CN114984858B - High-temperature high-pressure device of hexahedral top press - Google Patents
High-temperature high-pressure device of hexahedral top press Download PDFInfo
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- CN114984858B CN114984858B CN202210764367.5A CN202210764367A CN114984858B CN 114984858 B CN114984858 B CN 114984858B CN 202210764367 A CN202210764367 A CN 202210764367A CN 114984858 B CN114984858 B CN 114984858B
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- 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
- B01J3/067—Presses using a plurality of pressing members working in different directions
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Abstract
The invention discloses a high-temperature and high-pressure device of a hexahedral press, which comprises six top hammers of a hinged hexahedral press, six secondary press anvils with double chamfer structures, a cube synthetic block, an integral supporting frame and a cushion block for supporting and adjusting the positions of the secondary press anvils. Wherein the integral frame is provided with an anvil mounting channel for mounting the secondary anvil; the cushion blocks are adhered to the side surfaces of the secondary pressing anvils and used for adjusting the positions of the 6 secondary pressing anvils entering the supporting frame, so that the 6 secondary pressing anvils can synchronously pressurize the cube synthetic blocks. The invention overcomes the defect that the existing six-sided pressing machine needs to be replaced when being installed, is matched with an integral frame and a cushion block, is more beneficial to the stable and rapid assembly and accurate positioning of a high-pressure device, and adopts a double-chamfer structure pressing anvil to reasonably optimize the dimensional relationship of the pressing hammer, the pressing anvil and a synthetic block, thereby realizing the synthesis of high-temperature, high-pressure and large-volume samples.
Description
Technical Field
The invention belongs to the technical field of static high pressure, and particularly relates to a high-temperature high-pressure device of a hexahedral top press.
Background
High-pressure science has penetrated almost to the vast majority of leading-edge subject research, and is considered as the research field most likely to make a major scientific breakthrough in the future. In industry, the synthesis of superhard materials such as artificial diamond and cubic boron nitride is not separated from the high-pressure and high-temperature means, and the equipment mainly used in the synthesis is a large-cavity static high-pressure device. The large-cavity static high-pressure device mainly comprises a double-sided top press device and a multi-sided top press device.
In the multi-face top press device, the hinge type hexahedral top press is compact in structure, relatively simple in processing and installation and relatively low in manufacturing cost, but the highest pressure achieved by the hinge type hexahedral top press device is about 7GPa, so that the requirements of synthesis and high-pressure scientific development of novel superhard materials cannot be met. In recent years, he Duanwei et al (CN 100486684C) developed a six-octahedral static high pressure device (6-8 stage supercharging mode) based on a hinged hexahedral press, enabling the cavity pressure to reach 50GPa. Also based on hinged hexahedral press Zhu Pinwen et al (CN 102389750B) a six-hexahedral static high pressure device was developed(6-6 two stage boost mode) the chamber can be brought to the same pressure range as a six-eight pressure chamber. Although the pressure range of the hinge type hexahedral press is improved by several times by the 6-8 pressure cavity and the 6-6 pressure cavity designed by the former, the volume of the synthesized sample is far smaller than that of the hinge type hexahedral press, and the sample volume is reduced by 3 orders of magnitude (from 1000 mm) 3 Reduced to 1mm 3 ). Novel superhard materials such as Nanometer Polycrystalline Diamond (NPD) have wide application prospect due to excellent mechanical, optical and other properties, and the synthetic pressure is more than 10-12 GPa. Thus, the pressure of the hexahedral press was made to be 10GPa or more while having a large volume of sample (100 mm 3 ) Has important significance for industrialization of novel superhard materials such as NPD and the like.
Therefore, it is needed to design a high-temperature and high-pressure device of a hexahedral press, which can better consider the cavity pressure and the sample size, widen the application range of the hinged hexahedral press, and meet the requirements of novel superhard material synthesis and high-pressure scientific development. The high-temperature and high-pressure device of the hexahedral press, provided by the patent, has the advantages that the sample volume can reach 500mm under the pressure of 12GPa through the novel 6-6 secondary anvil design 3 Fills the range of the cavity pressure and the sample size which cannot be achieved by the prior hexahedral top press and the secondary pressurizing mode.
Disclosure of Invention
To achieve the purpose, a high-temperature and high-pressure device of a hexahedral top press is provided.
The high-temperature high-pressure device of the hexahedral press comprises six top hammers of a hinged hexahedral press, six secondary press anvils, a cube synthetic block, an integral supporting frame and a cushion block for supporting the secondary press anvils; the supporting frame is a hollow square structure with square edge sections, the square same as the solid square is removed relatively from the center of six faces of the supporting frame, and a channel formed by removing part is an anvil mounting channel; each secondary anvil passes through the anvil mounting channel and moves along the axis of the anvil under the drive of the corresponding anvil, so as to pressurize the cube synthesizing block; the cushion blocks are adhered to the side surfaces of the secondary pressing anvils and used for adjusting the positions of the 6 secondary pressing anvils entering the supporting frame, so that the lengths of the secondary pressing anvils entering the supporting frame are equal, and the synchronous pressurization of the 6 secondary pressing anvils on the cube synthetic blocks is realized.
Optionally, the side length of the hammer face of the top hammer is larger than the side length of the bottom face of the secondary anvil, the side length of the hammer face of the top hammer is smaller than the side length of the supporting frame, and the side length of the anvil face of the secondary anvil is smaller than the side length of the cube synthetic block.
Optionally, the ratio of the side length of the secondary anvil stock surface to the side length of the cube synthetic block is (0.5-0.8) to 1.0.
Optionally, the end face of the secondary anvil is of a double-chamfer structure, the first chamfer is smaller than 45 degrees and smaller than the second chamfer, and the first chamfer is used for forming a sealing edge when the secondary anvil extrudes the cube synthetic block.
Optionally, the first chamfer is 41 ° and the second chamfer is 46 °.
Optionally, the secondary anvil is made of tungsten carbide or sintered diamond; the pressure transmitting medium in the cube synthesis block is pyrophyllite, zirconia or magnesia; the cube synthesis block also comprises a heating pipe, and the cushion block is made of wood or pyrophyllite.
Optionally, the support frame is made of metal or polytetrafluoroethylene. For heating or resistance testing, materials such as non-conductive polytetrafluoroethylene are required.
The working process of the invention comprises the following steps:
after the cube composite block is assembled, the cube composite block and 6 secondary anvils are put into an integral supporting frame together, and a sample is positioned in the center of the cube composite block. And then, sticking a cushion block for supporting the secondary anvil on the outer side of the supporting frame and the side surface of the secondary anvil so as to ensure that the cube synthetic block is positioned at the centers of the six secondary anvils and the supporting frame and ensure that 6 secondary anvils advance synchronously in the pressurizing process. After the cube synthesis block, the secondary anvil, the supporting frame and the cushion block are assembled into a whole, the high-temperature high-pressure device and the high-temperature high-pressure device are placed in the center of the hexahedral top press. When the pressurizing is started, 6 top hammers of the hexahedral top press are used for pressurizing the high-temperature high-pressure device placed in the center, and 6 secondary anvil blocks are driven to pressurize the cube synthetic block and the sample positioned in the center of the synthetic block, so that the sample generates a high-pressure environment. The beneficial effects of the invention are as follows: (1) The novel six-sided press high-temperature high-pressure device is in a 6-stage pressurizing mode, and a one-stage top hammer of the hinged six-sided press is shared by the novel six-sided press high-temperature high-pressure device and the 6-8-stage pressurizing mode, so that the two modes can be freely switched, the technical defect that the top hammer needs to be replaced when the existing six-sided press is installed is overcome, the rapid assembly and the accurate positioning of the high-temperature high-pressure device are realized, and related experiments are completed with high efficiency. (2) The support frame used in the invention is integrated, and is matched with the cushion block to carry out position adjustment and accurate positioning of the secondary anvil, so that the cube synthetic block is ensured to be positioned at the center of a pressurizing area formed by the anvil surface of the secondary anvil, and synchronous pressurizing of six surfaces of the cube synthetic block is truly realized. In addition, after the integral support frame enables the secondary anvil and the cube synthetic block to be assembled, the integral stability of the integral support frame is better, even if the integral placement positions of the secondary anvil, the cube and the support frame after being assembled are not at the center of a space surrounded by the anvil face of the anvil, a certain anvil is firstly contacted with the secondary anvil, and the integral support frame can not be scattered in the process of pushing the secondary anvil, the cube and the support frame to approach toward the center, so that the integral support frame can still keep better integrity, ensure that the cube synthetic block is positioned at the center of a pressurizing area formed by the anvil face of the secondary anvil, and keep subsequent synchronous pressurizing. (3) According to the invention, the double-chamfer structure is arranged on the secondary anvil, so that the synthetic pressure and the synthetic size between the primary loading mode and the 6-8 secondary pressurizing mode of the hinge type hexahedral press are realized, the application range of the hinge type hexahedral press is widened, and the experimental cost is reduced. The synthesis pressure of the invention is more than 10GPa, the maximum diameter of the sample can reach 8mm, the synthesis pressure of the cavity and the size of the sample are well considered, and a plurality of application scenes such as resistance, differential heat and ultrasonic experiments under high temperature and high pressure can be satisfied.
Drawings
FIG. 1 is a schematic view of a structure of a high temperature and high pressure apparatus of a hexahedral press;
FIG. 2 is an assembled schematic view of a support frame + anvil + spacer;
FIG. 3 is a schematic diagram of a two-stage anvil structure;
in the figure: 1. a top hammer, a secondary anvil, a cube synthetic block, a supporting frame and a cushion block, wherein the top hammer is a secondary anvil; 21. the first chamfer, 22. The second chamfer, 23. The anvil face, 24. The third chamfer, 41. The anvil mounting channel.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without creating effort for a person skilled in the art.
The present invention will be described in further detail with reference to the following detailed description and the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
As shown in fig. 1 and 2, a high-temperature and high-pressure apparatus of a hexahedral press includes six rams 1 of a hinged hexahedral press, six secondary anvils 2, a cubic composite block 3, an integral support frame 4, and a pad 5 for supporting the secondary anvils.
Each anvil 1 corresponds to a secondary anvil 2. A cube synthesizing block 3 is arranged in the space surrounded by the 6 secondary anvils 2. Hammer face side length L of top hammer 1 C Is larger than the side length L of the bottom surface of the secondary anvil 2 D Hammer face side length L of top hammer 1 C Smaller than the side length L of the supporting frame 4 J Side length L of anvil surface of secondary anvil 2 Z Smaller than the side length L of the cube composite block 3 H . In order to ensure the pressurizing effect, the ratio of the side length of the anvil surface of the secondary anvil 2 to the side length of the cube synthesizing block 3 is generally (0.5-0.8) to 1.0. In this embodiment, the side lengths of the top hammer face, the bottom face of the secondary anvil and the support frame are 34mm, 32mm and 48mm, respectively.
The supporting frame 4 is a hollow square structure with square edge sections and square cross sections, the square is removed relatively from the center positions of six faces of the solid square, and a channel formed by removing part is an anvil mounting channel 41; each secondary anvil 2 passes through the anvil mounting channel 41 and moves along its own axis under the drive of its respective anvil 1, thereby pressurizing the cube synthesis block 3. The cushion block 5 is adhered to the side surface of the secondary anvil 2 and used for adjusting the positions of 6 secondary anvils 2 entering the supporting frame, so that the lengths of the secondary anvils 2 entering the supporting frame 4 are ensured to be equal, and the synchronous pressurization of the 6 secondary anvils on the cube synthesizing blocks 3 is further realized. As shown in fig. 2, the pad 5 is composed of 24 rectangular parallelepiped made of soft materials such as wood or pyrophyllite, and is used for supporting six secondary anvils 2 placed in the support frame 4. The four sides of each secondary anvil are respectively added with a cushion block, two opposite planes of the cushion blocks are respectively flush with the outer plane of the cube support frame and the outer plane of the secondary anvil, and the length of the side of the secondary anvil cannot exceed the outer edge part of the support frame.
The integral support frame is matched with the cushion block to carry out position adjustment and accurate positioning of the secondary anvil, so that the cube synthetic block is ensured to be positioned at the center of a pressurizing area formed by the anvil surface of the secondary anvil, and synchronous pressurizing of six surfaces of the cube synthetic block is truly realized. In addition, after the integral support frame enables the secondary anvil and the cube synthetic block to be assembled, the integral stability of the integral support frame is better, even if the integral placement positions of the secondary anvil, the cube and the support frame after being assembled are not at the center of a space surrounded by the anvil face of the anvil, a certain anvil is firstly contacted with the secondary anvil, and the integral support frame can not be scattered in the process of pushing the secondary anvil, the cube and the support frame to approach toward the center, so that the integral support frame can still keep better integrity, ensure that the cube synthetic block is positioned at the center of a pressurizing area formed by the anvil face of the secondary anvil, and keep subsequent synchronous pressurizing.
In order to ensure the sealing and holding of the cube synthesizing block 3 in the jacking process and further realize the high-pressure synthesis environment, the end face of the secondary anvil 2 generally adopts a double-chamfer structure, as shown in fig. 3. Wherein the first chamfer 21 < 45 DEG < the second chamfer 22. So that a sealing edge is easily formed at the first chamfer 21 upon pressing. By varying the angular extent of the first chamfer 21, different resultant pressures can be achieved. The smaller the end face the higher the pressure generated. Wherein, when the side length of the end face is 14mm and the side length of the cube synthetic block 3 is 20mm, the pressure of more than 12GPa can be generated, and the diameter and the height of the corresponding sample are 5-8mm. In this embodiment, the first chamfer 21 is 41 ° and the second chamfer is 46 °. For ease of installation, the edges of the secondary anvil 2 are also provided with a third chamfer 24.
The secondary anvil 2 is made of tungsten carbide or sintered diamond; the pressure transmitting medium in the cube synthesis block 3 is pyrophyllite, zirconia or magnesia.
The support frame 4 is made of metal or polytetrafluoroethylene. For heating or resistance testing, materials such as non-conductive polytetrafluoroethylene are required. And the supporting frame is not extruded in the pressurizing process, so that the supporting frame can be reused.
In the pressure loading process of the high-temperature high-pressure device of the hexahedral press, the hinge type hexahedral press drives the secondary anvil to pressurize the assembly, and the pressure is transmitted to the sample cavity through the pressure transmission medium to form a high-pressure environment in the sample cavity. The cube synthesis block 3 also comprises a heating pipe, wherein the heating pipe can be made of graphite, lanthanum chromate or rhenium metal, and the heating pipe generates heat through self resistance after passing current, so that a high-temperature environment is formed in the sample cavity. The conducting electrode is a molybdenum column or a steel plug which is arranged above and below the heating pipe, and the electrode is contacted with the anvil surface of the secondary anvil, so that current is transmitted to the heating pipe through the anvil.
The six secondary anvils of the novel high-temperature high-pressure device of the hexahedral press are independent and insulated, and can be used as electrodes for carrying out experiments such as resistance, differential heat, ultrasound and the like under high temperature and high pressure.
Claims (5)
1. The high-temperature and high-pressure device of the hexahedral press is characterized by comprising six top hammers of a hinged hexahedral press, six secondary press anvils, a cube synthetic block, an integral supporting frame and a cushion block for supporting the secondary press anvils; the supporting frame is a hollow square structure with square edge sections, the square same as the solid square is removed relatively from the center of six faces of the supporting frame, and a channel formed by removing part is an anvil mounting channel; each secondary anvil passes through the anvil mounting channel and moves along the axis of the anvil under the drive of the corresponding anvil, so as to pressurize the cube synthesizing block; the cushion blocks are adhered to the side surfaces of the secondary pressing anvils and used for adjusting the positions of 6 secondary pressing anvils entering the supporting frame, so that the lengths of the secondary pressing anvils entering the supporting frame are equal, and the synchronous pressurization of the 6 secondary pressing anvils on the cube synthetic blocks is realized; the end face of the secondary anvil is of a double-chamfer structure, wherein a first chamfer is used for forming a sealing edge when the secondary anvil extrudes a cube synthetic block, the first chamfer is 41 degrees, and the second chamfer is 46 degrees.
2. The high temperature and high pressure apparatus of claim 1, wherein the anvil face side length of the anvil is greater than the bottom face side length of the secondary anvil, the anvil face side length of the anvil is less than the side length of the support frame, and the anvil face side length of the secondary anvil is less than the side length of the cube composite block.
3. The high temperature and high pressure apparatus of a cubic press as set forth in claim 1 wherein the ratio of the side length of the anvil surface of the secondary anvil to the side length of the cube composite block is (0.5-0.8) to 1.0.
4. The high temperature and high pressure apparatus of the hexahedral press according to claim 1, wherein the secondary anvil is made of tungsten carbide or sintered diamond; the pressure transmitting medium in the cube synthesis block is pyrophyllite, zirconia or magnesia; the cube synthesis block also comprises a heating pipe, and the cushion block is made of wood or pyrophyllite.
5. The high temperature and high pressure apparatus of a hexahedral press according to claim 1, wherein the support frame is made of metal or polytetrafluoroethylene; the support frame used for heating or resistance testing experiments was made of polytetrafluoroethylene.
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CN110947340A (en) * | 2019-12-24 | 2020-04-03 | 内蒙古唐合科技有限公司 | Frame type cubic apparatus press |
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US20020025354A1 (en) * | 1998-03-10 | 2002-02-28 | Hall David R. | Reduced mass unitary cartridges with internal intensification for ultra high-pressure high-temperature press apparatus |
JP2006281289A (en) * | 2005-04-01 | 2006-10-19 | Sumitomo Heavy Industries Techno-Fort Co Ltd | Ultrahigh pressure generator, and member for storing object to be pressurized |
CN100581642C (en) * | 2006-06-05 | 2010-01-20 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Outer frame for hexahedral top press machine and hexahedral top press machine with outer frame |
CN101804313B (en) * | 2010-04-09 | 2012-12-19 | 四川大学 | Anvil-pre-sealing edge high pressure device |
CN102188935B (en) * | 2011-04-13 | 2013-05-29 | 四川大学 | Novel large-cavity high-pressure device |
CN102389750B (en) * | 2011-10-04 | 2013-10-23 | 吉林大学 | Ultra-high pressure device based on hinged-type hexahedral press |
CN106179124A (en) * | 2016-08-30 | 2016-12-07 | 四川大学 | A kind of anvil for producing high pressure |
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