製備高比表面積四氧化三錳粉末之研究

A study on the preparation hausmannite powder with high specific area surface

王誠華(Cheng-Hua Wang)

指導教授 ： 徐開鴻

國立臺北科技大學/工程學院/材料科學與工程研究所/碩士(2009年)

摘要

研究在於探討由CBM觸媒回收後得到的MnCl2，利用化學沉澱及溶液氧化製備高比表面積Mn3O4粉末。將回收的MnCl2與適量的鹼(NH4OH或NaOH)反應，生成中間產物Mn(OH)2，而後加入H2O2氧化沉澱得到Mn3O4粉末。初步試驗先比較NaOH與NH4OH兩個鹼液系統反應所得之四氧化三錳差別；而後選用NaOH為反應之鹼液進行田口實驗設計L9直交表試驗，初步獲得較佳的實驗參數，再進行調整。
實驗結果分別與四種市售產品進行BET比表面分析、雷射粒徑分析、XRD結構分析、ICP及EDTA成份分析、SEM表面形貌觀察等比較。結果顯示以1M MnCl2與2.4M NaOH反應後氧化得到的Mn3O4比表面積可達到26m2/g為最高。

關鍵字

四氧化三錳 ； 錳鋅鐵氧磁體 ； 鋰離子二次電池 ； 比表面積

並列摘要

This research focuses mainly on the preparation of haussmannite (Mn3O4) powders with high specific surface area. The whole process comprised of chemical precipitation and oxidation in solution. At first, MnCl2 was recovered by CBM catalyst and reacted with alkaline solution like NH4OH or NaOH. One intermediate product, Mn(OH)2,was formed. If H2O2 was subsequently added into the solution, Mn3O4 powders were obtained from the oxidation of Mn(OH)2.
Based on Taguchi method, one L9 orthogonal array was designed and implemented accordingly. A set of relatively practicable experimental conditions was decided and served as a basis for further adjustment of parameters.
The prepared samples were compared with four commercial products by means of 3.4.1 XRD分析 39
3.4.2 掃描式電子顯微鏡分析 39
3.4.3 雷射粒徑分析儀 (Mastersizer 2000) 39
3.4.4 發射光譜分析(ICP- Optima 2000) 40
3.4.5 離子層析儀(IC- DIONEX 2008 ) 40
3.4.5 BET比表面積測定儀(ASAP 2020) 41
第四章 結果與討論 42
4.1 使用不同鹼液合成Mn3O4粉末比較 42
4.1.1 實驗步驟差異 42
4.1.2 雷射粒徑分析 43
4.1.3 成份分析 46
4.1.4 XRD結構分析 46
4.1.5 SEM 粉體形貌觀察 48
4.1.6 綜合評估 49
4.2 田口實驗設計-L9直交試驗分析 50
4.2.1 L9直交表實驗統計分析 50
4.2.1.1 L9直交表實驗統計分析----比表面積 51
4.2.1.2 L9直交表實驗統計分析----Ｍn差值 55
4.2.2 反應後之溶液pHXRD, SEM, and ICP. The chemical composition was titrated by EDTA. Furthermore, the specific surface area and the distribution of particle size were also analyzed. . It was found that the specific surface area of Mn3O4 powders reaches its maximum (26 m2/g) when the concentrations of MnCl2 and NaOH were 1M and 2.4M, respectively.

並列關鍵字

hausmannite ； MnZn ferrite ； second Lithium batteries ； specific area surface

參考文獻

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