CN111876643A - Preparation method of high-strength and high-toughness WC-Fe-Ni hard alloy - Google Patents
Preparation method of high-strength and high-toughness WC-Fe-Ni hard alloy Download PDFInfo
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- CN111876643A CN111876643A CN202010781298.XA CN202010781298A CN111876643A CN 111876643 A CN111876643 A CN 111876643A CN 202010781298 A CN202010781298 A CN 202010781298A CN 111876643 A CN111876643 A CN 111876643A
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- 239000000956 alloy Substances 0.000 title claims abstract description 49
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 48
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 3
- 238000000465 moulding Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 230000003068 static effect Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
Abstract
The invention belongs to the field of hard alloy preparation, and discloses a preparation method of high-toughness WC-Fe-Ni hard alloy. Preparing mixed powder, then ball-milling, drying, sieving, filling into a graphite die and prepressing for molding; putting the obtained sample communicated with a graphite mold into a vibration sintering furnace, wherein the atmosphere in the furnace is vacuum or inert atmosphere, firstly applying constant pressure of 30-50 MPa to the sample, simultaneously heating to the sintering temperature of 1300-1320 ℃, and when the sintering temperature is reached, switching the constant pressure into vibration pressure for vibration sintering, wherein the average value of the vibration pressure is 30-50 MPa, the vibration amplitude of the vibration pressure is 10-50 MPa, the vibration frequency is 1-10 Hz, and the vibration sintering is carried out for 0.25-1 h; after the vibration sintering is finished, the vibration pressure is switched to constant pressure again, the heating is stopped, the furnace is cooled, and when the temperature in the vibration sintering furnace is reduced to 600-1000 ℃, the vibration sintering furnace is removedKeeping the pressure constant, and continuously and naturally cooling to room temperature along with the furnace to prepare the high-strength and high-toughness WC-Fe-Ni hard alloy. The hardness of the high-toughness WC-Fe-Ni hard alloy prepared by the invention is larger than or equal to 1900 MPa, and the fracture toughness is larger than or equal to 12.01 MPa.m1/2。
Description
Technical Field
The invention belongs to the technical field of hard alloy preparation, and particularly relates to a preparation method of high-toughness WC-Fe-Ni hard alloy.
Background
The WC-Fe-Ni hard alloy has the advantages of wide raw material source, low cost, small environmental pollution, higher hardness, wear resistance and corrosion resistance. Therefore, the WC-Fe-Ni hard alloy has important application prospect in the fields of cutting tools, petroleum mine drilling tools, precision dies, wear-resistant parts and the like. However, for the conventional WC-Fe-Ni hard alloy, the hardness and the toughness are mutually contradictory, and if one property is improved, the other property is inevitably sacrificed, so that the application of the hard alloy is greatly limited.
In order to solve the contradiction between the hardness and the toughness of the hard alloy and prepare the high-toughness WC-Fe-Ni hard alloy, researchers carry out a great deal of research to find that the materials with both high hardness and toughness can be obtained to a certain extent when the hard alloy with the gradient structure, the hard alloy with the double-crystal structure, the superfine/nano-crystal hard alloy and the hard alloy with the coating structure are prepared. However, the preparation methods are complicated in preparation process, complex in operation flow and high in production cost; the other method is to prepare the coating hard alloy, but the production process has strict requirements, huge equipment investment and higher production cost, and limits the large-scale industrial application of the high-toughness hard alloy.
In view of the above situation, in order to further expand the application of WC-Fe-Ni hard alloys, especially high-end application, it is urgently needed to develop a new preparation method of WC-Fe-Ni hard alloys with high toughness, so that the WC-Fe-Ni hard alloys not only have high hardness, but also have high fracture toughness and are suitable for industrial production.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of high-toughness WC-Fe-Ni hard alloy.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of high-strength and high-toughness WC-Fe-Ni hard alloy comprises the following steps:
(1) preparing mixed powder by using WC powder, Fe powder and Ni powder as raw materials, then carrying out ball milling, drying and sieving after ball milling, and filling the ball-milled powder into a graphite die for prepressing molding;
(2) putting a sample obtained after the pre-pressing forming in the step (1) into a vibration sintering furnace, wherein the atmosphere in the furnace is vacuum or inert atmosphere, firstly applying constant pressure of 30-50 MPa to the sample, simultaneously heating to the sintering temperature of 1300-1320 ℃, and when the sintering temperature is reached, switching the constant pressure into vibration pressure for vibration sintering, wherein the average value of the vibration pressure is 30-50 MPa, the vibration amplitude of the vibration pressure is 10-50 MPa, the vibration frequency is 1-10 Hz, and the vibration sintering is carried out for 0.25-1 h;
(3) and after the vibration sintering is finished, switching the vibration pressure to constant pressure again, stopping heating, cooling along with the furnace, removing the constant pressure when the temperature in the vibration sintering furnace is reduced to 600-1000 ℃, and naturally cooling to room temperature along with the furnace continuously to prepare the high-strength and high-toughness WC-Fe-Ni hard alloy.
Preferably, in the step (1), the grain diameter of the WC powder is 1-1.5 μm, and the grain diameters of the Fe powder and the Ni powder are 1-2 μm; in the mixed powder, the content of WC powder is 70-99.5 wt%, and the mass ratio of Fe/Ni is 1-3.
Preferably, in the step (1), the pressure of the pre-pressing forming is 5-20 MPa.
Preferably, in the step (1), the ball milling rotation speed is 120-150 rpm, the ball milling time is 15-24 hours, stainless steel balls with the diameter of 6-12 mm are added in the ball milling process, the mass ratio of ball materials is (3-5): 1, and 200-350 mL of absolute ethyl alcohol is added into every 1 kg of mixed powder as a ball milling medium.
Preferably, in the step (1), the drying is vacuum drying, the temperature of the vacuum drying is 40-60 ℃, and the time is 2-8 h.
Preferably, in the step (1), the powder is sieved by a sieve of 60-100 meshes.
Preferably, in the step (2), the temperature is increased to the sintering temperature at a temperature increasing speed of 2-8 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
(1) only applying vibration pressure in the sintering process of the high-toughness WC-Fe-Ni hard alloy, compared with the conventional high-toughness hard alloy, the method does not need additional working procedures, has simple process, is beneficial to large-scale production, and simultaneously reduces the production cost of the high-toughness hard alloy;
(2) the preparation method can obviously reduce the sintering temperature, shorten the sintering time, reduce the residual pores in the material, inhibit the growth of crystal grains and prepare the hard alloy material with high strength and high toughness;
(3) the hardness of the prepared high-strength and high-toughness WC-Fe-Ni hard alloy is not less than 1900 MPa, and the fracture toughness is not less than 12.01 MPa.m1/2The comprehensive performance of the developed high-strength and high-toughness hard alloy is superior to that of the traditional process method.
Drawings
FIG. 1 is an SEM photograph of a WC-Fe-Ni cemented carbide made in example 1.
FIG. 2 is an SEM image of a WC-Fe-Ni cemented carbide made in example 2.
FIG. 3 is an SEM image of a WC-Fe-Ni cemented carbide made in comparative example 1.
FIG. 4 is an SEM image of a WC-Fe-Ni cemented carbide made in comparative example 2.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
The vibratory sintering furnace in the following example was purchased from multi-field coupled experimental systems of all-readily available materials technologies, inc, and was model OPS-2020.
Example 1
In this embodiment, a WC-Fe-Ni cemented carbide with a binder phase content of 10 wt.% is selected, and the steps are as follows:
(1) taking WC powder (with the particle size of 1 mu m), Fe powder (with the particle size of 1 mu m) and Ni powder (with the particle size of 1 mu m) as raw materials, preparing mixed powder according to the component requirements that the content of the WC powder is 90 wt% and the mass ratio of Fe to Ni is 3, putting the weighed mixed powder on a planetary ball mill for ball milling, wherein the ball milling speed is 120 rpm, the ball milling time is 24 hours, adding stainless steel balls with the diameter of 8mm in the ball milling process, and adding 300 mL of absolute ethyl alcohol as a ball milling medium into 1 kg of the mixed powder;
(2) after ball milling and mixing, the slurry is put into a vacuum drying oven to be dried for 8 hours at the temperature of 60 ℃, the dried mixed powder is sieved under a 80-mesh sieve, and the sieved mixed powder is put into a graphite die to be pre-pressed and molded under the pressure of 5 MPa;
(3) putting the sample and the graphite mould into a vibration sintering furnace, wherein the atmosphere in the furnace is vacuum, and the vacuum degree is maintained at 1.0 multiplied by 10-3Pa, firstly applying a static constant pressure of 40 MPa to the sample, and simultaneously increasing the temperature to the sintering temperature of 1300 ℃ at a temperature rise speed of 8 ℃/min;
(4) when the sintering temperature is reached, immediately switching the static constant pressure into dynamic vibration pressure, wherein the median value of the vibration pressure is 40 MPa, the amplitude of the vibration pressure is 10 MPa, the vibration frequency is 5 Hz, and the vibration sintering time is 1 h;
(5) and after the vibration sintering is finished, switching the dynamic vibration pressure into the static constant pressure again, stopping heating, cooling along with the furnace, slowly discharging the static constant pressure until the pressure is 0 when the temperature in the vibration sintering furnace is reduced to 600 ℃, and continuously naturally cooling along with the furnace to room temperature to obtain the WC-Fe-Ni hard alloy.
FIG. 1 is an SEM image of the WC-Fe-Ni hard alloy, wherein the WC grain size is 0.60 μm, no obvious cavity exists in the structure, and the density is close to 100%.
Example 2
The difference from example 1 is that: in the step (4), the amplitude of the vibration pressure was 20 MPa, and the same was applied to example 1.
FIG. 2 is an SEM image of the WC-Fe-Ni hard alloy, wherein the WC grain size is 0.58 μm, no obvious cavity exists in the structure, and the density is close to 100%.
Comparative example 1
The difference from example 1 is that: in the step (4), the amplitude of the vibration pressure was 5 MPa, and the same was applied to example 1.
FIG. 3 is an SEM image of the WC-Fe-Ni hard alloy, wherein the WC grain size is 0.61 μm, no obvious cavity exists in the structure, and the density is close to 100%.
Comparative example 2
The WC-Fe-Ni hard alloy with 10 wt.% of binder phase is selected in the embodiment, and the steps are as follows:
(1) taking WC powder (with the particle size of 1 mu m), Fe powder (with the particle size of 1 mu m) and Ni powder (with the particle size of 1 mu m) as raw materials, preparing mixed powder according to the component requirements that the WC powder is 90 wt% and the Fe/Ni mass ratio is 3, placing the weighed mixed powder on a planetary ball mill for ball milling, wherein the ball milling rotation speed is 120 rpm, the ball milling time is 24 hours, adding stainless steel balls with the diameter of 8mm in the ball milling process, and adding 300 mL of absolute ethyl alcohol as a ball milling medium into each 1 kg of the mixed powder, wherein the mass ratio of the balls is 3: 1;
(2) after ball milling and mixing, the slurry is put into a vacuum drying oven to be dried for 8 hours at the temperature of 60 ℃, the dried mixed powder is sieved under a 80-mesh sieve, and the sieved mixed powder is put into a graphite die to be pre-pressed and molded under the pressure of 5 MPa;
(3) putting the sample and the graphite mould into a vibration sintering furnace, wherein the atmosphere in the furnace is vacuum, and the vacuum degree is maintained at 1.0 multiplied by 10-3Pa, applying a static constant pressure of 40 MPa to the sample, and raising the temperature to 1300 ℃ at a temperature rise speed of 8 ℃/min; when the sintering temperature is reached, maintaining the static constant pressure and preserving the heat for 1 h;
(4) and after the heat preservation is finished, stopping heating, cooling along with the furnace, slowly unloading the static constant pressure until the pressure is 0 when the temperature in the vibration sintering furnace is reduced to 600 ℃, and continuously cooling to the room temperature along with the furnace to prepare the WC-Fe-Ni hard alloy.
FIG. 4 is an SEM image of the WC-Fe-Ni hard alloy, wherein the size of WC crystal grains is 0.69 μm, the structure is thick, no obvious cavity exists, and the compactness is close to 100%.
The WC-Fe-Ni hard alloys prepared in example 1, example 2, comparative example 1 and comparative example 2 were subjected to a hardness fracture toughness test. The properties of the examples and comparative examples were tested in the same experimental procedure and the force properties of the examples and comparative examples are detailed in table 1 below.
As can be seen from Table 1: compared with the traditional sintering (comparative example 2), when the amplitude of the vibration pressure is 5 MPa (comparative example 1), the hardness of the material is obviously improved, but the fracture toughness of the material is not obviously improved, and when the amplitude of the vibration pressure is more than or equal to 10 MPa (examples 1 and 2), the hardness and the fracture toughness of the material are obviously improved, so that the hard alloy with high strength and high toughness can be prepared.
Claims (7)
1. A preparation method of high-strength and high-toughness WC-Fe-Ni hard alloy is characterized by comprising the following steps:
(1) preparing mixed powder by using WC powder, Fe powder and Ni powder as raw materials, then carrying out ball milling, drying and sieving after ball milling, and filling the ball-milled powder into a graphite die for prepressing molding;
(2) putting a sample obtained after the pre-pressing forming in the step (1) into a vibration sintering furnace, wherein the atmosphere in the furnace is vacuum or inert atmosphere, firstly applying constant pressure of 30-50 MPa to the sample, simultaneously heating to the sintering temperature of 1300-1320 ℃, and when the sintering temperature is reached, switching the constant pressure into vibration pressure for vibration sintering, wherein the average value of the vibration pressure is 30-50 MPa, the vibration amplitude of the vibration pressure is 10-50 MPa, the vibration frequency is 1-10 Hz, and the vibration sintering is carried out for 0.25-1 h;
(3) and after the vibration sintering is finished, switching the vibration pressure to constant pressure again, stopping heating, cooling along with the furnace, removing the constant pressure when the temperature in the vibration sintering furnace is reduced to 600-1000 ℃, and naturally cooling to room temperature along with the furnace continuously to prepare the high-strength and high-toughness WC-Fe-Ni hard alloy.
2. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the grain diameter of WC powder is 1-1.5 μm, and the grain diameters of Fe powder and Ni powder are 1-2 μm; in the mixed powder, the content of WC powder is 70-99.5 wt%, and the mass ratio of Fe/Ni is 1-3.
3. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the pressure of the pre-pressing forming is 5-20 MPa.
4. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the ball milling speed is 120-150 rpm, the ball milling time is 15-24 hours, stainless steel balls with the diameter of 6-12 mm are added in the ball milling process, the mass ratio of ball materials is (3-5): 1, and 200-350 mL of absolute ethyl alcohol is added into every 1 kg of mixed powder as a ball milling medium.
5. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the drying is vacuum drying, the temperature of the vacuum drying is 40-60 ℃, and the time is 2-8 hours.
6. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (1), sieving the mixture by a sieve of 60-100 meshes.
7. The method for preparing the high-toughness WC-Fe-Ni hard alloy as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the temperature is increased to the sintering temperature at the temperature increase speed of 2-8 ℃/min.
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