• 沒有找到結果。

3. Electrochemical synthesis of Pd–NiO nanoparticles in water-in-oil microemulsions

3.5 Acknowledgements

The authors would like to thank the National Science Council of the Republic of China, Taiwan, for financially supporting this research under Contract No. NSC 98-2221-E-151-033-MY2.

3.6 References

1 G. O. Mallory, and J. B. Hajdu, Electroless Plating: Fundamentals And Applications, Orlando (1990).

2 R. L. Zeller, and L. Salvati, Corrosion , 50, 457 (1994).

3 M. Bayes, I. Sinitskaya, K. Schell, and R. House, Trans. Inst. Met. Finish., 69, 140 (1991).

4 T. M. Harris, and Q. D. Dang, J. Electrochem. Soc., 140, 81 (1993).

5 G. F. Cui, N. Li, D. Y. Li, and M. L. Chi, J. Electrochem. Soc., 152, C669 (2005).

6 X. C. Wang, W. B. Cai, W. J. Wang, H. T. Liu, and Z. Z. Yu, Surf. Coat. Technol., 168, 300 (2003).

7 S. M. Mayanna, L. Ramesh, and B. S. Sheshadri, Trans. Inst. Met. Finish., 74, 66 (1996).

8 J. F. Hamilton, and R. C. Baetzold, Science, 205, 1213 (1979).

9 M. Paunovic, and M. Schlesinger, Fundamentals of Electrochemical Deposition John Wiley & Sons, Inc.

(2006).

10 C. L. Lee, C. M. Tseng, R. B. Wu, and K. L. Yang, Nanotechnol., 19, 4 (2008).

11 L. M. Abrantes, and J. P. Correia, J. Electrochem. Soc. 141, 2356 (1994).

12 J. Vandenmeerakker, J. Appl. Electrochem., 11, 395 (1981).

13 I. Ohno, O. Wakabayashi, and S. Haruyama, J. Electrochem. Soc., 132, 2323 (1985).

14 C. L. Lee, Y. C. Huang, C. C. Wan, Y. Y. Wang, Y. J. Ju, L. C. Kuo, and J. C. Oung, J. Electrochem. Soc., 152, C520 (2005).

15 C. L. Lee, Y. C. Huang, and L. C. Kuo, Electrochem. Commun., 8, 1021 (2006).

16 M. T. Reetz, and W. Helbig, J. Am. Chem. Soc., 116, 7401 (1994).

17 M. T. Reetz, W. Helbig, and S. A. Quaiser, Chem. Mater., 7, 2227 (1995).

18 I. Capek, Adv. Colloid Interface Sci. 110, 49 (2004),.

19 L. M. Neal, S. D. Jones, M. L. Everett, G. B. Hoflund, and H. E. Hagelin-Weaver, J. Mol. Cata. a-Chem.,, 325, 25 (2010).

20 J. F. Mulder, W. F. Stickle, P. E. Sobol, K. D. Bomben, and J. Chastain, Handbook of X-ray Phtoelectron Spectroscopy, Perkin-Elmer Corporation, Minnesota, (1992).

21 M. Paunovic, J. Electrochem. Soc., 124, 349 (1977).

22 A. J. Bard, and L. R. Faulkner, Electrochemical Methods, Wiley, New York (2001).

國際學術會議心得報告

計畫編號 NSC98-2221-E-151-033-MY2

計畫名稱 新化學鍍活化液合成與電化學特性之研究Ⅱ

與會人員及 服務機關

李建良 助理教授,國立高雄應用科技大學

會議時間地點 2010/11/1-2010/11/3, Tokyo, Japan 會議名稱 AsiaNano2010

發表論文題目 Electrochemical Synthesis of Pd/Ni Nanoparticles and Their Application as Catalyst for Electroless Ni Deposition

本年度參與國際學術研討會為

AsiaNano2010

會議在東京台場召開,本會議結合了 奈米材料先進製備技術、奈米粒子合成機構探討與前瞻應用,共多項會議,本 實驗室在會議中發表論文”

Electrochemical Synthesis of Pd/Ni Nanoparticles and Their Application as Catalyst for Electroless Ni Deposition

“,本論文以雙陽極定電 流電化學法來製備不同粒徑之鈀/鎳奈米粒子,此電化學合成實驗裝置以鈀片和 鎳片同時做為陽極電極,鉑片做為陰極,電解液為含有四辛基溴化銨( TOAB ) 之四氫呋喃溶液,以四辛基溴化銨包覆在聚集的金屬粒子外圍,製備出分散之 鈀/鎳合金奈米粒子,並經由調整加入微量去離水的含量,會改變粒子的結構,

可控制製備出奈米粒子的尺寸分佈,當加入的去離子水含量愈多,粒子尺寸愈 大,所製備出之粒徑分佈為 2.87 ~ 7.51 nm。此外,由於鎳易氧化的特性,在鈀/

鎳合金奈米粒子表面會有氧化鎳的生成。

以鈀/鎳合金奈米粒子在化學鍍鎳的沈積上,做為一新型催化劑,經比較所

製備出的鈀/鎳合金奈米粒子,發現最小尺寸的粒子具有最高的活性,為 1.84 ×

10

-2

cm

-2

.s

-1

。本次參與的研討會為一國際性研討會,會議期間與相關學者討論 外,亦參加了多場專題演講,也見識了日本學者對實驗的嚴謹度。此次會議中,

接觸到了不少有關貴金屬材料在電化學能源與感測上的研究,從中吸收到奈米

材料在許多領域的應用與相關知識,收穫良多。

Electrochemical Synthesis of Pd/Ni Nanoparticles and Their Application as Catalyst for Electroless Ni Deposition

Chen-Chung Wu, Chia-Chieh Syu, Chia-Chen Yang, Chien-Liang Lee*

Department of Chemical and Materials Engineering, National Kaohsiung University of Applied Science,

Kaohsiung 807, Taiwan [email protected]

Electroless nickel deposition is a catalytic reaction and an important industrial surface treatment method owing to its good corrosive protection, hardness and wear resistance [1]. Although the performance of an electroless process is influenced by numerous factors, including the composition of the deposition solution [2] and the choice of ligands [3], catalysis is the key factor in controlling the rate and mechanism of

electroless deposition [4].

In this study, Pd/Ni nanoparticles of various diameters were prepared in an electrochemical cell composed of two anodes and one cathode, at which both of Pd and Ni foil were simultaneously used as anodic

electrodes and Pt foil was used as cathodic foil. Their images observed by transmission electron microscope (TEM) are shown in Figure 1.

These alloy nanoparticles are electroreduced from nickel and palladium ion dissolved from Pd and Ni anodes and their diameters were controlled from 2.87 nm to 7.51 nm by the added H2O amount in a

tetrahydrofuran electrolyte containing micelles of tetraoctylammonium bromide (TOAB). The size of TOAB micelle has to be regulated. As the H2O amount increased, the structure of the TOABmicelle changed;

this caused the Pd/Ni nanoparticles to grow and be easily oxidized to NiO on the surface. This result was confirmed by X-ray photoelectron spectrum. Pd/Ni nanoparticles with oxidized surface were thus obtained.

Then, these alloy nanoparticles were tested as a

novel activator for electroless nickel deposition and the activities were in-situly measured by electrochemical quartz crystal microbalance. In a comparison between

the activities of Pd/Ni nanoparticles, the smallest Figure 1. TEM images of electroreduced Pd/Ni nanoparticles in TOAB/THF solution with various H2O amount. (A) 0 μl; (B) 20 μl; (C) 40 μl; (D) 80 μl; (E) 100 μl

nanoparticles had maximum activity, which reached to 1.84 × 10-2 (1/cm-2s-1).

References [1]. R. L. Zeller, Corrosion 50 (1994) 457.

[2]. M. Bayes, I. Sinitskaya, K.. Schell, R. House Trans. Inst. Met. Finish. 69 (1991) 140.

[3]. G. F. Cui, N. Li, D. Y. Li, M. Li, J. Electrochem. Soc. 152 (2005) C669.

[4]. J. F. Hamilton , R. C. Baetzold Science 205 (1979) 1213.

國科會補助計畫衍生研發成果推廣資料表

日期:2011/09/17

國科會補助計畫

計畫名稱: 新化學鍍活化液合成與電化學特性之研究(II) 計畫主持人: 李建良

計畫編號: 98-2221-E-151-033-MY2 學門領域: 電化學

無研發成果推廣資料

98 年度專題研究計畫研究成果彙整表

其他成果

(

無法以量化表達之成

果如辦理學術活動、獲 得獎項、重要國際合 作、研究成果國際影響 力及其他協助產業技 術發展之具體效益事 項等,請以文字敘述填 列。)

本年度計畫主要為利用雙陽極電化學法製備合金奈米膠體,並應用於化學鍍製 程中,在今年度迄今(2011/1-2011/8)已成功發表以計畫主持人通訊作者為主 11

篇 SCI 學術論文(含接受),影響因子總計 35.8,

計畫成果已受國際期刊主編與審查委員肯定。

另,活化液成果現已和國內廠商洽談技術轉移希冀輔導廠商建立新技術。

成果項目 量化 名稱或內容性質簡述

測驗工具(含質性與量性) 0

課程/模組 0

電腦及網路系統或工具 0

教材 0

舉辦之活動/競賽 0

研討會/工作坊 0

電子報、網站 0

目 計畫成果推廣之參與(閱聽)人數 0

國科會補助專題研究計畫成果報告自評表

請就研究內容與原計畫相符程度、達成預期目標情況、研究成果之學術或應用價 值(簡要敘述成果所代表之意義、價值、影響或進一步發展之可能性) 、是否適 合在學術期刊發表或申請專利、主要發現或其他有關價值等,作一綜合評估。

1. 請就研究內容與原計畫相符程度、達成預期目標情況作一綜合評估

■達成目標

□未達成目標(請說明,以 100 字為限)

□實驗失敗

□因故實驗中斷

□其他原因 說明:

2. 研究成果在學術期刊發表或申請專利等情形:

論文:■已發表 □未發表之文稿 □撰寫中 □無 專利:□已獲得 □申請中 ■無

技轉:□已技轉 ■洽談中 □無 其他:(以 100 字為限)

3. 請依學術成就、技術創新、社會影響等方面,評估研究成果之學術或應用價 值(簡要敘述成果所代表之意義、價值、影響或進一步發展之可能性)(以 500 字為限)

本年度計畫主要為利用雙陽極電化學法製備合金奈米膠體,並應用於化學鍍製程中,在今 年度迄今(2011/1-2011/8)已成功發表以計畫主持人通訊作者為主 11 篇 SCI 學術論文(含

接受),影響因子總計 35.8,

計畫成果已受國際期刊主編與審查委員肯定,另活化液成果現已和國內廠商洽談技術轉 移希冀輔導廠商建立新技術。

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