CN102517483B - Industrial production method for synthesizing cemented carbide block material in situ - Google Patents
Industrial production method for synthesizing cemented carbide block material in situ Download PDFInfo
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Abstract
The invention discloses an industrial production method for synthesizing a cemented carbide block material in situ, belonging to the technical field of cemented carbide. The industrial production method comprises the steps of: utilizing WO 2.9, Co3O4 and carbon black as raw materials, calculating a dosage ratio of the three raw materials by considering the evaporation capacity and wastage of Co and carbon wastage caused by carrying powder in an oxidizing gas during the preparation process according to the demand of a final Co content, ball grinding the raw materials to mix the same, and calculating the mass of the necessary raw material powder according to the material mass reduction and the sintering wastage coefficient k of the WC and Co powder during the sintering process; and utilizing the low sintering pressure at the primary application stage of a hot press sintering technique, a vacuum sintering technique or a low pressure sintering technique, periodically maintaining the temperature and periodically increasing the pressure to obtain the cemented carbide block material. The industrial production method of the invention has the advantages of simple technique steps, short process, energy saving and environmental friendly properties, and capability of realizing the large scale industrial production of the cemented carbide.
Description
Technical field
The invention belongs to the Wimet technical field, be specifically related to a kind of Wimet block material original position synthetic technology that is suitable for suitability for industrialized production.
Background technology
At present, Wimet block preparation methods the most commonly used is in the industrial production: with the reduction of tungsten oxide process and long high temperature cabonization Processing of Preparation WC powder; Cobalt/cobalt oxide powder is reduced Processing of Preparation go out the Co powder; And then two kinds of powder are carried out ball milling mix, compression moulding behind the adding binder; In agglomerating plant, carry out sintering densification at last and prepare the block Hardmetal materials.Yet, shortcoming such as this method exists operation many (at least five road master operations), long flow path (more than at least seven days), is easy to introduce impurity, energy-output ratio is big.
Zhang Jiuxing etc. proposed based on the synthetic method for preparing the WC-Co Wimet of discharge plasma sintering technique (Zhang Jiuxing, Wang Che, Zhang Guozhen, Zhong Taoxing, the plasma discharging original position is synthesized WC Wimet method, grant number ZL 200410003442.8; Zhang Jiuxing, Wang Che, Zhang Guozhen, Song Xiaoyan, Zhou Meiling, WC-Co Wimet in-situ synthetic method, publication number 200510105685, yet, present discharging plasma sintering equipment quantity both domestic and external is also very limited, and it is expensive, of paramount importance is that discharge plasma sintering technique still is in development at present, present stage can only be used for the preparation of small size sample in the laboratory scope, produce the also very big difficulty of existence in batches, and its sintering mechanism and the sintering technology of using always, as vacuum sintering, low pressure sintering, there is the essence difference in hot pressed sinterings etc., still can't promote the use of the preparation of industrialization scale.
Summary of the invention
The object of the present invention is to provide the synthetic industrialized preparing process of a kind of Wimet block material original position, solve complex process, long flow path, energy-intensive problem in the present hard carbide industry production.The present invention is raw material with tungsten oxide, cobalt/cobalt oxide and carbon black, requirement according to Co content in the final Wimet block material, steam output, waste and the powder of Co are brought the waste that oxidizing gas causes carbon in the consideration preparation process, calculate the amount ratio of above-mentioned three kinds of raw materials, and then utilize ball mill that raw material is carried out mixing and ball milling and handle; Specification of quality and sintering loss according to sintered specimen, calculate the quality of mixed powder, in sintering oven, carry out in-situ reducing carbonization and sintering densification after being filled into model, the innovative technology route of low sintering pressure of application initial stage and interim insulation, interim pressure boost, final to obtain fine and close, phase composite be WC and Co pure substance WC-Co Wimet block material mutually.The technological line that the present invention prepares WC-Co Wimet block material had both had outstanding advantages such as processing step is simple, flow process weak point, energy-conserving and environment-protective, can realize the large-scale industrialization production of Wimet again.Therefore, the present invention all has important practical value to scientific research and the technology industrialization in Wimet field.
The in-situ synthetic method that is suitable for the short flow process Wimet block material of commercial scale production provided by the invention may further comprise the steps:
(1) with WO
2.9, Co
3O
4With carbon black be raw material, reduction waste according to evaporation, waste and the C of Co in the requirement for preparing material C o content, the preparation process, calculate above-mentioned three kinds of raw material amount ratios, the mass percent of supposing Co is n% (n=6-20), the evaporation of Co amount and the loss that is pressed into mould are m% (m=0-3.0), the loss of carbon amount is p% (p=0-0.5), the mass ratio of three kinds of raw materials then is 1.18 (100-n-nm%): 1.36n (1+m%): (25.60-0.23n (1+m%)) (1+p%) carries out ball milling with raw material and mixes.
(2) specification of quality of the final blank of basis, consider mixed powder generation reduction and carbonization reaction in the sintering process, discharge gas and cause the minimizing of quality of materials and the sintering loss factor k (k=1.0-1.2) of powder, calculate the desired raw material powder quality, sample mass and raw material powder mass ratio are 1 behind the sintering: 1.35k (100-n-nm%) %.
(3) hot-pressing sintering technique is: a certain amount of mixed powder is put into mould, is that 10-50 ℃/min rises to 350-400 ℃ with the temperature rise rate, is incubated 0.5-1 hour, and pressure is 10-30MPa; Be warming up to 750-1000 ℃ then, be incubated 2-3 hour; Be warming up to 1200-1500 ℃ and increase sintering pressure to 30-80MPa, heat-insulation pressure keeping 30-90 minute with the temperature rise rate of 5-10 ℃/min again; At last, pressurize is cooled to below 1150 ℃, removes pressure, cool to room temperature.
Vacuum sintering technology is: after a certain amount of mixed powder is put into mould and colded pressing, mould and pressed compact are put into vacuum oven together, be warming up to 350-400 ℃ of insulation 0.5-1 hour, the speed with 5-10 ℃/min is warming up to 750-1000 ℃ then, is incubated 2-3 hour; Be warming up to 1300-1500 ℃ of insulation 1-5 hour again, cool to room temperature at last with the furnace.
Low pressure sintering technology is: be warming up to 350-400 ℃ of insulation 0.5-1 hour; Speed with 5-10 ℃/min is warming up to 750-1000 ℃ of insulation 2-3 hour then; Speed with 3-10 ℃/min is warming up to 1310-1470 ℃ subsequently, behind the insulation 20-40min, charges into 2-5MPa nitrogen or argon gas, heat-insulation pressure keeping 20-40min; Cool to room temperature at last with the furnace.
During hot-pressing sintering technique, the span of parameter m, p, k is: m=1.0-3.0, p=0-0.3, k=1.0-1.2.
During vacuum sintering technology, the span of parameter m, p, k: m=0-0.8, p=0-0.2, k=1.0-1.1.
During low pressure sintering technology, the span of parameter m, p, k: m=1.0-2.5, p=0.2-0.5, k=1.0-1.2.
The present invention is to be raw material with metal oxide and carbon black, and the preparation of industrialization technological line of the Wimet block material that the original position synthetics is mutually pure, fine and close is compared with existing Wimet preparation method, and the present invention has following advantage:
(1) the present invention compares with existing Wimet block material industry preparation method, on the basis that not increase equipment drops into, make preparation section be reduced to original 1/4th to 1/7th, flow process foreshortens to original 20-40%, simultaneously, can reduce the introducing of impurity in the production process, be beneficial to that acquisition is mutually pure, the Wimet of excellent property.
(2) the present invention prepares Wimet block material by the reaction in one-step synthesis, the effectively discharging of waste gas and waste liquid in the existing Wimet preparation process of minimizing, characteristics with flow process weak point, less energy consumption, energy-conserving and environment-protective, especially technical parameter controllability of the present invention is strong, the performance of the Wimet block material of adjustable final preparation;
(3) the present invention has taken into full account the evaporation of cobalt in the requirement of cobalt contents and the preparation process and the loss of loss and carbon, by accurate Theoretical Calculation, guarantees in the raw material reasonably Co content and carbon content; Calculate according to the Gibbs free energy of oxide compound and carbon reaction process, but the design optimization sintering process parameter is guaranteed abundant reduction and the carbonization of oxide powder, adopt lower pressure or do not pressurize in this stage, guarantee that the gas that reaction produces discharges smoothly; Under sintering temperature, be incubated at last, guarantee further reacting completely and reacting the sintering densification of back powder of unreacted powder, finally obtain the mutually pure and high Wimet block material of density of thing.
(4) the present invention compares with the patent " a kind of simple preparation method of superfine WC-Co composite powder (ZL 200610165554.2) fast " that this seminar prepares powder, exists essence different at preparation object, technological step with technical process.At first, existing patent is a kind of method for preparing powdered material, and the present invention is a kind of method for preparing block materials; Secondly, there is key difference in the material composition proportioning.The vacuum heat treatment temperature of existing powder process patent (ZL 200610165554.2) pulverizing process is relatively low, preparation process is not used mould, and the weight to final preparation powder is less demanding, therefore only need to determine according to the Co content of preparation powder ratio and the mixed carbon comtent of oxide compound, guarantee that the purity of phase gets final product.And the objective of the invention is to prepare the block materials that satisfies performance and dimensional requirement, except considering to prepare the Co content of powder, must be determined by experiment the evaporation of Co under the loss of Co in the preparation process and the high temperature, the loss of carbon, and the powder loss is to the influence of specimen size, with this ratio and mixed carbon comtent of determining oxide compound, could guarantee to obtain the mutually pure and qualified sample of size; At last, existing powder process patent (ZL 200610165554.2) is to prepare superfine WC-Co composite powder by vacuum heat treatment, must guarantee that in heat treatment process powdered reaction is complete, if the composite powder with this prepared is that the raw material sintering prepares the Wimet block, needing to increase ball-milling technology further mixes powder, and have only the densification process of WC and Co powder in the sintering process, there is not the reaction in process; The present invention is to be the new technology that the raw material one-step synthesis is prepared Wimet block material with the tungsten cobalt/cobalt oxide powder, reduction and carbonization and densification process carry out synchronously, can prepare traditional coarse-grain, thin crystalline substance and ultra-fine cemented carbide block materials respectively by the processing of oxide powder and the control of sintering process.This shows that the oxide compound reduction and carbonization of present technique and sintering process are intersected and carried out, and have reduced the introducing of impurity and have shortened technological process, guarantee the mutually pure and high-compactness of the Wimet block material for preparing.
(5) the present invention and discharge plasma sintering in-situ preparing technology (patent ZL 200410003442.8 and 200510105685) contrast has the essence difference.At first, on preparating mechanism, discharge plasma sintering is that the direct current pulse power source with pressure and high current low voltage directly is added on push-down head and the mould, powder self produced joule heating when electric current passed through, under the acting in conjunction in electric field, magnetic field, prepare Wimet block material by reaction sintering, and, because the surface action of electric current and the difference of material and mould electroconductibility, may cause the sample temperature inside inhomogeneous, and then cause its tissue and performance inhomogeneous; Secondly, discharge plasma sintering method only limits to the preparation of small size sample in the laboratory scope at present; And the present invention carries out at suitability for industrialized production equipment; the heat of powder derives from the heating original paper of equipment fully; reaction in the sintering process and sintering densification process are determined by sintering temperature substantially; therefore; original position building-up process of the present invention is easy to control, and especially technology itself can be used for the industrially scalable production of different size sample.
Description of drawings
The performance of the Wimet block material of table 1 the present invention preparation;
The XRD figure of the WC-6wt.%Co Wimet block material of preparation spectrum and stereoscan photograph among Fig. 1 embodiment 1;
XRD figure spectrum and the stereoscan photograph of the WC-10wt.%Co Wimet block material of Fig. 2 embodiment 2 preparations;
XRD figure spectrum and the stereoscan photograph of the WC-15wt.%Co Wimet block material of Fig. 3 embodiment 3 preparations;
The pattern photo of the WC-10wt.%Co cemented carbide powder of the metallographic structure photo of the WC-10wt.%Co Wimet block material of the present invention's preparation and ZL 200610165554.2 preparations among Fig. 4 comparative example 4;
The pattern photo of the WC-16wt.%Co cemented carbide powder of the fracture scanned photograph of the WC-16wt.%Co Wimet block material of the present invention's preparation and ZL 200610165554.2 preparations among Fig. 5 comparative example 5;
Adopt among Fig. 6 comparative example 6 the WC-6wt.%Co Wimet block material structure of the technology of the present invention preparation and hardness test position synoptic diagram, along sample axially and the regional sem photograph of Hardness Distribution radially, O point and A point;
Adopt the sem photograph in axial and hardness distribution radially, O point and the A point zone of the WC-6wt.%Co Wimet block material of ZL 200410003442.8 technology preparation among Fig. 7 comparative example 6.
Embodiment
Following examples have further been explained the present invention, but the present invention is not limited to following examples.
Among all embodiment all with WO
2.9, Co
3O
4With carbon black be raw material.Initial WO
2.9The median size of powder is about 40 microns, and purity is 99.5wt% (containing tungsten company limited by sea, Ganzhou produces), Co
3O
4The median size of powder is about 25 microns, and purity is 98.5wt% (being produced by the Beijing Chemical Plant), and the median size of carbon black powder is about 60 microns, and purity is 99.8wt% (being produced by Zhuzhou Hard Alloy Group Co Ltd).
Example 1: the finished product are WC-6wt.%Co (YG6) Wimet block material.Requirement according to Co content in the YG6 Wimet, according to Co loss 1.5% (m=1.5) in the hot pressed sintering, total carbon content increases by 0.2% (p=0.2) and the spillage of material coefficient is the physical condition of k=1.02, according to mass ratio be 110.81: 8.28: 24.20 with WO
2.9, Co
3O
4Carry out ball milling with carbon black and mix, and then be to be filled in the mould after 1: 1.29 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, in hot-pressed sintering furnace, carry out sintering.Its hot-pressing sintering technique parameter is: pressure 10MPa is that 30 ℃/min is warming up to 375 ℃ with temperature rise rate, is incubated 1 hour; Be warming up to 1000 ℃ then, be incubated 3 hours; Temperature rise rate with 10 ℃/min rises to 1450 ℃ again, and pressure boost is to 30MPa, heat-insulation pressure keeping 60 minutes; After last pressurize is cooled to 1050 ℃, removes pressure, be cooled to room temperature.Fig. 1 sees in XRD figure spectrum and the displaing micro tissue topography of the YG6 Wimet block material that is obtained by above-mentioned prepared, and material property parameter sees Table 1.
Example 2: the finished product are WC-10wt.%Co (YG10) Wimet block material.Requirement according to Co content in the YG10 Wimet, according to Co loss 0.3% (m=0.3) in the vacuum sintering, total carbon content increases by 0.15% (p=0.15) and the spillage of material coefficient is the physical condition of k=1.00, according to mass ratio be 106.16: 13.64: 23.64 with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, is after 1: 1.22 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, be filled into cold pressing in the mould after, mould and powder are carried out sintering together in vacuum sintering furnace.The processing parameter of vacuum sintering is: be warming up to 375 ℃, be incubated 1 hour; With the temperature rise rate to 950 of 8 ℃/min ℃, be incubated 2 hours then; Be warming up to 1400 ℃ again, be incubated 1.5 hours; Cool to room temperature at last with the furnace.Fig. 2 sees in XRD figure spectrum and the displaing micro tissue topography of the YG10 Wimet block material that is obtained by above-mentioned prepared, and material property parameter sees Table 1.
Example 3: the finished product are WC-15wt.%Co (YG15) Wimet block material.Requirement according to Co content in the YG15 Wimet, according to Co loss 2.5% (m=2.5) in the low pressure sintering, total carbon content increases by 0.3% (p=0.3) and the spillage of material coefficient is the physical condition of k=1.05, according to mass ratio be 99.86: 20.91: 22.05 with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, is to be filled in the mould after 1: 1.20 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, carries out sintering in the low pressure sintering stove.The processing parameter of sintering is: be warming up to 400 ℃ of insulations 1 hour; Speed with 7 ℃/min is warming up to 980 ℃ then, is incubated 3 hours; Temperature rise rate with 3 ℃/min is warming up to 1450 ℃ subsequently, behind the insulation 40min, charges into the 5MPa argon gas, heat-insulation pressure keeping 30min; Cool to room temperature at last with the furnace.Fig. 3 sees in XRD figure spectrum and displaing micro tissue topography by the YG15 Wimet block material of above-mentioned prepared, and material property parameter sees Table 1.
Example 4: with the contrast experiment of the existing patent (ZL 200610165554.2) of this seminar: be example with WC-10wt.%Co (YG10) Wimet.The present invention is according to Co loss 2.5% (m=2.5) in the hot pressed sintering, and total carbon content increases by 0.15% (p=0.15) and the spillage of material coefficient is the physical condition of k=1.1, is that 105.88: 13.97: 23.23 ratio is with WO according to mass ratio
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, is to be filled in the mould after 1: 1.33 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, carries out sintering in hot-pressed sintering furnace.Sintering process parameter is: pressure 20MPa is that 25 ℃/min is warming up to 350 ℃ with temperature rise rate, is incubated 0.5 hour; Be warming up to 850 ℃ then, be incubated 2.5 hours; Temperature rise rate with 10 ℃/min is warming up to 1420 ℃ again, and pressure boost is to 80MPa, heat-insulation pressure keeping 50 minutes; After last pressurize is cooled to 1150 ℃, removes pressure, be cooled to room temperature.The metallographic structure pattern that obtains block materials is seen Fig. 4 (a).According to the patent of this seminar " a kind of simple preparation method of superfine WC-Co composite powder (ZL 200610165554.2) fast ", according to certain mass ratio with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, be placed in the vacuum reaction stove in dry 25 hours in vacuum drying oven, is under the condition of 0.003Pa in vacuum tightness, is warming up to 1100 ℃ with the temperature rise rate of 30 ℃/min, is incubated 3.5 hours.The microtexture pattern of the YG10 cemented carbide powder powder material of preparation is seen Fig. 4 (b).
Example 5: with the contrast experiment of the existing patent (ZL 200610165554.2) of this seminar: be example with WC-16wt.%Co (YG16) Wimet.Requirement according to Co content in the YG16 Wimet, according to Co loss 0.6% (m=0.6) in the vacuum sintering, total carbon content increases by 0.1% (p=0.1) and the spillage of material coefficient is the physical condition of k=1.05, according to mass ratio be 99.00: 21.89: 21.89 with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, is after 1: 1.19 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, be filled into cold pressing in the mould after, mould and powder are carried out sintering together in vacuum sintering furnace.The processing parameter of vacuum sintering is: be warming up to 400 ℃, be incubated 0.5 hour; With the temperature rise rate to 900 of 5 ℃/min ℃, be incubated 2.5 hours then; Be warming up to 1450 ℃ again, be incubated 3 hours; Cool to room temperature at last with the furnace.The fracture apperance of the YG16 Wimet block material that is obtained by above-mentioned prepared is seen Fig. 5 (a).According to the patent of this seminar " a kind of simple preparation method of superfine WC-Co composite powder (ZL 200610165554.2) fast ", according to certain mass ratio with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, be placed in the vacuum reaction stove in dry 35 hours in vacuum drying oven, is under the condition of 0.004Pa in vacuum tightness, is warming up to 1150 ℃ with the temperature rise rate of 20 ℃/min, is incubated 4 hours.The microtexture pattern of the YG16 cemented carbide powder powder material of preparation is seen Fig. 5 (b).
Example 6: tissue and the performance uniformity contrast of the present invention and existing patent ZL 200410003442.8 preparation sample inside: the finished product are WC-6wt.%Co (YG6) the Wimet block material of φ 45 * 4mm.Requirement according to Co content in the YG6 Wimet, according to Co loss 2.0% (m=2.0) in the low pressure sintering, total carbon content increases by 0.3% (p=0.3) and the spillage of material coefficient is the physical condition of k=1.02, according to mass ratio be 110.78: 8.32: 24.19 with WO
2.9, Co
3O
4Carrying out ball milling with carbon black and mix, is to be filled in the mould after 1: 1.29 ratio is weighed the oxide compound mixed powder according to sample mass behind the sintering and mixed powder mass ratio, carries out sintering in the low pressure sintering stove.The processing parameter of sintering is: be warming up to 380 ℃ of insulations 1 hour; Speed with 6 ℃/min is warming up to 960 ℃ then, is incubated 2.5 hours; Temperature rise rate with 8 ℃/min is warming up to 1430 ℃ subsequently, behind the insulation 40min, charges into the 4MPa argon gas, heat-insulation pressure keeping 40min; Cool to room temperature at last with the furnace.The displaing micro tissue topography and the performance that are gone out YG6 Wimet block material different sites by above-mentioned prepared are seen Fig. 6: tissue and the synoptic diagram at hardness test position (as Fig. 6 a), along O point (sample center) and the regional sem photograph (as Fig. 6 O and 6A) of A point (specimen surface) as shown in the Hardness Distribution (as Fig. 6 b) of axially and radially (Y and the directions X among Fig. 6 a) of sample, Fig. 6 (a).
Preparation technology with patent ZL 200410003442.8 prepares sample: with the WO of mass percent 85%
3With 13% CoO powder add 15% carbon black mixed simultaneously routinely technology to add ethanol wetting, ball milling is to the granularity oven dry of back below 0.8 micron; The dress mould, in discharging plasma sintering equipment, carry out sintering, be evacuated to 4Pa, under 100 ℃/min, be rapidly heated to 850 ℃, be warming up to 1100 ℃ with 60 ℃/min then, treat that vacuum tightness returns to 4Pa, pressurization 50MPa, 1250 ℃ down after the insulation 2min cooling displaing micro tissue topography and the performance of WC Wimet block material different sites seen Fig. 7: the axially and radially hardness distribution of (Y and directions X shown in Fig. 6 a) of WC-6wt.%Co Wimet block material is seen Fig. 7 a, the sem photograph in O point shown in Fig. 6 (a) (sample center) and A point (specimen surface) zone is seen Fig. 7 O and 7A.
The different embodiment of table 1 prepare the performance perameter of Wimet
Claims (4)
1. the synthetic industrialized preparing process of Wimet block material original position is characterized in that, may further comprise the steps:
(1) with WO
2.9, Co
3O
4With carbon black be raw material, reduction waste according to evaporation, waste and the C of Co in the requirement for preparing material C o content, the preparation process, calculate above-mentioned three kinds of raw material amount ratios, the mass percent of supposing Co is n%, the evaporation of Co amount and the loss that is pressed into mould are m%, the loss of carbon amount is p%, the mass ratio of three kinds of raw materials then is 1.18 (100-n-nm%): 1.36n (1+m%): (25.60-0.23n (1+m%)) (1+p%), raw material is carried out ball milling mixing n=6-20, m=0-3.0, p=0-0.5;
(2) specification of quality of the final blank of basis, consider mixed powder generation reduction and carbonization reaction in the sintering process, discharge the sintering loss factor k that gas causes the minimizing of quality of materials and WC, Co powder, calculate the desired raw material powder quality, sample mass and raw material powder mass ratio are 1 behind the sintering: 1.35k (100-n-nm%) %, k=1.0-1.2;
(3) hot-pressing sintering technique is: a certain amount of mixed powder is put into mould, is that 10-50 ℃/min rises to 350-400 ℃ with the temperature rise rate, is incubated 0.5-1 hour, and pressure is 10-30MPa; Be warming up to 750-1000 ℃ then, be incubated 2-3 hour; Be warming up to 1200-1500 ℃ and increase sintering pressure to 30-80MPa, heat-insulation pressure keeping 30-90 minute with the temperature rise rate of 5-10 ℃/min again; At last, pressurize is cooled to below 1150 ℃, removes pressure, cool to room temperature;
Vacuum sintering technology is: after a certain amount of mixed powder is put into mould and colded pressing, mould and pressed compact are put into vacuum oven together, be warming up to 350-400 ℃ of insulation 0.5-1 hour, the speed with 5-10 ℃/min is warming up to 750-1000 ℃ then, is incubated 2-3 hour; Be warming up to 1300-1500 ℃ of insulation 1-5 hour again, cool to room temperature at last with the furnace;
Low pressure sintering technology is: be warming up to 350-400 ℃ of insulation 0.5-1 hour; Speed with 5-10 ℃/min is warming up to 750-1000 ℃ of insulation 2-3 hour then; Speed with 3-10 ℃/min is warming up to 1310-1470 ℃ subsequently, behind the insulation 20-40min, charges into 2-5MPa nitrogen or argon gas, heat-insulation pressure keeping 20-40min; Cool to room temperature at last with the furnace.
2. according to the method for claim 1, it is characterized in that during hot-pressing sintering technique, the span of parameter m, p, k is: m=1.0-3.0, p=0-0.3, k=1.0-1.2.
3. according to the method for claim 1, it is characterized in that, during vacuum sintering technology, the span of parameter m, p, k: m=0-0.8, p=0-0.2, k=1.0-1.1.
4. according to the method for claim 1, it is characterized in that, during low pressure sintering technology, the span of parameter m, p, k: m=1.0-2.5, p=0.2-0.5, k=1.0-1.2.
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| CN106346002A (en) * | 2016-11-16 | 2017-01-25 | 湖南文理学院 | Cemented carbide sintering process |
| CN106702249B (en) * | 2016-12-12 | 2018-05-22 | 南京航空航天大学 | A kind of preparation method of gradient-structure WC-Co hard alloy |
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| CN1232669C (en) * | 2004-03-12 | 2005-12-21 | 北京工业大学 | Method of WC hard alloy by electric discharge plasma in situ synthesis |
| CN101151386B (en) * | 2005-03-28 | 2010-05-19 | 京瓷株式会社 | Ultra-hard alloy and cutting tool |
| CN1749422A (en) * | 2005-09-30 | 2006-03-22 | 北京工业大学 | In-situ synthetic method for WC-Co hard alloy |
| CN100444997C (en) * | 2006-12-21 | 2008-12-24 | 北京工业大学 | Simple fast preparing process of superfine WC-Co composite powder |
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Application publication date: 20120627 Assignee: Beihard Technology (Xianghe) Co.,Ltd. Assignor: Beijing University of Technology Contract record no.: X2021990000686 Denomination of invention: Industrialized production method of in-situ synthesis of cemented carbide bulk materials Granted publication date: 20130807 License type: Exclusive License Record date: 20211111 |
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