N) -based metal ceramic is improved by 35-66%, the Hardness (HRA) is improved by 7-24%, the bending strength is improved by 35-83%, and the Ti (C, N) -based metal ceramic has uniform structure and no obvious holes.
2. The method of producing a Ti (C, N) -based cermet according to claim 1, characterized in that: nano Ti (C)0.5,N0.5) The mass percentages of the-WC-Co composite powder are that the nano titanium carbonitride accounts for 55-67%, the nano cobalt accounts for 8-15%, and the nano tungsten carbide accounts for 25-35%.
3. The method of producing a Ti (C, N) -based 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.
4. The method of producing a Ti (C, N) -based cermet according to claim 1, characterized in that: the drying temperature after ball milling is 70-90 ℃, and the drying time is 12-24 h.
5. The method of producing a Ti (C, N) -based cermet according to claim 1, characterized in that: the sintering of the metal ceramic is carried out under the condition of nitrogen, the heating rate is 100-minus-one DEG C/min, and the sintering temperature is 1300-minus-one DEG C1450 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110648963.2A CN113430410A (en) | 2021-06-10 | 2021-06-10 | Novel preparation method of Ti (C, N) -based metal ceramic |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110648963.2A CN113430410A (en) | 2021-06-10 | 2021-06-10 | Novel preparation method of Ti (C, N) -based metal ceramic |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6124040A (en) * | 1993-11-30 | 2000-09-26 | Widia Gmbh | Composite and process for the production thereof |
| 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 CN202110648963.2A patent/CN113430410A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6124040A (en) * | 1993-11-30 | 2000-09-26 | Widia Gmbh | Composite and process for the production thereof |
| 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 |
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| 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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