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Chloride-induced controllable method for preparing transition-metal silicide material with specific crystal phase

A technology of transition metals and silicides, applied in the direction of metal silicides, etc., can solve problems such as complex crystal phase composition

Inactive Publication Date: 2014-05-07
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since transition metal silicides need to be prepared by complex physical or chemical methods in a high-temperature, gas-solid multiphase system, the crystal phase composition of the product is usually relatively complex. Taking the preparation of nickel silicide as an example, the products are mostly nickel silicide (NiSi), silicide Nickel (Ni 2 Si), nickel silicide (Ni 3 Si) and other mixed crystal phases exist, and the existing preparation system is difficult to realize the synthesis of specific crystal phases for specific applications, especially single crystal phase transition metal silicide materials. This problem has become the main factor limiting the application of transition metal silicides. Therefore, the development of new systems or new methods capable of controllably synthesizing transition metal silicides with specific crystal phases plays an important supporting role in the industrial application of transition metal silicide materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Synthesis conditions and sample characteristics of single crystal phase CoSi

[0021] SiO impregnated with 3.0% barium chloride, 10.0% cobalt 2 (87.0%) Loaded precursors were placed in a quartz tube reactor, and high-purity hydrogen (H 2 ) after reduction treatment at 500°C for 2 hours, the SiCl 4 with H 2 The mixed gas (molar ratio is 1:6) is cut into the reactor, the volume space velocity is 10000 / min, the pressure is 0.3 MPa, the temperature is controlled at 900 degrees Celsius, and the CoSi single-phase silicide can be obtained after 6 hours of reaction; the material For catalytic SiCl 4 Hydrodechlorination reaction, resulting product SiHCl 3 The yield is 1.5 times that of the heterogeneous cobalt silicide (without introducing barium chloride) material.

Embodiment 2

[0022] Embodiment 2: single crystal phase Ni 3 Si synthesis conditions and sample characteristics

[0023] SiO impregnated with 1.0% barium chloride, 5.0% nickel 2 (94.0%) loaded precursor is placed in quartz tube reactor, with high-purity hydrogen (H 2 ) after reduction treatment at 500°C for 2 hours, the SiCl 4 with H 2 The mixed gas (molar ratio is 1:6) is cut into the reactor, the volume space velocity is 10000 / min, the pressure is 0.5 MPa, the temperature is controlled at 800 degrees Celsius, and Ni can be obtained after 8 hours of reaction 3 Si single-phase silicide; this material is used to catalyze SiCl 4 Hydrodechlorination reaction, resulting product SiHCl 3 The yield is twice that of the heterogeneous nickel silicide material.

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PUM

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Abstract

The invention relates to a chloride-induced controllable method for preparing a transition-metal silicide material with a specific crystal phase. The method comprises the steps of putting activated carbon which is dipped with barium chloride or calcium chloride and iron, copper, cobalt or nickel, or a silicon oxide precursor into a quartz tube reactor, firstly processing metal by using high-purity hydrogen gas (H2), carrying out full reduction at the temperature of 500 DEG C, then, introducing mixed gas of SiCl4 and H2, of which the mole ratio is 1: (6-8), into the reactor at the gaseous hourly space velocity of 5,000-20,000 / min and the pressure of 0.1-1.0MPa, and reacting for 3-8 hours while controlling the temperature to be 500-900 DEG C, thereby preparing transition-metal silicide. The transition-metal silicide prepared by the method can be expected to provide a support for the related researches and applications of transition-metal silicides with specific crystal phases.

Description

technical field [0001] The invention relates to a new method for controllably synthesizing a transition metal silicide material of a specific crystal phase, in particular a system for inducing the formation of a transition metal silicide material of a specific crystal phase by introducing a chloride salt and its controllable synthesis conditions. Background technique [0002] Transition metal (iron, copper, cobalt, nickel, etc.) silicides have important research and application values ​​in semiconductors, magnetic materials, solar energy, and catalytic industries. The applications of such materials in these fields are based on their special crystal phase structures. Since transition metal silicides need to be prepared by complex physical or chemical methods in a high-temperature, gas-solid multiphase system, the crystal phase composition of the product is usually relatively complex. Taking the preparation of nickel silicide as an example, the products are mostly nickel silici...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/06
Inventor 赵丹王冰邓圣军肖卫明陈超张宁
Owner NANCHANG UNIV
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