CN102965534A - Preparation method of hard alloy with ultra-coarse grains on surface - Google Patents
Preparation method of hard alloy with ultra-coarse grains on surface Download PDFInfo
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- CN102965534A CN102965534A CN2012104535124A CN201210453512A CN102965534A CN 102965534 A CN102965534 A CN 102965534A CN 2012104535124 A CN2012104535124 A CN 2012104535124A CN 201210453512 A CN201210453512 A CN 201210453512A CN 102965534 A CN102965534 A CN 102965534A
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Abstract
The invention relates to a preparation method of a hard alloy with ultra-coarse grains on the surface, belonging to the field of manufacturing of hard alloy materials. The preparation method comprises the following steps: selecting high-hardness refractory carbide powder as a raw material; and after controlling the carbon content, carrying out wet milling on the high-hardness refractory carbide powder and a binding metal or alloy powder mixture, drying, carrying out cold-press molding, dewaxing, carrying out carburization sintering in a high-carbon-potential atmosphere at 1400-1500 DEG C for 1-4 hours to obtain the hard alloy with ultra-coarse grains on the surface. The invention has the advantages of simple technique, low equipment investment and simple process control; the prepared alloy has the advantages of coarse grains on the alloy surface layer (the maximum grain fineness of the surface hard phase is up to 20 mu m) and favorable obdurability; and thus, the invention is suitable for preparing drilling or shielding hard metal products with requirements for high alloy surface hardness, high wear resistance, high impact toughness and fatigue resistance, and is suitable for industrial production.
Description
Technical field
The present invention relates to the preparation method that a kind of surface has extra-coarse grained Wimet.Be suitable for that requirement alloy surface hardness and wear resistance are high, impelling strength is high and the preparation of fatigue proof probing or shield structure hart metal product.Belong to Hardmetal materials manufacturing technology field.
Background technology
Wimet is described as " industry tooth ", has the characteristics such as high strength, high rigidity, antifatigue, corrosion-resistant, low thermal coefficient of expansion, is widely used in the industries such as mechanical workout, mining activities.Along with the continuous propelling to the Wimet flow of research, Wimet is just towards super thick and superfine crystal particle both direction development.Press the criteria for classification of the relevant Wimet of Sandvik company, the WC grain degree is that the Wimet of 3.5～4.9 μ m, 5.0～7.9 μ m, 8.0～14 μ m is respectively coarse grain, extra-coarse grained and extraordinarily thick crystal grain Wimet in the alloy.Under the identical condition of Co content, with respect in, coarse grain hard alloy, special, extra-coarse grained carbide alloy has larger thermal conductivity, higher fracture toughness property and preferably thermal fatigue resistance and thermal shock resistance, among the components of machine such as the punching die that is applied to toughness and thermal fatigue resistance, thermal shock resistance are had relatively high expectations, hot roll, and as the continuous rock drilling apparatus parts of exploitation soft rock under the extreme industrial and mineral condition.
In the actual recovery process, rock drilling Wimet work under bad environment, the situation of rock stratum and complexity thereof, the mode of its damage and inefficacy is also different.Research finds that the rock drilling Wimet occurs to lose efficacy following principal mode: impact fatigue, abrasive wear and thermal fatigue.For hard formation, the abrasive wear degree is relatively low, and alloy lost efficacy and mainly caused by impact and impact fatigue.Thick Wimet phase crystal grain makes Binder Phase distributed more widely because surface-area is less, is conducive to put forward heavy alloyed impelling strength.
The method of the super coarse-grain alloy of existing preparation mainly is ultrahigh-temperature carbonization (1800-2000 ℃) and super high sintering temperature (1450-1500 ℃), makes the whole grain fineness number of Wimet bring up to 8-14 μ m.Because the Wimet grain fineness number is got over high strength and hardness all can descend, and above-mentioned technique is also limited to the degree that improves the Wimet grain fineness number.The groundwork position of carbide drill tooth is the surface.As long as guarantee the toughness on surface, the military service performance that just can guarantee to bore tooth.Therefore, this has been researched and developed a kind of surface and has had the super coarse-grain alloy that grain fineness number reaches 20 μ m, and inner still in the normal alloy scope of 5-7 μ m.
Summary of the invention
The objective of the invention is the demand for reality, provide the surface that a kind of processing method is simple, facility investment is few, process control is easy to have the preparation method of extra-coarse grained Wimet.
A kind of surface of the present invention has the preparation method of extra-coarse grained Wimet, comprises the steps:
The first step: batching, batch mixing
The preparation total carbon is than the Wimet of the low 0.2-0.7wt% of balance carbon amount, and drying is granulated in wet-milling;
Second step: cold pressing, dewax
In the first step gained powder, add forming agent, mix rear coldmoulding; In nitrogen atmosphere, be heated to 850-950 ℃ and get rid of binder, obtain prefabricated Wimet;
The 3rd step: carbusintering is processed
Being embedded in prefabricated Wimet in the graphite granule or placing pressure is the alkyl gas atmosphere of 0.1-2MPa, heats carbusintering under the hydrogen atmosphere protection of the environment, comes out of the stove after cooling to normal temperature with the furnace; The carbusintering temperature is 1400 ℃-1500 ℃, soaking time 1h-4h.
A kind of surface of the present invention has the preparation method of extra-coarse grained Wimet, in the first step, described Wimet is by refractory metal W, Ti, Ta, Nb, a kind of poor carbon carbide and matrix metal Co among the Hf, Fe, a kind of for raw material prepares in Ni or its alloy, the total carbon of proportioning raw materials is than the Wimet of the low 0.2-0.7wt% of balance carbon amount; The mean particle size of each component in the described Wimet, metallic carbide are 1-5 μ m, and matrix metal or powdered alloy are 1-10 μ m; Carbon content is lower than the standard chemical variable of respective metal carbide in the described poor carbon carbide.
The present invention relates to the preparation method that a kind of surface has extra-coarse grained Wimet, in the first step, described wet-grinding technology and relative device parameter is: ball-milling medium is selected from a kind of in gasoline, alcohol, the acetone; Ball material mass ratio is 0.5-2:1; Rotational speed of ball-mill is 30-120 rev/min, Ball-milling Time 10-24 hour.
The present invention relates to the preparation method that a kind of surface has extra-coarse grained Wimet, in the second step, described forming agent is selected from a kind of in paraffin, the rubber, and forming agent accounts for powder quality 0.1-0.3%; Coldmoulding pressure is 100-300MPa.
The present invention adopts above-mentioned processing method, on the basis of normal preparation Wimet, by reducing rotational speed of ball-mill, reduce ball mill crushing efficient, increase Ball-milling Time and improve blend level, in order to avoid Wimet phase crystal grain by overcrushing, improves the homogeneity of final product surface microstructure size.Carbusintering to the carbide surface carburizing, makes its surface reach normal Wimet carbon content, guarantees intensity and the hardness of carbide surface; Adopt higher carbusintering temperature, and the proper extension soaking time, the broken hair growth is not large can to impel the less crystal grain of alloy surface further to dissolve recrystallize, finally obtains the Wimet that the surface has super coarse-grain.The carbide surface crystal grain that makes surpasses the size characteristic of conventional crystal grain, therefore has high tenacity and high-wearing feature.
In sum, technique of the present invention is simple, facility investment is few, process control is easy, the alloy surface coarse grains of preparation, has preferably obdurability, be suitable for that requirement alloy surface hardness and wear resistance are high, impelling strength is high and the preparation of fatigue proof probing or shield structure hart metal product, is suitable for suitability for industrialized production.
Description of drawings
Accompanying drawing 1 prepares the process flow sheet that the top layer has extra-coarse grained Wimet for the present invention;
Accompanying drawing 2 is the SEM picture behind the Wimet carbusintering in the embodiment of the invention 1;
Accompanying drawing 3 is the SEM picture behind the Wimet carbusintering in the embodiment of the invention 2;
Accompanying drawing 4 is the SEM picture behind the Wimet carbusintering in the embodiment of the invention 3.
Accompanying drawing 5 is the SEM picture behind the Wimet carbusintering in the embodiment of the invention 4.
As can be seen from Figure 2, behind the Wimet carbusintering of embodiment 1 preparation, the WC grain degree is between 5 μ m-18 μ m.
As can be seen from Figure 3, behind the Wimet carbusintering of embodiment 2 preparations, thick WC grain is more, and mean grain size is about 10 μ m.
As can be seen from Figure 4, behind the Wimet carbusintering of embodiment 3 preparations, the maximum grain fineness number of WC surpasses 20 μ m.
As can be seen from Figure 5, the 70%TiC-30%(Fe-16.7%Ni of embodiment 4 preparation) behind the Wimet carbusintering, the TiC mean grain size is between 8-10 μ m.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1
Adopting starting powder is that Fisher particle size is the WC powder of 2 μ m, poor carbon amount 0.4wt%, and purity is 99% cobalt powder, is made into WC-6Co wt.% alloying constituent, and ingredients by weight is 1kg.
Starting powder is put into the ball milling bucket carry out wet-milling, ball-milling medium is gasoline, and Ball-milling Time is 10h, and the gained powder is carried out drying, after colding pressing, 900 ℃ of nitrogen atmosphere dewaxings 1 hour, obtains prefabricated Wimet.It is heated to 1400 ℃ of insulations carried out carburizing treatment in 2 hours in methane and hydrogen mixed gas atmosphere, cooling obtains the surface and has extra-coarse grained Wimet fast in the hydrogen atmosphere protection of the environment.The SEM picture is seen accompanying drawing 2; Can draw from figure, the WC grain degree is between 5 μ m-18 μ m.
Embodiment 2
Adopting starting powder is that Fisher particle size is that WC powder, the purity of 2 μ m is 99% cobalt powder, adds the W powder, makes poor carbon amount be adjusted to 0.4wt%, is made into WC-6Co wt.% alloying constituent, and ingredients by weight is 1kg.
Starting powder is put into the ball milling bucket carry out wet-milling, ball-milling medium is gasoline, and Ball-milling Time is 14h, and the gained powder is carried out drying, after colding pressing, 900 ℃ of nitrogen atmosphere dewaxings 1 hour, obtains prefabricated Wimet.It is imbedded be heated to 1430 ℃ of insulations in the carbon dust carried out carbusintering in 1.5 hours and process in hydrogen atmosphere, cooling obtains the surface and has extra-coarse grained Wimet fast in the hydrogen atmosphere protection of the environment.The SEM picture is seen accompanying drawing 3; Can draw from figure, thick WC grain is more, and mean grain size is about 10 μ m.
Embodiment 3
Adopting starting powder is that Fisher particle size is that WC powder, the purity of 2 μ m is 99% cobalt powder, adds the W powder, makes poor carbon amount be adjusted to 0.5wt%, is made into WC-6Co wt.% alloying constituent, and ingredients by weight is 1kg.
Starting powder is put into the ball milling bucket carry out wet-milling, ball-milling medium is gasoline, and Ball-milling Time is 24h, and the gained powder is carried out drying, after colding pressing, 900 ℃ of nitrogen atmosphere dewaxings 1 hour, obtains prefabricated Wimet.It is imbedded be heated to 1460 ℃ of insulations in the carbon dust carried out carbusintering in 3.5 hours and process in hydrogen atmosphere, cooling obtains the surface and has extra-coarse grained Wimet fast in the hydrogen atmosphere protection of the environment.The SEM picture is seen accompanying drawing 4; Can draw from figure, the maximum grain fineness number of WC surpasses 20 μ m.
Embodiment 4
Starting powder is that granularity is that TiC powder (poor carbon amount is adjusted to 0.5wt%), the purity of 2 μ m is 99% Fe-16.7%Ni(atomic ratio) powder, be made into 70%TiC-30%(Fe-16.7%Ni) (weight ratio) alloying constituent, ingredients by weight is 1kg.
Starting powder is put into the ball milling bucket carry out wet-milling, ball-milling medium is gasoline, and Ball-milling Time is 24h, and the gained powder is carried out drying, after colding pressing, 700 ℃ of vacuum dewaxings 1 hour, obtains prefabricated Wimet.It is imbedded be heated to 1400 ℃ of insulations in the carbon dust carried out carbusintering in 3.5 hours and process in hydrogen atmosphere, cooling obtains the surface and has extra-coarse grained Wimet fast in the hydrogen atmosphere protection of the environment.The SEM picture is seen accompanying drawing 5; From figure, can draw the about 14 μ m of maximum grain fineness number.
Claims (4)
1. a surface has the preparation method of extra-coarse grained Wimet, comprises the steps:
The first step: batching, batch mixing
The preparation total carbon is than the Wimet of the low 0.2-0.7wt% of balance carbon amount, and drying is granulated in wet-milling;
Second step: cold pressing, dewax
In the first step gained powder, add forming agent, mix rear coldmoulding; In nitrogen atmosphere, be heated to 850-950 ℃ and get rid of binder, obtain prefabricated Wimet;
The 3rd step: carbusintering is processed
Being embedded in prefabricated Wimet in the graphite granule or placing pressure is the alkyl gas atmosphere of 0.1-2MPa, heats carbusintering under the hydrogen atmosphere protection of the environment, comes out of the stove after cooling to normal temperature with the furnace; The carbusintering temperature is 1400 ℃-1500 ℃, soaking time 1h-4h.
2. a kind of surface according to claim 1 has the preparation method of extra-coarse grained Wimet, it is characterized in that: in the first step, described Wimet is by refractory metal W, Ti, Ta, Nb, a kind of poor carbon carbide and matrix metal Co among the Hf, Fe, a kind of for raw material prepares in Ni or its alloy, the total carbon of proportioning raw materials is than the Wimet of the low 0.2-0.7wt% of balance carbon amount; The mean particle size of each component in the described Wimet, metallic carbide are 1-5 μ m, and matrix metal or powdered alloy are 1-10 μ m; Carbon content is lower than the standard chemical variable of respective metal carbide in the described poor carbon carbide.
3. a kind of surface according to claim 1 has the preparation method of extra-coarse grained Wimet, it is characterized in that: in the first step, described wet-grinding technology and relative device parameter is: ball-milling medium is selected from a kind of in gasoline, alcohol, the acetone; Ball material mass ratio is 0.5-2:1; Rotational speed of ball-mill is 30-120 rev/min, Ball-milling Time 10-24 hour.
4. a kind of surface according to claim 1 has the preparation method of extra-coarse grained Wimet, it is characterized in that: in the second step, described forming agent is selected from a kind of in paraffin, the rubber, and forming agent accounts for powder quality 0.1-0.3%; Coldmoulding pressure is 100-300MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630530A (en) * | 2015-01-29 | 2015-05-20 | 南京航空航天大学 | Preparation method of Ti(C, N)-based metal ceramic of gradient structure |
| CN107937861A (en) * | 2018-01-10 | 2018-04-20 | 自贡硬质合金有限责任公司 | A kind of hard alloy mends carbon method |
| CN111748709A (en) * | 2020-07-10 | 2020-10-09 | 山东三钻硬质合金有限公司 | Preparation method of ultra-coarse-grain high-strength hard alloy reclaimed material |
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| JPH07166288A (en) * | 1993-12-08 | 1995-06-27 | Hitachi Tool Eng Ltd | High strength sintered hard alloy having superfine-grained surface |
| CN101824574A (en) * | 2010-05-14 | 2010-09-08 | 山东硬质合金有限公司 | Method for preparing extra-coarse grained carbide alloy |
| CN101985717A (en) * | 2010-11-13 | 2011-03-16 | 湖南三三合金集团有限公司 | Method for preparing high-tenacity super-coarse-grained tungsten and cobalt hard alloy |
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2012
- 2012-11-13 CN CN2012104535124A patent/CN102965534A/en active Pending
Patent Citations (3)
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| JPH07166288A (en) * | 1993-12-08 | 1995-06-27 | Hitachi Tool Eng Ltd | High strength sintered hard alloy having superfine-grained surface |
| CN101824574A (en) * | 2010-05-14 | 2010-09-08 | 山东硬质合金有限公司 | Method for preparing extra-coarse grained carbide alloy |
| CN101985717A (en) * | 2010-11-13 | 2011-03-16 | 湖南三三合金集团有限公司 | Method for preparing high-tenacity super-coarse-grained tungsten and cobalt hard alloy |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630530A (en) * | 2015-01-29 | 2015-05-20 | 南京航空航天大学 | Preparation method of Ti(C, N)-based metal ceramic of gradient structure |
| CN107937861A (en) * | 2018-01-10 | 2018-04-20 | 自贡硬质合金有限责任公司 | A kind of hard alloy mends carbon method |
| CN111748709A (en) * | 2020-07-10 | 2020-10-09 | 山东三钻硬质合金有限公司 | Preparation method of ultra-coarse-grain high-strength hard alloy reclaimed material |
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Application publication date: 20130313 |