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A high-temperature and high-pressure preparation method of single-phase nanocubic-titanium boride

A high-temperature, high-pressure, nano-cubic technology is applied in the high-temperature and high-pressure preparation of a single-phase cubic-titanium boride, and the regulation of nanoscale grains. Effect of reaction time and small particle size

Active Publication Date: 2021-12-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is difficult to obtain nanometer-sized materials through traditional high-temperature sintering

Method used

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  • A high-temperature and high-pressure preparation method of single-phase nanocubic-titanium boride
  • A high-temperature and high-pressure preparation method of single-phase nanocubic-titanium boride
  • A high-temperature and high-pressure preparation method of single-phase nanocubic-titanium boride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] High-purity titanium powder (Ti) with a particle size of 50 to 100 nanometers and boron powder (B) with a particle size of 100 to 200 nanometers are mixed according to a molar ratio of 1:0.8, and the raw materials of the mixture are pressed by a hydraulic press according to the size of the synthesis cavity. Into a cylindrical shape (diameter 4mm, height 2.5mm), after the sample is pressed and formed, it is put into a synthesis chamber, and a six-sided hydraulic press is used to provide a high-temperature and high-pressure environment to synthesize the sample. In order to ensure the uniformity of the temperature of the synthesis chamber during the process of synthesizing the sample, the graphite heat pipe is used for side heating in the assembly chamber. At the same time, in order to ensure that the sample does not react with the heated graphite tube, the chamber of the synthesis sample is made of hexagonal boron nitride. Protect. The synthesis pressure is controlled to ...

Embodiment 2

[0027] Adopt the raw material identical with embodiment 1, mol ratio. The synthesis pressure was set to 1, 2, 3, 4, 5 GPa respectively, the synthesis temperature was 1000K, and other conditions and steps were the same as in Example 1. After stopping the heating, the sample is naturally cooled to room temperature and then the pressure is released. The X-ray diffraction results of the obtained sample are shown in Figure 4 , SEM test results see Figure 5 . c-TiB was prepared under these conditions (the remaining small amount of elemental Ti can be removed with hot sulfuric acid). From the SEM image of the sample, it can be found that the samples prepared under the pressure range of 1-5GPa are all nanoparticles, but when the pressure is greater than 3GPa, the samples are dense and difficult to crush.

Embodiment 3

[0029] Using the same raw materials as in Example 1, mixed according to the molar ratio of 1:1, the sample powder was pressed and formed using the same assembly as in Example 1, the synthesis pressure was 3.0GPa, and the synthesis temperature was set to 700K, 850K, and 1000K respectively. The pressure holding time was 30 minutes. After the heating was stopped, the sample was naturally cooled to room temperature and then the pressure was released. The X-ray diffraction results of the obtained sample are shown in Figure 6 . The sample prepared under this condition has already produced c-TiB at 850K, but there is more remaining Ti. With the increase of temperature, the content of c-TiB increases and the content of Ti decreases; at 1000K, the content of Ti is very small.

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Abstract

The high-temperature and high-pressure preparation method of a single-phase nano-cubic-titanium boride of the present invention belongs to the technical field of nano-binary boride preparation, and the raw materials are mixed with nano-titanium powder and nano-boron powder; cooled after being kept at high temperature and high pressure for 30 minutes The pressure is released, the obtained sample is ground into powder, and the remaining titanium powder is removed with hot sulfuric acid, and then washed and dried with water to obtain a single-phase nano-cubic titanium boride. The invention utilizes nanometer starting materials to effectively reduce the reaction energy, cross the generation interval of o-TiB, and prepare single-phase c-TiB. The method is simple and easy to operate, the sample has high purity, small and uniform particle size, and is suitable for subsequent industrial applications.

Description

technical field [0001] The invention belongs to the technical field of nanometer binary boride preparation, and relates to a method for preparing a cubic titanium boride (c-TiB) single phase at high temperature and high pressure and the regulation and control of nanoscale grains. Background technique [0002] TiB is a potential hard functional material due to its high melting point, high hardness, and good electrical conductivity. Its excellent physical properties come from the fact that Ti metal can provide abundant d-shell electrons, and there are diverse hybridization forms of B elements. Therefore, TiB is widely used in composite materials. For example, the composite materials of TiB and TiC exhibit excellent wear resistance; the composite materials of TiB and silicide enhance the performance of materials. At present, there are two phases in TiB, c-TiB and orthorhombic titanium boride (o-TiB), but it is difficult to prepare single-phase bulk materials, and there are few...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/04B82Y40/00
Inventor 朱品文连敏陶强董书山崔田李志慧
Owner JILIN UNIV
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