CN108585855B - Polycrystalline diamond sintered body of selenium catalyst and preparation method thereof - Google Patents
Polycrystalline diamond sintered body of selenium catalyst and preparation method thereof Download PDFInfo
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Abstract
A polycrystalline diamond sintered body of a selenium catalyst and a preparation method thereof relate to the technical field of superhard materials. A method of making a selenium catalyst polycrystalline diamond compact, comprising: grinding mixed powder consisting of 31.59-34.047 parts by weight of micron-sized diamond powder and 1.473-4.79 parts by weight of micron-sized selenium powder until the selenium powder becomes amorphous selenium powder; placing the mixed powder in a mould, and forming a blank under the conditions of room temperature and pressure of 5-20 MPa; sintering and curing the blank under the pressure of 6.5 GPa-12.5 GPa, wherein the sintering temperature is 1500-1900 ℃. The preparation method has simple process, and can prepare the polycrystalline diamond sintered body with high hardness.
Description
Technical Field
The invention relates to the technical field of superhard materials, in particular to a polycrystalline diamond sintered body of a selenium catalyst and a preparation method thereof.
Background
Polycrystalline diamond sintered bodies have been the main material for manufacturing cutting tools, dressers, dies and excavation bits because of their excellent mechanical properties such as extremely high hardness, wear resistance and impact resistance.
Most of the conventional polycrystalline diamond sintered bodies are formed by sintering diamond particles and a metal catalyst at high temperature and high pressure, but the conventional polycrystalline diamond sintered bodies have a complicated process flow, so that the cost is increased.
Disclosure of Invention
The invention aims to provide a polycrystalline diamond sintered body of a selenium catalyst, which has high hardness.
Another object of the present invention is to provide a method for preparing a polycrystalline diamond compact with a selenium catalyst, which is simple in process and can produce a polycrystalline diamond compact with high hardness.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a polycrystalline diamond sintered body of a selenium catalyst, which is prepared by sintering diamond powder and selenium powder, wherein gaps among diamond particles are filled with selenium and carbide of the selenium, and D-D bonds are formed among the diamond particles.
The invention also provides a preparation method of the polycrystalline diamond sintered body of the selenium catalyst, which comprises the following steps:
grinding mixed powder consisting of 31.59-34.047 parts by weight of micron-sized diamond powder and 1.473-4.79 parts by weight of micron-sized selenium powder until the selenium powder becomes amorphous selenium powder;
placing the mixed powder in a mould, and forming a blank under the conditions of room temperature and pressure of 5-20 MPa;
sintering and curing the blank under the pressure of 6.5 GPa-12.5 GPa, wherein the sintering temperature is 1500-1900 ℃.
The embodiment of the invention has the beneficial effects that: the invention discloses a selenium catalyst polycrystalline diamond sintered body and a preparation method thereof, wherein selenium powder is used as a catalyst, the selenium powder and diamond powder are mixed and sintered to successfully prepare the polycrystalline diamond sintered body, and the selenium has good oxidation resistance at room temperature, so that the impurities in the polycrystalline diamond sintered body using the selenium as the catalyst are less, the hardness of the polycrystalline diamond sintered body is improved, and the hardness can reach 68GPa or more. And the preparation process omits the processes of catalyst reduction treatment and vacuum presintering in the production process of the traditional metal catalyst polycrystalline diamond sintered body. Greatly simplifying the production process flow.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a scanning electron microscope photograph of selenium-polycrystalline diamond according to example 2 of the present invention;
fig. 2 is a graph showing the results of vickers hardness of the selenium-polycrystalline diamond of example 2 of the present invention.
Icon: 1-diamond particles; a 2-D-D bond; 3-selenium and selenium carbide.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The polycrystalline diamond sintered compact with a selenium catalyst and the method for producing the same according to the embodiment of the present invention will be described in detail.
Most of the conventional polycrystalline diamond sintered bodies are formed by sintering diamond particles and metal catalysts (such as iron, cobalt, and nickel) under high temperature and high pressure conditions. Oxidation is a major problem faced by metal catalysts. In the processes of generation, subpackaging, transportation and mixing with diamond powder, the metal catalyst is easy to oxidize to generate metal oxide, impurities are brought into the polycrystalline diamond sintered body, and therefore the performance of the polycrystalline diamond sintered body is reduced. In order to reduce the influence of catalyst oxidation, in the production process of the existing metal catalyst polycrystalline diamond sintered body, the powder of the metal catalyst needs to be subjected to hydrogen reduction treatment for several hours at the temperature of more than 700 ℃, and the pre-pressed assembly is put into a vacuum sintering furnace in hydrogen reduction atmosphere again before high-temperature and high-pressure sintering, and is subjected to vacuum treatment for several hours at the temperature of more than 900 ℃. This complicates the process flow for producing the polycrystalline diamond sintered body and increases the production cost.
In view of this, the present embodiment provides a polycrystalline diamond sintered body of a selenium catalyst, which is obtained by sintering diamond powder and selenium powder, wherein the spaces between diamond particles are filled with selenium and selenium carbide, and D-D bonds are formed between diamond particles.
The invention uses selenium powder as a catalyst, and the selenium powder and diamond powder are mixed and sintered to successfully prepare the polycrystalline diamond sintered body, wherein the selenium belongs to an oxygen element and has good oxidation resistance at room temperature, so that the impurities in the polycrystalline diamond sintered body using the selenium as the catalyst are less, and the performance of the polycrystalline diamond sintered body is improved.
A method of making a selenium catalyst polycrystalline diamond compact, comprising:
grinding mixed powder consisting of 31.59-34.047 parts by weight of micron-sized diamond powder and 1.473-4.79 parts by weight of micron-sized selenium powder until the selenium powder becomes amorphous selenium powder.
In this embodiment, diamond powder and selenium powder are mixed mainly by ball milling, and the mixed powder after ball milling is subjected to X-ray diffraction analysis to determine whether the selenium powder has been completely ball milled into amorphous selenium.
Further, in some embodiments, the selenium powder is present in an amount of 4.2% to 13.2% by weight. In some embodiments, the weight percentage of the selenium powder is 4.2% to 6.7%. It should be noted that the weight percentage of the selenium powder refers to the weight percentage of the selenium powder to the total amount of the selenium powder and the diamond powder.
In some embodiments, the diamond powder has a grain size of 0.2 to 7 μm, and the selenium powder has a grain size of 10 to 30 μm. In some embodiments, the diamond powder has a grain size of 2 to 5 μm.
Placing the mixed powder after ball milling in a mould, and forming into a blank under the conditions of room temperature and pressure of 5-20 MPa; sintering and curing the blank under the pressure of 6.5 GPa-12.5 GPa, wherein the sintering temperature is 1500-1900 ℃.
Selenium element used as a catalyst belongs to oxygen group elements, has good oxidation resistance at room temperature, and can not be oxidized in the processes of mixing, prepressing and assembling with diamond powder. The embodiment utilizes selenium powder as a catalyst, successfully prepares the polycrystalline diamond sintered body, and omits the processes of catalyst reduction treatment and vacuum pre-sintering in the production process of the traditional metal catalyst polycrystalline diamond sintered body. In addition, under the relatively high-temperature and high-pressure condition, namely the sintering temperature and pressure in the embodiment, selenium exists in the gaps of the diamond particles in a liquid state, so that the contact area of the selenium catalyst and the diamond is increased, more D-D bond bonds among the diamond particles are favorably formed, the density of the D-D bonds in the diamond sintered body is increased, and the mechanical property of the polycrystalline diamond sintered body is improved.
In the sintered body of polycrystalline diamond, the D-D bond means that diamond particles grow together from the particles under the action of a catalyst, and carbon atoms between the diamond particles are bonded together by chemical bonds of diamond, that is, D-D bonds.
Here, the room temperature refers to normal temperature or ordinary temperature, and in the present embodiment, the room temperature is 20 to 28 ℃.
In some embodiments, the sintering temperature is 1600 to 1850 ℃. The sintering time is 30-3600 s. In some embodiments, the sintering time is 100 to 1800 seconds. In some embodiments, the sintering time is 600 to 1000 seconds.
In some embodiments, the pressure for sintering and curing the blank is 9-12.5 GPa.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a polycrystalline diamond sintered body of a selenium catalyst, which comprises the following steps:
3.159g of diamond powder with the grain size of 2-5 microns and 0.479g of selenium powder with the grain size of 10-30 microns are weighed, wherein the weight percentage of the diamond powder is 86.8 percent, and the weight percentage of the selenium powder is 13.2 percent;
mixing the diamond powder and selenium powder to obtain mixed powder, putting the mixed powder into a tungsten carbide bottle filled with tungsten carbide balls, and then putting the tungsten carbide bottle into a CERTIPREP SPEX8000-D high-energy ball mill (Metuchen, NJ) for processing. Wherein the ball mill is located in a sealed glove box purged with argon. The ball milling of the mixed powder needs at least 10 hours until the selenium powder is completely ball milled into amorphous selenium, and the ball milled mixed powder is subjected to X-ray diffraction analysis to determine that the selenium powder is completely ball milled into the amorphous selenium.
Filling the mixed powder subjected to ball milling into a mold, and then maintaining the pressure on a double-sided jacking press at room temperature and under the pressure of 5MPa for 5min to form a blank;
and (2) placing the molded blank into a press (a 15MN three-column press) with an octahedral pressure cavity, keeping the pressure for 10min at room temperature under the pressure of 6.5GPa, then slowly raising the temperature while keeping the pressure, raising the temperature to 1500 ℃ within 5min, sintering for 30s at the temperature under the pressure, then reducing the temperature to room temperature within 10min, reducing the pressure to normal pressure within 15min, and recovering the sample to obtain the selenium-polycrystalline diamond sintered body.
Example 2
The embodiment provides a preparation method of a polycrystalline diamond sintered body of a selenium catalyst, which comprises the following steps:
weighing 3.404g of diamond powder with the grain size of 2-5 mu m and 0.147g of selenium powder with the grain size of 10-30 mu m, wherein the weight percentage of the diamond powder is 95.8 percent, and the weight percentage of the selenium powder is 4.2 percent;
mixing the diamond powder and selenium powder to obtain mixed powder, putting the mixed powder into a tungsten carbide bottle filled with tungsten carbide balls, and then putting the tungsten carbide bottle into a CERTIPREP SPEX8000-D high-energy ball mill (Metuchen, NJ) for processing. Wherein the ball mill is located in a sealed glove box purged with argon. The ball milling of the mixed powder needs at least 10 hours until the selenium powder is completely ball milled into amorphous selenium, and the ball milled mixed powder is subjected to X-ray diffraction analysis to determine that the selenium powder is completely ball milled into the amorphous selenium.
Filling the mixed powder subjected to ball milling into a mold, and then maintaining the pressure on a double-sided jacking press at room temperature and under the pressure of 20MPa for 5min to form a blank;
and (2) placing the molded blank into a press (a 15MN three-column press) with an octahedral pressure cavity, keeping the pressure for 10min at room temperature under the pressure of 12.5GPa, then slowly raising the temperature while keeping the pressure, raising the temperature to 1900 ℃ within 5min, sintering for 3600s at the temperature under the pressure, then reducing the temperature to the room temperature within 15min, reducing the pressure to the normal pressure within 6h, and recovering a sample to obtain the selenium-polycrystalline diamond sintered body.
Example 3
The embodiment provides a preparation method of a polycrystalline diamond sintered body of a selenium catalyst, which comprises the following steps:
3.334g of diamond powder with the grain size of 0.2-5 mu m and 0.239g of selenium powder with the grain size of 10-30 mu m are weighed, wherein the weight percentage of the diamond powder is 93.3 percent, and the weight percentage of the selenium powder is 6.7 percent;
mixing the diamond powder and selenium powder to obtain mixed powder, putting the mixed powder into a tungsten carbide bottle filled with tungsten carbide balls, and then putting the tungsten carbide bottle into a CERTIPREP SPEX8000-D high-energy ball mill (Metuchen, NJ) for processing. Wherein the ball mill is located in a sealed glove box purged with argon. The ball milling of the mixed powder needs at least 10 hours until the selenium powder is completely ball milled into amorphous selenium, and the ball milled mixed powder is subjected to X-ray diffraction analysis to determine that the selenium powder is completely ball milled into the amorphous selenium.
Filling the mixed powder subjected to ball milling into a mold, and then maintaining the pressure on a double-sided jacking press at room temperature and under the pressure of 10MPa for 1min to form a blank;
and (2) placing the molded blank into a press (a 15MN three-column press) with an octahedral pressure cavity, keeping the pressure for 10min at room temperature under the pressure of 10GPa, then slowly raising the temperature while keeping the pressure, raising the temperature to 1850 ℃ within 5min, sintering for 1800s at the temperature under the pressure, then reducing the temperature to room temperature within 10min, reducing the pressure to normal pressure within 6h, and recovering the sample to obtain the selenium-polycrystalline diamond sintered body.
Example 4
The embodiment provides a preparation method of a polycrystalline diamond sintered body of a selenium catalyst, which comprises the following steps:
3.231g of diamond powder with crystal grains of 5-10 mu m and 0.358g of selenium powder with crystal grains of 10-30 mu m are weighed, wherein the weight percentage of the diamond powder is 90 percent, and the weight percentage of the selenium powder is 10 percent;
mixing the diamond powder and selenium powder to obtain mixed powder, putting the mixed powder into a tungsten carbide bottle filled with tungsten carbide balls, and then putting the tungsten carbide bottle into a CERTIPREP SPEX8000-D high-energy ball mill (Metuchen, NJ) for processing. Wherein the ball mill is located in a sealed glove box purged with argon. The ball milling of the mixed powder needs at least 10 hours until the selenium powder is completely ball milled into amorphous selenium, and the ball milled mixed powder is subjected to X-ray diffraction analysis to determine that the selenium powder is completely ball milled into the amorphous selenium.
Filling the mixed powder subjected to ball milling into a mold, and then maintaining the pressure on a double-sided jacking press at room temperature and 15MPa for 4min to form a blank;
and (2) placing the molded blank into a press (a 15MN three-column press) with an octahedral pressure cavity, keeping the pressure for 10min at room temperature under the pressure of 9GPa, then slowly raising the temperature while keeping the pressure, raising the temperature to 1600 ℃ within 5min, sintering for 600s at the temperature and the pressure, then reducing the temperature to the room temperature within 15min, reducing the pressure to the normal pressure within 4h, and recovering the sample to obtain the selenium-polycrystalline diamond sintered body.
Test examples
(1) The microstructure of the selenium-polycrystalline diamond sintered body obtained in example 2 was subjected to a scanning electron microscope to obtain a microstructure shown in fig. 1.
Fig. 1 shows the results of analysis, and as can be seen from fig. 1, in the selenium-polycrystalline diamond sintered body, diamond particles 1 are bonded to each other by D-D bonds 2, and the diamond particles 1 are filled with selenium and selenium carbide 3.
(2) The hardness of the selenium-polycrystalline diamond sintered body prepared in this example 1 was measured by a MICRO4 microhardness tester (BUEH L ER L TD) by applying a load of 9.8N to the sample and holding the pressure for 15 seconds, making twelve indents on each sample, measuring the average hardness of the sample, and obtaining an average hardness of 21 GPa.
(3) Hardness of the selenium-polycrystalline diamond sintered body obtained in example 2 was measured using a MICRO4 microhardness tester (BUEH L ER L TD) by loading the sample with 2.45N, 4.9N, 9.8N, and 19.6N, respectively, and maintaining the pressure for 15 seconds for each loading, and the hardness of the sample was measured on the asymptotic hardness chart, as shown in FIG. 2, by taking the average value of the hardness.
As can be seen from fig. 2, the asymptotic hardness in fig. 2 is 68GPa, indicating that the selenium-polycrystalline diamond sintered body produced by the method of this embodiment has a better hardness.
In summary, the selenium powder is used as the catalyst, the selenium powder and the diamond powder are mixed and sintered, the polycrystalline diamond sintered body is successfully prepared, the selenium has good oxidation resistance at room temperature, so that the impurities in the polycrystalline diamond sintered body using the selenium as the catalyst are less, the hardness of the polycrystalline diamond sintered body is improved, and the hardness can reach 68GPa or above. And the preparation process omits the processes of catalyst reduction treatment and vacuum presintering in the production process of the traditional metal catalyst polycrystalline diamond sintered body. Greatly simplifying the production process flow.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The polycrystalline diamond sintered body is prepared by sintering diamond powder and selenium powder, wherein gaps among diamond particles are filled with selenium and carbide of the selenium, and D-D bonds are formed among the diamond particles.
2. A method of preparing a polycrystalline diamond sintered compact of a selenium catalyst, comprising:
grinding mixed powder consisting of 31.59-34.047 parts by weight of micron-sized diamond powder and 1.473-4.79 parts by weight of micron-sized selenium powder until the selenium powder becomes amorphous selenium powder;
placing the ground mixed powder into a die, and forming into a blank under the conditions of room temperature and pressure of 5-20 MPa;
sintering and solidifying the blank under the pressure of 6.5-12.5 GPa to obtain a polycrystalline diamond sintered body, wherein selenium and selenium carbide are filled in gaps of diamond particles, and D-D bonds are formed among the diamond particles, wherein the sintering temperature is 1500-1900 ℃.
3. The method for producing a selenium catalyst polycrystalline diamond sintered body according to claim 2, wherein the sintering time is 30 to 3600 s.
4. The method for producing a selenium-catalyzed polycrystalline diamond compact according to claim 2, wherein the sintering temperature is 1600 to 1850 ℃.
5. The method for producing a selenium catalyst polycrystalline diamond sintered body according to claim 2, wherein the pressure at which the blank is sintered and cured is 9 to 12.5 GPa.
6. The method for producing a selenium-catalyzed polycrystalline diamond sintered body according to claim 2, wherein the weight percentage of the selenium powder is 4.2% to 13.2%.
7. The method of producing a selenium-catalyzed polycrystalline diamond compact according to claim 6, wherein the weight percentage of the selenium powder is 4.2 to 6.7%.
8. The method for producing a selenium catalyst polycrystalline diamond sintered body according to claim 2, wherein the diamond powder has a crystal grain size of 0.2 to 10 μm.
9. The method for producing a selenium-catalyzed polycrystalline diamond sintered body according to claim 8, wherein the diamond powder has a crystal grain size of 2 to 5 μm.
10. The method for producing a polycrystalline diamond sintered body with a selenium catalyst according to claim 2, wherein the grain size of the selenium powder is 10 to 30 μm.
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