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Method for preparing Ti4O7

A nano, oxalic acid solution technology, applied in titanium oxide/hydroxide, electrical components, electrochemical generators, etc., can solve the problems of difficult to accurately control product quality, difficult to control product purity, difficult to industrialize production, etc. High rate performance, low cost, fine-grained effect

Active Publication Date: 2017-01-04
湖南科莱新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent application of Beijing University of Technology Publication No. CN102208658B uses the hydrogen reduction method, the process flow is complex and difficult to operate, the product quality is difficult to accurately control, the cost is high, and industrial production is difficult
The patent application of Sichuan University with publication number CN102642867 adopts the carbon reduction method, which not only uses toxic reagents such as benzaldehyde and phenylacetaldehyde, but the main problem is that the product purity is difficult to control after industrial production, and the product quality is not high

Method used

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  • Method for preparing Ti4O7
  • Method for preparing Ti4O7

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Experimental program
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Effect test

Embodiment 1

[0029] Take by weighing 378.18g oxalic acid (H 2 C 2 o 4 2H 2 O) Dissolve in 1L of pure water, heat up to 95°C in a water bath, add 95.734g of titanium powder, and stir vigorously (2000rpm) for 1 hour; cool and crystallize the reaction product, filter, and wash with pure water for 3 times, then put it in a vacuum drying oven at 100°C Dry it, put it into the atmosphere furnace, first pass in argon gas to exhaust the air, and then continue to pass in hydrogen gas, so that the amount of hydrogen in the furnace is not less than 30g (0.25kg / m 3 ). Raise the temperature to 900°C at a rate of 10°C / min (if the heating rate is too fast, the crystal grains will grow thicker, and if the heating rate is too slow, the production cycle will be lengthened), keep warm for 1.5h, cool with the furnace, take out the calcined powder and pulverize it to obtain high-purity simple Crystal Ti 4 o 7 Functional material, high purity ≥ 99%, fine particle size ≤ 100nm.

[0030] Depend on figure 1...

Embodiment 2

[0033] Take by weighing 378.18g oxalic acid (H 2 C 2 o 4 2H 2 O) Dissolve in 1L of pure water, heat up to 100°C in a water bath, add 95.734g of titanium powder, and stir vigorously (2000rpm) for 1 hour; cool and crystallize the reaction product, filter, and wash with pure water for 3 times, then put it in a vacuum drying oven at 100°C Dry it, put it into the atmosphere furnace, first pass in argon gas to exhaust the air, and then pass in hydrogen gas to make the amount of hydrogen in the furnace 60g, raise the temperature to 950°C at a rate of 10°C / min, keep it for 1h, cool with the furnace, and take it out The calcined powder is pulverized to obtain high-purity single crystal Ti 4 o 7 Functional material, high purity ≥ 99%, fine particle size ≤ 100nm. The test conductivity is 1980S / cm.

Embodiment 3

[0035] Take by weighing 316.5g oxalic acid (H 2 C 2 o 4 2H 2O) Dissolve in 1L of pure water, heat up to 80°C in a water bath, add 95.734g of titanium powder, and stir vigorously (2000rpm) for 2 hours; cool and crystallize the reaction product, filter, and wash with pure water for 3 times, then put it in a vacuum drying oven at 120°C Dry it, put it into the atmosphere furnace, first pass in argon gas to exhaust the air, and then pass in hydrogen gas, so that the amount of hydrogen in the furnace is not less than 30g, heat up to 1000 °C at a rate of 15 °C / min, keep it for 1 hour, and follow the furnace Cool, take out the calcined powder and pulverize to obtain high-purity Ti 4 o 7 Functional material, high purity ≥ 99%, fine particle size ≤ 100nm. The test conductivity is 1990S / cm.

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Abstract

The invention relates to a method for preparing Ti4O7. The method includes the following steps that titanium and an oxalic acid solution react at 60-100 DEG C, and a reaction product is obtained through cooling crystallization; then, the reaction product is roasted in a hydrogen atmosphere at 800-1000 DEG C, and Ti4O7 is obtained. According to the method, titanium powder and oxalic acid are adopted as raw materials, and the hydrogen atmosphere is adopted for high-temperature roasting, so that the fineness and performance of the product are guaranteed. By means of the method, environment-friendly high-purity nano-Ti4O7 which is high in purity (>=99%), small in particle size (<=100 nm) and high in chemical stability, acid-base resistance and conductivity can be obtained.

Description

technical field [0001] The invention belongs to the technical field of synthesis of new energy materials, in particular to a method for preparing high-purity nano-Ti 4 o 7 Methods. Background technique [0002] Titanium oxides can exist stably in a wide range of non-stoichiometric forms. Titanium oxide (Ti 3 o 5 、Ti 4 o 7 and Ti 5 o 9 ) is titanium dioxide with oxygen defects, with rutile-based TiO 2 The structure of the lattice. Among them Ti 4 o 7 The crystal structure of rutile titanium dioxide can be regarded as the matrix, and every 3 layers of TiO 2 After that is an oxygen deficient layer (TiO layer). Titanium oxide Several different titanium oxide compounds have high electrical conductivity, and at the same time have high chemical stability, and have good light absorption ability in the visible light region or ultraviolet light region, which makes them on the one hand become Excellent electrode materials and electrochemical catalyst support materials for...

Claims

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Application Information

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IPC IPC(8): C01G23/04H01M4/48H01M10/0525
CPCC01G23/04C01P2002/72C01P2004/03C01P2004/64C01P2006/40C01P2006/80H01M4/48H01M10/0525Y02E60/10
Inventor 张家松
Owner 湖南科莱新材料有限公司
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