CN103741000B - Ultra-fine Grained gradient hard alloy of a kind of rich surface cobalt and preparation method thereof - Google Patents
Ultra-fine Grained gradient hard alloy of a kind of rich surface cobalt and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to Wimet and manufacture field, be specifically related to Ultra-fine Grained gradient hard alloy of a kind of rich surface cobalt and preparation method thereof.The Ultra-fine Grained gradient hard alloy metallographic structure of rich surface cobalt of the present invention is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 10 ~ 40 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.2-0.4 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.2-2 times of Wimet nominal cobalt contents, not containing Emission in Cubic carbonitride in the gradient layer of rich surface cobalt; First preparation method prepares burden, and wet-milling is also pressed into material base, the rare gas element of charged pressure 5 ~ 10MPa before reaching liquid phase sintering conditions, and liquid phase sintering conditions is 1350 ~ 1500 DEG C.The present invention, by being filled with the gas of certain pressure in the liquid phase sintering stage, prepares the Ultra-fine Grained gradient hard alloy of rich surface cobalt, and refinement WC grain, obtains certain thickness rich surface cobalt layers, shorten the sintering period, reduce production cost.
Description
Technical field
The invention belongs to Wimet and manufacture field, be specifically related to Ultra-fine Grained gradient hard alloy of a kind of rich surface cobalt and preparation method thereof.
Background technology
Wimet is owing to having higher intensity and hardness, and the advantages such as wear resistance is better, are mainly used to make cutter, are widely used in machining field.In recent years, along with the development of Materials science, increasing difficult-to-machine material starts to obtain many application, therefore more and more higher requirement is proposed to the performance of work material inserted tool used, and along with the development of modern manufacturing industry, require that inserted tool is applicable to high-speed and continuous cutting etc., this just requires that inserted tool should have good wear resisting property, have good toughness and impact resistance again, traditional Wimet is all difficult to meet the demands in wear resisting property, intensity and toughness.According to Hall Page formula, crystal grain is less, and the intensity of material is larger, therefore by crystal grain thinning, improves Wimet intensity, and preparing the Wimet with Ultra-fine Grained is following main development direction.For in toughness and the exigent application of wear resistance, the Wimet with nanometer or micro-scale crystal grain has higher intensity, can better meet actual requirement.
In order to improve the wear resistance of inserted tool further, the inserted tool of application at present all needs to adopt chemical vapor deposition (CVD) or physical vapor deposition (PVD) in its plated surface last layer or multi-layer wear-resistant coating, as TiN, Al usually
2o
3deng.Temperature due to this coating technology is general all more than 800 DEG C, due to the difference of thermal expansivity between coatings and substrate, in process of cooling, certain thermal stresses can be produced between coatings and substrate, and then there will be some tiny cracks, in the cutting use procedure of cutter, these tiny cracks can be expanded to intrinsic silicon, cause cutter wear resisting property to reduce and tipping inefficacy, this just requires that matrix has higher toughness.In addition in order to improve the bonding strength between coatings and substrate, also require that there is between coatings and substrate good wettability.In order to address this problem, the hard alloy substrate with higher toughness of rich surface cobalt can be adopted, be commonly referred to rich surface cobalt gradient hard alloy.Because the gradient cladding cemented carbide substrate surfaces toughness of this rich surface cobalt is higher, the energy of crack propagation can be absorbed, slow down crackle to the expansion in matrix, the good wettability between rich surface cobalt layers and coating, thus improve and extend the performance and used life of Wimet.
The technology of this gradient hard alloy of current manufacture is referred to as gradient sintering, as United States Patent (USP) 4277283 and 4610931, nitrogenous additive is adopted to sinter in a vacuum, United States Patent (USP) 4548786 then adds nitrogen to gas is middle mutually, and both of these case all obtains the rich surface bonding phase region substantially not containing Emission in Cubic.United States Patent (USP) 4830930 obtains rich surface bonding phase region by carrying out decarburization after the sintering.These sintering process all adopt two-step sintering method (presintering and gradient sintering complete in two steps), and sintering atmosphere is without nitrogen vacuum.It is comparatively large that two-step sintering method prepares WC grain size in gradient hard alloy, and performance is lower, adds production cost in addition, is unfavorable for scale operation.
Summary of the invention
For prior art Problems existing, the invention provides Ultra-fine Grained gradient hard alloy of a kind of rich surface cobalt and preparation method thereof, by adopting a step sintering process, shorten Production Flow Chart, reduce production cost, by being filled with the rare gas element of certain pressure at liquid phase sintering holding stage, suppress growing up of WC grain, on the basis of refinement Wimet WC grain, prepare a kind of Ultra-fine Grained gradient hard alloy matrix with rich surface cobalt gradient layer.
The Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention, its composition is by mass percentage: 2-6%Ti (C, N), 6-15%Co, 0-0.5%VC, 0.2-0.8%Cr
3c
2with 0-0.5% carbon black, surplus is WC, its metallographic structure is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 10 ~ 40 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.2-0.4 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.2-2 times of Wimet nominal cobalt contents, not containing Emission in Cubic carbonitride in the gradient layer of rich surface cobalt.
The preparation method of the Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention carries out according to following steps:
(1) adopt the hard alloy material adding carbonitride to prepare burden, its composition is by mass percentage: 2-6%Ti (C, N), 6-15%Co, 0-0.5%VC, 0.2-0.8%Cr
3c
2with 0-0.5% carbon black, surplus is WC;
(2) wet-milling in wet-type ball mill is added after being mixed by above-mentioned raw materials, mixed slurry after wet-milling is left standstill 8 ~ 12h, then vacuum drying oven is put in 60 ~ 90 DEG C of insulation 1 ~ 2h, sieve with 40 eye mesh screens after dry, powder press after sieving and mould are pressed into material base, pressure is 5 ~ 20 tons, and the dwell time is 5 ~ 30s;
(3) material base is placed in vacuum oven, vacuum oven is evacuated down to below 10Pa to start to heat up, be warming up to 400 ~ 600 DEG C and be incubated 1 ~ 6h, pass into hydrogen simultaneously, carry out dewaxing, deoxidation, hydrogen afterwards in emptying furnace chamber continues to heat up, the rare gas element of charged pressure 5 ~ 10MPa before reaching liquid phase sintering conditions, liquid phase sintering conditions is 1350 ~ 1500 DEG C, 0.1 ~ 2h is incubated under inert gas pressure, cool to room temperature with the furnace after insulation terminates, obtain the Ultra-fine Grained gradient hard alloy of rich surface cobalt.
Wherein, the mean particle size of the WC powder of interpolation is 0.4 μm, and the mean particle size of Ti (C, N) powder is 0.2 ~ 1.5 μm, and the atomic ratio of C and N is the mean particle size of 0.5:0.5, Co powder is 1 μm, VC and Cr
3c
2the mean particle size of powder is less than 1 μm.
When step (2) carries out wet-milling, ratio of grinding media to material is (10 ~ 15): 1, and wet grinding media is alcohol, and rotating speed is 40 ~ 100r/min, and the wet-milling time is 48 ~ 72h.
Described rare gas element is argon gas.
Compared with prior art, feature of the present invention and beneficial effect are:
The ultra-fine cemented carbide matrix of rich surface cobalt of the present invention, main is hard phase with WC, and its average grain size is about 0.2 μm-0.4 μm, and is metallic binding phase with cobalt, add one or more carbonitride sosoloid, and add a kind of carbide containing V and Cr as grain inhibitor.Under a step sintering process, the rich surface cobalt layers thickness of acquisition is about 10 μm-40 μm, and not containing cubic carbides, the Binder Phase cobalt contents of rich surface cobalt layers is about the 1.2-2 of nominal binder phase content doubly.0.3 μm is about at the WC grain average grain size of rich surface cobalt layers and core.For in toughness and the exigent application of wear resistance, the Wimet with nano-micrometre grade crystal grain has higher intensity, coated cutting tool has higher wear resisting property, prepares the application that the gradient cladding inserted tool with Ultra-fine Grained expands Wimet for the performance improving Wimet and has a very big significance.
First, the inventive method comprises raw material configuration, ball milling, shaping and sintering four steps, described sintering step is followed successively by dewaxing deoxidation, heat up sintering, heat preservation sintering and cooling three phases, namely, in a step sintering process, by being filled with the gas of certain pressure in the liquid phase sintering stage, the Ultra-fine Grained gradient hard alloy of rich surface cobalt is prepared, refinement WC grain, obtain certain thickness rich surface cobalt layers, shorten the sintering period, reduce production cost;
Owing to being filled with the gas of certain pressure at liquid phase stage, facilitate the flowing of liquid phase, enable liquid phase fully fill space between WC powder particle at short notice, reduce the porosity of Wimet, improve the density of Wimet, and then improve the performance of Wimet; Reduce sintering temperature, growing up of WC grain can be suppressed, obtain ultra-fine cemented carbide matrix; Simultaneously due to the interpolation of nano-carbon titanium nitride powder and the existence of sintering pressure, reduce the dissolving decomposition temperature of titanium carbonitride, add the diffusion admittance of titanium carbonitride, facilitate the velocity of diffusion that in the Wimet of top layer, atom N is outside and Ti atom is inside, the room that liquid phase cobalt can stay after Fast Filling N and Ti atomic diffusion, be conducive to the formation of rich surface cobalt layers, obtain thicker rich surface cobalt gradient layer;
Secondly, the Ultra-fine Grained gradient hard alloy rich surface cobalt layers cobalt contents of rich surface cobalt prepared by the present invention is higher, and not containing Emission in Cubic, what make Wimet has good surface toughness and shock resistance, effectively can prevent the expansion of crackle;
Again, in the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the present invention, hard phase WC grain size is tiny, has higher intensity and wear resisting property.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 1;
Fig. 2 is the crystallite size analysis chart of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 1;
Fig. 3 is the metallographic structure figure of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 2;
Fig. 4 is the crystallite size analysis chart of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 2;
Fig. 5 is the metallographic structure figure of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 3;
Fig. 6 is the crystallite size analysis chart of the Ultra-fine Grained gradient hard alloy of rich surface cobalt prepared by the embodiment of the present invention 3.
Embodiment
Embodiment 1
The Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention, its composition is by mass percentage: 80%WC, 5%Ti (C, N), 14%Co, 0.3%VC, 0.7%Cr
3c
2its metallographic structure is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 15 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.32 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.4 times of Wimet nominal cobalt contents, not containing Emission in Cubic carbonitride in the gradient layer of rich surface cobalt.
The preparation method of the Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention carries out according to following steps:
(1) adopt the hard alloy material adding carbonitride to prepare burden, its composition range is by mass percentage: 80%WC, 5%Ti (C, N), 14%Co, 0.3%VC, 0.7%Cr
3c
2, the mean particle size of the WC powder of wherein adding is 0.4 μm, and the mean particle size of Ti (C, N) powder is 1.5 μm, and the mean particle size of matrix metal Co powder is 1 μm, grain inhibitor VC and Cr
3c
2the mean particle size of powder is less than 1 μm;
(2) wet-milling in wet-type ball mill is added after being mixed by above-mentioned raw materials, ratio of grinding media to material is 12:1, wet grinding media is alcohol, and rotating speed is 60r/min, and the wet-milling time is 60h, mixed slurry after wet-milling is left standstill 10h, then put into vacuum drying oven in 60 DEG C of insulation 2h, sieves with 40 eye mesh screens after dry, the powder press after sieving and mould are pressed into material base, pressure is 20 tons, and the dwell time is 5s;
(3) material base is placed in vacuum oven, vacuum oven is evacuated down to below 10Pa to start to heat up, be warming up to 400 DEG C and be incubated 6h, pass into hydrogen simultaneously, carry out dewaxing, deoxidation, hydrogen afterwards in emptying furnace chamber continues to heat up, the argon gas of charged pressure 9MPa before reaching liquid phase sintering conditions 1400 DEG C, and be incubated 1h, room temperature is cooled to the furnace after insulation terminates, obtain the Ultra-fine Grained gradient hard alloy that rich surface cobalt thickness is about 15 μm, WC grain average grain size is about 0.33 μm, and the hardness of Wimet is about
hV 30 1780, bending strength is about 2400 MPa, and as shown in Figure 1, crystallite size analysis chart as shown in Figure 2 for its metallographic structure figure.
Embodiment 2
The Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention, its composition is by mass percentage: 77.2%WC, 6%Ti (C, N), 15%Co, 0.5%VC, 0.8%Cr
3c
2, 0.5% carbon black, its metallographic structure is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 20 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.33 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.3 times of Wimet nominal cobalt contents, not containing Emission in Cubic carbonitride in the gradient layer of rich surface cobalt.
The preparation method of the Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention carries out according to following steps:
(1) adopt the hard alloy material adding carbonitride to prepare burden, its composition range is by mass percentage: 77.2%WC, 6%Ti (C, N), 15%Co, 0.5%VC, 0.8%Cr
3c
2, 0.5% carbon black, the mean particle size of the WC powder of wherein adding is 0.4 μm, and the mean particle size of Ti (C, N) powder is 0.2 μm, and the mean particle size of matrix metal Co powder is 1 μm, grain inhibitor VC and Cr
3c
2the mean particle size of powder is less than 1 μm;
(2) wet-milling in wet-type ball mill is added after being mixed by above-mentioned raw materials, ratio of grinding media to material is 10:1, wet grinding media is alcohol, and rotating speed is 70r/min, and the wet-milling time is 48h, mixed slurry after wet-milling is left standstill 8h, then put into vacuum drying oven in 90 DEG C of insulation 1h, sieves with 40 eye mesh screens after dry, the powder press after sieving and mould are pressed into material base, pressure is 5 tons, and the dwell time is 30s;
(3) material base is placed in vacuum oven, vacuum oven is evacuated down to below 10Pa to start to heat up, be warming up to 500 DEG C and be incubated 4h, pass into hydrogen simultaneously, carry out dewaxing, deoxidation, hydrogen afterwards in emptying furnace chamber continues to heat up, the argon gas of charged pressure 5MPa before reaching liquid phase sintering conditions 1350 DEG C, and be incubated 2h, room temperature is cooled to the furnace after insulation terminates, obtain the Ultra-fine Grained gradient hard alloy that rich surface cobalt thickness is about 20 μm, WC grain average grain size is about 0.33 μm, and the hardness of Wimet is about
hV 30 1800, bending strength is about 2600MPa, and as shown in Figure 3, crystallite size analysis chart as shown in Figure 4 for the metallographic structure figure of its correspondence.
Embodiment 3
The Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention, its composition is by mass percentage: 91.5%WC, 2%Ti (C, N), 6%Co, 0.2%Cr
3c
2, 0.3% carbon black, its metallographic structure is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 40 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.28 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.5 times of Wimet nominal cobalt contents, not containing Emission in Cubic carbonitride in the gradient layer of rich surface cobalt.
The preparation method of the Ultra-fine Grained gradient hard alloy of rich surface cobalt of the present invention carries out according to following steps:
(1) adopt the hard alloy material adding carbonitride to prepare burden, its composition range is by mass percentage: 91.5%WC, 2%Ti (C, N), 6%Co, 0.2%Cr
3c
2, 0.3% carbon black, the mean particle size of the WC powder of wherein adding is 0.4 μm, and the mean particle size of Ti (C, N) powder is 0.2 μm, and the mean particle size of matrix metal Co powder is 1 μm, grain inhibitor Cr
3c
2the mean particle size of powder is less than 1 μm;
(2) wet-milling in wet-type ball mill is added after being mixed by above-mentioned raw materials, ratio of grinding media to material is 15:1, wet grinding media is alcohol, and rotating speed is 80r/min, and the wet-milling time is 72h, mixed slurry after wet-milling is left standstill 12h, then put into vacuum drying oven in 80 DEG C of insulation 1.5h, sieves with 40 eye mesh screens after dry, the powder press after sieving and mould are pressed into material base, pressure is 10 tons, and the dwell time is 15s;
(3) material base is placed in vacuum oven, vacuum oven is evacuated down to below 10Pa to start to heat up, be warming up to 600 DEG C and be incubated 1h, pass into hydrogen simultaneously, carry out dewaxing, deoxidation, hydrogen afterwards in emptying furnace chamber continues to heat up, the argon gas of charged pressure 10MPa before reaching liquid phase sintering conditions 1500 DEG C, and be incubated 0.1h, room temperature is cooled to the furnace after insulation terminates, obtain the Ultra-fine Grained gradient hard alloy that rich surface cobalt thickness is about 40 μm, WC grain average grain size is about 0.28 μm, and the hardness of Wimet is about
hV 30 1830, bending strength is about 2800MPa, and as shown in Figure 5, crystallite size analysis chart as shown in Figure 6 for corresponding metallographic structure figure.
Claims (3)
1. a preparation method for the Ultra-fine Grained gradient hard alloy of rich surface cobalt, is characterized in that carrying out according to following steps:
(1) adopt the hard alloy material adding carbonitride to prepare burden, its composition is by mass percentage: 2-6%Ti (C, N), 6-15%Co, 0-0.5%VC, 0.2-0.8%Cr
3c
2with 0-0.5% carbon black, surplus is WC; The mean particle size of described WC powder is 0.4 μm, and the mean particle size of Ti (C, N) powder is 0.2 ~ 1.5 μm, and the atomic ratio of C and N is the mean particle size of 0.5:0.5, Co powder is 1 μm, VC and Cr
3c
2the mean particle size of powder is less than 1 μm;
(2) wet-milling in wet-type ball mill is added after being mixed by above-mentioned raw materials, mixed slurry after wet-milling is left standstill 8 ~ 12h, then vacuum drying oven is put in 60 ~ 90 DEG C of insulation 1 ~ 2h, sieve with 40 eye mesh screens after dry, powder press after sieving and mould are pressed into material base, pressure is 5 ~ 20 tons, and the dwell time is 5 ~ 30s;
(3) material base is placed in vacuum oven, vacuum oven is evacuated down to below 10Pa to start to heat up, be warming up to 400 ~ 600 DEG C and be incubated 1 ~ 6h, pass into hydrogen simultaneously, dewax, deoxidation, hydrogen afterwards in emptying furnace chamber continues to heat up, the rare gas element of charged pressure 5 ~ 10MPa before reaching liquid phase sintering conditions, liquid phase sintering conditions is 1350 ~ 1500 DEG C, 0.1 ~ 2h is incubated under inert gas pressure, room temperature is cooled to the furnace after insulation terminates, obtain the Ultra-fine Grained gradient hard alloy of rich surface cobalt, its metallographic structure is for core hard phase with WC and Emission in Cubic carbonitride, take cobalt as the gradient layer that Binder Phase forms 10 ~ 40 μm of thick rich surface cobalts, wherein in hard phase and gradient layer, the mean sizes of WC grain is 0.2-0.4 μm, cobalt contents in the gradient layer of rich surface cobalt is 1.2-2 times of Wimet nominal cobalt contents.
2. the preparation method of a kind of Ultra-fine Grained gradient hard alloy of rich surface cobalt according to claim 1, when it is characterized in that step (2) carries out wet-milling, ratio of grinding media to material is (10 ~ 15): 1, and wet grinding media is alcohol, rotating speed is (40 ~ 100) r/min, and the wet-milling time is 48 ~ 72h.
3. the preparation method of a kind of Ultra-fine Grained gradient hard alloy of rich surface cobalt according to claim 1, is characterized in that described rare gas element is argon gas.
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| CN105149591A (en) * | 2015-09-21 | 2015-12-16 | 安庆创跃电器有限公司 | Composite alloy blade production process |
| CN106048360B (en) * | 2016-07-11 | 2018-03-27 | 中南大学 | A kind of surface has hard alloy of double-deck gradient-structure and preparation method thereof |
| CN106566972B (en) * | 2016-11-10 | 2018-03-02 | 南京航空航天大学 | The preparation method of plate-like shape WC grains hard alloy with gradient-structure |
| CN107419151B (en) * | 2017-08-17 | 2019-01-04 | 东北大学 | Nanocrystalline gradient hard alloy of a kind of high rigidity surface layer richness WC and preparation method thereof |
| CN108274005B (en) * | 2018-02-08 | 2019-09-13 | 合肥工业大学 | A method of low cobalt, ultra-fine cemented carbide bar are prepared with nanometer WC-Co composite powder |
| CN109161711B (en) * | 2018-10-11 | 2020-09-01 | 郑州轻工业学院 | Superfine crystal gradient hard alloy with double-gradient-layer structure on surface and preparation method thereof |
| CN110306092A (en) * | 2019-08-13 | 2019-10-08 | 广东工业大学 | A kind of Graded-structure Cemented Carbides and its preparation method and application |
| CN112251658B (en) * | 2020-10-22 | 2021-11-26 | 常州润睿特种合金有限公司 | Ultrafine grain gradient hard alloy and preparation method and application method thereof |
| CN112846259B (en) * | 2021-01-05 | 2022-09-30 | 崇义章源钨业股份有限公司 | Cutter for steel turning and preparation method thereof |
| CN113444951A (en) * | 2021-03-19 | 2021-09-28 | 株洲力洲硬质合金有限公司 | Ultrafine grain gradient hard alloy and preparation method thereof |
| CN115725884B (en) * | 2021-08-30 | 2023-12-22 | 四川大学 | Gradient structure high cobalt YG hard alloy for forming die and preparation method |
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Application publication date: 20140423 Assignee: Shenyang ruiyide Coating Technology Co.,Ltd. Assignor: Northeastern University Contract record no.: X2023210000027 Denomination of invention: A Superfine Grain Gradient Cemented Carbide with Cobalt Rich Surface and Its Preparation Method Granted publication date: 20151104 License type: Common License Record date: 20230417 |