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Method for preparing negative thermal expansion Mn3 (Cu0.5Ge0.5)N bulk material

A technology of cu0.5ge0.5 and negative thermal expansion, which is applied in the field of rapid preparation of Mn3N bulk materials, can solve the problems of small powder compacted sample size, long preparation cycle, and long reaction time, so as to shorten the preparation cycle and reaction time Short, reduced reaction time effect

Inactive Publication Date: 2010-09-22
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of preparation method has the following limitations: the reaction time is long, and the usual reaction process is 780-850 ° C for 50-70 hours; the prepared powder compacted sample is small in size and low in strength; all use Mn 2 N is used as the starting material, while the preparation of Mn 2 The process of N compound is to carry out solid-gas reaction at 700-750°C for 60 hours, resulting in a long period of material preparation

Method used

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  • Method for preparing negative thermal expansion Mn3 (Cu0.5Ge0.5)N bulk material
  • Method for preparing negative thermal expansion Mn3 (Cu0.5Ge0.5)N bulk material
  • Method for preparing negative thermal expansion Mn3 (Cu0.5Ge0.5)N bulk material

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Experimental program
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Effect test

Embodiment 1

[0018] Mn powder and nitrogen are subjected to solid-gas reaction in a vacuum furnace, the nitrogen pressure in the furnace is 1.02MPa, the reaction temperature is 750°C, and the reaction time is 6 hours to obtain Mn 2 N 0.86 single phase powder. Will Mn 2 N 0.86 , Cu and Ge powders according to Mn 3 (Cu 0.5 Ge 0.5 ) The stoichiometric ratio of the N compound was weighed and mixed uniformly. The mixed powder was sintered under the protection of argon by spark plasma sintering. The process parameters were: sintering temperature 720°C, sintering pressure 60MPa, and heat preservation at sintering temperature for 30min.

[0019] The Mn that embodiment 1 prepares 3 (Cu 0.5 Ge 0.5 ) Phase analysis of N bulk material see figure 1 (a), negative thermal expansion performance test curve see figure 2 , and the characterization parameters of the negative thermal expansion properties of the material are shown in Table 1.

Embodiment 2

[0021] Mn powder and nitrogen were subjected to a solid-gas reaction in a vacuum furnace, the nitrogen pressure in the furnace was 1.04MPa, the reaction temperature was 800°C, and the reaction time was 5 hours to obtain Mn 2 N 0.86 single phase powder. Will Mn 2 N 0.86 , Cu and Ge powders according to Mn 3 (Cu 0.5 Ge 0.5 ) The stoichiometric ratio of N compounds was weighed and mixed evenly, and the mixed powder was sintered under the protection of argon by spark plasma sintering method. The process parameters were: sintering temperature 760°C, sintering pressure 50MPa, and heat preservation at sintering temperature for 20min.

[0022] The Mn that embodiment 2 prepares 3 (Cu 0.5 Ge 0.5 ) Phase analysis of N bulk material see figure 1 (b), negative thermal expansion performance test curve see image 3 , and the characterization parameters of the negative thermal expansion properties of the material are shown in Table 1.

Embodiment 3

[0024] Mn powder and nitrogen were subjected to a solid-gas reaction in a vacuum furnace. The nitrogen pressure in the furnace was 1.08 MPa, the reaction temperature was 1000 ° C, and the reaction time was 4 hours to obtain Mn 2 N 0.86 single phase powder. Will Mn 2 N 0.86 , Cu and Ge powders according to Mn 3 (Cu 0.5 Ge 0.5 ) The stoichiometric ratio of the N compound was weighed and mixed evenly, and the mixed powder was sintered under the protection of argon by spark plasma sintering. The process parameters were: sintering temperature 820°C, sintering pressure 30MPa, and heat preservation at sintering temperature for 5min.

[0025] The Mn that embodiment 3 prepares 3 (Cu 0.5 Ge 0.5 ) Phase analysis of N bulk material see figure 1 (c), negative thermal expansion performance test curve see Figure 4 , and the characterization parameters of the negative thermal expansion properties of the material are shown in Table 1.

[0026]

[0027] The Mn prepared in the emb...

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Abstract

The invention relates to a method for preparing a negative thermal expansion Mn3 (Cu0.5Ge0.5)N bulk material, which belongs to the technical field of novel functional materials and powder metallurgy. The prior method for preparing a Mn3 (Cu1-xGex)N compound has the problems of long preparation period, high energy-consumption and the like. The method comprises the following steps: preparing single-phase Mn2N0.86 compound powder through solid-gas reaction; evenly mixing the Mn2N0.86 compound powder with Cu and Ge powder according to the stoichiometric ratio of a Mn3 (Cu0.5Ge0.5)N compound; and performing sintering densification on the mixed powder under the protection of argon by using a spark plasma sintering (SPS) method so as to obtain the Mn3 (Cu0.5Ge0.5)N bulk material with negative thermal expansion characteristic. The method has the characteristics of short preparation period and low energy-consumption, and the prepared bulk material has high density.

Description

technical field [0001] The invention belongs to the technical field of new functional materials and powder metallurgy, in particular to a Mn with negative thermal expansion characteristics 3 (Cu 0.5 Ge 0.5 ) Rapid preparation method of N bulk materials. Background technique [0002] A new type of anti-perovskite structure material Mn with special negative thermal expansion (Negative Thermal Expansion, NTE) functional properties 3 AN (A=Cu, Zn, etc.), has unique advantages such as typical metal properties, isotropic thermal properties, negative thermal expansion coefficient and controllable temperature range of NTE, making it suitable for high-precision optical equipment, refraction grating, printed circuit Important potential in the field of military technology such as boards and heat sinks. In this type of compound, Mn doped with Ge 3 (Cu 1-x Ge x )N compounds have relatively better NTE properties, and their NTE onset temperature is around room temperature. With the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F3/105B22F9/16
Inventor 宋晓艳孙中华
Owner BEIJING UNIV OF TECH
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