SPS快速燒結制備含鉍玻璃及其性能研究
發(fā)布時間：2018-08-27 11:38
【摘要】：鉍離子摻雜玻璃自發(fā)現(xiàn)具有超寬帶近紅外發(fā)光性能以來受到了科研人員的廣泛關注,它很有可能制成超寬帶光纖放大器以解決現(xiàn)有稀土摻雜光纖放大器增益帶寬不足的問題,從而實現(xiàn)光纖通信的超大容量傳輸。目前對于鉍離子摻雜玻璃的研究主要集中在提高其發(fā)光性能和探討其發(fā)光機理等問題上,而摻鉍玻璃的制備方法是影響其性能的一個重要因素之一。鉍離子摻雜玻璃的制備多采用高溫熔融法,這種方法存在著熔融溫度高、熔融時間長等缺點,這對于制備鉍離子這種易揮發(fā)離子的摻雜玻璃來說十分不利。為此,我們提出采用新型的玻璃制備工藝來制備鉍離子摻雜玻璃。本文采用多孔材料結合新型的放電等離子體燒結(Spark Plasma Sintering,SPS)技術制備摻鉍玻璃。多孔材料因其具有大的比表面積而具有較高的燒結活性,和普通粉體材料相比它更容易燒結。放電等離子體燒結技術具有升溫速度快、燒結時間短、燒結過程中可以加壓等優(yōu)點。我們將多孔材料和SPS技術有機的結合在一起成功的探索出了一條低溫快速制備透明石英玻璃的新方法。這一低溫快速的制備方法對于鉍離子摻雜玻璃的制備十分有利。本工作首先通過微孔材料zsm-5燒結制備樣品的透明與不透明的轉變過程研究了不導電材料在sps燒結過程中的溫度分布,并采用ansys熱分析軟件對燒結過程中的溫度分布進行了模擬。二是以zsm-5和介孔材料sba-15為原料采用sps制備了石英玻璃。通過改變zsm-5粉體的燒結參數(shù),系統(tǒng)地研究了沸石分子篩zsm-5由有序結構變成無序結構的過程;通過拉曼光譜、紅外光譜以及同步輻射等測試技術分析了在有序無序轉變過程中zsm-5沸石分子篩結構的變化,并研究了這些結構變化對于樣品透過率、發(fā)光性能以及力學性能的影響。探索了sps燒結介孔材料sba-15制備石英玻璃樣品的燒結過程,并對燒結樣品的性能進行了研究。三是通過等體積浸漬法制備了不同濃度鉍鋁共摻雜的zsm-5粉體,采用sps技術對粉體進行燒結得到鉍離子摻雜zsm-5玻璃。系統(tǒng)地研究了鉍離子和鋁離子濃度對于摻鉍玻璃發(fā)光性能的影響,考察了不同激發(fā)波長對于樣品近紅外發(fā)光性能的影響,并結合實驗現(xiàn)象和相關實驗結果對鉍離子的近紅外發(fā)光機理進行了探討。四是采用不同的粉體制備工藝制備出了鉍離子單摻或鉍鋁共摻的sba-15粉體,然后采用sps技術對粉體進行燒結得到鉍離子摻雜的sba-15玻璃。系統(tǒng)地研究了不同粉體制備工藝對于樣品顏色和發(fā)光性能的影響。本文得到的主要研究成果和結論如下:(1)利用沸石分子篩zsm-5燒結制備樣品的透明與不透明的轉變過程研究了不導電材料在sps燒結過程中的溫度分布,研究發(fā)現(xiàn)樣品在徑向和軸向上都存在溫度梯度。1325℃燒結制備的樣品出現(xiàn)了中間透明邊緣不透明的現(xiàn)象,說明樣品存在徑向的溫度梯度,ansys熱分析軟件模擬結果表明樣品中心溫度比邊緣溫度高26℃;1315℃燒結制備的樣品出現(xiàn)了上表面透明部分大于下表面的現(xiàn)象,說明樣品存在軸向的溫度梯度,ansys熱分析軟件模擬結果表明樣品上表面的溫度比下表面高5℃。(2)采用sps技術對微孔分子篩zsm-5和介孔材料sba-15進行燒結,實驗表明兩種粉體都能成功制備出透明的玻璃樣品。對zsm-5粉體燒結的一系列樣品的研究表明:樣品的透過率隨燒結溫度的升高是逐漸增大的,1300℃燒結制備的樣品在250~1700nm范圍內(nèi)的透過率小于5%,當樣品的燒結溫度達到1350℃以上時,樣品完全透明透過率達到最大值,在近紅外區(qū)(780~1700nm)的透過率在80%以上,在紫外-可見光區(qū)(250~780nm)的透過率也能達到60%以上,但在300nm處出現(xiàn)了一個吸收峰;樣品的發(fā)光則相反,隨著燒結溫度的升高樣品的發(fā)光強度逐漸降低;采用同步輻射x射線衍射和透射電鏡的測試結果都表明即使在完全透明的樣品中仍存在著少量的未完全坍塌的zsm-5,從而產(chǎn)生了缺陷,造成了樣品的吸收和發(fā)光。對sba-15粉體燒結的樣品進行研究,發(fā)現(xiàn)在1050℃就能夠獲得完全透明的樣品。樣品在可見紫外區(qū)的透過率均能夠達到近90%,這一透過率值和傳統(tǒng)熔融法制備的石英玻璃基本相當,要好于zsm-5燒結制備的玻璃樣品,也明顯好于sps燒結納米二氧化硅和無定形二氧化硅制備的玻璃樣品。(3)采用sps燒結摻鉍zsm-5粉體成功制備出了摻鉍玻璃,制備出的鉍離子摻雜玻璃具有良好的近紅外發(fā)光性能。鉍離子摻雜濃度對于sps燒結制備的摻鉍玻璃發(fā)光性能的影響是十分復雜的,含鋁量少時,采用500和700nm的光激發(fā)都能夠得到較強的近紅外熒光發(fā)射,但800nm的光激發(fā)無法得到近紅外發(fā)射;含鋁量較多時,樣品采用500、700和800nm的光激發(fā)都能夠得到近紅外的熒光發(fā)射,但發(fā)光強度的變化規(guī)律是不同的,采用500、700nm的光激發(fā)產(chǎn)生的近紅外光的發(fā)光強度變化是一致的,而800nm激發(fā)產(chǎn)生的近紅外光的發(fā)光強度變化和它們不同。鋁離子對于鉍離子摻雜玻璃的性能具有十分大的影響,樣品的顏色會隨著鋁離子濃度的增加而加深;鋁離子含量在一定范圍內(nèi)的提高會增強500、700、800nm激發(fā)產(chǎn)生的近紅外發(fā)光的發(fā)光強度,但鋁離子的含量是不同的,500、700nm在鉍鋁比為1:3時就達到了最大值,而800nm在鉍鋁比為1:9時才達到最大值。有趣的是我們研究激發(fā)波長的影響時發(fā)現(xiàn)采用600nm的光激發(fā)摻鉍玻璃能夠產(chǎn)生熒光半高寬為273nm、發(fā)光峰位置為1207nm的近紅外發(fā)光,而且其發(fā)光強度要好于800nm激發(fā)產(chǎn)生的近紅外光。通過對實驗現(xiàn)象和結果的分析我們認為摻鉍玻璃在~1140nm處的發(fā)光是由于bi+的3p1→3p0的能級躍遷產(chǎn)生的,在~1240nm處的發(fā)光來自于bi0的2d3/2→4s3/2的能級躍遷,在~1440nm處的發(fā)光可以歸結為(bi2)2-的→3Π2g的能級躍遷。(4)采用不同的粉體制備工藝制備了鉍離子單摻雜的sba-15粉體和鉍鋁共摻雜的sba-15粉體,然后采用sps技術對粉體進行燒結得到了摻鉍玻璃。鉍離子單摻sba-15粉體制備的摻鉍玻璃在500、700和800nm的光激發(fā)下并沒有表現(xiàn)出近紅外發(fā)光性能,說明鋁離子等修飾劑對于摻鉍玻璃的近紅外發(fā)光性能是必不可少的。采用等體積浸漬法制備的鉍鋁共摻雜粉體燒結后樣品呈現(xiàn)出灰黑色,且隨著濃度的增加顏色逐漸加深,采用500、700nm的光激發(fā)樣品可以產(chǎn)生近紅外光,但800nm的光激發(fā)并沒有發(fā)現(xiàn)很明顯的發(fā)射現(xiàn)象。采用原位合成稀釋球磨制備的低濃度樣品的顏色和發(fā)光性能與等體積浸漬法制備樣品的顏色和性能基本一致。采用水熱法合成的鉍鋁共摻雜粉體制備的樣品在摻雜濃度為0.10mol%時,樣品的顏色呈現(xiàn)出灰黑色,XRD表明樣品中出現(xiàn)了鉍金屬,而當摻雜濃度大于0.30mol%時樣品呈現(xiàn)出紅色,且隨著鉍離子濃度的增加顏色逐漸加深,熒光性能測試表明紅色的樣品在500、700或800nm的光激發(fā)下都能夠產(chǎn)生強的熒光發(fā)射,而灰黑色樣品的發(fā)光性能很差,800nm的光激發(fā)時幾乎沒有熒光發(fā)射。采用不同的激發(fā)波長對0.90mol%的樣品進行測試發(fā)現(xiàn)大部分發(fā)光峰的峰值與ZSM-5制備的樣品相比都有一定程度的紅移,而且熒光半高寬變得更加的均勻,大多集中在230、240nm。對于低濃度SBA-15體系摻鉍樣品變成灰黑色的原因我們認為可能是鉍氧化物的熱分解作用、SBA-15表面的硅羥基或者粉體的燒結機理等因素造成的,也可能是這些因素共同作用的結果。
[Abstract]:Bismuth ion-doped glass has attracted much attention of researchers since it was found to have ultra-wideband near-infrared luminescence properties. It is possible to make ultra-wideband fiber amplifiers to solve the problem of insufficient gain bandwidth of existing rare earth-doped fiber amplifiers, so as to realize ultra-large capacity transmission of optical fiber communications. The research of glass is mainly focused on improving its luminescent properties and discussing its luminescent mechanism. The preparation method of bismuth-doped glass is one of the important factors affecting its properties. Bismuth-doped glasses are very disadvantageous for the volatile ion-doped glasses. Therefore, we propose a new glass preparation process to prepare Bismuth-doped glasses. In this paper, the porous materials combined with a new spark plasma sintering (SPS) technology are used to prepare Bismuth-doped glasses. Porous materials have a large specific surface area. The spark plasma sintering technology has the advantages of rapid heating, short sintering time and pressure during sintering process. We have successfully combined the porous materials and SPS technology to explore a rapid preparation of transparent quartz at low temperature. A new method for preparing bismuth ion-doped glass at low temperature and high speed is proposed. The temperature distribution of non-conductive materials during SPS sintering is studied by the transparent and opaque transition process of samples prepared by sintering microporous material zsm-5. The sintering process is analyzed by using ANSYS thermal analysis software. Temperature distribution in Zsm-5 was simulated. Secondly, quartz glass was prepared from ZSM-5 and mesoporous material SBA-15 by sps. By changing the sintering parameters of ZSM-5 powder, the process of zeolite zeolite ZSM-5 from ordered structure to disordered structure was systematically studied. Raman spectroscopy, infrared spectroscopy and synchrotron radiation were used to analyze the process. The structural changes of zeolite ZSM-5 during ordered disorder transformation were studied. The effects of these structural changes on the transmittance, luminescence and mechanical properties of the samples were investigated. The sintering process of mesoporous material SBA-15 was explored and the properties of the sintered samples were studied. Bismuth-doped ZSM-5 glasses were prepared by deposition impregnation method. Bismuth-doped ZSM-5 glasses were sintered by SPS technique. The effects of Bismuth ion and Al ion concentration on the luminescent properties of Bismuth-doped glasses were studied systematically. The influence of excitation wavelength on the Near-infrared Luminescent Properties of samples was investigated. The mechanism of near infrared luminescence of bismuth ion was discussed by experimental phenomena and correlative experimental results. Fourthly, different powder preparation techniques were used to prepare bismuth ion mono-doped or bismuth-aluminum co-doped SBA-15 powders. Then bismuth ion-doped SBA-15 glass was obtained by SPS technique. The main research results and conclusions are as follows: (1) the temperature distribution of non-conductive materials during SPS sintering was studied by using the transparent and opaque transition process of the samples prepared by zeolite ZSM-5 sintering, and the temperature gradients were found in both radial and axial directions. The results of ANSYS thermal analysis software simulation show that the center temperature of the sample is 26 degrees higher than the edge temperature; the transparent part of the upper surface is larger than the lower surface of the sample sintered at 1315 degrees Celsius, indicating that the sample has a radial temperature gradient. The results of ANSYS thermal analysis software simulation show that the temperature of the upper surface of the sample is higher than that of the lower surface by 5 (?) The transmittance of the sample increases gradually with the sintering temperature. The transmittance of the sample sintered at 1300 C is less than 5% in the range of 250 ~ 1700 nm. When the sintering temperature of the sample is above 1350 C, the transmittance of the sample reaches the maximum value. The transmittance in the near infrared region (780 ~ 1700 nm) is above 80%, and in the ultraviolet - visible region (25 - 1700 nm). The transmittance of 0~780 nm can reach over 60%, but an absorption peak appears at 300 nm. On the contrary, the luminescence intensity of the samples decreases with the increase of sintering temperature. The results of synchrotron radiation X-ray diffraction and transmission electron microscopy show that there are still a small amount of unfinished samples even in completely transparent samples. The samples sintered by SBA-15 powder were found to be completely transparent at 1050 C. The transmittance of the samples in the visible-ultraviolet region reached nearly 90%, which was almost the same as that of the quartz glass prepared by traditional melting method. (3) Bismuth-doped glass was successfully prepared by using sps-sintered bismuth-doped ZSM-5 powder, and the prepared bismuth-doped glass has good near-infrared luminescence properties. The influence of Al content on the luminescent properties of bismuth-doped glasses is very complex. When Al content is small, the near-infrared fluorescence can be obtained by 500 nm and 700 nm photoexcitation, but the near-infrared fluorescence can not be obtained by 800 nm photoexcitation. When Al content is high, the samples can be excited by 500,700 and 800 nm photoexcitation to obtain near-infrared fluorescence. The luminous intensity of the near infrared light excited by 500,700 nm is the same, but the luminous intensity of the near infrared light excited by 800 nm is different from them. Increasing the concentration of Al ions in a certain range will enhance the near-infrared luminescence intensity produced by 500,700,800 nm excitation, but the content of Al ions is different. 500,700 nm reaches the maximum when the ratio of Bi to Al is 1:3, and 800 nm reaches the maximum when the ratio of Bi to Al is 1:9. When the excitation wavelength is changed, it is found that the near-infrared luminescence can be produced by using 600 nm light to excite the bismuth-doped glass with a half-width of 273 nm and a peak position of 1207 nm, and the luminescence intensity is better than that of 800 nm light. The luminescence at ~1240 nm comes from the 2d_3/2 4s_3/2 energy level transition of Bi + at 3p_1 3p_0. The luminescence at ~1440 nm can be attributed to the 3 2G energy level transition of 2 of 2 of 2 of 2 of 2 of 2 of 3 2 of 2 of 2 of 2 of 2 of 2 of Bismuth-doped glass was obtained by SPS technique. Bismuth-doped glass prepared by SBA-15 powder doped with Bismuth ion did not exhibit Near-infrared Luminescent Properties under 500,700 and 800 nm light excitation, indicating that aluminum ion modifier is essential for Near-infrared Luminescent Properties of Bismuth-doped glass. Bismuth-doped glass was prepared by isovolumetric impregnation method. The samples sintered by bismuth-aluminium co-doped powders show gray-black color, and the color gradually deepens with the increase of concentration. The samples excited by 500,700 nm light can produce near-infrared light, but there is no obvious emission at 800 nm. The color and luminescent properties of low concentration samples prepared by in-situ synthesis dilution ball milling The color and properties of the samples prepared by hydrothermal method are basically the same as those prepared by isovolumetric impregnation method. When the doping concentration is 0.10mol%, the color of the samples is gray-black. XRD shows that there is bismuth metal in the samples, but when the doping concentration is more than 0.30mol%, the samples show red, and with the separation of bismuth. The fluorescence properties of the samples with different excitation wavelengths of 0.90 mol% showed that most of the samples with different excitation wavelengths produced strong fluorescence emission. The peak value of the distribution peak has a certain red shift compared with the sample prepared by ZSM-5, and the fluorescence half-width becomes more uniform, mostly concentrated at 230,240 nm. The sintering mechanism and other factors may also be the result of these factors.
【學位授予單位】：東華大學
【學位級別】：博士
【學位授予年份】：2016
【分類號】：TQ171.1
本文編號：2207157
[Abstract]:Bismuth ion-doped glass has attracted much attention of researchers since it was found to have ultra-wideband near-infrared luminescence properties. It is possible to make ultra-wideband fiber amplifiers to solve the problem of insufficient gain bandwidth of existing rare earth-doped fiber amplifiers, so as to realize ultra-large capacity transmission of optical fiber communications. The research of glass is mainly focused on improving its luminescent properties and discussing its luminescent mechanism. The preparation method of bismuth-doped glass is one of the important factors affecting its properties. Bismuth-doped glasses are very disadvantageous for the volatile ion-doped glasses. Therefore, we propose a new glass preparation process to prepare Bismuth-doped glasses. In this paper, the porous materials combined with a new spark plasma sintering (SPS) technology are used to prepare Bismuth-doped glasses. Porous materials have a large specific surface area. The spark plasma sintering technology has the advantages of rapid heating, short sintering time and pressure during sintering process. We have successfully combined the porous materials and SPS technology to explore a rapid preparation of transparent quartz at low temperature. A new method for preparing bismuth ion-doped glass at low temperature and high speed is proposed. The temperature distribution of non-conductive materials during SPS sintering is studied by the transparent and opaque transition process of samples prepared by sintering microporous material zsm-5. The sintering process is analyzed by using ANSYS thermal analysis software. Temperature distribution in Zsm-5 was simulated. Secondly, quartz glass was prepared from ZSM-5 and mesoporous material SBA-15 by sps. By changing the sintering parameters of ZSM-5 powder, the process of zeolite zeolite ZSM-5 from ordered structure to disordered structure was systematically studied. Raman spectroscopy, infrared spectroscopy and synchrotron radiation were used to analyze the process. The structural changes of zeolite ZSM-5 during ordered disorder transformation were studied. The effects of these structural changes on the transmittance, luminescence and mechanical properties of the samples were investigated. The sintering process of mesoporous material SBA-15 was explored and the properties of the sintered samples were studied. Bismuth-doped ZSM-5 glasses were prepared by deposition impregnation method. Bismuth-doped ZSM-5 glasses were sintered by SPS technique. The effects of Bismuth ion and Al ion concentration on the luminescent properties of Bismuth-doped glasses were studied systematically. The influence of excitation wavelength on the Near-infrared Luminescent Properties of samples was investigated. The mechanism of near infrared luminescence of bismuth ion was discussed by experimental phenomena and correlative experimental results. Fourthly, different powder preparation techniques were used to prepare bismuth ion mono-doped or bismuth-aluminum co-doped SBA-15 powders. Then bismuth ion-doped SBA-15 glass was obtained by SPS technique. The main research results and conclusions are as follows: (1) the temperature distribution of non-conductive materials during SPS sintering was studied by using the transparent and opaque transition process of the samples prepared by zeolite ZSM-5 sintering, and the temperature gradients were found in both radial and axial directions. The results of ANSYS thermal analysis software simulation show that the center temperature of the sample is 26 degrees higher than the edge temperature; the transparent part of the upper surface is larger than the lower surface of the sample sintered at 1315 degrees Celsius, indicating that the sample has a radial temperature gradient. The results of ANSYS thermal analysis software simulation show that the temperature of the upper surface of the sample is higher than that of the lower surface by 5 (?) The transmittance of the sample increases gradually with the sintering temperature. The transmittance of the sample sintered at 1300 C is less than 5% in the range of 250 ~ 1700 nm. When the sintering temperature of the sample is above 1350 C, the transmittance of the sample reaches the maximum value. The transmittance in the near infrared region (780 ~ 1700 nm) is above 80%, and in the ultraviolet - visible region (25 - 1700 nm). The transmittance of 0~780 nm can reach over 60%, but an absorption peak appears at 300 nm. On the contrary, the luminescence intensity of the samples decreases with the increase of sintering temperature. The results of synchrotron radiation X-ray diffraction and transmission electron microscopy show that there are still a small amount of unfinished samples even in completely transparent samples. The samples sintered by SBA-15 powder were found to be completely transparent at 1050 C. The transmittance of the samples in the visible-ultraviolet region reached nearly 90%, which was almost the same as that of the quartz glass prepared by traditional melting method. (3) Bismuth-doped glass was successfully prepared by using sps-sintered bismuth-doped ZSM-5 powder, and the prepared bismuth-doped glass has good near-infrared luminescence properties. The influence of Al content on the luminescent properties of bismuth-doped glasses is very complex. When Al content is small, the near-infrared fluorescence can be obtained by 500 nm and 700 nm photoexcitation, but the near-infrared fluorescence can not be obtained by 800 nm photoexcitation. When Al content is high, the samples can be excited by 500,700 and 800 nm photoexcitation to obtain near-infrared fluorescence. The luminous intensity of the near infrared light excited by 500,700 nm is the same, but the luminous intensity of the near infrared light excited by 800 nm is different from them. Increasing the concentration of Al ions in a certain range will enhance the near-infrared luminescence intensity produced by 500,700,800 nm excitation, but the content of Al ions is different. 500,700 nm reaches the maximum when the ratio of Bi to Al is 1:3, and 800 nm reaches the maximum when the ratio of Bi to Al is 1:9. When the excitation wavelength is changed, it is found that the near-infrared luminescence can be produced by using 600 nm light to excite the bismuth-doped glass with a half-width of 273 nm and a peak position of 1207 nm, and the luminescence intensity is better than that of 800 nm light. The luminescence at ~1240 nm comes from the 2d_3/2 4s_3/2 energy level transition of Bi + at 3p_1 3p_0. The luminescence at ~1440 nm can be attributed to the 3 2G energy level transition of 2 of 2 of 2 of 2 of 2 of 2 of 3 2 of 2 of 2 of 2 of 2 of 2 of Bismuth-doped glass was obtained by SPS technique. Bismuth-doped glass prepared by SBA-15 powder doped with Bismuth ion did not exhibit Near-infrared Luminescent Properties under 500,700 and 800 nm light excitation, indicating that aluminum ion modifier is essential for Near-infrared Luminescent Properties of Bismuth-doped glass. Bismuth-doped glass was prepared by isovolumetric impregnation method. The samples sintered by bismuth-aluminium co-doped powders show gray-black color, and the color gradually deepens with the increase of concentration. The samples excited by 500,700 nm light can produce near-infrared light, but there is no obvious emission at 800 nm. The color and luminescent properties of low concentration samples prepared by in-situ synthesis dilution ball milling The color and properties of the samples prepared by hydrothermal method are basically the same as those prepared by isovolumetric impregnation method. When the doping concentration is 0.10mol%, the color of the samples is gray-black. XRD shows that there is bismuth metal in the samples, but when the doping concentration is more than 0.30mol%, the samples show red, and with the separation of bismuth. The fluorescence properties of the samples with different excitation wavelengths of 0.90 mol% showed that most of the samples with different excitation wavelengths produced strong fluorescence emission. The peak value of the distribution peak has a certain red shift compared with the sample prepared by ZSM-5, and the fluorescence half-width becomes more uniform, mostly concentrated at 230,240 nm. The sintering mechanism and other factors may also be the result of these factors.
【學位授予單位】：東華大學
【學位級別】：博士
【學位授予年份】：2016
【分類號】：TQ171.1
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