本文關(guān)鍵詞： 儀器參數(shù) 數(shù)據(jù)初級處理程序 周期長度 粒子尺寸 簡易加熱爐　出處：《安徽大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：小角X射線散射(SAXS)是測量物質(zhì)內(nèi)部散射單元結(jié)構(gòu)信息的常用方法。本論文就SAXS方法開展了以下五個方面的研究:一.SAXS儀器參數(shù)和樣品散射角度標(biāo)定方法研究。大面積二維探測器已經(jīng)成為許多SAXS儀器的標(biāo)準(zhǔn)配置。當(dāng)SAXS儀器上的探測器和直通光垂直時,散射圖像具有圓對稱性,此時若有一個具有納米尺度的周期性結(jié)構(gòu)的樣品被測試,探測器將會收集到圓的衍射環(huán),圓中心點與直通光中心點重合;當(dāng)探測器傾斜時,散射圖像的圓對稱性就不復(fù)存在,圓的衍射環(huán)就會變成橢圓,橢圓中心點與直通光中心點不重合。樣品散射圖像對應(yīng)的散射角度或散射矢量標(biāo)定依賴于儀器參數(shù)的標(biāo)定,即需要知道樣品至探測器距離、探測器傾斜角度和直通光中心點坐標(biāo)這三個儀器參數(shù)。傳統(tǒng)的儀器參數(shù)標(biāo)定方法大都基于探測器垂直(或近似垂直)于直通光的設(shè)置,極少數(shù)涉及傾斜的情況,還沒有探測器傾斜角度的標(biāo)定方法報道。本研究發(fā)展了用標(biāo)準(zhǔn)樣品衍射環(huán)標(biāo)定探測器處于任意姿態(tài)下(垂直和傾斜)的儀器參數(shù)(探測器傾角或稱偏轉(zhuǎn)角、樣品至探測器距離、探測器上直通光斑中心)和樣品散射角度的方法,模擬建立了相應(yīng)的幾何關(guān)系,具體推導(dǎo)了相應(yīng)的計算公式,編譯了相應(yīng)的計算語句。以北京同步輻射1W2A小角站的實驗為例,用標(biāo)準(zhǔn)樣品SBA-]5標(biāo)定了 SAXS儀器參數(shù),用標(biāo)準(zhǔn)樣品硬脂酸銀驗證了該方法的可靠性。二.SAXS數(shù)據(jù)初級處理程序開發(fā)。SAXS實驗測試后,需對散射圖像進行初級數(shù)據(jù)處理,然后再進行進一步的樣品結(jié)構(gòu)參數(shù)計算。初級處理過程通常包括儀器參數(shù)標(biāo)定、散射角度標(biāo)定、二維圖像轉(zhuǎn)為一維數(shù)據(jù)、背底扣除、消模糊(準(zhǔn)直誤差校正)等幾個步驟。已有不少研究者開發(fā)了不同的數(shù)據(jù)初級處理軟件,但目前沒有一個軟件集成了上述五個功能,分散操作,麻煩費時;而且對于探測器傾斜的情況,還沒有相應(yīng)的軟件能計算探測器傾角進而計算其它儀器參數(shù)。為此,本研究開發(fā)了一款SAXS數(shù)據(jù)初級處理程序,用Matlab語言編寫,將上述五個功能集于一體,適合于探測器垂直或傾斜的任意姿態(tài),提高了數(shù)據(jù)初級處理的準(zhǔn)確性和自動化程度,且可實現(xiàn)批處理。三.周期性結(jié)構(gòu)樣品的周期長度d值測量。隨著科學(xué)的發(fā)展,越來越多的納米d值的材料被制備,當(dāng)d值為若干納米尺度時,對應(yīng)的衍射角則落在了小角散射的范圍。精確測定d值,對于認(rèn)識這類材料的結(jié)構(gòu),實現(xiàn)其結(jié)構(gòu)可控具有重要意義,因此成為了 SAXS的應(yīng)用方向之一。測量d值需要知道樣品至探測器的距離,但是探測內(nèi)部感光面的具體位置通常是不知道的,手工米尺測量距離的方法太過粗糙。本研究采用移動樣品或探測器的方法進行實驗,通過采集衍射環(huán)來計算d值,避免直接測量樣品至探測器距離來進行d值的計算,以期提高d值測量精度。詳細(xì)分析了移動樣品和移動探測器這兩種方法的區(qū)別,推導(dǎo)了相應(yīng)的計算公式,討論了探測器傾斜的影響,模擬分析了誤差變化規(guī)律,并用標(biāo)準(zhǔn)樣品進行了驗證。四.應(yīng)用SAXS測量溶液中粒子尺寸的一種新方法。SAXS是測量溶液中粒子尺寸的常用手段。實際測量中出于對散射強度的要求,溶液濃度不能太低,因此干涉效應(yīng)不可避免。傳統(tǒng)的處理干涉效應(yīng)的方法是制備并測量不同濃度的溶液,然后對散射曲線進行外推。傳統(tǒng)的方法不僅制備操作麻煩,而且外推散射曲線人為性較大。為此,本研究提出一種溶液中粒子尺寸測量的新方法。直接對任意濃度球形(或近似球形)粒子溶液的實測SAXS曲線進行變換,通過尋找峰位的方法來計算相應(yīng)于干涉效應(yīng)可忽略的無限稀釋溶液中粒子的尺寸。與傳統(tǒng)方法不同,該方法僅需要測量任意一種濃度的溶液,不需要知道溶液濃度,且不需要對實驗曲線進行外推延長。并對該方法進行了模擬和實驗驗證。五.一款SAXS原位測量專用簡易樣品加熱爐研制。原位加熱實驗是同步輻射SAXS領(lǐng)域的近年來研究熱點。本研究設(shè)計開發(fā)了一款SAXS原位測量專用簡易樣品加熱爐,它主要由溫控器、樣品池、固定架組成,采用擠壓密封的辦法,具備構(gòu)造簡略、操作容易的特點。采用該裝置分別進行了石墨烯溶液加熱和褐煤粉末加熱干燥的SAXS原位測試,實驗結(jié)果驗證了該加熱爐的實用性。
[Abstract]:Small angle X ray scattering (SAXS) is a common method for measuring material internal scattering unit structure information. This paper studies the following five aspects: the development of the SAXS method for calibration of a.SAXS instrument parameter and sample scattering angle. A large area of two-dimensional detector has become the standard configuration of many SAXS instruments. When the SAXS instrument. The detector and the straight vertical light, scattering image with circular symmetry, if has a nano scale periodic structure of the tested samples, the detector will collect diffraction ring round and round the center point and point light in the heart through coincidence; when the detector is tilted circular symmetry scattering image is not exist, will become an ellipse diffraction ring circle, ellipse center and straight optical center point do not coincide. The scattering angle of the corresponding scattering image of the sample or the scattering vector depends on the parameters of the calibration instrument calibration, which is required To know the sample to detector distance, tilt angle and light detector through the center coordinates of the three parameters of the instrument. The instrument parameters of traditional calibration methods are mostly based on the vertical detector (or near vertical) in the direct light settings for a few inclined, there were no reports of detector tilt angle calibration method was developed in this study. In any attitude detector calibration standard sample for diffraction ring (vertical and inclined) instrument parameters (detector angle or angle, sample to detector distance, the detector through the spot center) method and sample scattering angle, established the corresponding simulation geometry, deduced the corresponding calculation formula, compiled calculation statement corresponding. Using Beijing synchrotron radiation 1W2A small angle station experiment as an example, using the standard sample of SBA-]5 calibration of the SAXS instrument parameters, using standard sample silver stearate test The reliability of the method. The primary test program development two.SAXS.SAXS experimental data, the primary scattering image data processing, then the sample structure parameters for further calculations. The primary process includes instrument calibration, scattering angle calibration, two-dimensional image to one-dimensional data, background subtraction, deblurring (collimation error correction) of several steps. Many researchers have developed different primary data processing software, but does not currently have a software integration of the above five functions, decentralized operation, time-consuming and trouble; for the detector tilt, but also does not have the corresponding calculation software can calculate other parameters of angle detector instrument for., this study developed a SAXS primary data processing program, using Matlab language, the above five functions, suitable for vertical or inclined probe The arbitrary attitude, improve the degree of automation and accuracy of data processing and can achieve the primary, batch processing. Three. The cycle length of the periodic structure of D value of the sample measurement. With the development of science, more and more D nano materials were prepared, when the D value is some nano scale, the corresponding diffraction angle it falls on the range of small angle scattering. The accurate determination of D value, the cognitive structure of this type of materials, it is of great significance to achieve the controllable structure, which has become one of the application direction of SAXS. D measurements need to know the sample to detector distance, but the specific position detection of internal photosensitive surface is usually not known. A manual method of measuring distance is too rough. The method of moving the sample or detector experiments, through the acquisition of diffraction rings to calculate the D value, avoid the direct measurement of the sample to detector distance to D value meter Count, in order to improve the D value measurement accuracy. A detailed analysis of the differences between mobile and mobile detector samples of the two methods, and the corresponding calculating formulas are derived, the influence of detector tilt discussion, simulation analysis of the variation of the error, and verified by standard samples. Four. Using a new method of particle measurement solution SAXS size.SAXS is a commonly used method for measuring particles in solution. The size of the actual measurement based on scattering intensity, the concentration is too low, so the interference effect is inevitable. The traditional method of processing of the interference effect is the preparation and measurement of different concentration solution, and then extrapolating the scattering curves of the traditional method. Not only the preparation of complicated operation, and artificial scattering curve extrapolation is larger. Therefore, this study proposes a new solution method in the measurement of particle size. The spherical directly to any concentration (or nearly spherical ) measured SAXS particle solution of transformation, by looking for the method to calculate the peak particle solution corresponding to infinite dilution interference effect can be neglected in size. Unlike the traditional method, this method only needs the measurement of arbitrary a solution concentration, do not need to know the concentration of the solution, and does not need to extrapolate the experimental curve extended. And the method is simulated and verified by the experiments. The research and development of 5 SAXS in situ measurement special simple heating furnace. In situ heating experiment is the synchrotron radiation field of SAXS research in recent years. The research design and development of a simple SAXS in situ measurement special heating furnace, which is mainly composed of the thermostat, the sample pool, a fixed frame, the extrusion sealing method has simple structure, easy to operate features. Using this device were Shi Moxi solution heating and heating dry lignite powder SAXS In situ test, the experimental results verify the practicability of the reheating furnace.

【學(xué)位授予單位】：安徽大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O434.1

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