本文選題：稀土發(fā)光材料 + 氟化物　； 參考：《河北大學(xué)》2017年碩士論文

【摘要】：近年來(lái),新興的生物成像技術(shù)能夠?qū)崟r(shí)無(wú)損動(dòng)態(tài)監(jiān)測(cè)被標(biāo)記的細(xì)胞在活體小動(dòng)物體內(nèi)的活動(dòng)及反應(yīng),生物成像材料主要有量子點(diǎn)及納米上轉(zhuǎn)換材料等。但由于激發(fā)光源對(duì)組織的穿透能力較差,該應(yīng)用只能用于體表組織。X射線由于具有良好的組織穿透性,是進(jìn)行體內(nèi)生物成像的理想光源,但鑒于其對(duì)人體的危害性,輻射劑量不能過(guò)大,因此X射線激發(fā)下的長(zhǎng)余輝材料是很理想的生物成像材料。本論文的研究致力于尋找合適的材料,在低劑量X射線照射下實(shí)現(xiàn)長(zhǎng)時(shí)間的余輝發(fā)射。本文分別選用高溫固相法、水熱法和熱解法合成了氟化物為基質(zhì)的熒光材料,通過(guò)X射線衍射儀、掃描電子顯微鏡以及能譜儀對(duì)樣品的結(jié)構(gòu)形貌和組成進(jìn)行了分析;通過(guò)光譜儀對(duì)樣品的光譜性能進(jìn)行了分析;利用微弱光度計(jì)對(duì)樣品的余輝性能進(jìn)行了分析;利用熱釋光計(jì)量?jī)x對(duì)樣品的陷阱位置進(jìn)行了分析,其主要內(nèi)容如下:(1)采用高溫固相法合成了的NaYF_4:Pr~(3+)發(fā)光粉。探究了溫度、原料及氟源濃度對(duì)NaYF_4物相的影響,制備出了不同Pr~(3+)濃度摻雜的α相和β相的NaYF_4。分析了α(β)-NaYF_4:xPr~(3+)的XRD圖譜,對(duì)X射線發(fā)射譜、余輝衰減以及熱釋光曲線做了表征。在α-NaYF_4中,Pr~(3+)的最佳摻雜濃度為3%而在β-NaYF_4中最佳摻雜濃度為1%。Pr~(3+)在β-NaYF_4中的發(fā)光及余輝性能都要優(yōu)于α-NaYF_4。最后通過(guò)摻入Mg2+調(diào)節(jié)Pr~(3+)的發(fā)光,摻入Mg2+有利于β-NaYF_4:1%Pr~(3+)的發(fā)光的增強(qiáng)及余輝的延長(zhǎng)。(2)采用水熱法合成了NaYF_4:Pr~(3+)熒光粉。探究了氟源濃度及溶液pH值對(duì)NaYF_4物相及形貌的影響。分析了NaYF_4:Pr~(3+)的XRD、SEM和EDS圖譜,對(duì)X射線發(fā)射譜、余輝衰減以及熱釋光曲線做了表征。高的氟源濃度利于棒狀顆粒的產(chǎn)生,pH值越高,樣品顆粒越小。當(dāng)pH=5且氟釔比為1:8時(shí),NaYF_4:Pr~(3+)的發(fā)射峰及熱釋光峰值最強(qiáng),余輝時(shí)間也取得最大值。(3)通過(guò)熱解法制備了NaYF_4:Pr~(3+)熒光粉。樣品為純相的六角相NaYF_4,顆粒大小為30-40nm。采用水熱法制備了KYF_4:Pr~(3+)熒光粉。分析了KYF_4:Pr~(3+)的XRD、SEM圖譜,對(duì)X射線發(fā)射譜、余輝衰減以及熱釋光曲線做了表征。樣品為純相的KYF_4,顆粒大小為30-40nm。在X射線的激發(fā)下,樣品有有效的發(fā)光和余輝。
[Abstract]:In recent years, new biological imaging techniques can dynamically monitor the activities and responses of labeled cells in vivo, including quantum dots and nanoscale up-conversion materials. However, because of the poor penetration ability of the excitation light source to the tissue, the application can only be used in the surface tissue. Because of its good tissue penetration, it is an ideal light source for biological imaging in vivo, but in view of its harm to the human body, The radiation dose should not be too large, so the long afterglow material excited by X-ray is an ideal biomaterial. In this paper, the aim of this study is to find suitable materials for long time afterglow emission under low-dose X-ray irradiation. Fluorine based fluorescent materials were synthesized by high temperature solid phase method hydrothermal method and pyrolysis method respectively. The structure and composition of the samples were analyzed by X-ray diffractometer scanning electron microscope and energy spectrometer. The spectral properties of the sample were analyzed by spectrometer, the afterglow of the sample was analyzed by weak photometer, and the trap position of the sample was analyzed by thermoluminescence metrology. The main contents are as follows: (1) the NaYF_4:Pr~(3) luminescent powder was synthesized by high temperature solid state method. The effects of temperature, raw material and concentration of fluorine source on the phase of NaYF_4 were investigated. The 偽 phase doped with different Pr~(3 concentration and NaYF _ 4 with 尾 phase were prepared. The XRD spectra of 偽 (尾 -NaYF + 4: xPrH3) are analyzed. The X-ray emission spectra, afterglow decay and thermoluminescence curves are characterized. The optimum doping concentration of 偽 -NaYF4 is 3%, and the optimum doping concentration in 尾 -NaYF4 is 1%.Pr~(3). The luminescence and afterglow properties of 偽 -NaYF4 are better than 偽 -NaYF4. Finally, the luminescence of Pr~(3) was regulated by Mg2. The addition of Mg2 was beneficial to the enhancement of 尾 -NaYF4: 1) and the prolongation of afterglow. (2) NaYF_4:Pr~(3) phosphors were synthesized by hydrothermal method. The effects of fluorine concentration and pH value on the phase and morphology of NaYF_4 were investigated. The X-ray emission spectra, afterglow decay and thermoluminescence curves of NaYF_4:Pr~(3 were characterized. The higher the concentration of fluorine source is, the higher the pH value of the rod-like particles is, and the smaller the sample particles are. The emission peak and thermoluminescence peak of NaYF4: P _ (3) were the strongest when the ratio of pH=5 and fluorine yttrium was 1:8, and the afterglow time was also the maximum. (3) NaYF_4:Pr~(3) phosphors were prepared by pyrolysis. The sample is hexagonal phase NaYF4 with pure phase and particle size of 30-40 nm. KYF_4:Pr~(3) phosphors were prepared by hydrothermal method. The X-ray emission spectra, afterglow decay and thermoluminescence curves of KYF_4:Pr~(3 were characterized. The sample is pure phase KYF _ s _ 4 and the particle size is 30-40 nm. Under the excitation of X-ray, the sample has effective luminescence and afterglow.
【學(xué)位授予單位】：河北大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：O482.3

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