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Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal

A nickel submicron, solid-phase synthesis technology, applied in the direction of nickel sulfide, etc., can solve the problems of difficult industrialization of products, difficult organic solvent treatment, difficult separation of microemulsions, etc., and achieve excellent optics, low cost, and broad market prospects.

Inactive Publication Date: 2008-05-28
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The liquid phase method mainly includes solvothermal method and microemulsion method, and solvothermal method generally uses organic solvents as reaction solvents, which are difficult to handle; high-pressure tanks are used as reaction devices, so it is difficult to realize industrialization
In the microemulsion method, the selected microemulsion is formed by mixing various organic solvent components. Because the microemulsion is difficult to separate, it will pollute the environment, so it is difficult to realize the industrialization of the product.

Method used

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  • Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal
  • Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal
  • Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. According to a certain molar ratio of 1:1, respectively weigh 1.2442g (0.005mol) of nickel acetate and 0.3806g (0.005mol) of thiourea after grinding for 10 minutes, and put the two into a crucible to stir and mix evenly.

[0021] 2. Put the crucible containing the raw materials in a muffle furnace, react at 350°C for 3 hours, turn off the power, stop heating, and let it cool down to room temperature naturally.

[0022] 3. After grinding the cooled product, a black powdery hexagonal nickel sulfide submicron crystal is obtained.

[0023] As shown in Figure 1 and Figure 2, the structure and phase identification of the product was carried out using a German Bruker AXS D8 ADVANCEX-ray powder diffractometer (XRD, Cu K α radiation, λ=1.54056 Ȧ, 40kV, 200mA) for measurement. The morphology and size of the product were observed with a field emission scanning electron microscope (FESEM, 15kV) of S-4800 from Hitachi, Japan.

[0024] The results showed that:

[0025] Fig. 1: ...

Embodiment 2

[0028] 1. According to a certain molar ratio of 1:1, respectively weigh 1.2442g (0.005mol) of nickel acetate and 0.3806g (0.005mol) of thiourea after grinding for 10 minutes, and put the two into a crucible to stir and mix evenly.

[0029] 2. Put the crucible containing the raw materials in a muffle furnace, react at 400°C for 3 hours, turn off the power, stop heating, and let it cool down to room temperature naturally.

[0030] 3. After grinding the cooled product, a black powdery hexagonal nickel sulfide submicron crystal is obtained.

[0031] As shown in Figure 3 and Figure 4, the structure and phase identification of the product adopts German Bruker AXS D8 ADVANCEX-ray powder diffractometer (XRD, Cu K α radiation, λ=1.54056 Ȧ, 40kV, 200mA) for measurement. The morphology and size of the product were observed with a field emission scanning electron microscope (FESEM, 15kV) of S-4800 from Hitachi, Japan.

[0032] The results showed that:

[0033] Fig. 3: X-ray diffraction...

Embodiment 3

[0036] 1. According to a certain molar ratio of 1:1.5, respectively weigh 1.2442g (0.005mol) of nickel acetate and 0.5709g (0.0075mol) of thiourea after grinding for 10 minutes, and put the two into a crucible to stir and mix evenly.

[0037] 2. Put the crucible containing the raw materials in a muffle furnace, react at 400°C for 3 hours, turn off the power, stop heating, and let it cool down to room temperature naturally.

[0038] 3. After grinding the cooled product, a black powdery hexagonal nickel sulfide submicron crystal is obtained.

[0039] As shown in Figure 5 and Figure 6, the structure and phase identification of the product adopt German Bruker AXS D8 ADVANCEX-ray powder diffractometer (XRD, Cu K α radiation, λ=1.54056 Ȧ, 40kV, 200mA) for measurement. The morphology and size of the product were observed with a field emission scanning electron microscope (FESEM, 15kV) of S-4800 from Hitachi, Japan.

[0040] The results showed that:

[0041]Figure 5: X-ray diffract...

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Abstract

The invention relates to a low temperature solid phase synthesis method of hexagonal phase nickel purite submicron crystal. The molar ratios of nickel acetate and sulfur source of the invention are respectively 0.005molar and 0.005 to 0.0075molar, grinded nickel acetate and sulfur source powder are weighed and put into a crucible to stir until mixture is homogeneously mixed; the crucible which carries raw materials is put in a muffle furnace, reacts three hours at a temperature of 350 DEG C to 400 DEG C, and is naturally cooled to a room temperature; after being grinded, black powder hexagonal phase nickel purite submicron crystal is obtained. Defects of harsh conditions, high energy consumption, low yield, poor purity, expensive devices, high temperature, catalyst and virulent H2S gas, difficult processing of organic solvent, being difficult in industrialization and comparatively difficult in separating microemulsion, environment pollution, etc. of prior technique are overcome. The invention utilizes two reducing groups -NH2 at the sulfur source as protection, combing the advantage of liquid and solid fully contact and react in a heating up process, hexagonal phase NiS crystal product is directly synthesized by the muffle furnace at a low temperature condition in the air.

Description

technical field [0001] The invention relates to an inorganic functional material, in particular to a low-temperature solid-phase synthesis method of hexagonal nickel sulfide submicron crystals. Background technique [0002] NiS, black powder, melting point 797°C, relative density 5.3-5.65. There are three crystal forms, the α-type is an amorphous powder, which is extremely unstable in the air and is easily transformed into Ni(OH)S, the β-type is a hexagonal crystal, and the γ-type is a trigonal crystal, which can be converted into Ni(OH)S when heated to 396°C. β-type. [0003] As an advanced inorganic functional material, nickel sulfide has always been favored by people. NiS has special magnetic properties. When the temperature drops to the critical temperature, hexagonal NiS changes from a paramagnetic conductor to an antiferromagnetic semiconductor. The main characteristic of paramagnetic substances is that no matter whether there is an external magnetic field, there is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11
Inventor 张永才徐支有张明
Owner YANGZHOU UNIV
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