CN103866217A - Sub-zero treatment method for improving mechanical property of WC-Co (Wolfram Carbide) hard alloy - Google Patents

Sub-zero treatment method for improving mechanical property of WC-Co (Wolfram Carbide) hard alloy Download PDF

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CN103866217A
CN103866217A CN201410053649.XA CN201410053649A CN103866217A CN 103866217 A CN103866217 A CN 103866217A CN 201410053649 A CN201410053649 A CN 201410053649A CN 103866217 A CN103866217 A CN 103866217A
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wimet
hard alloy
liquid nitrogen
room temperature
vacuum
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CN103866217B (en
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陈礼清
张贺佳
孙静
王全兆
王文广
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Northeastern University China
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Abstract

The invention provides a sub-zero treatment method for improving mechanical property of WC-Co (Wolfram Carbide) hard alloy, and belongs to the technical field of materials. The method comprises the following steps of: (1) treating the WC-Co hard alloy by vacuum hardening, and taking out under room temperature; (2) treating the hardened WC-Co hard alloy by vacuum tempering; (3) wrapping the WC-Co hard alloy subjected to vacuum tempering, then transferring into a programmable sub-zero treatment box, cooling with liquid nitrogen as a refrigerant until the temperature reaches -196 DEG C, and maintaining the temperature for 10 to 25min; and (4) transferring the WC-Co hard alloy into a vessel containing liquid nitrogen within 2 minutes, maintaining temperature for 24 to 72 hours, and then taking out and recovering to room temperature. The method has the advantages that the final metallographic structure comprises WC particles, the second phase particles of a Co phase of a binding phase, the Co of an fcc (Face Center Cubic) crystal structure and the Co of a hcp (Hexagonal Close Packed) crystal structure; residual pressure stress is produced between WC particles and the surface of the hard alloy, which greatly improves the hardness, flexible strength and wear-resisting performance of the hard alloy; and the consumption of programmable equipment, the power consumption, and the dose of liquid nitrogen are also greatly reduced.

Description

A kind of cryogenic treating process that improves WC-Co Wimet mechanical property
Technical field
The invention belongs to material technology field, particularly a kind of cryogenic treating process that improves WC-Co Wimet mechanical property.
Background technology
Metal cutting technology and cutter, as gordian technique and basic equipment, are determining efficiency, precision, quality and the cost of machine tooling.Wimet is the tool material of being made up through powder metallurgy process of refractory metal compound and metal cakingagent, with its good performance more occasion substitute other cutter material.
Cemented Carbide Hardness, far above rapid steel, and has that high-flexural strength, chemical stability are good, thermotolerance advantages of higher; Lathe tools more than 90 % of developed country and milling cutters more than 55 % all adopt Hardmetal materials, and proportion is still increasing; Wimet is also used for manufacturing drill bit, end mill etc. in addition; As in the hard flank of tooth of processing, the complex cutting tool such as large module gear cutter and reamer, slotting cutter, broaching tool is also increasing.At present, inserted tool has occupied the dominant position in cutter market in the world, and proportion is up to 70 %, and the inserted tool ratio of China is relatively low.
China produces 1.6 ten thousand tons, Wimet at present per year, accounts for 40% left and right of global ultimate production.But the cutting tip output that hard metal article added value is the highest only has more than 3,000 tons, only account for 20%; According to the statistics of machine tool TIA of China, China's import inserted tool in 2010, account for 10,000,000,000 yuan, these import cutters have entered the high-end manufacture field of the key industrys such as China's aerospace, automobile and motorcycle, track traffic, electricity power, mould manufacture mostly.
China's Wimet high-end product is very few, and the technology stability of product and the stability of product are poor, and the Mineral resources of every ten thousand yuan of output values and energy-output ratio are 5 ~ 10 times of similar enterprise of developed country, and this present situation has caused the great attention of the Chinese government; Therefore, Hardmetal materials has been put into national new material industry " 12 " development program.
Along with the development of processing industry, modern cutter material is towards high precision, high speed cutting, DRY CUTTING and the future development such as reduce costs.In high-speed machining process, because cutter is bearing larger pressure and violent rubbing effect, cutter Fast Wearing is the main failure forms of cutter; Change frequently cutter, greatly reduce production efficiency, also increased production cost simultaneously.
The method of improving at present Cemented Carbide Properties mainly contains three directions: grain refining, coated carbides, interpolation rare metal and interpolation rare earth element; Although these methods have obtained certain research achievement, all have defect in various degree, and preparation technology's deficiency also limits the actual of novel hard alloy cutter material and has applied.
1) grain refining: only have at present minority enterprise can produce the Wimet of Ultra-fine Grained rank in batches, and it is very few especially to produce the enterprise of Nanograin Cemented Carbide in batches; Because cutter material Grain Refinement is still not mature enough, sintering process nanocrystal very easily grows into coarse grain, causes the strength of materials, hardness and abrasion resistance properties to decline, on the other hand, the price of the thinner Wimet of crystal grain is more expensive, makes to a certain extent it apply and is restricted.
2) coated carbides: cutter coat technique is still take chemical vapour deposition (CVD) and physical vapor deposition (PVD) as main.These two kinds of method comparison distinct issues are that the bonding strength between coating and matrix is low, and coating is easily peeled off, so coating can not be too thick, once and coating be worn away, cutter will rapid wearing; Current technology still fails fundamentally to solve carbide matrix material toughness and the poor problem of shock resistance.
3) add rare earth element: the interpolation of rare earth element can improve the microtexture of Wimet and improve its mechanical property, but due to the difference of addition manner, form, kind and quantity and the difference of research means, each research conclusion is different, the mechanism proposing is also variant, even conflicting.
Summary of the invention
Improve the problems referred to above that exist technically for existing Cemented Carbide Properties, the invention provides a kind of cryogenic treating process of the WC-Co of raising Wimet mechanical property, by by the quenching of WC-Co hard alloy vacuum, tempering and sub-zero treatment, significantly improve hardness, flexural strength and the wear resistance of Wimet, can reduce greatly liquid nitrogen usage quantity simultaneously.
The cryogenic treating process of raising WC-Co Wimet mechanical property of the present invention carries out according to the following steps:
1, WC-Co Wimet is carried out to vacuum hardening processing, vacuum tightness is 10 -1~ 10 -2pa, quenching temperature is 1170 ~ 1230 ℃, and Quenching Soaking Time is 20 ~ 30min, and quenchant is room temperature quenching oil, in the time that WC-Co Wimet is chilled to room temperature, takes out;
2, the WC-Co Wimet after quenching is carried out to vacuum tempering processing, control vacuum tightness 10 -1~ 10 -2pa, tempering temperature is 550 ~ 600 ℃, tempering insulation time is 30 ~ 60 min, then, with the speed cool to room temperature of 10 ~ 30 ℃/min, completes vacuum tempering;
3, the WC-Co Wimet after vacuum tempering is placed in program control deep cooling box by cotton and plastic wraps, take liquid nitrogen as refrigeration agent, is cooled to-196 ℃ with the cooling rate of 4 ~ 8 ℃/min, insulation 10 ~ 25min;
4, WC-Co Wimet in program control deep cooling box is taken out, then in the time of≤2min, be placed in the container that liquid nitrogen is housed, WC-Co Wimet is immersed in liquid nitrogen, insulation 24 ~ 72h, then takes out nature and returns to room temperature, completes sub-zero treatment.
In above-mentioned step 2, be with the speed cool to room temperature of 10 ~ 30 ℃/min that nitrogen-blow carries out cooling.
In above-mentioned step 3, WC-Co Wimet finishes to be controlled in 0.5h to the time that is placed in program control deep cooling box from vacuum tempering.
What method of the present invention adopted according to principle is:
There are face-centered cubic (fcc) α-Co and two kinds of crystalline structure of close-packed hexagonal (hcp) ε-Co in the pure cobalt of metal, when high temperature, exists with fcc form, and room temperature almost all exists with hcp form; Fcc metal slip plane is many, and plasticity is good, but hardness is low yielding, and frictional coefficient is large; Hcp metal slip plane is few, and hardness height is not yielding, and frictional coefficient is little, has good abrasion resistance properties; The hardness of Wimet mainly determined by hard and crisp WC, and bending strength is main relevant with Binder Phase Co.But due to the pinning effect of a large amount of WC particle to Co phase in Wimet, and cooling rate control bad (as too fast in a certain temperature section cooling rate) in temperature-fall period after sintering, make Co in the process of cooling from high temperature to low temperature, hinder the transformation of Co phase, room temperature retains the Co phase of a large amount of fcc structures, has reduced abrasion resistance properties; Sub-zero treatment can further make the Co of remaining fcc structure change mutually hcp structure into, and can produce larger surface compress residual stresses, improves the abrasion resistance properties of material; But it is compact that sub-zero treatment will be connected with thermal treatment, the ageing effect while transformation to reduce Binder Phase Co.
Adopt quench hot, the thermal treatment process of short period of time insulation: can the relatively large foreign atom such as C and W of solid solution at condition of high temperature cobalt metal, short period of time insulation can make WC particle be unlikely to grow up fast; When quenching due to quick cooling a large amount of foreign atoms be retained in Co mutually in, cobalt also exists with fcc structure formation mutually in a large number; In temper subsequently, can make a large amount of foreign atom short-distance movements of cobalt in mutually separate out, form a large amount of Second Phase Particles, disperse be distributed in cobalt mutually in, hinder dislocation motion, play second-phase strengthening effect, improved the abrasion resistance properties of metal; Reduce the lattice distortion of Co phase and the generation of micro-flaw simultaneously, in the slow process of cooling after tempering, make the Co of part fcc structure change mutually hcp structure into, further improved again the abrasion resistance properties of metal.
Wimet after tempering is put into program control deep cooling box sub-zero treatment as early as possible, to produce ageing effect in order to prevent that Binder Phase α-Co from changing in ε-Co process, room temperature longer transformation amount storage period is fewer, is similar to residual austenite ageing effect after the quenching of ferrous materials; There is literature research to show that the phase transformation of Co is also martensitic transformation, but this martensitic transformation that found through experiments Co is different from again ferrous materials, sharply cooling (as quenched) from high temperature to low temperature suppresses on the contrary α-Co and changes ε-Co into, if stop as long-time in room temperature also there will be the ageing effect of similar ferrous materials residual austenite; In deep cooling process, adopt program control deep cooling box slow cooling, be because metal easily becomes fragile when the low-temperature condition, can reduce the detrimental effect of thermal shocking to Wimet; Too fast in order to prevent that Wimet from heating up before moving on in liquid nitrogen vessel from program control deep cooling box by cotton and plastic wraps one, the 2nd, even if there is higher intensification, the cold shock absorption that plays of play producing while contacting with liquid nitrogen in Wimet moves into liquid nitrogen vessel, reduces thermal shock damage; The deep cooling principle of program control deep cooling box is to spray liquid nitrogen toward being equipped with in the casing of Wimet from liquid nitrogen bottle, absorbs heat to maintain low temperature by the latent heat of vaporization and the low temperature nitrogen of liquid nitrogen, and liquid nitrogen can not reuse, larger if long-time insulation expends amount of liquid nitrogen; So the Wimet of low-temperature condition is moved on to deep cooling insulation in the container that liquid nitrogen is housed, can largely reduce the volatilization of liquid nitrogen, after Wimet is taken out from liquid nitrogen, in container, remain liquid nitrogen and also can continue to use; Liquid nitrogen consumption can greatly reduce, and more the about amount of liquid nitrogen of meropodium is more remarkable for soaking time; As be incubated 48h, 5% left and right that liquid nitrogen consumption is program control deep cooling box; But the deep cooling effect of Wimet is not only relevant with technique, but also with Wimet crystal grain rank, the factors such as Co content are relevant.
The final metallographic structure of method of the present invention is the Co of WC particle, Co Second Phase Particles, fcc crystalline structure Co and the hcp crystalline structure in mutually; Between WC particle, have generation residual compressive stress with carbide surface, this series of combination has greatly improved hardness, bending strength and the abrasion resistance properties of Wimet; Program-controlled equipment loss and current consumption are also greatly reduced; And liquid nitrogen is nontoxic, pollution-free to air, there is the effect of energy-conserving and environment-protective.
Accompanying drawing explanation
Fig. 1 is the XRD material phase analysis figure of the raw material WC-12Co Wimet of employing in the embodiment of the present invention 1;
Fig. 2 is the XRD material phase analysis figure of the WC-12Co Wimet after the sub-zero treatment in the embodiment of the present invention 1;
Fig. 3 is the XRD material phase analysis figure of the WC-12Co Wimet after the sub-zero treatment in the embodiment of the present invention 2;
Fig. 4 is the XRD material phase analysis figure of the WC-12Co Wimet after the sub-zero treatment in the embodiment of the present invention 3.
Embodiment
The vickers hardness hv value of the WC-12Co Wimet in the embodiment of the present invention after sub-zero treatment is 1738 ~ 1791, and flexural strength is 2557 ~ 2651MPa.
The WC-Co Wimet of selecting in the embodiment of the present invention is commercial WC-12Co carbide chip, and crystal grain rank is thin brilliant, and its actual measurement vickers hardness hv value is 1621, and flexural strength is 2036MPa.
In the embodiment of the present invention, WC-12Co Wimet is carried out before XRD material phase analysis needing WC particle in Wimet to carry out selective electrolysis corrosion, otherwise the diffraction peak of Binder Phase Co will be affected almost and can not occur by WC particle; The document of caustic solution reference adopting be " stone ring English. in Wimet, lack X-ray diffraction---the electrolysis selective corrosion WC method [J] of content phase cobalt. physical and chemical inspection (physics fascicle), 1994,30 (4): 35-36+55. ".
In the embodiment of the present invention, electrolytic corrosion equipment is Electromet4.
In the embodiment of the present invention, program control deep cooling box is SLX-80 time variable control deep cooling box.
In the embodiment of the present invention, X-ray diffractometer is D8 DISCVER X-ray diffractometer.
The equipment of testing Vickers' hardness employing in the embodiment of the present invention is the omnipotent sclerometer of KB3000BVRZ-SA.
In the embodiment of the present invention, test the equipment I nstron1343 microcomputer-controlled hydraulic servo universal material experiment-machine that flexural strength adopts.
In the embodiment of the present invention, tested for hardness experiment is carried out according to " GB/T 4340.1-2009 Vickers Hardness Test of Metallic Materials part 1: test method ", and the experiment of test flexural strength is carried out according to GB/T 232-2010 " bend test of metal materials method " three-point bending.
In the embodiment of the present invention, wear resistance experiment adopts turning 45 rod iron material, then measures knife face average abrasion value VB thereafter, cutting speed Vc=130m/ min, depth of cut a p=0.2mm, amount of feed f=0.15mm/r, the cutting time is 60min, the WC-12Co Wimet tool flank wear VB value of sub-zero treatment is not 0.67mm.
The quenching oil adopting in the embodiment of the present invention is commercial industrial quenching oil.
Embodiment 1
WC-Co Wimet is carried out to vacuum hardening processing, and vacuum tightness is 10 -1~ 10 -2pa, quenching temperature is 1230 ℃, and Quenching Soaking Time is 20min, and quenchant is room temperature quenching oil, in the time that WC-Co Wimet is chilled to room temperature, takes out;
WC-Co Wimet after quenching is carried out to vacuum tempering processing, control vacuum tightness 10 -1~ 10 -2pa, tempering temperature is 550 ℃, and tempering insulation time is 60min, and then nitrogen-blow carries out the cooling speed cool to room temperature of WC-Co Wimet with 10 ℃/min that make, and completes vacuum tempering;
By the WC-Co Wimet after vacuum tempering, first with cotton parcel, skin is used plastic wraps again, is then placed in program control deep cooling box, take liquid nitrogen as refrigeration agent, is cooled to-196 ℃ with the cooling rate of 8 ℃/min, insulation 25min; WC-Co Wimet finishes to be controlled in 0.5h to the time that is placed in program control deep cooling box from vacuum tempering;
WC-Co Wimet in program control deep cooling box is taken out, in the time in 2min, be placed in the container that liquid nitrogen is housed, WC-Co Wimet is immersed in liquid nitrogen, place insulation 24h, then take out nature and return to room temperature, complete sub-zero treatment;
Raw material WC-Co Wimet is through the laggard row XRD analysis of excessive erosion, and thing phasor as shown in Figure 1;
The vickers hardness hv value of WC-12Co Wimet after treatment is 1738, and flexural strength is 2557Mpa, and rear knife face average abrasion amount VB value is 0.42mm, and XRD material phase analysis figure as shown in Figure 2.
Embodiment 2
WC-Co Wimet is carried out to vacuum hardening processing, and vacuum tightness is 10 -1~ 10 -2pa, quenching temperature is 1200 ℃, and Quenching Soaking Time is 25min, and quenchant is room temperature quenching oil, in the time that WC-Co Wimet is chilled to room temperature, takes out;
WC-Co Wimet after quenching is carried out to vacuum tempering processing, control vacuum tightness 10 -1~ 10 -2pa, tempering temperature is 570 ℃, and tempering insulation time is 45min, and then nitrogen-blow carries out the cooling speed cool to room temperature of WC-Co Wimet with 20 ℃/min that make, and completes vacuum tempering;
By the WC-Co Wimet after vacuum tempering, first with cotton parcel, skin is used plastic wraps again, is then placed in program control deep cooling box, take liquid nitrogen as refrigeration agent, is cooled to-196 ℃ with the cooling rate of 6 ℃/min, insulation 17min; WC-Co Wimet finishes to be controlled in 0.5h to the time that is placed in program control deep cooling box from vacuum tempering;
WC-Co Wimet in program control deep cooling box is taken out, in the time in 2min, be placed in the container that liquid nitrogen is housed, WC-Co Wimet is immersed in liquid nitrogen, place insulation 72h, then take out nature and return to room temperature, complete sub-zero treatment;
The vickers hardness hv value of WC-12Co Wimet after treatment is 1791, and flexural strength is 2651Mpa, and rear knife face average abrasion amount VB value is 0.31mm, and XRD material phase analysis figure as shown in Figure 3.
Embodiment 3
WC-Co Wimet is carried out to vacuum hardening processing, and vacuum tightness is 10 -1~ 10 -2pa, quenching temperature is 1170 ℃, and Quenching Soaking Time is 30min, and quenchant is room temperature quenching oil, in the time that WC-Co Wimet is chilled to room temperature, takes out;
WC-Co Wimet after quenching is carried out to vacuum tempering processing, control vacuum tightness 10 -1~ 10 -2pa, tempering temperature is 600 ℃, and tempering insulation time is 30min, and then nitrogen-blow carries out the cooling speed cool to room temperature of WC-Co Wimet with 30 ℃/min that make, and completes vacuum tempering;
By the WC-Co Wimet after vacuum tempering, first with cotton parcel, skin is used plastic wraps again, is then placed in program control deep cooling box, take liquid nitrogen as refrigeration agent, is cooled to-196 ℃ with the cooling rate of 4 ℃/min, insulation 10min; WC-Co Wimet finishes to be controlled in 0.5h to the time that is placed in program control deep cooling box from vacuum tempering;
WC-Co Wimet in program control deep cooling box is taken out, in the time in 2min, be placed in the container that liquid nitrogen is housed, WC-Co Wimet is immersed in liquid nitrogen, place insulation 48h, then take out nature and return to room temperature, complete sub-zero treatment;
The vickers hardness hv value of WC-12Co Wimet after treatment is 1784, and flexural strength is 2629Mpa, and rear knife face average abrasion amount VB value is 0.34mm, and XRD material phase analysis figure as shown in Figure 4;
WC-12Co Wimet, directly carries out sub-zero treatment by room temperature, and without high-temperature heat treatment process, the hardness of the product obtaining, flexural strength, abrasion resistance properties are all starkly lower than above-mentioned technique; XRD material phase analysis shows that ε-Co content only has subtle change compared with raw material.

Claims (3)

1. improve a cryogenic treating process for WC-Co Wimet mechanical property, it is characterized in that carrying out according to the following steps:
(1) WC-Co Wimet is carried out to vacuum hardening processing, vacuum tightness is 10 -1~ 10 -2pa, quenching temperature is 1170 ~ 1230 ℃, and Quenching Soaking Time is 20 ~ 30min, and quenchant is room temperature quenching oil, in the time that WC-Co Wimet is chilled to room temperature, takes out;
(2) the WC-Co Wimet after quenching is carried out to vacuum tempering processing, control vacuum tightness 10 -1~ 10 -2pa, tempering temperature is 550 ~ 600 ℃, tempering insulation time is 30 ~ 60 min, then, with the speed cool to room temperature of 10 ~ 30 ℃/min, completes vacuum tempering;
(3) the WC-Co Wimet after vacuum tempering is placed in program control deep cooling box by cotton and plastic wraps, take liquid nitrogen as refrigeration agent, is cooled to-196 ℃ with the cooling rate of 4 ~ 8 ℃/min, insulation 10 ~ 25min;
(4) WC-Co Wimet in program control deep cooling box is taken out, then in the time of≤2min, be placed in the container that liquid nitrogen is housed, WC-Co Wimet is immersed in liquid nitrogen, insulation 24 ~ 72h, then takes out nature and returns to room temperature, completes sub-zero treatment.
2. a kind of cryogenic treating process that improves WC-Co Wimet mechanical property according to claim 1, is characterized in that in described step (2), is that nitrogen-blow carries out cooling with the speed cool to room temperature of 10 ~ 30 ℃/min.
3. a kind of cryogenic treating process that improves WC-Co Wimet mechanical property according to claim 1, it is characterized in that in described step (3), WC-Co Wimet finishes to be controlled in 0.5h to the time that is placed in program control deep cooling box from vacuum tempering.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106914624A (en) * 2017-01-22 2017-07-04 苏州新锐合金工具股份有限公司 A kind of method for reducing hard alloy coefficient of friction
CN107937784A (en) * 2017-12-08 2018-04-20 吉林大学 A kind of cryogenic treating process of diamond composite
CN108034796A (en) * 2017-12-06 2018-05-15 中国兵器工业第五九研究所 A kind of high rigidity curved-surface structure mould accurate manufacture process
CN109795042A (en) * 2019-03-12 2019-05-24 吉林农业科技学院 A kind of tooling and crystal-cut component for crystal-cut
CN112301207A (en) * 2020-10-27 2021-02-02 蚌埠市利锋五金制品有限公司 Vacuum oil quenching heat treatment method for cutter
CN112496443A (en) * 2020-11-19 2021-03-16 中国航发沈阳黎明航空发动机有限责任公司 Alloy machine clamp combined broach and manufacturing method thereof
CN113134610A (en) * 2021-04-25 2021-07-20 四川德克普数控机床有限公司 Manufacturing method of rough skin milling cutter and five-axis numerical control grinding machine thereof

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CN1250751C (en) * 2002-09-13 2006-04-12 胡明 Bimetal saw band and hard alloy ultra-low temp. treatment process
CN103352112A (en) * 2013-07-12 2013-10-16 上海汇众汽车车桥系统有限公司 Cryogenic process for prolonging service life of jet-moulded high-speed steel milling cutter

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1250751C (en) * 2002-09-13 2006-04-12 胡明 Bimetal saw band and hard alloy ultra-low temp. treatment process
CN103352112A (en) * 2013-07-12 2013-10-16 上海汇众汽车车桥系统有限公司 Cryogenic process for prolonging service life of jet-moulded high-speed steel milling cutter

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106914624A (en) * 2017-01-22 2017-07-04 苏州新锐合金工具股份有限公司 A kind of method for reducing hard alloy coefficient of friction
CN106914624B (en) * 2017-01-22 2019-08-20 苏州新锐合金工具股份有限公司 A method of reducing hard alloy coefficient of friction
CN108034796A (en) * 2017-12-06 2018-05-15 中国兵器工业第五九研究所 A kind of high rigidity curved-surface structure mould accurate manufacture process
CN107937784A (en) * 2017-12-08 2018-04-20 吉林大学 A kind of cryogenic treating process of diamond composite
CN109795042A (en) * 2019-03-12 2019-05-24 吉林农业科技学院 A kind of tooling and crystal-cut component for crystal-cut
CN112301207A (en) * 2020-10-27 2021-02-02 蚌埠市利锋五金制品有限公司 Vacuum oil quenching heat treatment method for cutter
CN112496443A (en) * 2020-11-19 2021-03-16 中国航发沈阳黎明航空发动机有限责任公司 Alloy machine clamp combined broach and manufacturing method thereof
CN113134610A (en) * 2021-04-25 2021-07-20 四川德克普数控机床有限公司 Manufacturing method of rough skin milling cutter and five-axis numerical control grinding machine thereof

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