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Preparation of GRIN Glass Rods of Large Diameter

大直径GRIN玻璃棒的制备

基本信息

批准号：
63850014
负责人：
YAMANE Masayuki
金额：
$ 7.87万
依托单位：
TOKYO INSTITUTE OF TECHNOLOGY
依托单位国家：
日本
项目类别：
Grant-in-Aid for Developmental Scientific Research
财政年份：
1988
资助国家：
日本
起止时间：
1988 至 1989
项目状态：
已结题

项目摘要

On the purpose of preparing r-GRIN glass rods having a diameter larger than 10mm, the conditions on the various treatments for the preparation of the rods of PbO-K2O-B203-SiO2 system by sol-gel process have been studied.The results obtained were summarized as follows; (1) A bubble free gel of large size can be prepared by adding the mixture of acetic acid and aqueous lead acetate solution to a sol obtained by hydrolyzing a precursor solution consisted of tetraethoxysilane, tetramethoxysilane, and boronethoxide with aqubous hydrochloric acid of pH=2. (2) The pretreatment of the gel prior to the formation of concentrational gradient of lead should be made by aging the gel at 60 C in the mold, soaking in a solution of water-isopropanol system, and subsequent successive soaking in the solutions of isopropanol-acetonsystem (isopropanol/aceton=8/2, 5/5,0/10), in order to remove unnecessary water and acetic acid and to precipitate fine lead crystals on the micropore walls of the gel. (3) Formation of concentrational difference of lead in 4% between center and perimeter can be made by soaking the pretreated gel of about 35mm in diameter and 50mm in length in an ethanolic solution of potassium acetate for 4h. (4) A transparent bubble free GRIN glass rod of about 13mm in diameter and 20mm in length having a refractive index difference of about 0.05 between center and perimeter can be obtained by drying the gel in an atmosphere saturated with aceton, followed by sintering at 580 C.

以制备直径大于10mm的r-GRIN玻璃棒为目的，研究了溶胶-凝胶法制备pbo - k20 - b203 - sio2体系玻璃棒的各种处理条件。所得结果总结如下：(1)将四乙氧基硅烷、四甲氧基硅烷、硼氧基氧化物组成的前驱体溶液在pH=2的盐酸中水解得到的溶胶中加入乙酸和醋酸铅水溶液的混合物，可制得大粒径的无气泡凝胶。(2)凝胶在铅浓度梯度形成前的预处理应先在模具中60℃老化，然后在水-异丙醇体系溶液中浸泡，随后在异丙醇-丙酮体系（异丙醇/丙酮=8/ 2,5 /5,0/10）溶液中连续浸泡，以去除不必要的水和乙酸，并在凝胶微孔壁上沉淀细小的铅晶体。(3)将直径约35mm、长度约50mm的预处理凝胶在醋酸钾乙醇溶液中浸泡4h，可使铅在中心和周长之间形成4%的浓度差。(4)将凝胶在丙酮饱和气氛中干燥，580℃烧结，可得到直径约13mm，长约20mm，中心与周长折射率差约0.05的透明无气泡GRIN玻璃棒。