A new approach to produce high purity solar grade silicon (SOG-Si) using wet-chemical and electrochemical processes was proposed. First, diatomaceous earth was used as a source of silica and wet-chemical purification by acid leaching and solvent extraction processes were applied for eliminating heavy metal and light element such as boron, respectively. In particular, the solvent extraction using channel flow reactor demonstrated extremely high efficiency for eliminating boron to 7N (99.99999%) level purity. Secondly, the high-purity silica was reduced to silicon by the direct electrolysis method using molten CaCl 2 as an electrolyte and Si plate as cathode. We proposed the continuous electrolysis system by feeding silica granules to the Si cathode set at the bottom of the cell. It was confirmed that the reduction proceeded steadily to form crystalline Si with a sufficient reduction rate. We also attempted electrodeposition of Si films and have developed a process using KF-KCl + K 2 SiF 6 molten salt, from which uniform layer of Si with a thickness larger than 100 mm could be formed.
A novel approach toward the purification of silica and removal of boron impurities via solvent extraction with 2-ethyl-1,3-hexanediol using a microchannel device is presented. The microchannel, fabricated on Si substrates using lithographic techniques, had 100 μm width, 100 μm depth, and 10 mm length. Amorphous silica spiked with a trace amount of boric acid and refined diatomaceous earth used as silica feedstock were purified. Residual boron content was determined by inductively coupled argon plasma atomic emission spectrometry. Following extraction using a microchannel device, the residual boron content was less than 1.0 ppm for the former silica feedstock and than 2.5 ppm for the latter one, and the contact reaction period was 0.03 seconds for both type of silica feedstock. These are lower and significantly shorter due to much shorter diffusion distance and much larger specific interfacial area as compared to those observed when using a conventional separatory funnel, for both types of silica feedstock. Hence, it is suggested that microchannel devices can be utilized as an attractive approach toward the production of high-purity silica as a source for solar-grade silicon.
We present solvent extraction using a microchannel device for purification of silica, focusing upon boron extraction with 2-ethyl-1,3-hexanediol (EHD). Boron was successfully eliminated from the samples, which consists of silica and boric acid as well as refined diatomaceous earth. The residual boron content after the extraction using a microchannel device was lower than that using a conventional separatory funnel, although the contact reaction period was much shorter. It is suggested microchannel device is an attractive method to produce high-purified silica for solar grade silicon.
Elimination of boron species via solvent extraction with 2,2,4-trimethyl-1,3-pentandiaol was engaged in a flow-type device into which the aqueous solution dissolving diatomaceous earth, a candidate of the resource for high-purity silicon material. The flow-type device has a 2-stage channel with 1.0 mm width, 0.10 mm depth, and 25 mm length each, and the specific interfacial area is comparable to a typical microchannel device. Residual boron content in the aqueous solution decreased to less than 0.1 ppm after the solvent extraction under the restriction of short contact duration shorter than 100 ms. In addition, the analysis with density functional theory indicated that the number of neighbor carbon on the central carbon is one of the keys for improvement of reactivity of extractant. Hence, it is suggested that the flow-type microchannel device with solvent extraction with alkyldiol extractant can be utilized as an attractive approach toward the production of high-purity silica as a source for solar-grade silicon.
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