CN117923842A - Heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material - Google Patents
Heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material Download PDFInfo
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- CN117923842A CN117923842A CN202410060900.9A CN202410060900A CN117923842A CN 117923842 A CN117923842 A CN 117923842A CN 202410060900 A CN202410060900 A CN 202410060900A CN 117923842 A CN117923842 A CN 117923842A
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- dolomite
- pressure
- powder
- composite material
- heat
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 38
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 29
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 29
- 229910000514 dolomite Inorganic materials 0.000 claims abstract description 69
- 239000010459 dolomite Substances 0.000 claims abstract description 69
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 229910021523 barium zirconate Inorganic materials 0.000 claims abstract description 13
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 13
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical group [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910052582 BN Inorganic materials 0.000 description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial 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
- 238000000227 grinding Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials, which relates to the technical field of high-pressure synthesis of raw materials and auxiliary materials of superhard materials, wherein a certain amount of dolomite is taken and placed into a pulverizer to be pulverized, dolomite powder is obtained and then poured into disc-type stirring mill equipment, and then water glass liquid, a dispersing agent and barium zirconate powder are added according to a certain proportion to be mixed and stirred at a rotating speed to obtain dolomite composite powder; pressing the dolomite composite powder into dolomite lining pipe embryo by a four-column hydraulic press; and drying the dolomite lining pipe embryo, and pressing and embedding the dolomite lining pipe embryo into pyrophyllite blocks. The heat-insulating and pressure-maintaining composite material for high-temperature and high-pressure synthesis of the superhard material effectively increases the heat-insulating performance of the inner liner tube, well solves the heat-insulating and heat-preserving effects of the inner liner tube after the cavity is enlarged when the superhard material is synthesized, and simultaneously increases the productivity and reduces the consumption compared with the composite material which enlarges the effective cavity space of the synthesized superhard material.
Description
Technical Field
The invention relates to the technical field of high-pressure synthesis of raw materials and auxiliary materials of superhard materials, in particular to a heat-preservation pressure-maintaining composite material for high-temperature high-pressure synthesis of superhard materials.
Background
Superhard materials are generally materials having a vickers hardness of greater than 40 GPa. Due to its excellent hardness and wear resistance, superhard materials have been widely used in the fields of equipment manufacturing, petroleum, exploration, etc., and by virtue of its high hardness, various materials can be processed by cutting, slicing, grinding, etc.
The synthesis of superhard materials generally requires an extreme environment of high temperature and high pressure, which is currently generally produced domestically by a hexahedral press. In the production and manufacturing process of superhard material, pyrophyllite is used as a pressure transmission sealing medium of a high-pressure cavity, dolomite is used as a heat preservation medium of the high-pressure cavity, namely a dolomite lining pipe is embedded in the pyrophyllite block, and the dolomite lining pipe plays a role in pressure transmission and heat preservation. The dolomite can be decomposed slightly under the conditions of high temperature and high pressure, plays a certain role in pressurizing, has good heat preservation, and is widely applied to the field of synthesizing superhard materials.
Along with the large-scale development of the hexahedral top press, the high-pressure synthesis cavity is enlarged, so that the uniformity of a temperature field in the high-pressure synthesis cavity is ensured, the heat loss is reduced, the requirement of superhard material conversion can be met by a dolomite lining pipe with better heat preservation effect, and in order to stably synthesize the superhard material, the wall thickness of the dolomite lining pipe is thickened in a common method, so that the effective synthesis cavity is reduced, and the synthesis yield of the superhard material is reduced.
The patent CN114455930B discloses a preparation method of a dolomite composite material, which adopts a certain amount of zirconia powder added into dolomite powder, effectively increases the heat insulation performance of a lining pipe on the basis of not affecting the pressure transmission performance of the dolomite, but the zirconia can change phase under the high temperature condition, and has a certain influence on the uniformity of a pressure field of a high-pressure synthesis cavity, thereby affecting the synthesis quality of superhard materials.
Therefore, it is necessary to provide a new heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials to solve the technical problems.
Disclosure of Invention
The invention mainly aims to provide a heat-preservation pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials, which solves the problems that zirconium oxide can generate phase change under the high-temperature condition, and the uniformity of a pressure field of a high-pressure synthesis cavity is influenced to a certain extent, so that the synthesis quality of the superhard materials is influenced.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a heat-preservation pressure-maintaining composite material for high-temperature high-pressure synthesis of superhard materials comprises the following steps:
step one: preparing a proper amount of dolomite, a dispersing agent, barium zirconate powder and water glass liquid;
Step two: placing a certain amount of dolomite into a pulverizer to pulverize, and then filtering through a filter screen to obtain dolomite powder, wherein the granularity of the dolomite powder is 10-40 mu m;
Step three: pouring the crushed dolomite powder into disc type stirring mill equipment, adding water glass liquid and a dispersing agent according to a certain proportion, and then adding barium zirconate powder according to a certain proportion together to carry out rotating speed mixing and stirring in the disc type stirring mill equipment to obtain dolomite composite powder;
Step four: placing the mixed dolomite composite powder into a mould on a four-column hydraulic press, and pressing the dolomite composite powder into a dolomite lining pipe embryo through the four-column hydraulic press;
step five: placing the pressed dolomite lining pipe embryo into a drying box for drying, wherein the drying temperature is 200-300 ℃;
step six: and pressing and embedding the dried dolomite lining pipe into pyrophyllite blocks to prepare the pyrophyllite composite blocks.
Preferably, the dispersing agent in the third step is sodium polyacrylate, and the dosage proportion of the dispersing agent is 0% -0.9%.
Preferably, the granularity of the barium zirconate powder in the third step is in the range of 10-30 μm.
Preferably, the dosage proportion of the barium zirconate powder in the step three is 10-50%.
Preferably, the water glass liquid in the third step is used in an amount of 5-10%.
Preferably, the rotating speed of the pulverizer in the second step is 1200rpm, and the mixing and stirring time is 3-4h.
Compared with the prior art, the invention has the following beneficial effects:
1. Compared with the related art, the invention provides a heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials, which comprises the following components: barium zirconate has a small thermal expansion coefficient (8.7x10 -6℃-1, 25-1080 ℃), a lower thermal conductivity than magnesium oxide, a higher melting point (2700 ℃), a lower chemical reaction activation energy, good thermal shock resistance and excellent corrosion resistance, has a low thermal conductivity of 5.2Wm -1K-1 at room temperature and has excellent properties such as excellent mechanical strength and structural integrity at temperatures close to the melting point. The invention effectively increases the heat preservation performance of the lining pipe on the basis of not affecting the dolomite pressure transmission performance, thus the wall thickness of the lining pipe is not required to be thickened, the heat insulation effect of the lining pipe when the super-hard material is synthesized after the cavity is enlarged is well solved, and meanwhile, compared with the method which enlarges the effective cavity space of the synthesized super-hard material, the invention increases the productivity, reduces the consumption and realizes the advantages of energy saving and synergistic production.
Drawings
FIG. 1 is a general flow chart of the present invention;
FIG. 2 is a flow chart of a second step of the present invention;
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Examples
As shown in fig. 1 and 2, a heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials is prepared by placing 300g of dolomite into a pulverizer for pulverizing, and then filtering by a filter screen to obtain dolomite powder with the granularity of 10 mu m; pouring the crushed dolomite powder into a disc type stirring mill device, adding 5% of water glass liquid and 1% of sodium polyacrylate dispersant, adding 10% of barium zirconate powder, mixing and stirring at a rotating speed in the disc type stirring mill device for 3 hours, and finally obtaining dolomite composite powder; placing the mixed dolomite composite powder into a die on a four-column hydraulic press, and pressing the mixed dolomite composite powder into a dolomite lining tube embryo through the four-column hydraulic press, wherein the pressing pressure is 30MPa; placing the pressed dolomite lining pipe embryo into a drying box for drying, wherein the drying temperature is 200 ℃; and pressing and embedding the dried dolomite lining pipe into pyrophyllite blocks to prepare the pyrophyllite composite blocks. Under the same conditions, the high temperature and high pressure bonding is carried out to form the cubic boron nitride product, and compared with a pure dolomite tube, the yield of the cubic boron nitride product is improved by about 1 percent.
Examples
As shown in fig. 1 and 2, a heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials is prepared by placing 300g of dolomite into a pulverizer for pulverizing, and then filtering by a filter screen to obtain dolomite powder with the granularity of 20 mu m; pouring the crushed dolomite powder into a disc type stirring mill device, adding 7% of water glass liquid and 3% of sodium polyacrylate dispersant, adding 30% of barium zirconate powder, mixing and stirring at a rotating speed in the disc type stirring mill device for 4 hours, and finally obtaining dolomite composite powder; placing the mixed dolomite composite powder into a die on a four-column hydraulic press, and pressing the mixed dolomite composite powder into a dolomite lining tube embryo through the four-column hydraulic press, wherein the pressing pressure is 40MPa; placing the pressed dolomite lining pipe embryo into a drying box for drying, wherein the drying temperature is 300 ℃; and pressing and embedding the dried dolomite lining pipe into pyrophyllite blocks to prepare the pyrophyllite composite blocks. Under the same conditions, the high temperature and high pressure are adopted to form the cubic boron nitride product, and compared with a pure dolomite tube, the yield of the cubic boron nitride product is improved by about 1.5%.
Examples
As shown in fig. 1 and 2, a heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard materials is prepared by placing 300g of dolomite into a pulverizer for pulverizing, and then filtering by a filter screen to obtain dolomite powder with the granularity of 40 mu m; pouring the crushed dolomite powder into a disc type stirring mill device, adding 10% of water glass liquid and 3% of sodium polyacrylate dispersant, adding 50% of barium zirconate powder, mixing and stirring at a rotating speed in the disc type stirring mill device for 4 hours, and finally obtaining dolomite composite powder; placing the mixed dolomite composite powder into a die on a four-column hydraulic press, and pressing the mixed dolomite composite powder into a dolomite lining tube embryo through the four-column hydraulic press, wherein the pressing pressure is 40MPa; placing the pressed dolomite lining pipe embryo into a drying box for drying, wherein the drying temperature is 300 ℃; and pressing and embedding the dried dolomite lining pipe into pyrophyllite blocks to prepare the pyrophyllite composite blocks. Under the same conditions, the high temperature and high pressure bonding is carried out to form the cubic boron nitride product, and compared with a pure dolomite tube, the yield of the cubic boron nitride product is improved by about 2 percent.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The heat-preservation pressure-maintaining composite material for high-temperature high-pressure synthesis of the superhard material is characterized by comprising the following steps of:
step one: preparing a proper amount of dolomite, a dispersing agent, barium zirconate powder and water glass liquid;
Step two: placing a certain amount of dolomite into a pulverizer to pulverize, and then filtering through a filter screen to obtain dolomite powder, wherein the granularity of the dolomite powder is 10-40 mu m;
Step three: pouring the crushed dolomite powder into disc type stirring mill equipment, adding water glass liquid and a dispersing agent according to a certain proportion, and then adding barium zirconate powder according to a certain proportion together to carry out rotating speed mixing and stirring in the disc type stirring mill equipment to obtain dolomite composite powder;
Step four: placing the mixed dolomite composite powder into a mould on a four-column hydraulic press, and pressing the dolomite composite powder into a dolomite lining pipe embryo through the four-column hydraulic press;
step five: placing the pressed dolomite lining pipe embryo into a drying box for drying, wherein the drying temperature is 200-300 ℃;
step six: and pressing and embedding the dried dolomite lining pipe into pyrophyllite blocks to prepare the pyrophyllite composite blocks.
2. The thermal-insulation pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material according to claim 1, wherein the thermal-insulation pressure-maintaining composite material is characterized in that: in the third step, the dispersing agent is sodium polyacrylate, and the dosage proportion of the dispersing agent is 0% -0.9%.
3. The thermal-insulation pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material according to claim 2, wherein the thermal-insulation pressure-maintaining composite material is characterized in that: and in the third step, the granularity range of the barium zirconate powder is 10-30 mu m.
4. A thermal insulation and pressure maintaining composite material for high temperature and high pressure synthesis of superhard material according to claim 3, wherein: in the third step, the dosage proportion of the barium zirconate powder is 10-50%.
5. The heat and pressure preserving composite material for high temperature and high pressure synthesis of superhard material according to claim 4, wherein: the dosage proportion of the water glass liquid in the step three is 5% -10%.
6. The heat and pressure preserving composite material for high temperature and high pressure synthesis of superhard material according to claim 5, wherein: the rotating speed of the pulverizer in the second step is 1200rpm, and the mixing and stirring time is 3-4h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410060900.9A CN117923842A (en) | 2024-01-16 | 2024-01-16 | Heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410060900.9A CN117923842A (en) | 2024-01-16 | 2024-01-16 | Heat-preserving and pressure-maintaining composite material for high-temperature and high-pressure synthesis of superhard material |
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