CN109569435B - High-temperature high-pressure synthesis cavity - Google Patents
High-temperature high-pressure synthesis cavity Download PDFInfo
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- CN109569435B CN109569435B CN201811542365.1A CN201811542365A CN109569435B CN 109569435 B CN109569435 B CN 109569435B CN 201811542365 A CN201811542365 A CN 201811542365A CN 109569435 B CN109569435 B CN 109569435B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
Abstract
The invention discloses a high-temperature high-pressure synthesis cavity which comprises two half cavities, wherein the two half cavities are oppositely buckled to form a cavity body, the half cavities are cuboid, the half cavities are made of pyrophyllite, through holes are formed in the centers of the upper surface and the lower surface of the half cavities, magnesium oxide layers are embedded in the rest surfaces of the half cavities, and high-temperature components are arranged in the through holes. According to the invention, the magnesium oxide layer is embedded on the pyrophyllite to form the composite block assembly combining the pyrophyllite and the magnesium oxide layer, the pyrophyllite enables the assembly to have good sealing performance under high pressure, and the magnesium oxide has relatively higher bulk modulus relative to the pyrophyllite, and the magnesium oxide is used as a pressure transmission medium, so that the pressure of the anvil can be effectively transmitted to the inside of the cavity, and the pressure in the cavity can reach a higher level. The high-temperature component has good heat preservation and heating performance, ensures the concentration of heat and prevents the heat from diffusing to the top hammer.
Description
Technical Field
The invention relates to the technical field of superhard composite materials, in particular to a high-temperature high-pressure synthesis cavity.
Background
The synthesis of diamond, cubic boron nitride and other superhard and superhard composite materials mostly adopts a cubic press, 6 anvil hammers surround a cubic body, and a pressure transmission medium cavity with corresponding size can be placed in the cubic body. When the cubic press works, 6 jack hammers act on the cubic pressure transmission medium and generate high pressure in the cavity. During loading, part of the pressure transfer medium is squeezed, and the medium distributed among the 6 top hammers forms sealing edges at 12 edges of the cube. Part of external loading force directly acts on the pressure transmission medium through the top hammer surface to generate high pressure in the high-pressure cavity; the other part acts on the sealing edge area, and the sealing of the high-pressure cavity is formed by the internal friction force of the sealing edge material and the friction force between the sealing edge material and the outer surface of the anvil. People generate high pressure through high-pressure equipment and a synthesis cavity, and the high pressure and the high temperature are a limit condition for material synthesis through auxiliary heating.
High quality products and high performance materials require higher synthesis pressures and more stable temperature environments. In the aspect of pressure, people invent a plurality of methods to improve the pressure inside the synthetic cavity in production, so that the pressure inside the cavity for production is stabilized at about 6 GPa. The method for improving the internal pressure of the cavity is divided into two methods: 1. the performance of the equipment is improved; 2. the structure of the synthetic cavity is improved. The method for improving the performance of the equipment comprises the following steps: the cylinder diameter of the six-surface jack is enlarged, the area of a jack hammer is reduced, and the like; the method for improving the structure of the synthesis cavity mainly comprises the following steps: the method comprises the steps of adopting a pressurizing unit, additionally arranging a pre-sealing edge, changing and assembling materials of internal components and the like. In production, however, the diameter of the press cylinder cannot be further enlarged when the diameter is enlarged to a certain extent, and the top hammer can reach the self-stress limit when the diameter is reduced to a certain extent, so that the top hammer is easy to crack and cause loss; the modes of adopting a pressurizing unit, additionally arranging a sealing edge and the like also bring problems of cost increase, unstable production and the like to production. Temperature aspect: the heating material is a material which has high resistivity and is not easy to be compressed, and at present, the adopted graphite material is easy to be compressed under the high-pressure condition.
Disclosure of Invention
The invention aims to provide a high-temperature high-pressure synthesis cavity to solve the problems in the prior art and enable high temperature and high pressure to be formed in the cavity.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a high-temperature high-pressure synthesis cavity which comprises two half cavities, wherein the two half cavities are oppositely buckled to form a cavity body, the half cavities are cuboid, the half cavities are made of pyrophyllite, through holes are formed in the centers of the upper surface and the lower surface of the half cavities, magnesium oxide layers are embedded in the other surfaces of the half cavities, and high-temperature components are arranged in the through holes.
Preferably, the high-temperature assembly comprises a shielding pipe, an isobaric pipe, a heating pipe and a heat insulation pipe which are sequentially arranged from inside to outside along the circumferential direction of the through hole, shielding sheets are arranged at two ends of the shielding pipe, isobaric sheets are arranged at two ends of the isobaric pipe, heating sheets are arranged at two ends of the heating pipe, heat insulation rings are arranged at two ends of the heat insulation pipe, a conducting strip is arranged on the outer side of the through hole in the axial direction, and a steel bowl is arranged on the outer side of the conducting strip in the axial direction.
Preferably, the shielding tube is a hexagonal boron nitride tube, the shielding sheet is a molybdenum cup, a niobium cup or a zirconium cup, and the thicknesses of the shielding tube and the shielding sheet are 0.5-2 mm.
Preferably, the isobaric tube is a zirconium dioxide tube, the isostatic pressing sheet is a zirconium dioxide sheet, the thickness of the isobaric tube and the isostatic pressing sheet is 1-5mm, and the content of zirconium dioxide in the isobaric tube and the isostatic pressing sheet is 5-30%.
Preferably, the heating pipe and the heating sheet are made of graphite, and the thickness of the heating pipe and the heating sheet is 0.5-3 mm.
Preferably, the heating pipe and the heating sheet are made of tantalum foil, and the thickness of the heating pipe and the thickness of the heating sheet are 0.01-0.2 mm.
Preferably, the thermal insulation pipe and the thermal insulation ring are made of zirconia, and the thickness of the thermal insulation pipe and the thermal insulation ring is 1-3 mm.
Preferably, the length and width of the half cavity are both a, the height of the half cavity is a/2, the sizes of the upper surface and the lower surface of the half cavity are a × a, and the sizes of the rest surfaces of the half cavity are a × a/2; the minimum distances from the upper end face, the left end face and the right end face of the magnesium oxide layer to the surfaces of the adjacent half cavities are g, and g is more than or equal to 3mm and less than or equal to 20 mm; the thickness of the magnesium oxide layer embedded into the semi-cavity is d, and d is more than or equal to 5mm and less than or equal to 20 mm; the thickness of the pyrophyllite at the position where each surface of the semi-cavity is overlapped with the magnesium oxide layer is e, and e is more than or equal to 0mm and less than or equal to 5 mm.
Preferably, the lower end face of the magnesium oxide layer is flush with the lower surface of the semi-cavity, angles formed by the upper end face of the magnesium oxide layer and the horizontal direction, the left end face of the magnesium oxide layer and the vertical direction, and the right end face of the magnesium oxide layer and the vertical direction are all theta, and theta is greater than or equal to 0 degree and less than or equal to 30 degrees; the length and the width of the outer side surface of the magnesium oxide layer are respectively greater than the length and the width of the inner side surface of the magnesium oxide layer.
Preferably, the lower surfaces of the two half cavities are attached to each other.
Compared with the prior art, the invention has the following technical effects:
according to the invention, the magnesium oxide layer is embedded on the pyrophyllite to form the composite block assembly combining the pyrophyllite and the magnesium oxide layer, the pyrophyllite enables the assembly to have good sealing performance under high pressure, and the magnesium oxide has relatively higher bulk modulus relative to the pyrophyllite, and the magnesium oxide is used as a pressure transmission medium, so that the pressure of the anvil can be effectively transmitted to the inside of the cavity, and the pressure in the cavity can reach a higher level. The high-temperature component has good heat preservation and heating performance, ensures the concentration of heat and prevents the heat from diffusing to the top hammer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram of a high temperature and high pressure synthesis chamber of the present invention;
FIG. 2 is an exploded view of a high temperature, high pressure synthesis chamber of the present invention;
FIG. 3 is a schematic view of a half-cavity of the present invention;
FIG. 4 is a schematic cross-sectional view of a half-cavity of the present invention;
wherein: 1-half cavity, 2-magnesium oxide layer, 3-heat insulation pipe, 4-heating pipe, 5-isobaric pipe, 6-shielding pipe, 7-shielding sheet, 8-isobaric pressing sheet, 9-heating sheet, 10-heat insulation ring, 11-conducting sheet and 12-steel bowl.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The invention aims to provide a high-temperature high-pressure synthesis cavity, which is used for solving the problems in the prior art and enabling high temperature and high pressure to be formed in the cavity.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example one
As shown in fig. 1-4: the embodiment provides a synthetic cavity of high temperature high pressure, including two half cavity 1, two relative locks of half cavity 1 form the cavity, and half cavity 1 is the cuboid, and half cavity 1 adopts the pyrophyllite to make, and the center department of the upper surface of half cavity 1 and lower surface is provided with the through-hole, and the diameter of through-hole is b, and b is 40 mm, and all the other each sides of half cavity 1 are inlayed and are had magnesium oxide layer 2, are provided with high temperature assembly in the through-hole. The high-temperature assembly comprises a shielding pipe 6, an isobaric pipe 5, a heating pipe 4 and a heat insulation pipe 3 which are sequentially arranged from inside to outside along the circumferential direction of the through hole, shielding sheets 7 are arranged on the inner sides of two ends of the shielding pipe 6, the shielding pipe 6 is a hexagonal boron nitride pipe, the shielding sheets 7 are molybdenum cups, niobium cups or zirconium cups, and the size of the shielding pipe 6 is
The size of the shielding plate 7 is
The isobaric tube 5 is provided with isobaric sheets 8 at the inner sides of two ends, the isobaric tube 5 is a zirconium dioxide tube, the isobaric sheets 8 are zirconium dioxide sheets, and the size of the isobaric tube 5 is
The size of the equal-pressure sheet 8 is
The content of zirconium dioxide in the isobaric tube 5 and the isobaric plate 8 is 5-30%. The heating sheets 9 are arranged on the inner sides of the two ends of the heating pipe 4, the heating pipe 4 and the heating sheets 9 are made of graphite, and the size of the heating pipe 4 is
The heating sheet 9 has a size of
The inner sides of both ends of the heat-insulating pipe 3 are provided with heat-insulating rings 10, the heat-insulating pipe 3 and the heat-insulating rings 10 are made of zirconia, and the heat-insulating pipe 3 has a size of
The size of the heat insulating ring 10 is
The heat insulation pipe 3 and the heat insulation ring 10 enable the cavity to have good heat insulation performance, ensure the concentration of heat, prevent the heat from diffusing to the top hammer and conduct electricity. The heat insulating ring 10 is provided with a conductive sheet 11 on the outside in the axial direction of the through-hole, and the conductive sheet 11 has a size of
The conducting strip 11 is provided with a steel bowl 12 along the axial outer side of the through hole, and the size of the steel bowl 12 is
In this embodiment, the length and width of the half cavity 1 are both a, a is 60mm, the height of the half cavity 1 is a/2, the dimensions of the upper surface and the lower surface of the half cavity 1 are a × a, and the dimensions of the rest surfaces of the half cavity 1 are a × a/2; the minimum distance from the upper end face, the left end face and the right end face of the magnesium oxide layer 2 to the surface of the adjacent half cavity 1 is g, and g is 10 mm; the thickness of the magnesium oxide layer 2 embedded into the half cavity 1 is d, and d is 10 mm; the thickness of the pyrophyllite at the position where each surface of the half cavity 1 is overlapped with the magnesium oxide layer 2 is e, and the e is 0 mm. The lower end face of the magnesium oxide layer 2 is flush with the lower surface of the semi-cavity 1, the angles formed by the upper end face of the magnesium oxide layer 2 and the horizontal direction, the left end face of the magnesium oxide layer 2 and the vertical direction, and the right end face of the magnesium oxide layer 2 and the vertical direction are all theta, and theta is more than or equal to 0 degree and less than or equal to 30 degrees; the length and width of the outer side surface of the magnesium oxide layer 2 are respectively greater than the length and width of the inner side surface. The outer surface of the magnesium oxide layer 2 had a length of 2f and a width of f, where f was 20 mm and f + g was a/2. The lower surfaces of the two half cavities 1 are attached to form a high-temperature high-pressure synthesis cavity, and the top hammer applies pressure to six surfaces of the high-temperature high-pressure synthesis cavity.
Example two
The embodiment provides a synthetic cavity of high temperature high pressure, including two half cavity 1, two relative locks of half cavity 1 form the cavity, and half cavity 1 is the cuboid, and half cavity 1 adopts the pyrophyllite to make, and the center department of the upper surface of half cavity 1 and lower surface is provided with the through-hole, and the diameter of through-hole is b, and b is 55 mm, and all the other each sides of half cavity 1 are inlayed and are had magnesium oxide layer 2, are provided with high temperature assembly in the through-hole. The high-temperature assembly comprises a shielding pipe 6, an isobaric pipe 5, a heating pipe 4 and a heat insulation pipe 3 which are sequentially arranged from inside to outside along the circumferential direction of the through hole, shielding sheets 7 are arranged on the inner sides of two ends of the shielding pipe 6, the shielding pipe 6 is a hexagonal boron nitride pipe, the shielding sheets 7 are molybdenum cups, niobium cups or zirconium cups, and the size of the shielding pipe 6 is
The size of the shielding plate 7 is
The isobaric tube 5 is provided with isobaric sheets 8 at the inner sides of two ends, the isobaric tube 5 is a zirconium dioxide tube, the isobaric sheets 8 are zirconium dioxide sheets, and the size of the isobaric tube 5 is
The size of the equal-pressure sheet 8 is
The content of zirconium dioxide in the isobaric tube 5 and the isobaric plate 8 is 5-30%. Heating sheets 9 are arranged on the inner sides of the two ends of the heating pipe 4, the heating pipe 4 and the heating sheets 9 are made of tantalum foil, and the heating pipe 4 and the heating sheets 9The thickness of the heating plate 9 was 0.1 mm. The inner sides of both ends of the heat-insulating pipe 3 are provided with heat-insulating rings 10, the heat-insulating pipe 3 and the heat-insulating rings 10 are made of zirconia, and the heat-insulating pipe 3 has a size of
The size of the heat insulating ring 10 is
The heat insulation pipe 3 and the heat insulation ring 10 enable the cavity to have good heat insulation performance, ensure the concentration of heat, prevent the heat from diffusing to the top hammer and conduct electricity. The heat insulating ring 10 is provided with a conductive sheet 11 on the outside in the axial direction of the through-hole, and the conductive sheet 11 has a size of
The conducting strip 11 is provided with a steel bowl 12 along the axial outer side of the through hole, and the size of the steel bowl 12 is
In this embodiment, the length and width of the half cavity 1 are both a, a is 75mm, the height of the half cavity 1 is a/2, the dimensions of the upper surface and the lower surface of the half cavity 1 are a × a, and the dimensions of the rest surfaces of the half cavity 1 are a × a/2; the minimum distance from the upper end face, the left end face and the right end face of the magnesium oxide layer 2 to the surface of the adjacent half cavity 1 is g, and g is 10 mm; the thickness of the magnesium oxide layer 2 embedded into the half cavity 1 is d, and d is 8 mm; the thickness of the pyrophyllite at the position where each surface of the half cavity 1 is overlapped with the magnesium oxide layer 2 is e, and the e is 4.5 mm. The lower end face of the magnesium oxide layer 2 is flush with the lower surface of the semi-cavity 1, the angles formed by the upper end face of the magnesium oxide layer 2 and the horizontal direction, the left end face of the magnesium oxide layer 2 and the vertical direction, and the right end face of the magnesium oxide layer 2 and the vertical direction are all theta, and theta is more than or equal to 0 degree and less than or equal to 30 degrees; the length and width of the outer side surface of the magnesium oxide layer 2 are respectively greater than the length and width of the inner side surface. The outer surface of the magnesium oxide layer 2 had a length of 2f and a width of f, where f was 27.5 mm and f + g was a/2. The lower surfaces of the two half cavities 1 are attached to form a high-temperature high-pressure synthesis cavity, and the top hammer applies pressure to six surfaces of the high-temperature high-pressure synthesis cavity.
In the embodiment, the magnesium oxide layer 2 is embedded on the pyrophyllite to form a composite block assembly combining the pyrophyllite and the magnesium oxide layer 2, the pyrophyllite enables the cavity to have good sealing performance under high pressure, the magnesium oxide has relatively high bulk modulus relative to the pyrophyllite, and the magnesium oxide is used as a pressure transmission medium, so that the pressure of the anvil can be effectively transmitted into the cavity, and the pressure in the cavity can reach 8-10 GPa. The high-temperature component has good heat preservation and heating performance, so that heat generated by the heating material is locked in the high-temperature high-pressure cavity and is not radiated outwards, the heat loss is reduced, and a sample can be synthesized in a higher and more stable temperature environment. In addition, the heat insulation material also plays a role in heat insulation, so that the heat transferred to the hard alloy top hammer is reduced, and the hammer consumption is reduced. Ensuring the concentration of heat and preventing the heat from spreading to the top hammer.
The principle and the implementation mode of the present invention are explained by applying specific examples in the present specification, and the above descriptions of the examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (9)
1. A high-temperature high-pressure synthesis cavity is characterized in that: the structure comprises two half cavities which are oppositely buckled to form a cavity, wherein the half cavities are cuboid, the half cavities are made of pyrophyllite, through holes are formed in the centers of the upper surface and the lower surface of the half cavities, magnesium oxide layers are embedded in the rest surfaces of the half cavities, and high-temperature components are arranged in the through holes;
the high-temperature assembly comprises a shielding pipe, an isobaric pipe, a heating pipe and a heat insulation pipe which are sequentially arranged from inside to outside along the circumferential direction of the through hole, shielding sheets are arranged at two ends of the shielding pipe, isobaric sheets are arranged at two ends of the isobaric pipe, heating sheets are arranged at two ends of the heating pipe, heat insulation rings are arranged at two ends of the heat insulation pipe, a conductive sheet is arranged on the outer side of the through hole in the axial direction, and a steel bowl is arranged on the outer side of the through hole in the axial direction.
2. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the shielding tube is a hexagonal boron nitride tube, the shielding sheet is a molybdenum cup, a niobium cup or a zirconium cup, and the thickness of the shielding tube and the thickness of the shielding sheet are 0.5-2 mm.
3. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the isobaric tube is a zirconium dioxide tube, the isostatic pressing piece is a zirconium dioxide piece, the thickness of the isobaric tube and the isostatic pressing piece is 1-5mm, and the content of zirconium dioxide in the isobaric tube and the isostatic pressing piece is 5-30%.
4. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the heating pipe and the heating sheet are made of graphite, and the thickness of the heating pipe and the thickness of the heating sheet are 0.5-3 mm.
5. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the heating pipe and the heating sheet are made of tantalum foil, and the thickness of the heating pipe and the thickness of the heating sheet are 0.01-0.2 mm.
6. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the thermal insulation pipe and the thermal insulation ring are made of zirconium oxide, and the thickness of the thermal insulation pipe and the thermal insulation ring is 1-3 mm.
7. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the length and the width of the half cavity are both a, the height of the half cavity is a/2, the sizes of the upper surface and the lower surface of the half cavity are a x a, and the sizes of the rest surfaces of the half cavity are a x a/2; the minimum distances from the upper end face, the left end face and the right end face of the magnesium oxide layer to the surfaces of the adjacent half cavities are g, and g is more than or equal to 3mm and less than or equal to 20 mm; the thickness of the magnesium oxide layer embedded into the semi-cavity is d, and d is more than or equal to 5mm and less than or equal to 20 mm; the thickness of the pyrophyllite at the position where each surface of the semi-cavity is overlapped with the magnesium oxide layer is e, and e is more than or equal to 0mm and less than or equal to 5 mm.
8. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the lower end face of the magnesium oxide layer is flush with the lower surface of the semi-cavity, the angles formed by the upper end face of the magnesium oxide layer and the horizontal direction, the left end face of the magnesium oxide layer and the vertical direction, and the right end face of the magnesium oxide layer and the vertical direction are all theta, and theta is more than or equal to 0 degree and less than or equal to 30 degrees; the length and the width of the outer side surface of the magnesium oxide layer are respectively greater than the length and the width of the inner side surface of the magnesium oxide layer.
9. The high-temperature high-pressure synthesis chamber according to claim 1, wherein: the lower surfaces of the two half cavities are attached to each other.
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| CN111545132B (en) * | 2020-05-11 | 2022-08-19 | 中国有色桂林矿产地质研究院有限公司 | Ultrahigh pressure synthesis cavity |
| CN114768681A (en) * | 2022-04-20 | 2022-07-22 | 中国有色桂林矿产地质研究院有限公司 | Pressure transmission device for superhard composite material |
| CN115041096B (en) * | 2022-06-07 | 2023-08-15 | 中国工程物理研究院核物理与化学研究所 | High-temperature high-pressure device of two-sided press |
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