CN103627942A - Preparation method for high-performance WC-Co nanocrystal cemented carbide - Google Patents
Preparation method for high-performance WC-Co nanocrystal cemented carbide Download PDFInfo
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- CN103627942A CN103627942A CN201310090726.4A CN201310090726A CN103627942A CN 103627942 A CN103627942 A CN 103627942A CN 201310090726 A CN201310090726 A CN 201310090726A CN 103627942 A CN103627942 A CN 103627942A
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Abstract
A disclosed preparation method for high-performance WC-Co nanocrystal cemented carbide comprises: taking nanometer tungsten carbide (WC) powder, ultrafine cobalt (Co) powder and ultrafine vanadium carbide (Cr2C3) powder as raw material powders, employing an alcohol wet grinding technology, and performing vacuum sintering and hot isostatic pressing sintering to prepare the WC-Co nanocrystal cemented carbide. By employing the above method for preparing nanocrystal cemented carbide, WC crystal grain structure is complete and clearly visible, by employing a method prescribed in ISO4499-2 for calculating two hundred or more WC crystal grains and averaging, the WC average crystal grain is less than 150 nm, the hardness HV30 is 1900 or more, the strength TRS is 4000 MPa or more and the metallographic structure is A02B00C00. The technology is simple, the process control is convenient, the production cost is low, and the prepared nanocrystal cemented carbide has the advantages of high densification degree and excellent performances.
Description
Technical field
The present invention relates to Hardmetal materials manufacturing technology field, particularly relate to a kind of preparation method of high-performance WC-Co Nanograin Cemented Carbide.
Background technology
Around crystal grain thinning, produce the large focus in the research and development ，Shi world today Wimet technical field of ultra-fine and nanostructure Wimet.The close grain of Wimet of realizing at present batch production is 0.2 μ m.
In nano hard alloy preparation process, adopting high quality nano raw material powder is unusual the key link.The preparation method of nano-powder is a lot, and in theory, any multicrystal method of fine crystal particle size of manufacturing can be used for manufacturing nano-powder.Laboratory adopts mechanical alloying method, fixed bed reaction method, be dried-fluidized bed process etc. of spraying to prepare nanometer WC powder or WC-Co composite powder conventionally, but because it is too complicated or be subject to device-restrictive easily to introduce impurity or technique, can suitability for industrialized production composite powder only have spraying dry-fluidized bed process, the defect of this method is freely to join Co, causes alloying constituent single.
Concerning nano hard alloy base material, sintering circuit will determine the quality of alloy mass.Because nano raw material powder model system has very large surface energy, in traditional liquid sintering process, for reducing system surfaces energy, WC grain will be grown up rapidly, therefore many scholar's research the sintering technologies such as the microwave sintering of nano hard alloy, rapid thermal pressed sintering, discharge plasma sintering, object is to accelerate sintering rate, shorten sintering time, reduce sintering temperature, to control growing up of WC grain, but this will cause, sintering process will be abundant not, alloy grain growth is perfect not, cannot realize industrial application.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art, a kind of preparation method of high-performance WC-Co Nanograin Cemented Carbide is provided, is with nanometer WC powder, ultra-fine Co powder, VC powder and Cr
3c
2powder is as raw material powder, utilize alcohol wet-grinding technology and relative device, through vacuum sintering and HIP sintering, thereby prepare the high-performance nano cemented carbide that grain fineness number is less than 150 nanometers, have technique simple, process control is easy, and production cost is low, the Nanograin Cemented Carbide densification degree of preparing is high, the feature of excellent performance.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of high-performance WC-Co Nanograin Cemented Carbide, comprises the steps:
A. compound is produced step; This step is to select mean particle size to be less than the Cr that the WC powder of 400nm, Co powder that mean particle size is less than 1.5um, the equal granularity of VC powder peace that mean particle size is less than 1.5um are less than 1.5um
3c
2powder is raw material, and wherein, Co powder accounts for the 3wt%～30wt% of total raw material, and VC powder accounts for the 0wt%～2.0wt% of total raw material, Cr
3c
2powder accounts for the 0wt%～2.0wt% of total raw material, and surplus is WC powder; And paraffin makees binder, and the addition of the paraffin 0.5wt%～3.5wt% that is described total raw material; Then, make medium in roller ball mill, carry out wet-milling with raw spirit, the ratio of grinding media to material of Wimet mill ball and solid material is 2:1～10:1, and the liquid-solid ratio of raw spirit and solid material is 100～600mL/kg; Ball milling carries out vacuum-drying and is prepared into compound after 30～120 hours;
B. pressing step; The compound that previous step is made is pressed into pressed compact; Wherein, pressing pressure is 100～250MPa;
C. sintering step; The pressed compact that previous step is made sinters WC-Co Nanograin Cemented Carbide into.
Further, described compound is produced step and is also comprised compound is crossed to 80 eye mesh screens.
Further, at compound, cross after 80 eye mesh screens, also comprise that compound is put into nodulizer to roll and within 3～15 minutes, carry out pelletization treatment.
Described pressing step is that the compound that previous step is prepared is pressed into round bar shape pressed compact.
Described sintering step is first the pressed compact suppressing to be carried out to vacuum sintering, sintering temperature is controlled at 1000～1400 ℃, soaking time is controlled at 0.5～2 hour, and then carry out HIP sintering, sintering temperature is controlled at 1200～1400 ℃, soaking time is controlled at 0.5～2 hour, and sintering pressure is controlled at 50～200MPa.
The preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention, to adopt purple tungsten local reduction way to produce, with nanometer tungsten carbide (WC) powder, ultra-fine cobalt (Co) powder, ultra-fine vanadium carbide (VC) powder and ultra-fine chromium carbide (Cr3C2) powder are as raw material powder, utilize alcohol wet-grinding technology and relative device, through vacuum sintering and HIP sintering, prepare WC-Co Nanograin Cemented Carbide, the Nanograin Cemented Carbide that adopts aforesaid method to prepare, WC grain tissue improves and is high-visible, adopt 200 above WC grain of method measurement calculating of ISO4499-2 regulation to average, calculate WC average crystal grain and be less than 150nm, hardness HV30 is more than 1900, intensity TRS is more than 4000MPa, metallographic structure is A02B00C00.
The invention has the beneficial effects as follows, owing to having adopted with nanometer tungsten carbide (WC) powder, ultra-fine cobalt (Co) powder, ultra-fine vanadium carbide (VC) powder and ultra-fine chromium carbide (Cr
3c
2) powder is as raw material powder, and utilize alcohol wet-grinding technology and relative device, and through vacuum sintering and HIP sintering, prepare WC-Co Nanograin Cemented Carbide, compared with prior art, there is following beneficial effect:
Nano hard alloy method is prepared in laboratory: adopt preparation nanometer WC or the WC-Co composite powders such as machine-alloying, thermochemistry synthesis method, adopt the techniques such as microwave sintering, low temperature hot-press sintering, discharge plasma sintering to realize alloy densification, but this Fast Sintering is often difficult to realize real alloy densification, weave construction is not good, alloy property is not high, can not realize industrial applications;
When the inventive method is prepared Nanograin Cemented Carbide, raw material powder obtains by suitability for industrialized production, adopt the wet-milling of alcohol paraffin, vacuum sintering and HIP sintering technique, whole processing technology routine is compact, equipment is connected closely, is easy to realize industrialized mass production.The Nanograin Cemented Carbide densification degree of preparation is high, excellent performance, and it is perfect, high-visible that WC grain is organized, and WC grain size is less than 150 nanometers.Have technique simple, process control is easy, and production cost is low, and the Nanograin Cemented Carbide densification degree of preparing is high, the feature of excellent performance.
Below in conjunction with drawings and Examples, the present invention is described in further detail; But the preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention is not limited to embodiment.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of embodiment mono-WC powder of the present invention;
Fig. 2 is the stereoscan photograph of embodiment mono-Co powder of the present invention;
Fig. 3 is the stereoscan photograph of embodiment mono-Nanograin Cemented Carbide of the present invention;
Fig. 4 is the stereoscan photograph of embodiment bis-Nanograin Cemented Carbides of the present invention;
Fig. 5 is the stereoscan photograph of embodiment tri-Nanograin Cemented Carbides of the present invention.
Embodiment
Embodiment mono-,
Referring to shown in Fig. 1 to Fig. 3, the preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention, comprises the steps:
A. compound is produced step: selecting median size is the WC(wolfram varbide of 70nm) powder (as shown in Figure 1), the Co(cobalt that to add median size be 0.8um) the VC(vanadium carbide of powder (as shown in Figure 2), median size 1 μ m) Cr of the equal particle diameter 1 μ m of powder peace
3c
2(chromium carbide) powder is raw material, and wherein, Co powder accounts for the 12wt% of total raw material, and VC powder accounts for the 0.50wt% of total raw material, Cr
3c
2the 0.5wt% of powder total raw material, surplus is nanometer WC powder, above four kinds of powder (WC powder, Co powder, VC powder and Cr
3c
2powder) form total raw material; Additional paraffin is made binder, and the addition of the paraffin 2wt% that is above-mentioned total raw material; Then, make medium in roller ball mill, carry out wet-milling mixing with raw spirit, the ratio of grinding media to material of Wimet mill ball and solid material is 4:1, and the liquid-solid ratio of raw spirit and solid material is 300mL/kg; Ball milling carries out vacuum-drying after 60 hours; Cross after 80 mesh sieves, in nodulizer, roll and within 3 minutes, be prepared into compound;
B. pressing step: the compound preparing in previous step is pressed into round bar shape pressed compact, and wherein pressing pressure is 150MPa;
C. sintering step: the pressed compact suppressing is carried out to vacuum sintering, and sintering temperature is controlled at 1250 ℃, and soaking time is controlled at 1 hour, carry out again HIP sintering, sintering temperature is controlled at 1350 ℃, and soaking time is controlled at 0.5 hour, and sintering pressure is controlled at 150MPa.
Adopt aforesaid method to prepare Nanograin Cemented Carbide, adopt the method measurement of ISO4499-2 regulation to calculate WC average crystal grain 131nm, see Fig. 3, hardness HV30 is 2002, intensity TRS is that 4172MPa, metallographic structure are A02B00C00.
Embodiment bis-,
Shown in Figure 4, the preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention, comprises the steps:
A. compound is produced step: selecting median size is the WC powder of 100nm, Co powder, the VC powder of median size 1 μ m and the Cr of median size 1 μ m that interpolation median size is 0.8um
3c
2powder is raw material, and wherein, Co powder accounts for the 13wt% of total raw material, and VC powder accounts for the 1.3wt% of total raw material, Cr
3c
2the 0.9wt% of powder total raw material, all the other are nanometer WC powder; Additional paraffin is made binder, and the addition of the paraffin 2wt% that is above-mentioned total raw material; Then, make medium in roller ball mill, carry out wet-milling mixing with raw spirit, the ratio of grinding media to material of Wimet mill ball and solid material is 5.5:1, and the liquid-solid ratio of raw spirit and solid material is 350mL/kg; Ball milling carries out vacuum-drying after 80 hours; Cross after 80 mesh sieves, in nodulizer, roll and within 3 minutes, be prepared into compound;
B. pressing step: the compound preparing in previous step is pressed into round bar shape pressed compact, and wherein pressing pressure is 180MPa;
C. sintering step: the pressed compact suppressing is carried out to vacuum sintering, and sintering temperature is controlled at 1280 ℃, and soaking time is controlled at 0.5 hour, carry out again HIP sintering, sintering temperature is controlled at 1340 ℃, and soaking time is controlled at 1 hour, and sintering pressure is controlled at 150MPa.
Adopt aforesaid method to prepare Nanograin Cemented Carbide, WC average crystal grain 149nm, is shown in Fig. 4, and hardness HV30 is 1920, intensity TRS is that 4015MPa, metallographic structure are A02B00C00.
Embodiment tri-,
Shown in Figure 5, the preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention, comprises the steps:
A. compound is produced step: selecting median size is the WC powder of 200nm, Co powder, the VC powder of median size 1 μ m and the Cr of median size 1 μ m that interpolation median size is 0.6um
3c
2powder is raw material, and wherein, Co powder accounts for the 10wt% of total raw material, and VC powder accounts for the 0.45wt% of total raw material, Cr
3c
2the 0.6wt% of powder total raw material, all the other are nanometer WC powder; Additional paraffin is made binder, and the addition of the paraffin 2wt% that is above-mentioned total raw material; Then, make medium in roller ball mill, carry out wet-milling mixing with raw spirit, the ratio of grinding media to material of Wimet mill ball and solid material is 7:1, and the liquid-solid ratio of raw spirit and solid material is 400mL/kg; Ball milling carries out vacuum-drying after 100 hours; Cross after 80 mesh sieves, in nodulizer, roll and within 8 minutes, be prepared into compound;
B. pressing step: the compound preparing in previous step is pressed into round bar shape pressed compact, and wherein pressing pressure is 200MPa;
C. sintering step: the pressed compact suppressing is carried out to vacuum sintering, and sintering temperature is controlled at 1280 ℃, and soaking time is controlled at 1 hour, carry out again HIP sintering, sintering temperature is controlled at 1350 ℃, and soaking time is controlled at 1 hour, and sintering pressure is controlled at 120MPa.
Adopt aforesaid method to prepare Nanograin Cemented Carbide, WC average crystal grain 152nm, is shown in Fig. 5, and hardness HV30 is 2058, intensity TRS is that 4018MPa, metallographic structure are A02B00C00.
The preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention is to adopt purple tungsten local reduction way to produce, with nanometer tungsten carbide (WC) powder, ultra-fine cobalt (Co) powder, ultra-fine vanadium carbide (VC) powder and ultra-fine chromium carbide (Cr
3c
2) powder is as raw material powder, utilize alcohol wet-grinding technology and relative device, through vacuum sintering and HIP sintering, prepare WC-Co Nanograin Cemented Carbide, the Nanograin Cemented Carbide that adopts aforesaid method to prepare, WC grain tissue improves and is high-visible, and the method measurement of employing ISO4499-2 regulation is calculated 200 above WC grain and is averaged, calculate WC average crystal grain and be less than 150nm, hardness HV30 is more than 1900, intensity TRS is that 4000MPa is above, metallographic structure is A02B00C00.
Above-described embodiment is only used for further illustrating the preparation method of a kind of high-performance WC-Co Nanograin Cemented Carbide of the present invention; but the present invention is not limited to embodiment; any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment, all fall in the protection domain of technical solution of the present invention.
Claims (5)
1. a preparation method for high-performance WC-Co Nanograin Cemented Carbide, is characterized in that: comprise the steps:
A. compound is produced step; This step is to select mean particle size to be less than the Cr that the WC powder of 400nm, Co powder that mean particle size is less than 1.5um, the equal granularity of VC powder peace that mean particle size is less than 1.5um are less than 1.5um
3c
2powder is raw material, and wherein, Co powder accounts for the 3wt%～30wt% of total raw material, and VC powder accounts for the 0wt%～2.0wt% of total raw material, Cr
3c
2powder accounts for the 0wt%～2.0wt% of total raw material, and surplus is WC powder; And paraffin makees binder, and the addition of the paraffin 0.5wt%～3.5wt% that is described total raw material; Then, make medium in roller ball mill, carry out wet-milling with raw spirit, the ratio of grinding media to material of Wimet mill ball and solid material is 2:1～10:1, and the liquid-solid ratio of raw spirit and solid material is 100～600mL/kg; Ball milling carries out vacuum-drying and is prepared into compound after 30～120 hours;
B. pressing step; The compound that previous step is made is pressed into pressed compact; Wherein, pressing pressure is 100～250MPa;
C. sintering step; The pressed compact that previous step is made sinters WC-Co Nanograin Cemented Carbide into.
2. the preparation method of high-performance WC-Co Nanograin Cemented Carbide according to claim 1, is characterized in that: further, described compound is produced step and also comprised compound is crossed to 80 eye mesh screens.
3. the preparation method of high-performance WC-Co Nanograin Cemented Carbide according to claim 2, is characterized in that: further, at compound, cross after 80 eye mesh screens, also comprise that compound is put into nodulizer to roll and within 3～15 minutes, carry out pelletization treatment.
4. the preparation method of high-performance WC-Co Nanograin Cemented Carbide according to claim 1, is characterized in that: described pressing step is that the compound that previous step is prepared is pressed into round bar shape pressed compact.
5. the preparation method of high-performance WC-Co Nanograin Cemented Carbide according to claim 1, it is characterized in that: described sintering step is first the pressed compact suppressing to be carried out to vacuum sintering, sintering temperature is controlled at 1000～1400 ℃, soaking time is controlled at 0.5～2 hour, and then carry out HIP sintering, sintering temperature is controlled at 1200～1400 ℃, and soaking time is controlled at 0.5～2 hour, and sintering pressure is controlled at 50～200MPa.
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| CN106041092A (en) * | 2016-08-19 | 2016-10-26 | 合肥东方节能科技股份有限公司 | Method for low-pressure sintering formation of guide wheel of guide fitting based on WC-10Co cemented carbide |
| CN106086575A (en) * | 2016-08-26 | 2016-11-09 | 洛阳金鹭硬质合金工具有限公司 | A kind of steel bonded carbide and preparation method thereof |
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Application publication date: 20140312 |