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Method for preparing nanometer Ti4O7 powder

A powder and nano-technology, applied in the field of preparation of nano-Ti4O7 powder, can solve the problems of low electrical conductivity and activity, difficult industrialized production, complicated technological process, etc., and achieve the effect of convenient industrialized production, easy control and simple process

Active Publication Date: 2014-01-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

U.S. Patent No. 4,422,917 discloses an electrode material, an electrode, and an electrochemical cell. A Ti-containing 4 o 7 、Ti 5 o 9 ,, Ti 6 o 11 and other multi-component titanium oxide mixtures, because the product is not a single-phase Ti 4 o 7 , and the particle size is relatively coarse, so the conductivity and activity are not high; Chinese patent CN 102208658A discloses a nano-Ti 4 o 7 Process for the preparation of particles using tetraethyl silicate as SiO 2 The precursors were coated in TiO 2 The surface of the powder is then heat-treated in a reducing atmosphere, and the surface-coated silicon is used to inhibit the growth of the product particles, and the silicon-containing nano-Ti is prepared 4 o 7 Particles, and then remove the SiO in the product by alkali or hydrofluoric acid etching 2 , although this method obtains nano-Ti with a single phase composition 4 o 7 Powder, but the process is complex and difficult to control, so industrial production is difficult and costly

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  • Method for preparing nanometer Ti4O7 powder
  • Method for preparing nanometer Ti4O7 powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the present embodiment, the component of raw material and the percentage by weight of each component are as follows:

[0025] Nano titanium dioxide powder 96.2%

[0026] Nano carbon black powder 3.7%

[0027] Benzaldehyde 0.1%

[0028] The process steps are as follows:

[0029] (1) Put the nano-titanium dioxide powder, nano-carbon black powder and benzaldehyde measured by the above weight percentage into the drum type ball mill, add a ball diameter of WC-8wt% Co cemented carbide balls, the ball-to-material ratio is 8:1, add wet grinding medium absolute ethanol, the addition of absolute ethanol to submerge nano titanium dioxide powder, nano carbon black powder, benzaldehyde and cemented carbide The ball is limited, wet milling and dispersing is carried out at normal pressure and room temperature, the speed of the ball mill is controlled at 20 rpm, and the wet milling and dispersing time is 90 hours. After the nano-titanium dioxide powder, nano-carbon black powder ...

Embodiment 2

[0033] In the present embodiment, the component of raw material and the percentage by weight of each component are as follows:

[0034] Nano titanium dioxide powder 96.1%

[0035] Nano carbon black powder 2.9%

[0036] Phenylacetaldehyde 1%

[0037] The process steps are as follows:

[0038] (1) Put the nano-titanium dioxide powder, nano-carbon black powder and phenylacetaldehyde measured by the above weight percentage into the roller mill, add a ball diameter of WC-8wt% Co cemented carbide balls, the ball-to-material ratio is 5: 1, adding wet grinding medium is industrial alcohol, and its addition is to submerge nano-titanium dioxide powder, nano-carbon black powder, phenylacetaldehyde and cemented carbide balls. Under normal pressure and room temperature, carry out wet milling and dispersing, control the speed of the ball mill at 30 rpm, and mill for 80 hours. After the nano-titanium dioxide powder, nano-carbon black powder and phenylacetaldehyde are mixed evenly, sieve ...

Embodiment 3

[0041]In the present embodiment, the component of raw material and the percentage by weight of each component are as follows:

[0042] Nano Titanium Dioxide Powder 96%

[0043] Nano carbon black powder 3.9%

[0044] Cinnamaldehyde 0.1%

[0045] The process steps are as follows:

[0046] (1) Put the nano-titanium dioxide powder, nano-carbon black powder and cinnamic aldehyde measured by the above weight percentage into the high-energy ball mill, add a ball diameter of WC-8wt% Co cemented carbide balls, the ball-to-material ratio is 10:1, add wet grinding medium absolute ethanol, the addition of absolute ethanol to submerge nano titanium dioxide powder, nano carbon black powder, cinnamaldehyde and cemented carbide Balls as the limit, ball milling for 10 hours, when the nano-titanium dioxide powder, nano-carbon black powder and cinnamic aldehyde are mixed evenly, sieve to separate the cemented carbide balls to obtain a mixed slurry, and then dry at 80°C for 1 hour;

[0047] ...

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Abstract

The invention discloses a method for preparing nanometer Ti4O7 powder. The weight percentages of various raw materials are as follows: 96-97 percent of titanium dioxide powder, 2.9-3.9 percent of nanometer black powder and 0.1-1 percent of aromatic aldehyde. The process comprises the following steps: (1) putting titanium dioxide powder, nanometer black powder and aromatic aldehyde which are measured according to the weight percentages into a ball mill; adding a grinding ball body and a grinding medium for wet milling and dispersion at the constant pressure and the room temperature; separating the grinding ball body after the titanium dioxide powder, the nanometer black powder and the aromatic aldehyde are uniformly mixed so as to obtain mixed slurry; and then drying the mixed slurry for 1-3 hours at the temperature of between 60 and 80 DEG C; and (2) filling the mixture prepared in the step (1) into a heating furnace; and heating the mixture to be at 800-1150 DEG C under a vacuum condition or a condition that inertia gas flows and performing reduction reaction for 1-4 hours at the temperature; and cooling the mixture to the room temperature along with the furnace after the reaction time is up.

Description

technical field [0001] The invention belongs to the field of nanomaterials, in particular to a nanometer Ti 4 o 7 Method of powder preparation. Background technique [0002] Ti 4 o 7 It is a single-phase titanium black, which has excellent thermodynamic stability and electrical conductivity, and can be used as an electrode material for lithium batteries, lithium-air batteries and fuel cells, so it has attracted extensive attention. However, as an electrode material, not only high conductivity, but also high specific surface area and activity are required. U.S. Patent No. 4,422,917 discloses an electrode material, an electrode, and an electrochemical cell. A Ti-containing 4 o 7 、Ti 5 o 9 ,, Ti 6 o 11 and other multi-component titanium oxide mixtures, because the product is not a single-phase Ti 4 o 7 , and the particle size is relatively coarse, so the conductivity and activity are not high; Chinese patent CN 102208658A discloses a nano-Ti 4 o 7 Process for the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/04B82Y40/00
Inventor 叶金文刘颖朱瑞杰
Owner SICHUAN UNIV
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