CN117965938A - Beta-layer-removed hard alloy and preparation method thereof - Google Patents
Beta-layer-removed hard alloy and preparation method thereof Download PDFInfo
- Publication number
- CN117965938A CN117965938A CN202410015712.4A CN202410015712A CN117965938A CN 117965938 A CN117965938 A CN 117965938A CN 202410015712 A CN202410015712 A CN 202410015712A CN 117965938 A CN117965938 A CN 117965938A
- Authority
- CN
- China
- Prior art keywords
- nitrogen
- parts
- hard alloy
- sintering
- containing reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 44
- 239000000956 alloy Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000012495 reaction gas Substances 0.000 claims abstract description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007789 gas Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000000748 compression moulding Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- 238000001238 wet grinding Methods 0.000 claims abstract description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005121 nitriding Methods 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
The invention discloses a beta-layer removed hard alloy and a preparation method thereof, which relate to the technical field of hard alloys and comprise the following steps: mixing the following hard alloy raw materials in parts by weight, wherein the hard alloy raw materials contain no nitrogen, and the hard alloy raw materials comprise 80-85 parts of WC, 3-7 parts of (Ti, W) C, 5-8 parts of Co, 1-3 parts of TaC and 1-3 parts of NbC; s2: wet milling, spray drying, and compression molding to obtain pressed compact; removing the forming agent from the pressed compact by H 2 positive pressure, heating to 150-350 ℃ in vacuum, sintering in atmosphere at 1270-1350 ℃ by nitrogen-containing reaction gas, heating to 1420-1490 ℃ in vacuum, sintering for 0.5-1.5H, cooling to 1000-1100 ℃ after sintering, and introducing mixed gas of CH 4 and H 2. According to the invention, nitrogen-containing reaction gas is introduced into the nitrogen-free reaction raw material under the micro-pressure atmosphere for nitriding treatment, and at the same time, carbon-containing gas is added in a trace amount, and a certain amount of carbon elements are further provided in the cooling process, so that the gradient of the beta-removing layer is adjusted, an effective toughness area is formed on the surface of the alloy, and the performance of the alloy is improved.
Description
Technical Field
The invention relates to the technical field of hard alloy, in particular to a beta-layer removed hard alloy and a preparation method thereof.
Background
When continuously cutting carbon steel and alloy steel, the friction between the cutting and the front cutter surface of the cutter is large, and the average temperature of the cutting area is high, so that the hard alloy cutter is required to have higher high-temperature hardness. Wear resistance, adhesion resistance and oxidation resistance.
In order to improve the service life and cutting performance of the hard alloy cutting tool, a thin layer of high-hardness wear-resistant material such as TiN, tiC, ti (C, N) or Al 2O3 is coated on the surface of the alloy by adopting a chemical vapor deposition and physical vapor deposition method. However, the coated tool materials are susceptible to cracking during cooling due to thermal stresses due to the different coefficients of thermal expansion of the different materials.
In order to prevent as far as possible material failure due to crack initiation and propagation to obtain a high performance cemented carbide cutting tool material, the alloy substrate is typically gradient sintered prior to coating, and the gradient sintered coating substrate forms ductile regions of cubic phase deficient carbides and carbonitrides in its surface region, with a corresponding binder content higher than the coating substrate. Therefore, research into this process technology is required.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a beta-layer-removed hard alloy and a preparation method thereof.
The technical scheme of the invention is as follows:
the preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: mixing the following hard alloy raw materials in parts by weight, wherein the hard alloy raw materials contain no nitrogen, and the hard alloy raw materials comprise 80-85 parts of WC, 3-7 parts of (Ti, W) C, 5-8 parts of Co, 1-3 parts of TaC and 1-3 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: removing the forming agent from the pressed compact by H 2 positive pressure, heating to 150-350 ℃ in vacuum, sintering in atmosphere at 1270-1350 ℃ by nitrogen-containing reaction gas, heating to 1420-1490 ℃ in vacuum, sintering for 0.5-1.5H, cooling to 1000-1100 ℃ after sintering, and introducing mixed gas of CH 4 and H 2.
As a preferred embodiment of the present invention, in step S3, the pressure of the nitrogen-containing reaction gas is controlled to 50-150mbar.
In a preferred embodiment of the present invention, in step S3, the nitrogen-containing reaction gas is nitrogen.
As a preferable mode of the present invention, in the step S3, the nitrogen-containing reaction gas contains methane in a proportion of 0.5 to 3 vt%.
As a preferable scheme of the invention, in the step S3, the volume ratio of CH 4 and H 2 in the mixed gas is 1-3:1.
As a preferable scheme of the invention, in the step S3, the time for introducing the mixed gas at 1000-1100 ℃ is 20-40min.
The beneficial effects of the invention are as follows: according to the invention, nitrogen-containing reaction gas is introduced into the nitrogen-free reaction raw material under the micro-pressure atmosphere for nitriding treatment, and at the same time, carbon-containing gas is added in a trace amount, and a certain amount of carbon elements are further provided in the cooling process, so that the gradient of the beta-removing layer is adjusted, an effective toughness area is formed on the surface of the alloy, the diffusion of cracks in the alloy is prevented, and the performance of the alloy is improved.
Detailed Description
Embodiments of the present invention are described in detail below. The following examples are illustrative only and are not to be construed as limiting the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The technical scheme of the invention is further described in the following specific examples.
Example 1
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 50mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in an amount of 0.5 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Example 2
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 100mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in an amount of 0.5 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Example 3
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 150mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in an amount of 0.5 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Example 4
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 100mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in a proportion of 1 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Example 5
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 100mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in an amount of 1.5 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Example 6
The variation made on the basis of example 4 is in particular that the nitrogen-containing reaction gas contains methane in a proportion of 2 vt%.
Example 7
The variation made on the basis of example 4 is in particular that the nitrogen-containing reaction gas contains methane in a proportion of 3 vt%.
Example 8
The changes made on the basis of example 4 are in particular the volume ratio of CH 4 and H 2 in the gas mixture being 2:1.
Example 9
The variation made on the basis of example 4 is in particular the volumetric ratio of CH 4 and H 2 in the gas mixture of 3:1.
Comparative example 1 (Nitrogen-containing reaction gas containing no carbon-containing gas)
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating is carried out to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating is carried out to 1420 ℃ for sintering for 1H, after sintering is finished, cooling is carried out to 1100 ℃, and mixed gas of CH 4 and H 2 is introduced.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 100mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
Comparative example 2 (no mixed gas was introduced during the cooling stage)
The preparation method of the beta-layer removed hard alloy comprises the following steps:
S1: the following hard alloy raw materials without nitrogen are adopted for mixing, by weight, 80 parts of WC, 3 parts of (Ti, W) C, 5 parts of Co, 2 parts of TaC and 2 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: the pressed compact is subjected to positive pressure H 2 to remove the forming agent, vacuum heating to 150 ℃, then atmosphere sintering is carried out at 1270 ℃ through nitrogen-containing reaction gas, finally vacuum heating to 1420 ℃ and sintering for 1H, and furnace cooling is carried out.
In step S3, the pressure of the nitrogen-containing reaction gas is controlled at 100mbar.
In step S3, the nitrogen-containing reaction gas is nitrogen.
In step S3, the nitrogen-containing reaction gas contains methane in a proportion of 1 vt%.
In step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1:1.
In step S3, the time for introducing the mixed gas is 20 minutes.
The above examples and comparative examples were subjected to performance tests, and the test results are shown in table 1.
Table 1 results of performance tests of examples and comparative examples
From the above table, the performance of the examples is better than that of the comparative examples, probably for the following reasons: the nitrogen-containing reaction gas is introduced into the nitrogen-containing reaction raw material under the micro-pressure atmosphere for nitriding treatment, and the carbon-containing gas is added in a trace amount, so that a certain amount of carbon elements are further provided in the cooling process, the gradient of the beta-removing layer is adjusted, an effective toughness area is formed on the surface of the alloy, the diffusion of cracks in the alloy is prevented, and the performance of the alloy is improved.
The foregoing examples have shown only the preferred embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be pointed out that various other corresponding changes and modifications can be made by those skilled in the art in light of the above description of the technical solution and the idea, and all such changes and modifications are intended to be within the scope of the invention as defined in the appended claims.
Claims (6)
1. The preparation method of the beta-layer removed hard alloy is characterized by comprising the following steps of:
S1: mixing the following hard alloy raw materials in parts by weight, wherein the hard alloy raw materials contain no nitrogen, and the hard alloy raw materials comprise 80-85 parts of WC, 3-7 parts of (Ti, W) C, 5-8 parts of Co, 1-3 parts of TaC and 1-3 parts of NbC;
s2: wet milling, spray drying, and compression molding to obtain pressed compact;
S3: removing the forming agent from the pressed compact by H 2 positive pressure, heating to 150-350 ℃ in vacuum, sintering in atmosphere at 1270-1350 ℃ by nitrogen-containing reaction gas, heating to 1420-1490 ℃ in vacuum, sintering for 0.5-1.5H, cooling to 1000-1100 ℃ after sintering, and introducing mixed gas of CH 4 and H 2.
2. The method of claim 1, wherein in step S3, the pressure of the nitrogen-containing reaction gas is controlled to be 50-150mbar.
3. The method of claim 1, wherein in step S3, the nitrogen-containing reaction gas is nitrogen.
4. The method of claim 1, wherein in step S3, the nitrogen-containing reaction gas contains methane in an amount of 0.5 to 3 vt%.
5. The method of claim 1, wherein in step S3, the volume ratio of CH 4 to H 2 in the mixed gas is 1-3:1.
6. The method of claim 1, wherein in step S3, the mixed gas is introduced at 1000-1100 ℃ for 20-40min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410015712.4A CN117965938A (en) | 2024-01-05 | 2024-01-05 | Beta-layer-removed hard alloy and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410015712.4A CN117965938A (en) | 2024-01-05 | 2024-01-05 | Beta-layer-removed hard alloy and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117965938A true CN117965938A (en) | 2024-05-03 |
Family
ID=90865370
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410015712.4A Pending CN117965938A (en) | 2024-01-05 | 2024-01-05 | Beta-layer-removed hard alloy and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117965938A (en) |
-
2024
- 2024-01-05 CN CN202410015712.4A patent/CN117965938A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Endler et al. | Interlayers for diamond deposition on tool materials | |
| Konyashin | PVD/CVD technology for coating cemented carbides | |
| CN103403222A (en) | Coating layer for cutting tool | |
| JPH07103468B2 (en) | Coated cemented carbide and method for producing the same | |
| CN101974713A (en) | Method for preparing gradient cemented carbide with cubic carbide free layer | |
| CN114645171B (en) | Multi-principal-element alloy-diamond grinding tool material and preparation method and application thereof | |
| CN110408830B (en) | Ti (C, N) -based metal ceramic material and carbon balance control method thereof | |
| CN111482622A (en) | Coated cutting tool and preparation method thereof | |
| Richter et al. | Characterisation and wear behaviour of TiN-and TiCxN1-x-coated cermets | |
| WO2005121398A1 (en) | Thin diamond film coating method and cemented carbide member coated with diamond thin film | |
| CN117965938A (en) | Beta-layer-removed hard alloy and preparation method thereof | |
| EP0045291B1 (en) | Method of making a coated cemented carbide body and body produced in such a manner | |
| CN111893457A (en) | Coated cutting tool and preparation method thereof | |
| US4869929A (en) | Process for preparing sic protective films on metallic or metal impregnated substrates | |
| CN104249153A (en) | Hard alloy sintering method based on multi-atmosphere control and sintering product thereof | |
| JP2001316819A (en) | Hard amorphous carbon film and production method therefor | |
| CN110656301A (en) | Preparation method of controllable nitriding-PVD (physical vapor deposition) composite coating for high-speed steel tool | |
| EP0198464B1 (en) | Coated silicon nitride cutting tool and process for making | |
| CN113718226A (en) | Preparation method of hard alloy material surface diamond layer, hard alloy material and application thereof | |
| JP2006247751A (en) | Diamond film removing method and manufacturing method of diamond film coated member | |
| JP4133150B2 (en) | Method for producing diamond film-coated member | |
| JPH07243023A (en) | Cutting tool made of surface treated tungsten carbide-base sintered hard alloy, excellent in breaking resistance | |
| JPH0222453A (en) | Surface-treated tungsten carbide-base sintered hard alloy for cutting tool | |
| JPH05339731A (en) | Production of material having hard low-friction layer on its surface | |
| JPH0394062A (en) | Diamond-coated sintered hard alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication |