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研究生:黃楷熒
研究生(外文):Kai-Ying Huang
論文名稱:化學還原法生成鎳絲及其反應機制探討
論文名稱(外文):Chemical synthesis of Nickel fibers and the study of the mechanism
指導教授:周更生周更生引用關係
指導教授(外文):Kan-Sen Chou
學位類別:碩士
校院名稱:國立清華大學
系所名稱:化學工程學系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2004
畢業學年度:92
語文別:中文
論文頁數:63
中文關鍵詞:鎳絲化學還原機制
相關次數:
  • 被引用被引用:2
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  • 下載下載:40
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這份研究主要是對本實驗室首度提出以化學方法製造鎳絲進行改進及探討。該方法係使用鎳的鹽類溶液為原料,在鹼性環境下,使用聯氨為還原劑,以及其他必要添加劑(例如PAA及NaBH4),並且在磁場中反應。根據觀察,溶液中的鎳離子首先還原成具有磁性的鎳微粒,這些鎳微粒沿著磁力線排列並互相連結生成絲狀產物。鎳絲的粗細主要受反應速率的影響,反應愈慢產物愈細,而反應速率會隨著pH值的增加而減緩。PAA的存在確保產物不會互相凝聚,但濃度過高亦會影響鎳微粒在軸向的凝聚而生成短棒狀產物。目前藉由不同配方,可生成直徑0.5、1、2μm的鎳絲。NaBH4的添加有助於克服產生新成核點的高活化能,降低反應溫度及時間。透過電性研究,明顯看出鎳絲的導電度會隨著直徑減小而大幅降低,且理論極限值大約只有塊材的30%,這可能是由於硼參雜於鎳絲中,以及鎳金屬氧化的影響。

此外,本研究亦對生成鎳絲的反應機制加以分別探討,透過觀察結果顯示在還原反應中存在兩種鎳的化合物或錯離子,例如Ni(OH)2與Ni(N2H4)32+,並分別進行還原生成金屬鎳。藉由瞭解其個別的反應活化能,可進一步控制反應速率並生成良好絲狀產物。
Abstract
In this work, we tried to improve as well as to understand the chemical method for synthesizing nickel fibers that was first found in our laboratory. The chemical method utilized nickel chloride solution as precursor, hydrazine in an alkaline solution as a reducing agent, and other necessary additives (such as PAA and NaBH4) to obtain the claimed nickel fibers under the influence of magnetic field. According to our observation, the nickel ion was first reduced to form magnetic nickel particles, and then aggregated along the magnetic line of force to form fibrous products. The diameter of the nickel fibers depended mostly on the reaction rate: with a slower reaction rate the diameter became smaller. The reaction rate was slower with increasing pH values. The use of PAA can prevent aggregation of the nickel particles, however, too much PAA would also affect the aggregation along the magnetic line and thus formed rod-like products. By changing the concentration of reactants, we could synthesize nickel fibers of diameters of 0.5, 1, and 2μm. The addition of NaBH4 lowered the activation energy of nucleation and therefore enabled us to obtain nickel fiber at a lower temperature. Electrical conductivity studies showed that these fibers could have at best about 30% of that for bulk nickel material. It was suspected to be caused by the inclusion of boron into the nickel fibers and also the oxidation of the nickel fibers.

In addition, we also discussed the reaction mechanism leading to the formation of nickel fibers. Our results showed that there are two types of nickel compound or complex preceding the chemical reduction, i.e. Ni(OH)2 and Ni(N2H4)32+ and they were reduced independently into nickel. Knowing their individual activation energy, we could have a better control over the reaction rate and thus the characteristics of nickel fibers.
摘要 1
Abstract 2

第一章 緒論 3
第二章 文獻回顧 5
2-1 金屬絲的製備方法 5
2-1.1陽極處理氧化鋁生成法 5
2-1.2共聚合體生成法 6
2-1.3超音波生成法 7
2-2 鎳絲的製備方法 8
2-2.1 Polyol Process 8
2-2.2 模版(template)生成法 9
2-2.3 化學還原法 10
2-3化學還原法生成鎳絲之產物性質 11
2-4 研究方向 12
第三章 實驗 13
3-1 實驗藥品 13
3-2 實驗儀器 14
3-3 實驗原理 15
3-4 實驗步驟 16
3-4.1 不同介面活性劑對鎳絲生成的影響 17
3-4.2 提高Na2CO3濃度對鎳絲生成的影響 18
3-4.3 氫硼酸鈉對鎳絲生成的影響 18
3-4.4 PAA濃度對鎳絲生成的影響 19
3-4.5 提高Ni2+濃度對鎳絲生成的影響 20
3-4.6 N2H6用量對鎳絲生成的影響 20
3-4.7加入NH3對鎳絲生成的影響 21
3-4.8 放大反應系統 22
3-4.8.1 E2組放大實驗 23
3-4.8.2 G1組放大實驗 24
3-4.9溶液中各反應之探討 25
3-4.9.1 N2H3COO-離子的生成 25
3-4.9.2 以Ni(N2H4)32+為前驅鹽進行還原反應 25
3-4-9.3 以Ni(OH)2為前驅鹽進行還原反應 26
3-4-10 鎳絲導電度分析 26
第四章 結果與討論 27
4-1 不同介面活性劑對鎳絲生成的影響 27
4-2 提高Na2CO3濃度對鎳絲生成的影響 29
4-3 氫硼酸鈉對鎳絲生成的影響 30
4-4 PAA濃度對鎳絲生成的影響 33
4-5 提高Ni2+濃度對鎳絲生成的影響 34
4-6 降低N2H4濃度對鎳絲生成的影響 37
4-7加入NH3對鎳絲生成的影響 38
4-8 放大反應系統 39
4-9 溶液中各反應之探討 41
4-9.1 N2H3COO-錯離子的生成 42
4.9-2以Ni(N2H4)32+為前驅鹽進行還原反應 44
4.9-3以Ni(OH)2為前驅鹽進行還原反應 47
4-10導電性分析 54
4-11產物性質鑑定 55
第五章 結論 60
第六章 參考文獻 61
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