本文選題：水熱法　切入點：兩步水熱法　出處：《南京航空航天大學(xué)》2010年碩士論文　論文類型：學(xué)位論文

【摘要】： 本文分別采用異丙醇輔助水熱法和兩步水熱法在240oC下成功合成了鈣鈦礦結(jié)構(gòu)的(K,Na)NbO_3無鉛壓電陶瓷粉體。采用X射線衍射儀(XRD)和掃描電子顯微鏡(SEM)研究了原料中K/(K+Na)和(K+Na)/Nb摩爾比對產(chǎn)物粉體的物相結(jié)構(gòu)和微觀形貌的影響。結(jié)果表明異丙醇輔助水熱法易于合成富鉀或富鈉的單相(K,Na)NbO_3固溶體。而合成K/Na接近1的(K,Na)NbO_3固溶體時,得到的粉體為富鉀的(K,Na)NbO_3固溶體和富鈉的(K,Na)NbO_3固溶體多相共存的混合物。然而兩步水熱法可以通過調(diào)節(jié)第二步水熱反應(yīng)中原料的比例很好的控制產(chǎn)物中K/Na的比例。對富鉀的(K,Na)NbO_3固溶體和富鈉的(K,Na)NbO_3固溶體多相共存的混合物在不同的溫度進行后期熱處理實驗,XRD結(jié)果顯示在900 oC下保溫兩個小時后物相由最初的多相共存轉(zhuǎn)變?yōu)閱蜗嗟?K,Na)NbO_3固溶體。 為了提高(K,Na)NbO_3的壓電性能,在水熱合成(K,Na)NbO_3粉體的基礎(chǔ)上,對其進行了Sb元素的摻雜,成功得到了單相的(K_(0.7)Na_(0.3))(Nb_(0.95)Sb_(0.05))O_3粉體。采用XRD、Raman散射和SEM等方法研究了Sb元素摻雜對水熱合成(K,Na)(Nb, Sb)O_3粉體的物相結(jié)構(gòu)和形貌的影響。結(jié)果表明隨著Sb元素摻雜量的增加,得到粉體的物相從富鉀相和富鈉相共存逐漸轉(zhuǎn)變?yōu)閱蜗嗟?K, Na)(Nb, Sb)O_3固溶體,并且其形貌由無規(guī)團聚狀變化為規(guī)則的六角狀形貌。本文還進行了240oC時不同反應(yīng)時間下水熱合成(K, Na)(Nb, Sb)O_3粉體的實驗,通過測試不同反應(yīng)時間得到的產(chǎn)物的物相結(jié)構(gòu)和粉體形貌,我們提出了一種可能的(K, Na)(Nb, Sb)O_3固溶體的水熱合成機理,探討了Sb元素摻雜對物相結(jié)構(gòu)和形貌的影響機制。 以水熱法合成的單相的K (Nb_(0.95)Sb_(0.05))O_3和Na (Nb_(0.95)Sb_(0.05))O_3粉體為原料,采用傳統(tǒng)燒結(jié)工藝制備了無鉛壓電陶瓷。與傳統(tǒng)固相法相比,水熱法制備的壓電陶瓷其體內(nèi)氣孔率下降,密度增大,晶界強度增強,出現(xiàn)穿晶斷裂。運用阻抗分析儀和鐵電分析儀測試其介電、壓電、鐵電性能,得到壓電常數(shù)d33為146pC/N,機電耦合系數(shù)kp為42%左右,品質(zhì)因數(shù)Qm為63左右,相對介電常數(shù)εr為750,介電損耗tanδ為0.03,并且剩余極化強度Pr有較明顯的提高,達到了30μC/cm2以上。
[Abstract]:Lead-free piezoelectric ceramic powders with perovskite structure have been successfully synthesized by isopropanol assisted hydrothermal method and two-step hydrothermal method at 240oC, respectively. K _ (+) K _ (+) Na) in raw materials has been studied by X-ray diffractometer (XRD) and scanning electron microscopy (SEM). The effects of molar ratio of K and K Na)/Nb on the phase structure and micromorphology of the product powders were investigated. The results showed that the potassium rich or sodium rich monophase KNbO3 solid solution was easy to be synthesized by isopropanol assisted hydrothermal method, and when the K / Na ratio was close to 1, the K / Na NbO _ 3 solid solution could be synthesized, and when the K / Na ratio was close to 1, the NbO _ 3 solid solution could be synthesized by isopropanol assisted hydrothermal method. The obtained powder is a mixture of potassium rich Knao NbO _ 3 solid solution and sodium rich K _ 2O _ 3 solid solution. However, the two-step hydrothermal method can control the ratio of K / Na in the product very well by adjusting the ratio of the raw material in the second step hydrothermal reaction. The XRD results show that the phase changes from the initial multiphase coexistence to the single-phase KNaNbO3 solid solution after holding at 900oC for two hours after post-heat treatment at different temperatures for the mixture of KNaNaNbO3 solid solution and sodium rich KNaNbO3 solid solution at different temperatures, and the XRD results show that the phase changes from the initial multiphase coexistence to the single-phase KNaNbO3 solid solution after holding at 900oC for two hours. In order to improve the piezoelectric properties of NbO3, the SB element was doped on the basis of hydrothermal synthesis of NbO3 powder. In this paper, we have successfully obtained the single-phase single phase KDD-0.7NaTi-0.3NbStack-0.95SbStack-0.05SnO3 powder. The effect of SB doping on the phase structure and morphology of Sb)O_3 powder was studied by means of XRD-Raman scattering and SEM. The results show that with the increase of SB doping amount, the effect of SB doping on the phase structure and morphology of Sb)O_3 powder is studied. The results show that the effect of SB doping on the phase structure and morphology of Sb)O_3 powder is studied with increasing the doping amount of SB element, and the effect of SB element doping on the phase structure and morphology of Sb)O_3 powder is studied. The phase of powder was gradually changed from the coexistence of potassium rich phase and sodium rich phase to a single phase solid solution of K, Na-Nb, Sb)O_3. Moreover, the morphologies of the products changed from random agglomeration to regular hexagonal morphologies. Experiments were also carried out on the hydrothermal synthesis of K, Na-Nb, Sb)O_3 powders at different reaction times at 240 OC. The phase structure and morphology of the products obtained at different reaction times were tested. We propose a possible hydrothermal synthesis mechanism of K, Na-Nb, Sb)O_3 solid solution, and discuss the influence mechanism of SB doping on the phase structure and morphology. The lead-free piezoelectric ceramics were prepared by traditional sintering process from the single phase K-NbDX 0.95 SbO _ 3 and Na _ NbM _ (0.95) SbDO _ 3 powders synthesized by hydrothermal method. Compared with the conventional solid state method, the bulk porosity and density of the piezoelectric ceramics prepared by hydrothermal method decreased and the density increased. The dielectric, piezoelectric and ferroelectric properties were measured by impedance analyzer and ferroelectric analyzer. The piezoelectric constant D33 was 146pC / N, the electromechanical coupling coefficient (KP) was about 42%, and the quality factor (QM) was about 63. The relative dielectric constant 蔚 r is 750, the dielectric loss tan 未 is 0.03, and the residual polarization intensity pr is obviously increased to more than 30 渭 C / cm 2.
【學(xué)位授予單位】：南京航空航天大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2010
【分類號】：TQ174.75

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