以改良無電鍍法製備鈀複合膜及其氫氣過濾的表現探討

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研究生：	王鈞毅 Wang, Jun-Yi
論文名稱：	以改良無電鍍法製備鈀複合膜及其氫氣過濾的表現探討 Modified electroless plating for Pd composite membrane preparation and its performance discussion in hydrogen separation
指導教授：	黃金花 Huang, Jin-Hua
口試委員:	黃倉秀 Huang, Tsung-Shiew 陳翰儀 Chen, Han-Yi 羅一翔 Lo, I Hsiang 黃國晏 Huang, Kuo-Yen
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2022
畢業學年度：	110
語文別：	英文
論文頁數：	98
中文關鍵詞：	氫氣、鈀、多孔不鏽鋼、無電電鍍
外文關鍵詞：	hydrogen, palladium, porous stainless steel, electroless plating
相關次數：	點閱：3 下載：0
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本研究內容共分成三部份。首先，本研究有別於傳統無電鍍液，使用了不含EDTA（Ethylenediaminetetraacetic acid）的無電鍍液進行鈀複合膜的製備。在研究中首先使用一次性添加聯胺的方法，透過系統地改變鍍液體積與聯胺濃度，以期能找出最適本無電鍍系統的參數。實驗結果發現，使用6.75 mM聯胺與180 mL鍍液可以得到表現最佳的鈀複合膜，其氫氣滲透率可達4.4 x 10-3 mol/m2sPa0.5 ，選擇率可達1.6 x 104，但穩定性不佳。接著，為了改良前述製備方式，無電鍍的流程被更改成分批添加由高至低濃度的聯胺，用以控制反應速度在期望的範圍。經此改良的無電鍍法所得到的鈀複合膜，擁有相比前者更高的選擇率與長期穩定性。
在第二部份的研究中，筆者嘗試將使用過且性能已經略微衰退的鈀膜管進行額外的層狀雙氫氧化合物（LDH）層生長。儘管鈀膜管部分表面積在經過LDH層生長後遭到覆蓋，其最終的氫氣滲透率並無太大變化，但氮氣漏氣率則呈現大幅的改善。因此，在鈀複合膜外生長LDH層，可以作為一個改善或修補鈀複合膜的流程。
第三部份的研究則為將鈀複合膜實際應用於甲醇重組氣的過濾實驗。結果發現使用擁有較高選擇率的鈀膜管進行過濾時，可以明顯減少雜氣的濃度，且在過濾實驗中，一氧化碳的濃度變化會更敏感的隨著選擇率的高低改變。其次，若將水氣從重組器中移除，鈀膜管的過濾能力呈顯著的提升。最後，有生長額外LDH層的鈀膜管也被用於重組器過濾，並且證明額外使用LDH層修飾的鈀膜管確實擁有較強的過濾能力。上述鈀膜管，最終在進行7-10天的長期測試後，確定本研究中的鈀膜管即使應用在重組器的環境中，仍可以保有一定的長期穩定性。

This dissertation contains three parts of researches. The first part of researches aimed to fabricate high-performance Pd composite membranes via electroless plating (ELP) with EDTA (Ethylenediaminetetraacetic acid)-free bath. Initially, both bath volume and hydrazine concentration were systematically varied to find the optimal parameters for membrane preparation. After measuring of the as-fabricated membrane tubes, the ELP with 180 mL bath volume and 6.75 mM hydrazine is believed to be the most suitable parameters for this study. ELP process was then modified in order to obtain better performance of membrane tubes. As a result, preparation of Pd membrane tubes with modified ELP showed great improvement of plating yield, better H2/N2 selectivity and long term stability.
In the second research, additional LDH (Layered double hydroxides) layers were grown onto used and little degraded Pd membrane tubes. No evident hydrogen permeance degradation was observed on the LDH modified Pd membranes. Moreover, the H2/N2 selectivity improved, indicating effective defects blocking by the LDH layer. Since the LDH layer growth is facile, it is appealing to improve performance of membrane tubes by adding extra LDH.
For the last research, membrane tubes obtained from the previously mentioned ELP system were applied to test their performances in the atmosphere of methanol reformate gas. Membrane tubes with higher H2/N2 values showed better ability of hydrogen separation in the atmosphere of reformate gas. The effects of steam in reformate gas were also discussed in the study. Reformate gas after steam removal was introduced into selected membrane tubes. The results showed that the hydrogen separation can be improved by removing steam from the reformate gas. Finally, membrane tubes were applied to undergo 7-10 days long-term stability tests. It was found that the LDH modified membrane tubes showed improved long-term stability, suggesting the as-fabricated membrane tubes were suitable for practical use.

Chinese Abstract ...................................................................  I
English Abstract ................................................................... II
Acknowledge .................................................................. III
Table of contents ................................................................... IV
List of Figures .................................................................. VII
List of Tables ................................................................. VIII
Chapter 1 Introduction .................................................................... 1
Chapter 2 Literature review .................................................................... 6
2.1 Pd-H system .................................................................... 6
2.2 Porous support used for Pd composite membranes ................................................................... 10
2.2.1 Intermetallic diffusion barriers ................................................................... 12
2.2.2 Surface modification of microporous supports ................................................................... 14
2.3 Methods to synthesize composite Pd membranes ................................................................... 18
2.3.1 Supported foils ................................................................... 19
2.3.2 Magnetron sputtering......................................................... 20
2.3.3 Chemical vapor deposition ................................................................... 22
2.3.4 Electroplating ................................................................... 24
2.3.5 Electroless plating ................................................................... 26
Chapter 3 Experimental section ................................................................... 33
3.1 Pretreatment of the porous stainless steel substrates ................................................................... 33
3.2 Substrate modification ................................................................... 36
3.2.1 Alumina substrate modification ................................................................... 36
3.2.2 Substrate modification by LDH growth ................................................................... 38
3.3 Electroless plating ................................................................... 40
3.4 Permeance and thermal stability measurements ................................................................... 43
3.5 Membrane characterization ................................................................... 45
Chapter 4 ELP of Pd composite membrane with EDTA-free bath ................................................................... 47
4.1 Problems and objectives ................................................................... 47
4.2 Results and discussion ................................................................... 49
4.2.1 Plating with varied bath volume and hydrazine concentration ................................................................... 49
4.2.2 Modified electroless plating ................................................................... 56
4.2.3 Performance and stability test ................................................................... 58
4.3 Conclusion ................................................................... 60
Chapter 5 H2 filtration of composite membrane with external LDH layer ................................................................... 61
5.1 Problems and objectives ................................................................... 61
5.2 Results and discussion ................................................................... 62
5.2.1 Additional growth of LDH layer onto Pd surface ................................................................... 62
5.2.2 Discussion of performance improvement........................................................ 64
5.3 Conclusion ................................................................... 66
Chapter 6 H2 separation for methanol reforming with various selectivity of Pd composite membranes ................................................................... 67
6.1 Problems and objectives ................................................................... 67
6.2 Results and discussion ................................................................... 68
6.2.1 Performance of H2 separation with Pd composite membrane ................................................................... 68
6.2.2 Performance of H2 separation with LDH/Pd composite membrane
................................................................... 76
6.3 Conclusion ................................................................... 80
Chapter 7 Conclusions ................................................................... 82
Chapter 8 Recommendations ................................................................... 85
References ................................................................... 87
Curriculum Vitae ................................................................... 98
List of Figures
Figure 2.1. Pd – H phase diagram ................................................................... 19
Figure 2.2. Pore size distribution for 0.1, 0.2 and 0.5 m grade PSS supports
................................................................... 25
Figure 3.1. Schematic and pictures of the PSS tubes ................................................................... 43
Figure 3.2. Procedure of membrane fabrication ................................................................... 44
Figure 3.3. Alumina particles surface modification apparatus ................................................................... 46
Figure 3.4. Schematic of one loop of the activation process. ................................................................... 50
Figure 3.5. Experimental setup for hydrogen permeation flux measurements
................................................................... 53
Figure 3.6 Samples cut from membrane tubes prior to SEM observation ................................................................... 56
Figure 4.1. SEM image of membrane from (a) 120 mL bath, 6.75 mM hydrazine. (b) 240 mL bath, 6.75 mM hydrazine.. ................................................................... 62
Figure 4.2. Thermal stability tests of the membranes were prepared from bath volume of 180 mL and: (a) 6.75 mM; (b) 9 mM hydrazine ................................................................... 64
Figure 4.3. Schematics of the two approaches: (a) original ELP; (b) modified ELP
................................................................... 66
Figure 4.4. Schematics illustrating the stacking behaviors of Pd with slow and fast plating rates. ................................................................... 66
Figure 4.5. Thermal stability test of the Pd membrane prepared using the EDTA-free bath and the sequential addition of ................................................................... 68
Figure 5.1. Top view SEM images of extra LDH surface modification on Pd membrane with magnification of (a) 1000 and (b) 3000.
................................................................... 74
List of Tables
Table 3.1. Compositions of the activation solutions ................................................................... 49
Table 3.2. The electroless Pd plating bath compositions Component ................................................................... 49
Table 4.1. performances of various membranes prepared using different bath volumes and hydrazine concentrations ................................................................... 57
Table 4.2. Performance of membranes by original ELP and modified ELP ................................................................... 66
Table 5.1. Properties and performances of various membranes prepared using different bath volumes and hydrazine concentrations. ................................................................... 70
Table 6.1. Performance of 6 tubes for prior to reformate gas filtration test hydrazine
................................................................... 76
Table 6.2. Concentration and flux measured at atmospheric pressure prior to reformate gas filtration
................................................................... 78
Table 6.3. Composition of permeate gas from methanol reformate gas
................................................................... 78
Table 6.4.Concentration of permeate gas of tube D with and without condensation
................................................................... 80
Table 6.5. N2 and H2 flux of tube C measured at pressure difference of 4 atm and 400°C in a 10-day span.
................................................................... 82
Table 6.6. H2 permeance and H2/N2 of tubes before addition LDH layer growth
................................................................... 84
Table 6.7 H2 permeance and H2/N2 of tubes before and after additional LDH layer growth
................................................................... 84
Table 6.8. Concentration of permeate gas of samples without extra LDH growth (sample G) and with extra LDH growth (sample H)
................................................................... 86
Table 6.9. H2 and N2 flux measured at 4 atm and 380°C in the long-term test of sample G (no additional LDH growth)
................................................................... 86
Table 6.10. H2 and N2 flux measured at 4 atm and 380°C in the long-term test of sample H (with additional LDH growth)
................................................................... 86
                                

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