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Method for synthesizing Ti3B2N by adopting Pb fluxing agent

A technology of flux and mixing materials, which is applied in chemical instruments and methods, boron compounds, nitrogen compounds, etc., can solve the problems of high synthesis temperature, high production cost at high temperature, and immature synthesis technology, so as to reduce the synthesis temperature and synthesis method. Simple and easy to operate, the effect of reducing production costs

Inactive Publication Date: 2018-07-13
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent application 2016100610872 discloses a new ceramic crystal Ti 3 B 2 N and its preparation method, the application uses a high-temperature solid-state reaction method to synthesize Ti 3 B 2 N, but the application requires a higher synthesis temperature of 1100-1200°C, which is not conducive to the actual production of the product, and the high-temperature production cost is higher, and the synthesis technology disclosed in the application is still immature, and needs to be further improved

Method used

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  • Method for synthesizing Ti3B2N by adopting Pb fluxing agent
  • Method for synthesizing Ti3B2N by adopting Pb fluxing agent
  • Method for synthesizing Ti3B2N by adopting Pb fluxing agent

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Embodiment 1

[0049] The present embodiment provides a kind of adopting Pb flux to synthesize Ti 3 B 2 N method to synthesize Ti 3 B 2 The method of N includes the following steps:

[0050] 1) Weigh TiH respectively 2 Powder, amorphous B powder and hexagonal BN powder, spare;

[0051] and TiH 2 The molar ratio of TiH powder, amorphous B powder and hexagonal BN powder 2 :B:BN=3:1:1;

[0052] 2) the TiH taken in step 1) 2 Powder, amorphous B powder and hexagonal BN powder are put into a container and mixed and stirred evenly to obtain a mixture;

[0053] TiH 2 Powder, amorphous B powder and hexagonal BN powder are put into the container and mixed and stirred evenly. The process is: in TiH 2 powder, amorphous B powder, and hexagonal BN powder were mixed and stirred, then absolute ethanol was added, mixed and stirred for 18 hours, and then dried naturally. Wherein, the addition amount of absolute ethanol must satisfy that this absolute ethanol liquid level completely submerges higher...

Embodiment 2

[0061] The difference between this embodiment and embodiment 1 is: TiH 2 powder, amorphous B powder, hexagonal BN powder, the molar ratio of the three raw materials TiH 2 :B:BN=2.5:1.3:1.3. Others are the same as in Example 1.

[0062] The XRD pattern of the product prepared in this embodiment is shown in Figure 4 . Although still containing Ti 3 B 2 N.TiB 2 and TiN three phases, but the comparison between Example 2 and Example 1 shows that in the sample synthesized in Example 2, Ti 3 B 2 The content of N is reduced compared with that in Example 1.

Embodiment 3

[0064] The difference between this embodiment and Embodiment 1 is that the heating temperature of the quartz tube containing the sample is 600°C. Others are the same as in Example 1.

[0065] The XRD pattern of the product prepared in this embodiment is shown in Figure 5 . Although this example still contains Ti 3 B 2 N.TiB 2 and TiN three phases, but in the sample synthesized in Example 3, Ti 3 B 2 The content of N is reduced compared with that in Example 1.

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Abstract

The invention provides a method for synthesizing Ti3B2N by adopting a Pb fluxing agent. The method comprises the following steps: separately weighing TiH2 powder, amorphous B powder and hexagonal BN powder, wherein a molar ratio of the three raw materials, i.e., the TiH2 powder, the amorphous B powder and the hexagonal BN powder is (2.5 to 3.5): (0.7 to 1.3): (0.7 to 1.3); mixing and uniformly stirring the weighed TiH2 powder, amorphous B powder and hexagonal BN powder in a container, thus obtaining a mixture; adding metal Pb powder which is 15 to 30 percent of the weight of the mixture into the mixture and is to be used as a fluxing agent, uniformly mixing, tabletting, placing tablets into a quartz pipe, vacuumizing, charging Ar gas, and sealing; heating the quartz pipe to 600 to 900 DEGC, and preserving the heat for 12 to 24 hours, thus obtaining a sample; and naturally cooling the sample to room temperature along with the furnace temperature, removing the residual Pb in the sampleby adopting diluted hydrochloric acid, thus obtaining Ti3B2N. By adding the Ph powder fluxing agent, the synthetic temperature of the Ti3B2N is successfully decreased to 600 to 900 DEG C, so that thesynthetic temperature of the TI3B2N can be apparently decreased, which is very important for the actual application. The method is suitable for the industrialized mass production, and the production cost is decreased.

Description

technical field [0001] The invention belongs to the field of structural materials, and in particular relates to a method for synthesizing Ti with Pb flux. 3 B 2 N 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 patent application 2016100610872 discloses a new ceramic crystal Ti 3 B 2 N and its preparation method, the application uses a high-temperature solid-state reaction method to synthesize Ti 3 B 2 N, but this application requires a higher synthesis temperature of 1100-1200°C, which is not conducive to the actual production of products, and the high-temperature production cost is relatively high, and the synthesis technology disclosed in this application is still immature and needs to be further improved. [000...

Claims

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Application Information

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IPC IPC(8): C01B35/14C04B35/58C04B35/622
CPCC01B21/0602C01B35/146C01P2002/72C04B35/58014C04B35/622C04B2235/6562C04B2235/6567
Inventor 胡前库吴庆华周爱国王李波陈进峰侯一鸣秦双红
Owner HENAN POLYTECHNIC UNIV
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