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Large-scale preparation method of single-phase NiS2 powder

A powder and single-phase technology, which is applied in the field of large-scale preparation of single-phase NiS2 powder, can solve problems such as powder synthesis difficulties, and achieve the effects of good conductivity, simple process, and uniform particle size

Active Publication Date: 2020-05-08
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For single-phase NiS 2 The difficulty of powder synthesis, the purpose of the present invention is to provide a high-performance single-phase NiS 2 The large-scale preparation method of powder, the present invention synthesizes NiS by high-temperature solid-phase method 2 Powder, using the principle that elemental sulfur will sublimate at a high temperature above 450°C, remove excess elemental sulfur, and finally obtain high-performance single-phase NiS 2 Powder

Method used

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  • Large-scale preparation method of single-phase NiS2 powder
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  • Large-scale preparation method of single-phase NiS2 powder

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Embodiment 1

[0028] Such as figure 1 The process flow shown, a single-phase NiS 2 The large-scale preparation method of powder, the preparation method comprises the following steps: commercially available metal nickel powder and sublimation sulfur powder are initial raw materials, first weigh 10Kg metal nickel powder and 25Kg sublimation sulfur powder and fully mix, under Ar atmosphere, The mixed powder was placed in a graphite crucible with a cover, and the crucible was placed in a tubular atmosphere furnace, and the temperature was raised to 680 °C at a heating rate of 5 °C / min, kept for 2 hours, and then cooled to room temperature with the furnace. Collect synthetic materials for grinding and sieving, and conduct XRD and differential thermal tests. The XRD result is NiS 2 phase, without other impurity phases, the result of differential heat is that the elemental sulfur content is 2.1wt%, and then the sulfur removal process is carried out: under the Ar atmosphere, the sieved NiS 2 The ...

Embodiment 2

[0030] Such as figure 1 The process flow shown, a single-phase NiS 2The large-scale preparation method of powder, the preparation method comprises the following steps: commercially available metal nickel powder and sublimated sulfur powder are the initial raw materials, first weigh 10Kg metal nickel powder and 15Kg sublimated sulfur powder to fully mix, under Ar atmosphere, The mixed powder was placed in a graphite crucible with a cover, and the crucible was placed in a tubular atmosphere furnace. The temperature was raised to 650 °C at a heating rate of 5 °C / min, kept for 2 hours, and then cooled to room temperature with the furnace. Collect synthetic materials for grinding and sieving, and conduct XRD test, the result has NiS 2 phase and NiS phase. Weigh 3Kg of sublimated sulfur powder and mix it with the synthetic powder, and then re-synthesize, the synthesis system is the same as above, until all the metallic nickel is synthesized into NiS 2 until. The differential the...

Embodiment 3

[0032] Such as figure 1 The process flow shown, a single-phase NiS 2 The large-scale preparation method of powder, the preparation method comprises the following steps: commercially available metal nickel powder and sublimated sulfur powder are the initial raw materials, first weigh 10Kg metal nickel powder and 35Kg sublimated sulfur powder to fully mix, under Ar atmosphere, The mixed powder was placed in a graphite crucible with a cover, and the crucible was placed in a tubular atmosphere furnace. The temperature was raised to 600 °C at a heating rate of 10 °C / min, kept for 2 hours, and then cooled to room temperature with the furnace. Collect synthetic materials for grinding and sieving, and conduct XRD test, the result is NiS 2 Mutually. The differential thermal analysis of the obtained powder shows that the sulfur content is greater than 0.2wt%. Desulfurization process: under Ar atmosphere, sieved NiS 2 The powder was placed in a graphite crucible, and the crucible was...

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Abstract

The invention discloses a large-scale preparation method of single-phase NiS2 powder. The preparation method comprises the steps of 1) mixing metal nickel powder and sublimed sulfur powder in proportion; 2) performing high-temperature solid-phase synthesis heat treatment on the mixed powder in a protective gas atmosphere; 3) carrying out grinding, sieving and phase characterization on the synthesized powder, if a phase characterization result shows that sulfur is insufficient, supplementing sublimed sulfur powder for mixing, and carrying out high-temperature solid-phase synthesis again according to the condition in the step (2) until metal nickel is completely synthesized into a NiS2 phase; and 4) performing differential thermal analysis on the NiS2 powder synthesized in the step 3), if the differential thermal analysis shows that the mass percentage content of elemental sulfur is higher than 0.2%, removing redundant elemental sulfur through high-temperature heat treatment until the mass percentage content of elemental sulfur is lower than 0.2%. The process is simple, large-scale production can be achieved, the obtained NiS2 powder is high in purity, high in conductivity and uniform in particle size, and a foundation is laid for obtaining high-power thermal batteries.

Description

technical field [0001] The invention belongs to the field of thermal battery positive electrode materials, in particular, the invention relates to a single-phase NiS used for thermal battery positive electrode materials 2 A large-scale preparation method of powder. Background technique [0002] Thermal batteries are also called molten salt batteries. The electrolyte is a non-conductive solid at room temperature. Long-term storage and heating activation are its two major features, which are of great significance in both military and civilian fields. In civil fields such as fire alarm power supply, harsh environment, high temperature geothermal and power supply of various measuring instruments in the process of oil and gas drilling and exploration. [0003] The thermal battery was invented by Dr. Erb of Germany during World War II. In 1970, the Marine Technology Research Center of the British Admiralty used sulfur as the positive electrode material of the new thermal battery....

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M6/20C01G53/11
CPCC01G53/11H01M4/5815H01M6/20
Inventor 褚颖朱永平赵丽利王学营
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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