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Ultrafine diamond micropowder synthesis method

A technology of diamond micropowder and synthesis method, which is applied in the direction of diamond, etc., which can solve the problems of high cost, low purity and low diamond yield of ultrafine micropowder, and achieve narrow grain size distribution range, high purity and high yield. high effect

Active Publication Date: 2020-03-10
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has a series of thorny problems, such as extremely low diamond yield, low purity and serious adsorption of impurities on the surface
Therefore, the ultrafine diamond powder synthesized by this method often needs to undergo extremely complicated follow-up treatments before it can be further applied to the ultrafine grinding and polishing of precision components, which naturally leads to the high cost of this ultrafine powder. high

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  • Ultrafine diamond micropowder synthesis method
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  • Ultrafine diamond micropowder synthesis method

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Experimental program
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Effect test

Embodiment 1

[0037] A method for synthesizing ultrafine diamond powder, comprising the following steps:

[0038] Step 1. Sample pre-compression: use a tablet press to press the precursor to a density of 1.1-1.35g / m 3 , the precursors include naphthalene, anthracene, nitrogen anthracene, phenanthroline;

[0039] Step 2. Pressurization: Boost the pressure from normal pressure to the target pressure, keep the pressure under the target pressure, heat during the pressure keeping stage, and after the pressure keeping is completed, reduce the pressure to normal pressure to obtain ultrafine diamond powder.

[0040] In the step 2, the target pressure is 10Gpa-13Gpa, and the pressure is maintained at the target pressure for 100min-300min. The holding time is slightly longer than the total heating time.

[0041] Further, the heating process in the pressure holding stage in the step 2 is as follows: firstly, the temperature is raised to 620°C-650°C, the heating rate is 10-20°C / s, and the temperature...

Embodiment 2

[0048] Naphthalene synthetic ultrafine diamond powder:

[0049] Press the precursor naphthalene to a density of 1.23 g / m using a tablet press 3, first increase the pressure from normal pressure to the target pressure of 13Gpa, and heat at the target pressure. , the heating rate is 0.5°C / min, and the temperature is kept at 680°C for 120 minutes; then the temperature is raised to 720°C, and the heating rate is 0.5°C / min; finally, the temperature is raised to the target temperature of 1680°C at 10°C / s, and annealed after holding at the target temperature for 5s , after the pressure holding is completed, the pressure is reduced to normal pressure to obtain diamond powder.

[0050] Carry out Raman, XRD, FE-SEM characterization to the material synthesized in above-mentioned embodiment 2, obtain its basic experiment characterization data figure respectively as follows figure 1 , figure 2 , image 3 shown, from figure 1 Raman Peak is located at 1331.6cm -1 , figure 2 The XRD ...

Embodiment 3

[0052] Naphthalene synthetic ultrafine diamond powder:

[0053] Press the precursor naphthalene to a density of 1.18 g / m using a tablet press 3 , from normal pressure to the target pressure of 12.5Gpa, heating at the target pressure, the heating process is as follows: first raise the temperature to 640°C, the heating rate is 10°C / s, keep the temperature at 640°C for 18 minutes; then raise the temperature to 690°C ℃, the heating rate is 0.8°C / min, and the temperature is kept at 690°C for 100 minutes; then the temperature is raised to 730°C, and the heating rate is 0.6°C / min; finally, the temperature is raised to the target temperature of 1800°C at 25°C / s, and the temperature is kept at the target temperature for 300s. After the fire, after the pressure holding is completed, the pressure is reduced to normal pressure to obtain diamond powder.

[0054] The FE-SEM scanning image of the product of embodiment 3 is as Figure 4 shown, and the appearance characterized by FE-SEM Fi...

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Abstract

The invention discloses an ultrafine diamond micropowder synthesis method including: (1) pretabletting of sample: tabletting a precursor into the density of 1.1-1.35 g / m<3> with a tabletting machine,the precursor including naphthalene, anthracene, acridine, and phenanthroline; (2) pressurization: increasing the pressure from normal pressure to target pressure and maintaining the pressure under the target pressure, heating the sample during the pressure maintenance, and after the pressure maintenance, reducing the pressure to the normal pressure to prepare the ultrafine diamond micropowder, the target pressure being 10-13 GPa, and the pressure maintenance lasting for 100-300 min under the target pressure. The method is free of use of metal catalysts, so that introduction of metal impurities is avoided; the ultrafine diamond micropowder with grain size being less than or equal to 10 [mu]m and having excellent crystal appearance development. The method avoid the time and labor consumingprocesses such as mechanical crushing and shaping treatment and is high in yield of diamond. The ultrafine diamond micropowder is high in purity and is narrow in distribution range of the granularity.The product can satisfy the requirement of ultrafine grinding and polishing for various types of precision instruments without complex subsequent processing.

Description

technical field [0001] The invention relates to the technical field of diamond synthesis, in particular to a method for synthesizing ultrafine diamond powder. Background technique [0002] Diamond is currently the material with the highest hardness known, and is widely used in cutting, grinding, grinding and polishing of various hard materials such as cemented carbide, ceramics, gemstones, and optical crystals. Diamond micropowder usually refers to diamond powder materials with a grain size distribution in the range of 0.1 μm to 54 μm. It is mainly used for ultra-precision finishing (grinding and polishing) of the workpiece surface and is the most important application form of diamond. Diamond powder with a grain size of less than 15 μm is also called ultrafine diamond powder. This powder is suitable for ultrafine grinding and polishing of single crystal silicon wafers for semiconductor integrated circuits, computer disks, and various optoelectronic crystal components. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/26
CPCC01B32/26
Inventor 刘童李振臧金浩
Owner ZHENGZHOU UNIV
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