CN107879341B - Diamond subzero treatment method - Google Patents
Diamond subzero treatment method Download PDFInfo
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- CN107879341B CN107879341B CN201711067632.XA CN201711067632A CN107879341B CN 107879341 B CN107879341 B CN 107879341B CN 201711067632 A CN201711067632 A CN 201711067632A CN 107879341 B CN107879341 B CN 107879341B
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Abstract
The invention discloses a diamond subzero treatment method, which comprises the steps of placing diamonds with the granularity of 30/35 meshes and 35/40 in a liquid nitrogen subzero box, carrying out subzero treatment, reducing the temperature of the liquid nitrogen subzero box from 20 ℃ to-180 ℃ in steps, slowly heating to room temperature, then heating to 120 ℃ after preserving the temperature for a period of time, and finally slowly returning the temperature to the room temperature. The invention can obviously improve the integral static pressure strength of 30/35-mesh and 35/40-mesh diamond groups, and the number of diamond particles with the static pressure strength in the range of 600-800 MPa after cryogenic treatment is improved by about 20 percent. The cryogenic treatment can permanently change the internal crystal structure of the material, improve the dislocation condition of the crystal and release part of residual stress, thereby affecting the performance of the material.
Description
Technical Field
The invention relates to a cryogenic treatment method for diamond, in particular to a method for improving the performance of a diamond material through liquid nitrogen cryogenic treatment, and belongs to the field of materials science.
Background
The cryogenic treatment is a technique of placing an object to be treated (material) in a specific ultralow temperature environment to change the microstructure and structure of the object to be treated (material), thereby improving the material performance to a certain extent. The minimum treatment temperature can reach-196 ℃. In the beginning of the 20 th century, the primary application of cryogenic technology in the field of aviation was mainly in the application of liquid oxygen chemical rocket oxidizers and the use of refrigeration equipment in spacecraft, as well as liquid oxygen fuels, nuclear power rocket propellants and the like. Later researchers began attempting to apply cryogenic techniques to portions of the materials being processed, which increased the safety of the aircraft in high pressure vessels and the stability of some critical component performance.
China is the first major country for producing ultra-hard materials (artificial diamond and cubic boron nitride) in the world at present, but the strength of the artificial diamond has a great space for improving. The artificial diamond contains impurities such as B, Ni, Mn, Co, Si, Al, Ca, Mg and the like due to existence of a melting medium in the growth process, thereby showing different colors and performances. The impurities in diamond are often aligned along the axis of symmetry of the crystal, and are often distributed in the form of lines, flakes, rods or particles. The diamond has impurities inside, and crystal defects, lattice dislocations and the like formed during the crystal growth process reduce the performance of the diamond to various degrees. In particular, the hydrostatic strength of diamond, which has a significant effect on the working performance of diamond tools, decreases as the amount of impurities, defects, and residual stress therein increases. Therefore, there is a need to find a method for post-treating diamond to improve its performance.
The cryogenic treatment can permanently change the internal crystal structure of the material, improve the dislocation condition of the crystal and release part of residual stress, thereby affecting the performance of the material.
Disclosure of Invention
The invention aims to provide a cryogenic treatment method for diamond. The artificial diamond particles are treated by means of a liquid nitrogen cryogenic treatment process, so that the internal tissue structure of the artificial diamond particles is changed, and the static pressure strength of the artificial diamond particles is improved. The comparison of the static pressure strength of the diamond particles before and after the cryogenic treatment proves that the cryogenic treatment process can obviously improve the overall static pressure strength of two batches of diamond particles with the granularity of 30/35 meshes and 35/40 meshes. After 30/35-mesh batches of diamond particles are subjected to liquid nitrogen cryogenic treatment, the average static pressure strength value is improved by 23.17%, and the quantity of diamond particles with the static pressure strength within the range of 600-800 MPa after the cryogenic treatment is improved by about 20% compared with that before the cryogenic treatment; after 35/40-mesh batches of diamond particles are subjected to liquid nitrogen cryogenic treatment, the average static pressure intensity value is improved by 1.21%, the number of diamond particles with the static pressure intensity within the range of 600-800 MPa after the cryogenic treatment is improved by about 20% compared with the number of diamond particles before the cryogenic treatment, and meanwhile, the number of diamond particles with the static pressure intensity within the range of 200-400 MPa is reduced by 1 time compared with the number of diamond particles before the cryogenic treatment. The increase of the static pressure strength of the diamond will make contribution and change to the huge application markets (such as mechanical processing, oil and gas drilling, geological drilling, stone processing and the like).
The subzero treatment method of the diamond in the invention is that the granularity of the diamond to be treated is 30/35 meshes and 35/40 meshes, and the treatment method comprises the following steps: placing diamond with the granularity of 30/35 meshes and diamond with the granularity of 35/40 meshes in a liquid nitrogen cryogenic box, carrying out cryogenic treatment, reducing the temperature of the cryogenic box from 20 ℃ at room temperature to-180 ℃ step by step, slowly heating to room temperature, then heating the cryogenic box to 120 ℃ after preserving the temperature for a period of time, and finally slowly returning the cryogenic box to the room temperature.
The specific treatment method comprises the following steps: placing diamonds with particle sizes of 30/35 meshes and 35/40 meshes in a liquid nitrogen cryogenic box, and reducing the temperature of the cryogenic box from 20 ℃ to-80 ℃ within 15 min; keeping the temperature at-80 deg.C for 20 min; reducing the temperature from-80 ℃ to-180 ℃ within 15 min; keeping the temperature at-180 ℃ for 20 min; increasing the temperature from-180 ℃ to 20 ℃ within 30 min; keeping the temperature at 20 ℃ for 20 min; increasing from 20 deg.C to 120 deg.C within 15 min; keeping the temperature at 120 ℃ for 20 min; naturally cooling from 120 ℃ to 20 ℃.
The invention has the beneficial effects that:
tests prove that the cryogenic treatment process can obviously improve the integral static pressure strength of two batches of diamonds of 30/35 meshes and 35/40 meshes, and the quantity of diamond particles with the static pressure strength within the range of 600-800 MPa after the cryogenic treatment is improved by about 20 percent compared with that before the cryogenic treatment. The cryogenic treatment can permanently affect the internal crystal structure of the material and release part of residual stress, thereby changing the material performance and being a great driving force for huge material markets.
Drawings
FIG. 1 is a static pressure intensity profile of 30/35 mesh un-cryogenically treated diamond.
FIG. 2 is a static pressure intensity distribution curve of 30/35 mesh cryogenic diamond.
FIG. 3 is a static pressure intensity profile of 35/40 mesh un-cryogenically treated diamond.
FIG. 4 is a static pressure intensity distribution curve of 35/40 mesh cryogenically treated diamond.
Detailed Description
Two kinds of artificial diamond with different grain sizes of 30/35 meshes and 35/40 meshes are adopted. And (3) screening and grouping two diamonds with different granularities, placing the diamonds in a liquid nitrogen cryogenic box, and carrying out cryogenic treatment.
The specific treatment method comprises the following steps: the temperature of the liquid nitrogen deep cooling box is reduced from 20 ℃ to-80 ℃ within 15 min; keeping the temperature at-80 deg.C for 20 min; reducing the temperature from-80 ℃ to-180 ℃ within 15 min; keeping the temperature at-180 ℃ for 20 min; increasing the temperature from-180 ℃ to 20 ℃ within 30 min; keeping the temperature at 20 ℃ for 20 min; increasing from 20 deg.C to 120 deg.C within 15 min; keeping the temperature at 120 ℃ for 20 min; naturally cooling from 120 ℃ to 20 ℃. And (4) carrying out strength test on the treated diamond particles by using an intelligent particle strength tester.
The increase of the hydrostatic hardness of the artificial diamond after the low-temperature cycle treatment is caused by the irreversible change of the original stress-strain state of the crystal caused by the defect structure adjustment of the crystal lattice. The residual stress in the diamond is usually generated under the conditions of high pressure and high temperature in the formation process of the artificial diamond, and the residual stress belongs to the category of microscopic thermal stress. Meanwhile, the diamond contains a certain amount of impurities, and the difference of the thermal expansion coefficients of the impurities and the diamond crystals is also an important reason for the generation of internal stress. And for different treatment processes with different particle sizes, the release degree of the internal stress is different, so that the treatment effect is different.
The experimental results of the 30/35 mesh diamond are shown in fig. 1 and 2, and fig. 1 is a static pressure intensity distribution curve of 30/35 mesh diamond particles without cryogenic treatment; FIG. 2 is a static pressure intensity distribution curve of 30/35 mesh cryogenically treated diamond particles.
The static pressure intensity curve height of the 30/35-mesh subzero treatment diamond is improved to some extent compared with that of the diamond which is not subzero treated, and the number of the diamonds with the static pressure intensity within the range of 600-800 MPa after treatment is improved by about 20 percent; the average hydrostatic strength of the diamond is improved by 23.17 percent. This demonstrates that cryogenic treatment has some effect on the properties of the diamond particles.
The experimental results of the 35/40-mesh diamond are shown in fig. 3 and 4, and fig. 3 is a static pressure intensity distribution curve of 35/40-mesh diamond without cryogenic treatment; FIG. 4 is a static pressure intensity distribution curve of 35/40 mesh cryogenically treated diamond.
The overall curve height of the hydrostatic strength of the diamond treated by the 35/40-mesh deep cooling is improved compared with that of the diamond not treated by the deep cooling. The average static pressure intensity value is improved by 1.21%, the number of diamond particles with the static pressure intensity within the range of 600-800 MPa after the deep cooling treatment is improved by about 20% compared with the number of diamond particles before the deep cooling treatment, and meanwhile, the number of diamond particles with the static pressure intensity within the range of 200-400 MPa is reduced by 1 time compared with the number of diamond particles before the deep cooling treatment. The integral hydrostatic strength of the batch of diamond is proved to be obviously improved after the deep cooling treatment.
The static pressure strength of the 30/35-mesh and 35/40-mesh diamond groups after cryogenic treatment is remarkably improved, and the static pressure strength is improved most in the range of 600-800 MPa. The cryogenic treatment improves the overall hydrostatic strength of the diamond stack to some extent.
The obtained experimental result can prove that the static pressure strength of the diamond treated at low temperature is improved, so that the diamond has good application prospect: the drilling life of the drill bit can be prolonged without additional cost and modification of the manufacturing process of the drill bit.
The cryogenic treatment experiment of the diamond shows that the change of the strength performance of the diamond is explained to a great extent, and the microstructure of the diamond, such as crystal form, crystal face, defect, dislocation and the like, is changed under the low-temperature process. The cryogenic treatment can change the strength of the artificial diamond, release partial internal residual stress of the crystal and improve the stress condition of the crystal in the diamond.
The low temperature treatment of the artificial diamond by using the low temperature treatment technology before the drill bit is manufactured by the artificial diamond has great advantages. The working capacity of the drill bit is improved due to the increase of the static pressure hardness of the artificial diamond embedded in the drill bit.
Claims (1)
1. A diamond cryogenic treatment method, the granularity of the diamond to be treated is 30/35 meshes and 35/40 meshes, and the treatment method comprises the following steps: placing diamonds with a granularity of 30/35 meshes and 35/40 meshes in a liquid nitrogen deep cooling box, and reducing the temperature of the liquid nitrogen deep cooling box from 20 ℃ to-80 ℃ within 15 min; keeping the temperature at-80 deg.C for 20 min; reducing the temperature from-80 ℃ to-180 ℃ within 15 min; keeping the temperature at-180 ℃ for 20 min; increasing the temperature from-180 ℃ to 20 ℃ within 30 min; keeping the temperature at 20 ℃ for 20 min; increasing from 20 deg.C to 120 deg.C within 15 min; keeping the temperature at 120 ℃ for 20 min; naturally cooling from 120 ℃ to 20 ℃.
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