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基于結(jié)晶法的YAG粉末制備及其燒結(jié)特性

發(fā)布時間:2018-05-17 03:30

  本文選題:YAG + 粉末。 參考:《華中科技大學(xué)》2015年碩士論文


【摘要】:釔鋁石榴石(Y3Al5O12,YAG)是一種重要的激光基質(zhì)材料。相對于YAG單晶,YAG透明陶瓷因其高穩(wěn)定性、低制造成本和易大濃度摻雜等特點引起了國內(nèi)外學(xué)者的濃厚興趣,近年來在許多場合已經(jīng)取代了YAG單晶得到實際應(yīng)用。高透明YAG陶瓷是制備高質(zhì)量YAG激光陶瓷的前提。而YAG粉末的燒結(jié)特性是影響YAG陶瓷透光率的重要因素之一。因而本論文主要研究目的是探究出一種簡單高效、適合工業(yè)化生產(chǎn)的YAG粉末合成方法。利用此方法可以在較低溫度下合成成分均勻、分散良好、大小適宜的YAG粉末,從而為制備YAG透明陶瓷打下良好的基礎(chǔ)。本文首先以硝酸鹽體系為原材料采用結(jié)晶法來合成YAG粉末,具體研究內(nèi)容分為三部分:(1)硝酸鹽過程。僅僅以Y(NO3)3和Al(NO3)3為原材料,利用二者在水中的大溶解度,通過加熱攪拌它們的水溶液,制得Y(NO3)3和Al(NO3)3混合較均勻的結(jié)晶前驅(qū)體。此結(jié)晶前驅(qū)體經(jīng)950oC煅燒后,合成了純相YAG粉末。制得的YAG粉末經(jīng)1550oC燒結(jié)后,樣品中晶粒組成了許多“晶粒團”,“晶粒團”內(nèi)部晶粒排列整齊,氣孔含量很少,而“晶粒團”之間卻留有非常大的氣孔。(2)Y2O3過程。在硝酸鹽過程基礎(chǔ)上,在原材料中加入2 wt.%Y2O3納米粉體,結(jié)晶前驅(qū)體經(jīng)過850oC煅燒制備出了純相YAG粉末,此過程制備的粉末與硝酸鹽過程制備的粉末具有相似的團聚性和燒結(jié)特性。(3)Y-PAA過程。在Y2O3過程基礎(chǔ)上,在原材料中加入占固體材料50 wt.%的聚丙烯酸(Polyacrylic acid,[C3H4O2]n,PAA),經(jīng)過700oC煅燒合成了分散較好的、純相的YAG粉末。此過程合成的粉末經(jīng)1550oC燒結(jié)后無“晶粒團”出現(xiàn),但是晶粒排列不致密。為了進一步改善粉體的燒結(jié)特性,接著利用硫酸鹽+硝酸鹽體系為原材料采用結(jié)晶方法來合成YAG粉末。此過程中以相對廉價的Y(NO3)3、Al(NO3)3和Al2(SO4)3為原材料,通過蒸發(fā)其水溶液的溶劑,使混合溶液中的離子發(fā)生重組而結(jié)晶析出飽和鹽,按照鹽的不同結(jié)晶析出順序構(gòu)成了三層核殼結(jié)構(gòu)的結(jié)晶前驅(qū)體,并通過煅燒此結(jié)晶前驅(qū)體來合成YAG粉末。實驗過程中發(fā)現(xiàn),增加原材料中SO2-4的含量,有利于改善粉末分散性,但不利于獲得純相的YAG粉末。當(dāng)原材料中n(SO2-4)/n(Y3+)=1.5時,煅燒1050oC合成的粉末分散性較優(yōu)。此粉末經(jīng)1550oC燒結(jié)后平均晶粒尺寸約為1.02um,晶粒分布均勻,表現(xiàn)出最佳的燒結(jié)特性。綜合分析以上幾種方法制備的YAG粉末的顆粒大小、分散性,及其燒結(jié)特性,總結(jié)出對粉末燒結(jié)特性影響較大的因素分別為:(1)分散性。只有高分散的粉末才能在燒結(jié)時發(fā)生同步生長,從而使得晶粒大小分布均勻,晶粒間氣孔含量較少。(2)顆粒大小。粉末一次顆粒越小,粉末的燒結(jié)活性越高;但粉末一次顆粒太小,又將會使得燒結(jié)中晶粒發(fā)生異常長大,使得晶粒分布不均勻。
[Abstract]:Yttrium aluminum garnet (Y _ 3AL _ 5o _ 12) is an important laser matrix material. Compared with YAG crystal transparent ceramics, because of its high stability, low manufacturing cost and easy to doped with large concentration, it has attracted great interest of scholars at home and abroad. In recent years, YAG single crystals have been replaced by YAG in many applications. High transparent YAG ceramics are the prerequisite for the preparation of high quality YAG laser ceramics. The sintering characteristic of YAG powder is one of the important factors affecting the transmittance of YAG ceramics. Therefore, the main purpose of this paper is to explore a simple and efficient synthesis method of YAG powder suitable for industrial production. The method can be used to synthesize YAG powders with uniform composition, good dispersion and appropriate size at low temperature, thus laying a good foundation for the preparation of YAG transparent ceramics. In this paper, YAG powder was synthesized by crystallization method using nitrate system as raw material. The specific research contents are divided into three parts: 1) nitrate process. Using only Y(NO3)3 and Al(NO3)3 as raw materials, using their high solubility in water and stirring their aqueous solution by heating, a more homogeneous crystal precursor of Y(NO3)3 and Al(NO3)3 was prepared. After calcined with 950oC, the pure phase YAG powder was synthesized. After the YAG powder was sintered by 1550oC, many "grain clusters" were formed in the samples. The grains in the "grain clusters" were arranged neatly and the porosity content was very small, but there was a very large process of porosity. On the basis of nitrate process, the pure phase YAG powder was prepared by 850oC calcination of the crystal precursor by adding 2 wt.%Y2O3 nano-powder into the raw material. The powders prepared by this process have similar agglomeration and sintering properties to those prepared by nitrate process. On the basis of Y2O3 process, polyacrylic acidate (50 wt.%) was added into the raw material, [C3H4O2] nacidic acid, [C3H4O2] PAA, was calcined by 700oC to synthesize well dispersed and pure phase YAG powder. The powder synthesized by this process did not appear "grain agglomeration" after 1550oC sintering, but the grain arrangement was not compact. In order to further improve the sintering properties of the powder, YAG powder was synthesized by crystallization method using sulfate nitrate system as raw material. In this process, the relatively cheap Yanno _ 3N _ 3O _ 3AlN _ 3N _ 3O _ 3 and Al2(SO4)3 were used as raw materials to crystallize and precipitate saturated salts by evaporating their aqueous solution solvent and recombination of the ions in the mixed solution. The crystal precursor with three layers of core-shell structure was formed according to the different crystallization precipitation order of salt, and the YAG powder was synthesized by calcining the crystal precursor. It was found in the experiment that increasing the content of SO2-4 in raw materials was beneficial to improve the dispersibility of the powder, but was not conducive to obtaining pure phase YAG powder. When n(SO2-4)/n(Y3 = 1.5 in raw materials, the dispersion of powders synthesized by calcination of 1050oC is better. The average grain size of the powder sintered by 1550oC is about 1.02um, and the grain distribution is uniform, showing the best sintering characteristics. The particle size, dispersity and sintering properties of YAG powders prepared by the above methods are analyzed. The factors that have a great influence on the sintering properties of YAG powders are concluded as follows: 1) dispersity. Only the highly dispersed powder can grow synchronously during sintering, so that the grain size distribution is uniform and the porosity content between grains is less. The smaller the primary particle is, the higher the sintering activity of the powder is, but the smaller the primary particle is, the more abnormal the grain growth will be and the uneven distribution of the grain will occur.
【學(xué)位授予單位】:華中科技大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ174.65

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