氮氯雙摻雜硫銀鍺礦硫化物固態電解質之空氣穩定性及介面穩定性研究

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研究生：	謝承翰 Cheng-Han Hsieh
論文名稱：	氮氯雙摻雜硫銀鍺礦硫化物固態電解質之空氣穩定性及介面穩定性研究 N, Cl Dual-doped argyrodite Li6PS5Cl sulfides for enhanced air stability and interface stability
指導教授：	黃炳照 Bing-Joe Hwang 吳溪煌 She-Huang Wu 蘇威年 Wei-Nien Su
口試委員:	黃炳照 Bing-Joe Hwang 吳溪煌 She-Huang Wu 蘇威年 Wei-Nien Su
學位類別：	碩士 Master
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	中文
論文頁數：	151
中文關鍵詞：	固態電解質、硫化物、硫銀鍺礦、雙摻雜、空氣穩定性、離子電導率
外文關鍵詞：	solid electrolyte, sulfide, argyrodite, dual doping, air stability, ionic conductivity
相關次數：	點閱：245 下載：1
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近年來，全固態鋰金屬電池因其高能量密度和更高的安全性而得到廣泛的研究。在固態電解質中，硫化物基固態電解質的離子電導率較高，因此比其他型態的固態電解質更受到關注。近來許多團隊將研究硫化物固態電解質的方向著重於介面以及空氣穩定性，使電解質保留原先的離子電導率。然而，硫化物基固態電解質的高濕度敏感特性，在接觸水氣時會產生有毒的硫化氫氣體，使其合成時需要在極低水氣的條件下，才能維持樣品的穩定性及再現性。
在本論文中，第一部分我們以Li6PS5Cl (LPSC)為基底將S2-用Cl- 取代，並藉由機械球磨和固態燒結製備而成，再利用同步輻射中心的 in-situ XRD 來探討燒結溫度對結晶度及雜相的影響，進一步優化燒結條件，再以液態氮快速降溫，證明可以保留固態電解質在高溫下的晶相，開發出過量氯Li5.4PS4.4Cl1.6，超越商業用LPSC的離子電導率，從2 mS/cm提升到8 mS/cm，第二部分我們以過量氯Li5.4PS4.4Cl1.6為基底將S2-用N3-取代，合成出雙摻雜於argyrodite之硫化物固態電解質：Li5.4+y PS4.4-y Ny Cl1.6 ( 0≦y≦0.2) 。這項工作表明，固體電解質的離子電導率可以透過用氯離子取代硫離子來提高，而且在摻雜氮離子到過量氯中後發現離子電導率不會下降很多，同時可以提高空氣穩定性以及提高介面穩定性，第三部分我們會探討如何要將1g製程放大成5g製程，實驗中發現進行放大製程時，必須減少球磨的速率和時間，否則球磨速率和時間太長會導致粉末在球磨後沉積在球磨罐中，使粉末回收率大幅下降，在多次實驗後可以獲得相近的導離率和導電率，這樣就可以確定合成平台的穩定性，並且解決同一批粉末在進行測試時會有不夠的問題。不論是過量氯或是有摻雜的固態電解質，都可以利用放大製程來製備。同時為了避免壓碇碎裂的問題，在此也有探討將粉末與PTFE進行混合，最終在導離率與粉末碎裂問題的抉擇下，採用粉末+0.1 (wt%) PTFE作為最佳值。

In recent years, all-solid-state lithium metal batteries (ASSLMBs) have been extensively studied due to their high energy density and improved safety. Among solid-state electrolytes, sulfide-based solid-state electrolytes have higher ionic conductivity, so they have attracted more attention than other types of solid-state electrolytes. Recently, many teams have focused on the direction of the research on sulfide solid-state electrolytes, focusing on interfacial stability and air stability and enabling the electrolyte to retain the original conductivity. However, the high humidity sensitivity of sulfide-based solid electrolytes will produce toxic hydrogen sulfide gas when exposed to moisture, so that the stability and reproducibility of the sample must be maintained under extremely low moisture conditions during synthesis.
In the first part, we used Li6PS5Cl (LPSC) as the substrate to replace S2- with Cl-, and prepared it by mechanical ball milling and solid-state sintering. The influence of crystallinity and impurity phase, further optimize the sintering conditions, and then prove that the crystal phase of the solid electrolyte at high temperature can be preserved by rapid cooling of liquid nitrogen, and develop chlorine-rich Li5.4PS4.4Cl1.6, which exceeds the conductivity of commercial LPSC, from 2 mS/cm to 8 mS/cm. In the second part, we use chlorine-rich Li5.4PS4.4Cl1.6 as the substrate to replace S2- with N3-, and synthesize dual-doped: Li5.4+y PS4.4-y NyCl1.6 (0≦y≦0.2). This work shows that the ionic conductivity of solid electrolytes can be improved by substituting chlorine ions for sulfur, and that the conductivity does not decrease much after doping nitrogen ions, while improving water-oxygen stability and interface stability. In the third part, we will discuss how to scale up the 1g process into a 5g process. In the experiment, we found that the speed and time of ball milling must be reduced when the process is scaled up. Otherwise, the speed and time of ball milling will be too long, and the powder will be deposited in the ball mill tank after ball milling, so the powder recovery rate dropped significantly.Similar conductivity and conductivity can be obtained after multiple experiments, so that the stability of the synthesis platform can be confirmed, and the problem of insufficient testing of the same batch of powder can be solved. Both chlorine-rich and dual-doped solid electrolytes can be prepared using scale-up processes. At the same time, in order to avoid the problem of pallet crushing, it is also discussed here to mix the powder with PTFE. Finally, under the choice of conductivity and powder fragmentation, the powder + 0.1 (wt%) PTFE is used as the optimal value.

目錄
摘要................................................................................i
ABSTRACT......................................................................... iii
致謝................................................................................v
目錄..............................................................................vii
圖目錄............................................................................xi
表目錄...........................................................................xvii
第一章 緒論.........................................................................1
1 鋰離子電池發展...................................................................1
2 全固態電池......................................................................3
3 固態電解質......................................................................5
3.1氧化物固態電解質........................................................7
3.2硫化物固態電解質........................................................8
3.3鹵化物固態電解質.......................................................10
第二章 文獻回顧.....................................................................13
1 硫銀鍺礦固態電解質..............................................................13
1.1發展歷程......................................................................13
1.2晶格結構......................................................................14
1.3鋰離子在結構中傳導途徑.........................................................14
2 硫銀鍺礦之合成方式..............................................................18
2.1熔體淬火法....................................................................18
2.2機械式球磨法...................................................................18
2.3濕化學合成法...................................................................19
3 硫銀鍺礦之改質..................................................................21
3.1陰離子摻雜-鋰空位 .............................................................21
3.2陽離子摻雜-錯位 ...............................................................24
3.3雙離子摻雜....................................................................26
4 全固態電池之未來展望及挑戰.......................................................30
5 研究動機與目的..................................................................31
6     Roadmap....................................................................32
第三章 實驗方法及實驗儀器............................................................33
1 實驗藥品.......................................................................33
2 實驗儀器設備及配件..............................................................34
3 實驗步驟.......................................................................35
3.1 Li6+xPS5-xNxCl (x=0.05, 0.1, 0.15, 0.2)合成..................................35
3.2 Li5.4+yPS4.4-yNyCl1.6 (y=0.05, 0.1, 0.15, 0.2)合成...........................36
3.3 Li5.4+yPS4.4-yNyCl1.6 (y = 0, 0.05, 0.1, 0.15, 0.2) 放大製程.................38
3.4硫化物固態電解質錠片之製備.....................................................40
4  KP-cell 型電池組裝 ...........................................................41
4.1鋰對稱電池組裝.................................................................41
4.2混合正極之製備與半電池組裝......................................................42
5 材料結構及特性鑑定分析...........................................................43
5.1非臨場X射線繞射 (Ex-situ XRD)分析..............................................43
5.2原位X射線繞射 (In-situ XRD)分析...............................................45
5.3拉曼散射光譜分析儀.............................................................46
5.4空氣穩定性測試.................................................................47
6 材料電化學特性分析..............................................................49
6.1交流阻抗分析...................................................................49
6.2鋰對鋰對稱電池充放電測試........................................................49
6.3循環伏安分析...................................................................50
6.4線性掃描伏安法.................................................................50
7 材料表面分析............................................................51
7.1 X射線光電子能譜...............................................................51
第四章 結果與討論...................................................................53
1 由原位X射線繞射優化合成條件......................................................53
2 氮摻雜於硫銀鍺礦................................................................58
2.1氮摻雜比例對結構的影響..........................................................58
2.2氮摻雜比例對振動頻率的影響之分析................................................70
2.3氮摻雜比例與電導率之關係........................................................71
2.4空氣穩定性測試.................................................................74
3 氮氯雙摻雜於硫銀鍺礦............................................................76
3.1氮摻雜比例對結構的影響..........................................................76
3.2氮摻雜比例對振動頻率的影響之分析................................................89
3.3氮摻雜比例與電導率之關係.......................................................90
3.4空氣穩定性測試.................................................................93
4固態電解質之電化學分析............................................................96
4.1循環伏安法測試.................................................................96
4.2鋰對稱電池循環測試............................................................100
4.3極限電流密度測試..............................................................102
4.4循環前後硫化物固態電解質的材料表面組成和化學狀態.................................104
5硫化物固態電解質之放大製程...............................................107
5.1 Li5.4 PS4.4 Cl1.6與Li5.55 PS4.25 N0.15 Cl1.6放大製程條件探討.107
5.2 Li5.4 PS4.4 Cl1.6與Li5.55 PS4.25 N0.15 Cl1.6摻混PTFE前後之電導
率.........................................................109
6 經放大製程之材料電化學分析..............................................114
6.1 Li5.4 PS4.4 Cl1.6與Li5.55 PS4.25 N0.15 Cl1.6摻混PTFE前後之極限電流密度測試....114
7綜合討論.......................................................................116
第五章 結論.......................................................................119
第六章 未來展望....................................................................121
第七章 參考文獻....................................................................123

                                

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