Method for preparing compact metal oxide ceramic film based on in situ reaction

A technology of oxide ceramics and dense metals, which is applied in the field of metal oxide ceramic thin films, can solve the problems of many closed pores, limit the use of membrane materials, and it is difficult to obtain dense ceramic thin films, so as to simplify the process steps and make the carrier gas environment friendly , good dispersion effect

Inactive Publication Date: 2008-07-09
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing spraying method needs to synthesize the phase-formed ceramic powder first, and then spray the synthetic powder to form a film. It is difficult to obtain a dense ceramic film with a relatively small film thickness (such as 5 μm-10 μm). The ceramic film after sintering There are many closed pores, which limits the application field of membrane materials

Method used

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  • Method for preparing compact metal oxide ceramic film based on in situ reaction
  • Method for preparing compact metal oxide ceramic film based on in situ reaction
  • Method for preparing compact metal oxide ceramic film based on in situ reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: On NiO-BaCe 0.8 SM 0.2 o 2.9 Preparation of BaCe on substrate 0.8 SM 0.2 o 2.9 film

[0014] Formulating BaCe 0.8 SM 0.2 o 2.9 Slurry: Weigh the raw material BaCO 3 , CeO 2 and Sm 2 o 3 , so that the ratio of the amount of raw materials (molar ratio) is BaCO 3 : CeO 2 :Sm 2 o 3 =1:0.8:0.1, using absolute ethanol as solvent, the rare earth metal oxide CeO 2 and Sm 2 o 3 Alkaline earth metal carbonate BaCO 3 Powder: absolute ethanol: triethanolamine mixed uniformly according to the mass ratio of 8:100:0.5, ball milled for 24 hours; then add polyethylene glycol and dibutyl phthalate according to the mass ratio of 0.5:0.5:0.2 and polyvinyl butyral, and then ball milled for 24 hours to form a slurry; the slurry prepared above was sprayed with a sprayer using nitrogen as a carrier gas, and heated to a temperature of 200°C-300°C and kept at this temperature with A thin layer of loose metal oxides and metal carbonates is formed on the surface of t...

Embodiment 2

[0018] Example 2: On NiO-BaCe 0.8 SM 0.2 o 2.9 Preparation of Ba on the substrate 3 Ca 1.18 Nb 1.82 o 9-σ film

[0019] Prepare Ba 3 Ca 1.18 Nb 1.82 o 9-σ Slurry: Weigh the raw material BaCO 3 , CaCO 3 and Nb 2 o 5 , so that the ratio of the amount of raw materials (molar ratio) is BaCO 3 : CaCO 3 : Nb 2 o 5 =3:1.18:0.91, using absolute ethanol as solvent, the transition metal oxide Nb 2 o 5 and alkaline earth metal carbonate BaCO 3 and CaCO 3 Powder: absolute ethanol: triethanolamine is mixed uniformly according to the mass ratio of 6:100:0.5, ball milled for 24 hours; then add polyethylene glycol and dibutyl phthalate according to the mass ratio of 0.5:0.5:0.25 and polyvinyl butyral, and then ball milled for 24 hours to form a slurry; use a sprayer to spray the prepared slurry with air as the carrier gas, and heat it to a temperature of 200°C-300°C and keep it at this temperature. A layer of loose metal oxide and metal carbonate layer is formed on the s...

Embodiment 3

[0023] Example 3: On NiO-BaCe 0.8 SM 0.2 o 2.9 Preparation of Ba on the substrate 3 Ca 1.18 Nb 1.82 o 9-σ film

[0024] Prepare Ba 3 Ca 1.18 Nb 1.82 o 9-σ Slurry: Weigh the raw material BaCO 3 , CaCO 3 and Nb 2 o 5 , so that the ratio of the amount of raw materials (molar ratio) is BaCO 3 : CaCO 3 : Nb 2 o 5 =3:1.18:0.91, using absolute ethanol as solvent, the transition metal oxide Nb 2 o 5 and alkaline earth metal carbonate BaCO 3 and CaCO 3 Powder: absolute ethanol: triethanolamine according to the mass ratio of 15:100:1, mix evenly, ball mill for 24 hours; then add polyethylene glycol and dibutyl phthalate according to the mass ratio of 1:1:0.5 and polyvinyl butyral, and then ball milled for 24 hours to form a slurry; the slurry prepared above was sprayed with a sprayer using air as the carrier gas, and heated to a temperature of 200°C-300°C and kept at the temperature. A layer of loose metal oxide and metal carbonate layer is formed on the surface. ...

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Abstract

The invention discloses a process for preparing ceramic films of fine and compact metal oxide which is based on reaction in-situ, which is characterized by mixing metal oxide powder and alkaline earth metal carbonate which are mixed with each other according to stoichiometric proportion, absolute ethyl alcohol and trolamine according to mass ratio of 5-15:100:0.5-1, then, ball grinding and mixing the mixture uniformly, wherein the metal oxide is rear earth oxide or / and transition metal oxide. Then, the mixture is added with polyethylene glycol with mass ratio of 0.5-1, dibutyl orthophthalates with mass ratio of 0.5-1, polyvinyl butyral with mass ratio of 0.2-0.5. Slurry which is ball ground and mixed uniformly is sprayed on a ceramic base at temperature between 200DEG C-300DEG C, wherein the ceramic base is provided with agglutinating property contractibility, and then, the ceramic base is sintered at temperature between 1350DEG C-1450DEG C under reaction in-situ to densify. The process completes film forming and phase forming of the ceramic in one step, which is simple in operation, further, the thickness of the ceramic films can be controlled between 5 mum-30 mum, and heat matching problems between different bases and film materials are partially resolved.

Description

technical field [0001] The invention belongs to the technical field of metal oxide ceramic thin films, in particular to a method for preparing dense metal oxide ceramic thin films based on in-situ reactions. Background technique [0002] According to the introduction of American "Power Sources" (Journal of Power Sources, 164, 2007, 567-571; and 170, 2007, 38-41;), the preparation methods of inorganic membrane materials include: powder dry pressing sintering method, tape casting method, rolling rod method, extrusion method, chemical vapor deposition method, physical vapor deposition method, electroless plating method, spray method, etc. Among them, the spray method is one of the film preparation methods that has received more attention. It has the advantages of easy process control, low cost, large film forming area, etc., and can be used in industrial production. However, the existing spraying method needs to first synthesize the phase-formed ceramic powder, and then use t...

Claims

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Application Information

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IPC IPC(8): C04B35/64C04B35/01C04B35/50
Inventor 毕磊刘卫张尚权方曙民
Owner UNIV OF SCI & TECH OF CHINA
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