本文選題：Pb基反鐵電材料 + 溶膠-凝膠法�。� 參考：《內(nèi)蒙古工業(yè)大學(xué)》2015年碩士論文

【摘要】：制備高功率密度、大容量電容器的關(guān)鍵是尋求一種同時具有能量存儲密度、高儲能效率(即低能量損耗)及快速存放電行為的材料。Pb基反鐵電材料就是這樣的相變材料,其在溫度、電場及應(yīng)力的誘導(dǎo)下可以實現(xiàn)反鐵電態(tài)(AFE)與順電態(tài)(P)和AFE與鐵電態(tài)(FE)之間的快速轉(zhuǎn)變,呈現(xiàn)出雙電滯回線,從而可以實現(xiàn)能量的存儲與釋放。論文采用溶膠-凝膠技術(shù)合成了成分不同、但均具有純相鈣鈦礦結(jié)構(gòu)的Pb基反鐵電陶瓷粉,并將陶瓷粉燒結(jié)成陶瓷。借助差熱-熱重分析儀(DSC-TG),X射線衍射儀(XRD),掃描電子顯微鏡(SEM)、拉曼測試儀(Ramam)等對陶瓷粉的組成結(jié)構(gòu)進行了表征,采用介電性能測試儀和鐵電性能測試儀對陶瓷的電性能進行了測試。探討了鉛過量、添加劑的種類及含量對Pb基陶瓷粉的結(jié)構(gòu)及微觀形貌的影響,獲得了合成純相鈣鈦礦結(jié)構(gòu)PZ陶瓷粉的最優(yōu)工藝參數(shù)。分析了La3+、Ti4+、La3+和Ti4+的混合摻雜對鈣鈦礦結(jié)構(gòu)Pb基反鐵電陶瓷粉的合成溫度、晶粒尺寸、微觀形貌及電性能的影響。論文采用溶膠-凝膠法制備了不同鉛過量的PZ陶瓷粉。實驗發(fā)現(xiàn),制備鈣鈦礦結(jié)構(gòu)的PZ時,鉛的最佳過量值為3%。鈣鈦礦結(jié)構(gòu)PZ陶瓷粉的最佳合成工藝為:煅燒溫度為900℃,保溫時間為2h。但實驗合成的PZ粉體團聚現(xiàn)象嚴(yán)重�？紤]到鈣鈦礦結(jié)構(gòu)PZ的合成溫度太高、且粉體團聚現(xiàn)象嚴(yán)重,論文探討了DEA和PEG對PZ陶瓷粉的相變溫度、晶粒尺寸、顆粒形貌等的影響。實驗發(fā)現(xiàn),DEA的添加有助于降低單一鈣鈦礦結(jié)構(gòu)PZ陶瓷粉的合成溫度。在Pb過量3%的PZ陶瓷粉中添加10%的DEA,保溫2h時,單一鈣鈦礦結(jié)構(gòu)PZ陶瓷粉的合成溫度從900℃降至580℃。添加10%的PEG,PZ陶瓷粉團聚的顆粒分散效果明顯。元素?fù)诫s的結(jié)果表明,添加La3+、Ti4+后,晶格畸變致使鈣鈦礦結(jié)構(gòu)的Pb基反鐵電材料的晶粒細(xì)化,合成溫度降低。PLZ陶瓷粉的合成溫度為540℃,晶粒尺寸的理論計算值為35.47nm。PZT陶瓷粉的合成溫度為600℃,晶粒尺寸的理論計算值為47.50nm。PLZT陶瓷粉的合成溫度為580℃,晶粒尺寸的理論計算值為45.43nm。Ramam譜的測試結(jié)果表明,室溫下,鈣鈦礦結(jié)構(gòu)PZ的相結(jié)構(gòu)為反鐵電正交相,PLZ的相結(jié)構(gòu)為反鐵電四方相,PZT的相結(jié)構(gòu)為反鐵電正交相,PLZT的相結(jié)構(gòu)為反鐵電四方相。電性能的測試結(jié)果表明,PZ陶瓷的居里溫度TC為226℃;介電常數(shù)ε為2264;場致開關(guān)場強EA-F=13.4 KV/cm,EF-A=10.2 KV/cm;飽和極化PS=11.28 UC/cm2。PLZ陶瓷的TC為151℃;介電常數(shù)ε為3489;場致開關(guān)場強EA-F=9.9 KV/cm,EF-A=6.6KV/cm;飽和極化PS=12.26 UC/cm2。PZT陶瓷的TC為230℃;ε為2641,場致開關(guān)場強EA-F=12.1 KV/cm,EF-A=7.4KV/cm;PS=19.41 UC/cm2。PLZT的TC降低至148℃;介電常數(shù)ε為3196;場致開關(guān)場強EA-F=7.4 KV/cm,EF-A=3.8KV/cm;飽和極化PS=22.49UC/cm2。
[Abstract]:The key to fabricating high power density and large capacity capacitors is to find a material with high energy storage density, high energy storage efficiency (I. E. low energy loss) and fast storage behavior. Pb-based antiferroelectric materials are such phase change materials. Under the inducement of temperature, electric field and stress, the antiferroelectric state (AFE) and the paraelectric state (P) and the AFE and the ferroelectric state (FE) can be transformed rapidly, showing a double hysteresis loop, so that the energy can be stored and released. Pb-based antiferroelectric powders with pure phase perovskite structure were synthesized by sol-gel technique and sintered into ceramics. The structure of ceramic powder was characterized by differential thermogravimetric analyzer (DSC-TG) X-ray diffraction (XRD), scanning electron microscope (SEM) and Raman tester (Ramam). The effects of excessive lead and the kinds and contents of additives on the microstructure and microstructure of Pb-based ceramic powders were discussed. The optimum technological parameters for the synthesis of PZ ceramic powders with pure phase perovskite structure were obtained. The effects of mixed doping of La _ 3 and Ti _ 4 on the synthesis temperature, grain size, microstructure and electrical properties of perovskite Pb-based antiferroelectric ceramic powders were analyzed. In this paper, PZ ceramic powder with different lead overdose was prepared by sol-gel method. It is found that the optimum excess value of lead is 3 when PZ with perovskite structure is prepared. The optimum synthesis process of perovskite PZ ceramic powder is as follows: calcination temperature is 900 鈩，

本文編號：2073166