CN115821099A - Preparation method of hard alloy - Google Patents
Preparation method of hard alloy Download PDFInfo
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- CN115821099A CN115821099A CN202211506419.5A CN202211506419A CN115821099A CN 115821099 A CN115821099 A CN 115821099A CN 202211506419 A CN202211506419 A CN 202211506419A CN 115821099 A CN115821099 A CN 115821099A
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- 239000000956 alloy Substances 0.000 title claims abstract description 26
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 65
- 239000002994 raw material Substances 0.000 claims description 27
- 239000003966 growth inhibitor Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- 229910009043 WC-Co Inorganic materials 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000005056 compaction Methods 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005452 bending Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 150000001247 metal acetylides Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
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Abstract
The invention discloses a preparation method of hard alloy, belonging to the technical field of hard alloy production. The average WC grain size after sintering is in the range of 0.4um to 1.6um. Under the condition of not changing the traditional fine grain hard alloy production process, WC particles in the alloy structure are fine and uniform, the average grain size of the alloy produced by the method can reach 0.4-1.6um, and the bending strength and hardness of the alloy can be effectively improved. Under the same process conditions, the hardness of the sample in the embodiment of the invention can reach 1600HV3, the bending strength can reach 3250 +/-200 MPa, and the performance of the hard alloy is effectively improved.
Description
Technical Field
The invention belongs to the technical field of production of hard alloys, and particularly relates to a preparation method of a hard alloy.
Background
Cemented carbides for metal cutting have experienced a development history of nearly 70 years, and one of the biggest inventions in this field is a thin coating with TiC, tiN, al-O components, which can greatly improve the metal removal rate of the tool. The development of cemented carbide coating manufacturing technology has gone through a history from the first high temperature chemical vapor deposition (HT-CVD) to low deposition temperatures (MT-CVD) and Physical Vapor Deposition (PVD). While the thickness and adhesion of the coating is improved, the composition of the substrate is constantly changing. Previously these substrates normally constituted an effective part of the tool, however, today the main function of the substrate material was to carry the coating, which is an effective cutting material. The coated substrate, usually in the form of a removable insert, is mounted on the tool and, once the coating has worn, can be easily replaced.
The development of cemented carbide substrate materials has experienced a progression from the use of composite polycrystalline diamond, carbides, nitrides to the use of WC-Co cemented carbide substrates. The demand for WC grains during sintering of cemented carbides is also increasing. Cemented carbide with a grain size of less than 1.3um is generally defined as fine-grained cemented carbide, with a grain size of less than 0.5um as ultra-fine-grained cemented carbide, and with a grain size of less than 0.2um as nano-cemented carbide. Ultra-fine grain WC-Co cemented carbides have been developed and used for drilling holes in composite printed circuits or similar applications, which require special machining methods to complete; but the traditional preparation process has the defects of long flow, large energy consumption, accumulated defects, poor product quality stability and the like.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a preparation method of a hard alloy, wherein the average WC grain size after sintering is in the range of 0.4-1.6um, so that the performance of the WC-Co hard alloy is improved. The method comprises the following steps:
(1) supply of WC powder raw material: the WC powder raw material with round particles and the average grain size of 0.5-1.5um is used, the ultrafine powder often has aggregation phenomenon, the effect of the powder is greatly influenced when the WC powder raw material is used, and the WC powder raw material needs to be de-agglomerated or is easy to de-agglomerate.
(2) Provision of Co powder feedstock: a round-grained and narrow-size-distribution Co powder feedstock is used, which has been de-agglomerated or is easily de-agglomerated, the average grain size of the Co powder being less than the average grain size of the WC powder and less than the average grain size of the grain growth inhibitor powder.
(3) Mixing and compacting: uniformly mixing and compacting the WC powder raw material obtained in the step (1), the Co powder raw material obtained in the step (2) and the grain growth inhibitor to form a compact.
(4) And (3) sintering: and (4) sintering the compact obtained in the step (3) to obtain a hard alloy sample.
The WC powder raw material in the step (1) is produced in a reduction or carburization mode, and the original WC average grain size of the WC powder raw material is 0.5-1.5um. The average grain diameter of the Co powder in the step (2) is 0.5-1.0um. The grain growth inhibitor in the step (2) is Cr 3 C 2 Or is VC + Cr 3 C 2 . The mixing mode in the step (3) is to grind by a grinding machine for 3-4h; the compaction pressure of the powder in the step (3) is 110-115MPa. The sintering temperature in the step (4) is 1300-1400 ℃, and the heat preservation time is 5-10min.
The WC-Co-based hard alloy prepared by the method has the average grain size range of 0.4-1.6um after sintering.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for preparing WC-Co-based hard alloy by sintering, wherein the average WC grain size after sintering is in the range of 0.4-1.6um, and the performance is improved. Under the condition of not changing the traditional fine grain hard alloy production process, WC particles in the alloy structure are fine and uniform, the average grain size of the alloy produced by the method can reach 0.4-1.6um, and the bending strength and hardness of the alloy can be effectively improved.
Detailed Description
The invention is further illustrated, but is not in any way limited, by the following specific examples. The particle size of the sample was measured by a Fisher-Tropsch particle size analyzer (model WLP-216, supplied by Dandong Huayu instruments Co., ltd.) according to the standard GB/T3249-2022 method for measuring Fisher particle size of metal and compound powders thereof. Testing the three-point bending strength of the hard alloy on a CMT5105 universal testing machine according to the standard GB/T232-2010 metal material bending test method, wherein the loading rate is 4mm/min; the Durascan full-automatic Vickers hardness is adopted to measure the hardness according to the standard GB/T4340.1-1999 Metal Vickers hardness part 1: the hardness of the hard alloy is tested according to the test method, the loading force is 3kg, and the pressure maintaining time is 10-15 s.
Example 1
A method of making a cemented carbide, the method comprising the steps of:
(1) supply of WC powder: WC powder with round particles and narrow particle size distribution is used, the WC powder raw material is de-agglomerated or easy to de-agglomerate. The WC powder raw material is produced by a reduction or carburization mode, and the original WC average grain size (FSSS) of the WC powder raw material is 0.7um.
(2) Provision of Co powder: using a round-grained and narrow-size-distribution Co powder feedstock that has been de-agglomerated or is readily de-agglomerated, the Co powder having an average grain size that is less than the average grain size of the WC powder and less than the average grain size of the grain growth inhibitor powder; the grain growth inhibitor is added to the Co powder as part of the binder and alloyed therewith to provide a rounded Co powder after alloying with the at least one grain growth inhibitor. The average grain diameter of the Co powder is 0.65um. The grain growth inhibitor is Cr 3 C 2 。
(3) Mixing and compacting: mixing the WC powder obtained in the step (1), the Co powder obtained in the step (2) and a grain growth inhibitor according to the mass percentage shown in the table 1; uniformly mixing the raw materials, and grinding the raw materials by using a grinding machine in a mixing mode for 3 hours; then, the mixture is compacted at a pressure of 110MPa to form a compact.
(4) And (3) sintering: and (4) sintering the compact obtained in the step (3), wherein the sintering temperature is 1400 ℃, and the heat preservation time is 10min, so that a hard alloy sample is obtained.
TABLE 1 raw material proportioning scheme
Comparative example 1
The preparation of cemented carbide samples was carried out using the prior art with the experimental protocol shown in table 2.
Table 2 prior art experimental protocols
The same process as in example 1 was used to sinter the same batch of samples of example 1 and comparative example 1 in the same state, except that the compacting pressure of the powder was adjusted to 145MPa and the milling time was adjusted to 30 hours. The hardness of the above samples is detected to be 1600+25HV3.
Samples (5.5X 6.5X 21 mm) prepared after the sintering of example 1 and comparative example 1 respectively are subjected to a three-point bending test to obtain an average value of results, and the bending strength of comparative example 1 in the prior art is 2725 +/-300 MPa; while the bending strength of the example 1 of the present invention is 3250 ± 200MPa, it is shown that the performance of the cemented carbide is effectively improved.
Example 2
A method of making a cemented carbide, the method comprising the steps of:
(1) providing a WC powder raw material: WC powder with round particles and narrow particle size distribution is used, the WC powder raw material is de-agglomerated or easy to de-agglomerate. The WC powder raw material is produced by a reduction or carburization mode, and the original WC average grain size (FSSS) of the WC powder raw material is 1.0um.
(2) Provision of Co powder feedstock: using a round-grained and narrow-size-distribution Co powder feedstock that has been de-agglomerated or is readily de-agglomerated, the Co powder having an average grain size that is less than the average grain size of the WC powder and less than the average grain size of the grain growth inhibitor powder; the grain growth inhibitor is added to the Co powder as part of the binder and alloyed therewith to provide a grain growth inhibitor with at least one of the grain growth inhibitorsRound Co powder after alloying. The average grain diameter of the Co powder is 0.8um. The grain growth inhibitor is Cr 3 C 2 。
(3) Mixing and compacting: mixing the WC powder raw material obtained in the step (1), the Co powder obtained in the step (2), a grain growth inhibitor and compensating carbon according to the mass percentage shown in the table 3; uniformly mixing the raw materials, and grinding the raw materials by using a grinding machine in a mixing mode for 4 hours; then, the mixture was compacted at a pressure of 115MPa to form a compact.
(4) And (3) sintering: and (4) sintering the compact obtained in the step (3), wherein the sintering temperature is 1350 ℃, and the heat preservation time is 8min, so that a hard alloy sample is obtained.
Table 3 raw material proportioning scheme
Comparative example 2
The preparation of cemented carbide samples was carried out using the prior art with the experimental protocol shown in table 4.
Table 4 prior art experimental protocol
The same process as in example 2 was used to compact the same test inserts at 18% compression, the compaction pressure of the powder was adjusted to 160MPa only, the milling time was adjusted to 30 hours, and the same conditions were used to sinter the same batch of samples of example 2 and comparative example 2 in the same state of sintering. The hardness of the above samples is 1750+25HV3 by detection.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (7)
1. A method for preparing a hard alloy, characterized in that the method comprises the following steps:
(1) providing a WC powder raw material: using a WC powder feedstock having round particles and an average grain size of 0.5-1.5um, which has been de-agglomerated or is susceptible to de-agglomeration;
(2) provision of Co powder feedstock: using a round-grained and narrow-size-distribution Co powder feedstock that has been de-agglomerated or is readily de-agglomerated, the Co powder having an average grain size that is less than the average grain size of the WC powder and less than the average grain size of the grain growth inhibitor powder; adding grain growth inhibitor as part of the binder to the Co powder and alloying therewith to provide a rounded Co powder alloyed with at least one grain growth inhibitor;
(3) mixing and compacting: uniformly mixing and compacting the WC powder raw material obtained in the step (1), the Co powder raw material obtained in the step (2) and a grain growth inhibitor to form a compact;
(4) and (3) sintering: and (4) sintering the compact obtained in the step (3) to obtain a hard alloy sample.
2. The method for preparing a cemented carbide according to claim 1, wherein: the WC powder raw material in the step (1) is produced by a reduction or carburization mode, and the original WC average grain size of the WC powder raw material is 0.5-1.5 mu m.
3. The method for preparing a cemented carbide according to claim 1, wherein: the average grain diameter of the Co powder in the step (2) is 0.5-1.0 μm.
4. The method for preparing a cemented carbide according to claim 1, wherein: the grain growth inhibitor in the step (2) is Cr 3 C 2 Or is VC + Cr 3 C 2 。
5. The method for preparing a cemented carbide according to claim 1, wherein: the mixing mode in the step (3) is to grind by a grinding machine for 3-4h; the compaction pressure of the powder in the step (3) is 110-115MPa.
6. The method for preparing a cemented carbide according to claim 1, wherein: the sintering temperature in the step (4) is 1300-1400 ℃, and the heat preservation time is 5-10min.
7. A WC-Co based cemented carbide produced by the method according to any one of claims 1 to 6, having a WC average grain size after sintering in the range of 0.4 to 1.6 μm.
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