本文選題：Nd:YAG透明陶瓷 + 燒結(jié)助劑��； 參考：《西安電子科技大學(xué)》2015年博士論文

【摘要】：隨著陶瓷制備技術(shù)的高速發(fā)展,Nd:YAG透明陶瓷作為固體激光材料,自出現(xiàn)以來,在工業(yè)、醫(yī)療、國(guó)防等領(lǐng)域得到了廣泛的應(yīng)用。本文采用固相反應(yīng)真空燒結(jié)法,以高純Al_2O_3、Y_2O_3和Nd_2O_3為原料,利用X射線衍射分析、掃描電鏡、分光光度計(jì)和導(dǎo)熱儀等儀器,分別對(duì)陶瓷樣品的物相、顯微結(jié)構(gòu)和熱性能進(jìn)行了表征,研究了Nd:YAG激光陶瓷的關(guān)鍵技術(shù)、激光性能和熱性能,為Nd:YAG激光陶瓷的國(guó)產(chǎn)化提供了實(shí)驗(yàn)依據(jù)。以高純Al_2O_3、Y_2O_3和Nd_2O_3為原料,采用固相反應(yīng)法,添加不同含量的TEOS制備Nd:YAG透明陶瓷。得到在1750℃燒結(jié)30h,添加0.3wt%TEOS的樣品致密化程度較高,有個(gè)別氣孔分布在晶粒內(nèi)部,晶界上無雜質(zhì)相生成,平均晶粒尺寸為30μm左右,在1064nm處的透過率為72.32%。在添加TEOS的基礎(chǔ)上添加不同質(zhì)量分?jǐn)?shù)的MgO作為復(fù)合燒結(jié)助劑制備陶瓷,得到添加0.3wt%TEOS+0.3wt%MgO的陶瓷樣品,在1730℃燒結(jié)30h,致密化程度高,晶界上無雜質(zhì)相生成,平均晶粒尺寸為25μm,晶粒均勻,在1064nm處的透過率為78.46%,高于僅添加TEOS的樣品在1064nm處透過率值(72.32%)。這主要是因?yàn)镸gO加入起到抑制晶粒生長(zhǎng),增加晶界密度,為氣孔的排出提供更多通道,所以陶瓷的透過率得到提高。對(duì)于B_2O_3和SiO_2作為復(fù)合燒結(jié)助劑,在保持添加總量不變的情況下,通過改變B~(3+):Si4+比例(0.5,1.0,2.0),研究了其對(duì)樣品顯微結(jié)構(gòu)及透過率的影響。得到當(dāng)B~(3+):Si4+=0.5,在1700℃燒結(jié)30h的樣品其致密度較高,在1064nm處的透過率為76.87%,晶界干凈,晶粒均勻。這主要是因?yàn)锽_2O_3通過降低液相的粘度來提高樣品的致密化速率,使得陶瓷快速到達(dá)理論致密度值,所以添加B_2O_3能降低陶瓷的燒結(jié)溫度。采用固相反應(yīng)法、化學(xué)共沉淀法以及溶膠—凝膠法在不同燒結(jié)溫度下合成了Nd:YAG粉體,進(jìn)而使用Nd:YAG粉體制備陶瓷樣品,通過對(duì)比陶瓷樣品的顯微形貌及測(cè)量其透過率值,選擇固相反應(yīng)法制備Nd:YAG透明陶瓷。通過對(duì)Y_2O_3粉體的預(yù)處理、改進(jìn)素坯成型方式及改變燒結(jié)制度,制備厚尺寸Nd:YAG激光陶瓷。使用冷等靜壓成型的素坯相對(duì)密度為51.6%,高于雙向軸壓的素坯相對(duì)密度。以素坯成型為基礎(chǔ),設(shè)計(jì)模具,實(shí)現(xiàn)了Nd~(3+)濃度的梯度摻雜。由于粉體顆粒尺寸、燒結(jié)活性、比表面積值不同,使用不同處理方式的Y_2O_3粉體合成YAG相的溫度不同。從化學(xué)沉淀法處理到1200℃熱處理,合成YAG相的溫度依次提高50℃。采用不同處理方法的Y_2O_3粉體,使用冷等靜壓法制備的素坯在1730℃燒結(jié)30h,得到的陶瓷樣品顯微結(jié)構(gòu)差異明顯。以1200℃熱處理2h的Y_2O_3粉體為原料,得到的樣品晶粒尺寸均勻,大小約為15μm,氣孔含量少,在1064nm處透過率為78.46%。對(duì)1200℃熱處理2h的Y_2O_3粉體為原料制備的樣品,通過改變燒結(jié)制度,得到升溫速率為1℃/min,保溫時(shí)間為30h燒結(jié)成的陶瓷樣品顯微結(jié)構(gòu)中晶粒內(nèi)部的氣孔基本排除完全,在1064nm和400nm處的透過率分別為83.59%、80.82%,達(dá)到了作為激光材料透明度的要求。選用平行平面諧振腔,端面泵浦的方式,成功實(shí)現(xiàn)了Nd:YAG透明陶瓷1064nm的激光輸出,其中泵浦閾值為1.15w,最大輸出功率為1.54w,相應(yīng)的光—光轉(zhuǎn)換效率為18.4%,斜效率為21.3%。同時(shí)采用LFA—447的Nanoflash導(dǎo)熱儀來測(cè)量不同透過率及不同晶粒尺寸的陶瓷樣品的熱擴(kuò)散系數(shù)、比熱值,并計(jì)算出陶瓷樣品的熱導(dǎo)系數(shù)。得到陶瓷樣品的熱導(dǎo)率隨著氣孔率的增大(即透過率減小)而減小,并隨著晶粒尺寸的增大(即晶界密度的減小)而增大,為制備高熱導(dǎo)率的陶瓷樣品提供參數(shù)指標(biāo)。
[Abstract]:With the rapid development of ceramic preparation technology, Nd:YAG transparent ceramics, as solid laser materials, have been widely used in the fields of industry, medical treatment and national defense since they appeared. In this paper, the solid phase reaction vacuum sintering method was used, with high purity Al_2O_3, Y_2O_3 and Nd_2O_3 as raw materials, using X ray diffraction analysis, scanning electron microscope, spectrophotometer and guide. The phase, microstructure and thermal properties of the ceramic samples were characterized by heat instrument and other instruments. The key technologies, laser properties and thermal properties of Nd:YAG laser ceramics were studied. The experimental basis for the localization of Nd:YAG laser ceramics was provided. The high purity Al_2O_3, Y_2O_3 and Nd_2O_3 were used as raw materials, and the solid phase reaction was used to add different content of TEO. Nd:YAG transparent ceramics were prepared by S. The samples were sintered at 1750 C for 30h, and the densification degree of the samples added with 0.3wt%TEOS was high. There were some pores in the grain and no impurity phase on the grain boundary. The average grain size was about 30 m, and the transmittance at 1064nm was 72.32%. on the basis of adding TEOS. The ceramics were prepared by sintering aids, and the 0.3wt%TEOS+0.3wt%MgO ceramic samples were obtained. The densification degree was high at 1730 C for 30h. The densification degree was high and the grain boundary was not formed. The average grain size was 25 m, the grain was uniform and the transmittance at 1064nm was 78.46%, which was higher than that of the samples with TEOS only at 1064nm (72.32%). This is mainly due to MgO plus. In order to suppress the grain growth, increase the grain boundary density and provide more channels for the discharge of the pores, the transmittance of the ceramics is improved. For B_2O_3 and SiO_2 as a composite sintering additive, the microstructure and transmittance of the samples are studied by changing the amount of B~ (3+): Si4+ (0.5,1.0,2.0). When B~ (3+): Si4+=0.5, the density of the samples sintered at 1700 C for 30h is higher, the transmittance at 1064nm is 76.87%, the grain boundary is clean and the grain is uniform. This is mainly because B_2O_3 increases the densification rate of the sample by reducing the viscosity of the liquid phase and makes the ceramics reach the theoretical density value at a fast speed, so the addition of B_2O_3 can reduce the pottery. The sintering temperature of porcelain was prepared by solid phase reaction, chemical coprecipitation and sol-gel synthesis of Nd:YAG powders at different sintering temperatures. Then the ceramic samples were prepared by using Nd:YAG powder system. By comparing the microstructure of the ceramic samples and measuring the transmittance of the ceramics, the transparent Nd:YAG ceramics were prepared by the solid phase reaction method, and Y_2O_3 was prepared by the method of solid phase reaction. The thick size Nd:YAG laser ceramics are prepared by the pretreatment of the powder, improving the forming mode of the plain billet and changing the sintering system. The relative density of the plain blank with cold isostatic pressure is 51.6%, which is higher than the relative density of the billet. Based on the forming of the plain billet, the mold is designed to achieve the gradient doping of the concentration of Nd~ (3+). The temperature of YAG phase synthesized by Y_2O_3 powder with different treatment methods is different. The temperature of the synthetic YAG phase is increased by 50 degrees centigrade by the chemical precipitation process to 1200 C heat treatment. The ceramic samples prepared by the cold isostatic pressure method by cold isostatic pressure method are sintered at 1730 C for 30h. The microstructure difference is obvious. With the Y_2O_3 powder of heat treated 2H at 1200 C as raw material, the grain size of the sample is uniform, the size is about 15 mu m, the gas pore content is little, the transmittance at 1064nm is 78.46%. to the Y_2O_3 powder of 2H at 1200 C heat treatment 2h, and the heating rate is 1 C /min and the heat preservation time is obtained by changing the sintering system. The pores in the microstructures of the 30h sintered ceramic samples are basically eliminated completely, and the transmittance at 1064nm and 400nm is 83.59%, 80.82% respectively, reaching the requirement of the transparency of the laser materials. The laser output of the Nd:YAG transparent ceramic 1064nm is successfully realized by using the parallel plane resonant cavity and the end pump mode. The pump threshold is 1.15w, the maximum output power is 1.54w, the corresponding light to light conversion efficiency is 18.4%, the oblique efficiency is 21.3%. and the LFA 447 Nanoflash thermal conductivity meter is used to measure the thermal diffusivity of the ceramic samples with different transmittance and different grain sizes, the specific heat value and the thermal conductivity of the ceramic samples are calculated. The ceramic samples are obtained. The thermal conductivity decreases with the increase of the porosity (that is, the transmittance decrease), and increases with the increase of grain size (i.e. the decrease of grain boundary density), which provides parameters for the ceramic samples prepared with high thermal conductivity.

【學(xué)位授予單位】：西安電子科技大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ174.1

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