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A kind of ball milling processing raw material to synthesize high-purity ti 3 b 2 nMaterial method

A high-purity, raw material technology, applied in chemical instruments and methods, boron compounds, inorganic chemistry, etc., can solve the problems of high impurities in N samples, and achieve the effects of fast diffusion, reduced content, and fast reaction speed

Active Publication Date: 2021-04-27
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a kind of ball mill treatment raw material synthetic high-purity Ti 3 B 2 approach to N materials to at least address Ti in existing synthetic methods 3 B 2 The N sample has many impurities, thus greatly improving the Ti 3 B 2 Purity and content of N material, for Ti 3 B 2 The practical application of N materials has very good practical significance

Method used

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  • A kind of ball milling processing raw material to synthesize high-purity ti <sub>3</sub> b <sub>2</sub> nMaterial method
  • A kind of ball milling processing raw material to synthesize high-purity ti <sub>3</sub> b <sub>2</sub> nMaterial method
  • A kind of ball milling processing raw material to synthesize high-purity ti <sub>3</sub> b <sub>2</sub> nMaterial method

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Effect test

Embodiment 1

[0076] This embodiment provides a kind of ball mill treatment raw material synthetic high-purity Ti 3 B 2 N material method, preparation of Ti 3 B 2 The method of N includes the following steps:

[0077] 1) Weigh nano-Ti powder, amorphous B powder and hexagonal BN powder respectively, and set aside;

[0078] And the molar ratio of the three raw materials of the nano-Ti powder, the amorphous B powder and the hexagonal BN powder Ti: B: BN=3: 1: 1;

[0079] 2) put the nano-Ti powder, amorphous B powder and hexagonal BN powder weighed in step 1) into a ball mill jar, and the grinding balls adopt agate balls, and agate balls include large balls and small balls, and the diameters of large balls and small balls are 15mm and 5mm respectively, the number ratio of large balls and small balls is 1:5, and the weight ratio of balls to water is 2:1:1, the speed of the ball mill is 300r / min, and the ball mill tank is filled with Ar gas inert gas as a protection Inert gas, ball milled on...

Embodiment 2

[0085] The difference between this embodiment and embodiment 1 is that the ball milling time in step 2) is 60 h, and the other preparation steps are the same as in embodiment 1, and will not be repeated here.

[0086] The product XRD spectrum that this embodiment prepares sees image 3 , containing Ti 3 B 2 Two phases of N and TiN, and the XRD pattern in Example 1 shows that the sample also contains Ti 3 B 2 There are two phases of N and TiN, and the ratio of the two phases basically does not change. It shows that when other parameters are the same, the ball milling time is 48 or 60h. Ti 3 B 2 N sample; at the same time, after ball milling for a certain time to make the raw material amorphized, increasing the ball milling time cannot continue to improve Ti 3 B 2 The purity of the N material.

Embodiment 3

[0088] The difference between this example and Example 1 lies in: in step 4), the temperature is raised to 1200° C. at a rate of 8° C. / min under a nitrogen atmosphere; other preparation steps are the same as those of Example 1, and will not be repeated here.

[0089] The XRD pattern of the sample prepared in this embodiment is shown in Figure 4 , containing Ti 3 B 2 N and TiN two phases, the XRD patterns of Example 3 and Example 1 are similar, indicating that under the same conditions of other parameters, the sintering temperature of 1250 ° C and 1200 ° C can obtain Ti 3 B 2 N samples.

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Abstract

The invention provides a method of ball milling raw materials to synthesize high-purity Ti 3 B 2 The method for N material, comprises the steps: the TiH that weighs respectively 2 Powder, amorphous B powder and hexagonal BN powder are mixed and stirred, and the weighed mixture is put into a ball mill tank, and balls and water are put into the ball mill tank according to a certain proportion, and inert gas is filled as a protective gas for ball milling. ;Take out the sample after ball milling, dry it in a drying oven to obtain a powdery raw material sample; finally raise the temperature to 1200-1300°C under an inert protective atmosphere, keep it warm and cool it to room temperature to obtain high-purity Ti 3 B 2 N material. In the present invention, by improving the synthesis process, the raw materials can be mixed at the nanometer level by using ball milling treatment, so that the raw materials can be mixed more uniformly, and the raw materials can be amorphized, so that the reaction can be carried out more easily, the impurity phase in the reaction product can be reduced, and the impurities in the sample can be successfully removed. TiB 2 Impurities, for Ti 3 B 2 The future practical application of N materials is very important.

Description

technical field [0001] The invention belongs to the field of structural materials, and in particular relates to a method of ball milling raw materials to synthesize high-purity Ti 3 B 2 N material method. Background technique [0002] Ti 3 B 2 N is a new type of ternary layered compound, which has high modulus (Young's modulus 430.22 GPa, shear modulus 181.06 GPa), high strength and so on. At the same time, Ti 3 B 2 N has a very low density (theoretical density 4.80g / cm 3 ). [0003] Chinese invention patent applications 2016100610872 and 2016106036190 respectively disclose "a new type of ceramic crystal Ti 3 B 2 N and its preparation method" and "a synthetic high-purity Ti 3 B 2 The method of N" all adopts high-temperature solid-state reaction preparation method; Chinese invention patent applications 2018101697425, 201810169743X, 2018101517916 and 2018101697410 disclose the use of low melting point metals Al, Pb, Sn and Zn as fluxes to synthesize Ti 3 B 2 N's m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/14
CPCC01B35/146
Inventor 胡前库吴庆华周爱国王李波侯一鸣秦双红
Owner HENAN POLYTECHNIC UNIV
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