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Method for preparing transparent calcium fluoride ceramic

A technology of transparent ceramics and calcium fluoride, which is applied in the field of preparation of transparent calcium fluoride ceramics, which can solve the problems of inability to mass-produce and low output, and achieve the effect of light agglomeration, uniform distribution and improved densification

Inactive Publication Date: 2011-07-20
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] At present, the most researched fluoride nanopowder synthesis method is the microemulsion method, because the yield is too low to be mass-produced

Method used

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  • Method for preparing transparent calcium fluoride ceramic
  • Method for preparing transparent calcium fluoride ceramic
  • Method for preparing transparent calcium fluoride ceramic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] According to the preparation process figure 1 As shown, take the same volume of 2M Ca(NO 3 ) 2 Solution and 4M KF solution, using direct chemical precipitation method to remove Ca(NO 3 ) 2 The solution was slowly poured into the KF solution, and at the same time, the suspension of calcium fluoride nanopowder was obtained by the mixing method of magnetic stirring at a speed of 400 rpm, and then stood for 20 hours, washed with water or alcohol, centrifuged, and dried under vacuum at 80°C And other steps to prepare calcium fluoride nano-powder with an average crystal grain size of 25 nm. The content of the obtained calcium fluoride nano powder and the sintering aid is n(CaF 2 ): n(LiF):n(NaF)=97:2.5:0.5; mix evenly with alcohol in a mortar, put it in a mold, and press molding with an axial pressure of 30MPa to obtain a blank with a diameter of 16mm. The green body is kept at 500℃ for 2 hours at a heating rate of 10℃ / min in a vacuum sintering furnace, and the vacuum degree i...

Embodiment 2

[0043] According to the preparation process figure 1 , Take the same volume of 2M Ca(NO 3 ) 2 Solution and 4M KF solution, the nano powder preparation process was as described in Example 1, and the calcium fluoride nano powder with an average crystal grain size of 25 nm was prepared. The molar ratio of sintered powder is n(CaF 2 ):n(LiF):n(NaF)=97:0.5:2.5; Use alcohol to mix evenly in a mortar, put it into a mold, and press it into a shape with an axial pressure of 30MPa to obtain a blank with a diameter of 16mm. The green body is heated to 10 o C / min heating rate, heat preservation at 500℃ for 2 hours, vacuum degree is 10 -3 Pa; The obtained semi-finished product is placed in a hot isostatic pressing furnace at a temperature rise rate of 20°C / min, kept at 800°C for 2 hours, the pressurizing medium is nitrogen, the pressure is 200MPa, and the temperature is reduced to room temperature at a rate of 15°C / min.

[0044] After the obtained samples are rough-grinded with different type...

Embodiment 3

[0046] According to the preparation process figure 1 , Take the same volume of 2M Ca(NO 3 ) 2 Solution and 4M KF solution, the nano powder preparation process was as described in Example 1, and the calcium fluoride nano powder with an average crystal grain size of 25 nm was prepared. The molar ratio of sintered powder is n(CaF 2 ):n(LiF):n(NaF)=97:2:1; Use alcohol to mix evenly in a mortar, put it in a mold, and press it into a shape with an axial pressure of 30MPa to obtain a blank with a diameter of 16mm. The green body is kept at 500℃ for 2 hours at a heating rate of 10℃ / min in a vacuum sintering furnace, and the vacuum degree is 10 -3 Pa; The obtained semi-finished product is placed in a hot isostatic pressing furnace at a temperature rise rate of 20°C / min, kept at 800°C for 2 hours, the pressurizing medium is nitrogen, the pressure is 200MPa, and the temperature is reduced to room temperature at a rate of 15°C / min.

[0047] After rough grinding of the obtained samples with d...

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Abstract

The invention relates to a method for preparing transparent calcium fluoride ceramic, comprising the steps of nano raw powder synthesizing, vacuum sintering, heat treatment and product finishing, wherein the adopted sintering powder is nano powder which is synthesized by adopting a chemical reaction precipitation method and has the grain size of 20-70nm; the adopted sintering auxiliary is lithiumfluoride (0.5-5mol%) and sodium fluoride (0.5-3mol%); the processes are adopted, of the prepared transparent calcium fluoride ceramic prepared by vacuum sintering and heat aftertreatment has the density of not lower than 99.5% and the transmittance in visual and near infrared bands of lower than 75%, thus the ceramic is an ideal transparent material. The invention has the advantages that the raw material yield is high, the operation is simple and the ceramic transmittance is high.

Description

Technical field [0001] The present invention relates to the field of non-oxide transparent ceramics, in particular to a method for preparing transparent calcium fluoride ceramics by nano-synthesis technology, vacuum sintering, and hot isostatic pressing post-treatment process. Background technique [0002] In recent years, research on transparent ceramics has been very active at home and abroad, such as: [0003] Literature 1 (Ikesue A, Kinoshita T, Kamata K, Yoshida K. Fabrication and Optical Properties of High-Performance Polycrystalline Nd:YAG Ceramics for Solid-State Lasers[J]. J Am Ceram Soc . 1995,78(4):1033-1040.) announced the preparation of yttrium aluminum garnet (Y 3 Al 5 O 12 ) The transparent ceramic method has an optical transmittance close to single crystal. [0004] Literature 2 (Apetz R, Bruggen MPB. Transparent Alumina: A Light-Scattering Model[J]. J Am Ceram Soc . 2003,86(3):480-486.) announced the solid-phase method to prepare alumina transparent ceramics, and est...

Claims

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Application Information

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IPC IPC(8): C04B35/553C04B35/622
Inventor 宋京红智广林梅炳初周卫兵李威威
Owner WUHAN UNIV OF TECH
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