CN113373337A - Preparation method of multi-element superfine metal ceramic - Google Patents
Preparation method of multi-element superfine metal ceramic Download PDFInfo
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- CN113373337A CN113373337A CN202110649127.6A CN202110649127A CN113373337A CN 113373337 A CN113373337 A CN 113373337A CN 202110649127 A CN202110649127 A CN 202110649127A CN 113373337 A CN113373337 A CN 113373337A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 23
- 239000002184 metal Substances 0.000 title claims abstract description 23
- 239000000919 ceramic Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 26
- 239000002114 nanocomposite Substances 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 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 9
- 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
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000009768 microwave sintering Methods 0.000 claims abstract description 9
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 9
- 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 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
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 239000011651 chromium Substances 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 239000011195 cermet Substances 0.000 claims description 34
- 239000013078 crystal Substances 0.000 claims description 12
- 238000001035 drying Methods 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
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910003470 tongbaite Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 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
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000002131 composite material Substances 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
- 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
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (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 preparation of superfine metal ceramics, and relates to a preparation method of multi-element superfine metal ceramics. 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 them, placing them in microwave sintering furnace and making microwave in-situ synthesis so as to obtain Ti (C)0.5,N0.5)‑WC‑V8C7‑Cr3C2-Co nanocomposite powder. b. And (b) weighing a certain amount of the nano composite powder prepared in the step (a), and sintering in discharge plasma sintering equipment to finally prepare the superfine Ti (C, N) -based metal ceramic. The metal ceramic is relatively traditionalThe Hardness (HRA) of the metal ceramic prepared by the method is improved by 8-25%, the bending strength is improved by 47-85%, and the fracture toughness is improved by 32-65%. 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 multielement 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 multi-element 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 multi-element superfine cermet 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 them, placing them in microwave sintering furnace and making microwave in-situ synthesis so as to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder;
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 multielement 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 multi-element superfine cermet, Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2The microwave sintering process of the-Co nano composite powder is carried out under the protection of flowing inert gas, the sintering temperature is 1100-1300 ℃, and the heat preservation time is 0.5-2h。
In the method for preparing the multi-element 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 multi-element superfine cermet, the drying temperature is 65-90 ℃ after ball milling, and the drying time is 12-24 h.
The sintering method for preparing the multi-element superfine cermet provided by the invention is carried out 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 multi-element superfine metal ceramic, the preparation method has the advantages that:
(1) the crystal grains of the metal ceramic are distributed uniformly and are fine. The multi-element Ti (C, N) -based nano composite powder containing the hard phase, the binding phase and the composite grain inhibitor is synthesized in situ by adopting a microwave method, so that the uniform dispersion of all components can be fundamentally realized, the growth of Ti (C, N) grains can be effectively inhibited, and the hard alloy with uniform grain distribution and fine grains can be obtained.
(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 the mass percentage, uniformly mixing, and placing in a microwave sintering furnace for microwave in-situ synthesis to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder. Weighing the nano composite powder according to the amount, mixing (high-energy ball mill), drying (70 ℃, 20 h), and sintering (60-250 ℃/min, 1350-. The cermet is oppositeCompared with the traditional method, the Hardness (HRA) of the metal ceramic is improved by 8-25%, the bending strength is improved by 47-85%, and the fracture toughness is improved by 32-65%. 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 percent, uniformly mixing, and placing in a microwave sintering furnace for microwave in-situ synthesis to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder. Weighing the nano composite powder according to the amount, mixing (high-energy ball mill), drying (75 ℃, 18 h), and sintering (60-250 ℃/min, 1350-. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 8-25%, the bending strength is improved by 47-85%, and the fracture toughness is improved by 32-65%. 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 the mass percentage, uniformly mixing, and placing in a microwave sintering furnace for microwave in-situ synthesis to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder. Weighing the nano composite powder according to the amount, mixing (high-energy ball mill), drying (80 ℃, 16 h), and sintering (60-250 ℃/min, 1350-. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 8-25%, the bending strength is improved by 47-85%, and the fracture toughness is improved by 32-65%. 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 the mass percentage, uniformly mixing, and placing in a microwave sintering furnace for microwave in-situ synthesis to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder. Weighing the nano composite powder according to the amount, mixing (high-energy ball mill), drying (85 ℃, 14 h), and sintering (60-250 ℃/min, 1350-. Compared with the cermet prepared by the traditional method, the Hardness (HRA) of the cermet is improved by 8-25%, the bending strength is improved by 47-85%, and the fracture toughness is improved by 32-65%. 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 multi-element 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 them, placing them in microwave sintering furnace and making microwave in-situ synthesis so as to obtain Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2-Co nanocomposite powder;
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.
2. The method for preparing multi-element ultrafine cermet according to claim 1, characterized in that: the superfine Ti (C, N) -based metal ceramic comprises, by mass, 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.
3. The method for preparing multi-element ultrafine cermet according to claim 1, characterized in that: the preparation of Ti (C)0.5,N0.5)-WC-V8C7-Cr3C2The microwave sintering process of the-Co nano composite powder is carried out under the protection of flowing inert gas, the sintering temperature is 1100-1300 ℃, and the heat preservation time is 0.5-2 h.
4. The method for preparing multi-element ultrafine 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 multi-element ultrafine 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 multi-element ultrafine 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386759A (en) * | 2022-08-26 | 2022-11-25 | 西安工业大学 | Ti (C7, N3)/TiB 2/WC micro-nano composite metal ceramic cutter material and preparation method thereof |
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- 2021-06-10 CN CN202110649127.6A patent/CN113373337A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115386759A (en) * | 2022-08-26 | 2022-11-25 | 西安工业大学 | Ti (C7, N3)/TiB 2/WC micro-nano composite metal ceramic cutter material and preparation method thereof |
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Application publication date: 20210910 |