Technology of preparing nanometer composite oxide by mechanical grinding

A composite oxide and nanocomposite technology, applied in the fields of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problem of not mentioning the solid-phase chemical reaction between components, reducing the specific surface area of ​​the composite oxide, and being unsuitable for large-scale industrialization. Production and other problems, to avoid high temperature decomposition route, perfect crystal structure and low cost

Inactive Publication Date: 2006-11-29
张润铎
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Problems solved by technology

However, high temperature will lead to a significant decrease in the specific surface area of ​​the composite oxide and an increase in the grain size, which seriously affects its practical application and excellent performance.
A series of preparation methods (for example: solution-gel method, co-precipitation method, citrate complexation method, spray drying method, freeze-drying method, etc.) have been tried to adopt in order to improve the specific surface area of ​​composite oxides, but these preparation methods There are many problems such as complex process, high cost, serious pollution, etc., which are not suitable for large-scale industrial production
At the same time, the above methods can only be used to increase the specific surface area of ​​the composite oxide to a level of 30 square meters per gram.
[0003] The mechanical ball milling method is mainly used in the superfine pulverization of metals (Chinese patent, application number 02137646.8) and metal oxides (Chinese patent, application number 01134340.0), while the U.S. patent (patent number 4134852) only mentions the use of ball milling to disperse various oxides, forming a homogeneous precursor mixture without mentioning any solid-phase chemical reactions between the components during ball milling

Method used

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  • Technology of preparing nanometer composite oxide by mechanical grinding
  • Technology of preparing nanometer composite oxide by mechanical grinding
  • Technology of preparing nanometer composite oxide by mechanical grinding

Examples

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Effect test

example 1

[0044] Lanthanum nitrate and ferric nitrate according to the molecular formula LaFeO 3 The molar ratios indicated in were weighed, mixed, and transferred to stainless steel tanks. A metal ball about 5 times the weight of the mixed material is placed, and the vibration frequency generated by the ball is 800 times per minute. This process is wet grinding, and the amount of water added is 0.5 times of the amount of material. Grinding is carried out under closed conditions without introducing other gases, and the grinding time is 24 hours. The obtained material was dried at 110°C for 3 hours, calcined at 700°C for 5 hours, then sodium hydroxide was added, and fine grinding was continued for 20 hours. After primary washing with ammonia water, filtering, secondary washing with deionized water, filtering, and drying at 110°C for 5 hours, the product was obtained.

example 2

[0046] Lanthanum nitrate, chromium oxide, copper chloride according to LaCr 0.8 Cu 0.2 o 4 The molar ratio of the various atoms shown in the molecular formula is weighed. Preliminary mixing, transferred to a stainless steel grinding tank, and at the same time, metal balls about 8 times the weight of the mixed material were added into the tank, and ball milling was performed at a vibration frequency of 1000 times per minute. The process is dry grinding. The grinding process continuously replenishes air into the grinding tank. The primary grinding time is 20 hours, and then sodium chloride is added to continue fine grinding for 20 hours. After preliminary washing with 10% sodium hydroxide solution, filtering, secondary washing with deionized water, filtering, and drying at 110° C. for 5 hours, the product was obtained.

example 3

[0048] Magnesium carbonate and alumina powders are weighed and simply mixed according to the atomic molar ratio of Mg and Al shown in the molecular formula MgAl204, and added to a stainless steel grinding jar together with metal balls 8 times the amount of the mixed material. The vibration frequency generated by the sphere is 1500 vibrations per minute. Grinding was carried out in an atmosphere of 20% oxygen, and the primary grinding time was 15 hours. The obtained material was dried at 110°C for 3 hours, calcined at 700°C for 5 hours, then ammonium chloride was added, and the fine grinding was continued for 20 hours. Preliminary washing with 5% acetic acid, filtering, secondary washing with deionized water, filtering, and drying at 110° C. for 5 hours to obtain the product.

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Abstract

A process for preparing the nano-class composite oxide from perovskite, spinel, scheelite, heteropoly acid, etc by mechanical grinding features that the collision, squeezing and kneading between high-energy metallic balls can trigger the solid-state chemical reaction between simple oxides at lower temp to generate nano-class composite oxide. It includes such steps as proportional mixing, high-energy ball grinding while solid-phase reaction, fine grinding, washing and drying.

Description

technical field [0001] The invention relates to a preparation method of a nanocomposite oxide, belonging to the fields of nanomaterials and solid-state chemistry. The technology has simple process, low cost and energy consumption, high degree of automation and production efficiency, low environmental pollution, excellent physical and chemical properties of the product, and stable product quality. technical background [0002] Composite oxides are a new multi-component oxide with a definite structure prepared by chemical synthesis of two or more simple oxides. They have unique electrical, magnetic, superconducting, and catalytic properties. Broad prospects. Composite oxides are usually prepared by firing (800-1400°C) to form a specific crystal phase structure at high temperature. However, high temperature will lead to a significant decrease in the specific surface area of ​​the composite oxide and an increase in the grain size, which seriously affects its practical applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/01C01G1/02B02C17/00B82B3/00
Inventor 张润铎
Owner 张润铎
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