高性能Nd:YAG激光透明陶瓷的制備及激光實(shí)驗(yàn)
本文選題:Nd:YAG 切入點(diǎn):熱處理 出處:《西安電子科技大學(xué)》2015年碩士論文
【摘要】:摻釹釔鋁石榴石(Nd:YAG)多晶陶瓷可避其單晶和玻璃之劣勢而集兩者之優(yōu)勢于一身,具有良好的光學(xué)性能和機(jī)械強(qiáng)度以及穩(wěn)定的物理化學(xué)性質(zhì),被廣泛應(yīng)用于激光增益介質(zhì)及透明窗口材料。本論文選用高純商業(yè)氧化釔、氧化鋁、氧化釹為原料,以正硅酸乙酯和氧化鎂為燒結(jié)助劑,采用固相反應(yīng)法,利用真空燒結(jié)技術(shù),在高溫下制備1at%Nd:YAG激光透明陶瓷。實(shí)驗(yàn)中,我們深入研究和討論了原料Y_2O_3不同溫度熱處理對樣品透過率的影響及其機(jī)理;運(yùn)用高能球磨機(jī)制備了粒度較小、尺寸均一的Y_2O_3粉體,并使用其制備了實(shí)驗(yàn)樣品且展開了相關(guān)分析;運(yùn)用冷等靜壓技術(shù)制備樣品素坯,并與傳統(tǒng)手動壓片對比中體現(xiàn)其優(yōu)勢;將真空燒結(jié)過程的升溫階段和保溫階段分而研究,在詳細(xì)對比分析其現(xiàn)象和探討機(jī)理中,確定最佳升溫速率和保溫時間;探究了退火處理影響樣品透過率的內(nèi)因;最終進(jìn)一步改進(jìn)實(shí)驗(yàn)方案,制得高質(zhì)量實(shí)驗(yàn)樣品,并搭建出光系統(tǒng),對樣品進(jìn)行出光試驗(yàn)。最終我們得到如下結(jié)論:1)基于電鏡掃描圖(SEM)的觀察,氧化釔原料顆粒為有斷層的塊狀結(jié)構(gòu),且有大量空隙存在于斷層之中,這些空隙在一定程度上會形成樣品內(nèi)部影響透過率的氣孔。對氧化釔進(jìn)行熱處理,能有效消除這些空隙,進(jìn)而減少樣品內(nèi)氣孔的形成而提高樣品透明度。2)通過高能球磨機(jī)球磨處理,可得到粒度較小、尺寸均一的Y_2O_3原料粉體,理論上講,粒度減小則比表面積增大,活性增強(qiáng),可促進(jìn)燒結(jié)過程的進(jìn)行并提高其致密化程度。3)運(yùn)用冷等靜壓機(jī)壓片,可使得樣品素坯具有良好的致密性和均勻性,一方面可在燒結(jié)前最大程度減少樣品內(nèi)部的氣孔,另一方面良好的均勻性有利于樣品在燒結(jié)過程中形成尺寸均勻的晶粒,而減少光在樣品內(nèi)部的損耗,從而提高樣品透過率。4)燒結(jié)過程升溫速率為1℃/1.5min,既可為樣品內(nèi)氣孔排出提供足夠時間,又不至于晶粒生長過大晶界數(shù)量減少而減少氣孔排出通道,此升溫速率下制備的樣品透過率高。5)燒結(jié)過程中保溫時間的延長,有利于氣孔的最大化排出和增加樣品的致密性,進(jìn)而提高樣品透過率。在實(shí)驗(yàn)對比中發(fā)現(xiàn),保溫時間超過30h后,樣品透過率增加極其微小,綜合考慮實(shí)驗(yàn)成本和要求,將30h確定為實(shí)驗(yàn)的最佳保溫時間。6)退火處理可有效消除樣品內(nèi)的氧空位和應(yīng)力,提高樣品在可見光范圍內(nèi)的透過率。7)最后的出光實(shí)驗(yàn)不理想,分析其原因一方面可能是陶瓷樣品閾值問題,微小氣孔和雜質(zhì)構(gòu)成的第二相形成光的散射和吸收中心,降低樣品對808nm波長入射光的吸收利用;另一方面可能是樣品的實(shí)際厚度較薄,小于波長為808nm光進(jìn)入樣品體內(nèi)強(qiáng)度將為原強(qiáng)度1/e時的吸收長度,以致不能產(chǎn)生足夠能量來穩(wěn)定發(fā)射波長為1064nm激光。
[Abstract]:Neodymium doped yttrium aluminum garnet (Nd:YAG) polycrystalline ceramics can avoid the disadvantages of the single crystal and glass and set their advantages in one, with physical and chemical properties, optical properties and good mechanical strength and stability, is widely used in laser gain medium and a transparent window material. The use of high pure commercial yttrium oxide, aluminum oxide, neodymium oxide as raw materials, using TEOS and Magnesium Oxide as sintering additive by solid phase reaction method by vacuum sintering technology, the preparation of 1at%Nd:YAG transparent laser ceramic at high temperature. In the experiment, we studied and discussed the raw materials of Y_2O_3 with different heat treatment temperature on the sample transmittance of the effect and mechanism of small size; by using high energy ball mill, Y_2O_3 powder with uniform size, and using the same experimental samples were prepared and analyzed; samples blank by cold isostatic pressing technology, and with the traditional manual The advantages of tablet contrast; temperature stage vacuum sintering process and heat preservation and research, in the detailed comparative analysis of the phenomenon and to explore the mechanism, determine the optimal heating rate and holding time; to explore the effect of annealing the sample through the rate of internal cause; finally further improve the experiment, make high quality experiment the sample, and build a system of light, light of test samples. Finally we get the following conclusions: 1) scanning electron microscope (SEM) based on the observation of yttrium oxide particles as raw materials, fault block structure, and there is a large gap exists in the fault, the gap formed inside the sample through the effect rate porosity to some extent. Heat treatment of yttrium oxide, can effectively eliminate these gaps and reduce the formation of pores in the samples and improve the sample.2) by high energy ball milling transparency, particle can be obtained Small, Y_2O_3 powder with uniform size, in theory, particle size reduces the surface area increase, enhanced activity, can promote the sintering process and improve the densification of.3) by cold isostatic press press, can make the sample blank with good compactness and uniformity, on the one hand before sintering to minimize pores inside the sample, even on the other hand is beneficial to the formation of uniform grain size of samples during sintering process, and reduce the loss of light inside the sample, thereby improving the sample transmittance.4) sintering process heating rate is 1 DEG /1.5min, can provide enough time for the sample air discharge, without excessive grain growth and reduce the grain boundary to reduce the number of air outlet channel, the heating rate of the sample prepared by high rate.5) prolongation of the sintering process, the maximum benefit of stomata Discharge and increase the density of the sample, and then improve the sample transmittance. Found in the experiment, the holding time is over 30h, the sample transmittance increase is extremely small, considering the experimental cost and requirements, identify 30h as the best heat preservation time.6 experiment) annealing treatment can effectively eliminate the oxygen vacancies within the sample and force, improve the transmittance of the.7 samples in the visible range) the last light experiment is not ideal, analyzed the reason on the one hand may be ceramic sample thresholds, made of tiny pores and impurity of the second phase into light scattering and absorption in the heart, reduce the sample to 808nm the wavelength of incident light absorbed by another; may be the actual thickness of the sample is thinner, smaller than the wavelength of 808nm light intensity will enter the sample body absorption strength of 1/e, the length of the original, so that cannot produce enough energy to stabilize the emission wavelength of 1064nm laser.
【學(xué)位授予單位】:西安電子科技大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ174.1
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