由石英晶體的XRD圖課件

由石英晶體的XRD圖解析出該晶體的結(jié)構(gòu)唐家業(yè)SA08014019由石英晶體的XRD圖唐家業(yè)主要內(nèi)容IndexingPawleyfittingStructuresolutionRietveldrefinement主要內(nèi)容Indexing

INDEXING導(dǎo)入實(shí)驗(yàn)數(shù)據(jù)File/Import/Examples/Reflex/ExperimentalData/Bruker/Quartz.raw文件。如下圖所示：INDEXING導(dǎo)入實(shí)驗(yàn)數(shù)據(jù)File/Import

INDEXING將導(dǎo)入的石英衍射譜，去背底，平滑，剝離Ka2產(chǎn)生的衍射峰。具體操作如下：INDEXING將導(dǎo)入的石英衍射譜，去背底，平滑，剝離

INDEXINGINDEXING

INDEXING

Quartz(BackgroundRemoved)(Smoothed)(Stripped)圖如下：INDEXINGQuartz(Ba

INDEXING打開ReflexPowderIndexing對(duì)話框，利用粉末衍射譜中的峰位確定晶系和估計(jì)晶格常數(shù)。操作步驟如下：INDEXING打開ReflexPowder

INDEXINGINDEXING

INDEXING得到的晶胞如下：INDEXING得到的晶胞如下：Pawleyfitting打開PowderRefinement對(duì)話框。選擇Setup條目并點(diǎn)擊Convergencequality右側(cè)的More...按鈕，打開RefinementConvergence

Options窗口。將Numberofcycles值從2改為5，點(diǎn)擊OK。

Convergencequality選項(xiàng)提供了一種快捷的，單擊選擇所有參數(shù)設(shè)置的方法，它控制著模擬的速度和精確度。Pawleyfitting打開PowderRPawleyfitting

U,V,W,NA,NB和ZeroPointLineShift。將AsymmetryCorrection從None改成-Baldinozzi，允許P1,P2,P3和P4參數(shù)的精修。20個(gè)背底系數(shù)的精修在默認(rèn)狀態(tài)下都處于打開狀態(tài)。PawleyfittingU,V,W,Pawleyfitting調(diào)節(jié)好相應(yīng)的參數(shù)后，點(diǎn)擊Refine.Pawleyfitting調(diào)節(jié)好相應(yīng)的參數(shù)后，點(diǎn)擊RefiPawleyfittingPawleyfittingPawleyfitting初步得到結(jié)果Rwp=2.90%，在誤差范圍內(nèi)。Pawleyfitting初步得到結(jié)果Rwp=2.90%，Pawleyfitting將得到的結(jié)果尋找空間群為P4/NBMPawleyfitting將得到的結(jié)果尋找空間群為P4/NPawleyfitting對(duì)得到的結(jié)果再次精修，得到結(jié)果Rwp=2.83%，誤差減小。Pawleyfitting對(duì)得到的結(jié)果再次精修，得到結(jié)果RStructureSolution嘗試往晶胞中添加原子。步驟：BuildCrystalsRebuildCrystal

OptionstabIgnorespecialpositionsRebuildStructureSolution嘗試往晶胞中添加原子。步StructureSolution添加原子：畫出Si原子，拷貝后黏貼到empty_cell_P6.xsd一次，同時(shí)畫出O原子，拷貝后黏貼到empty_cell_P6.xsd兩次StructureSolution添加原子StructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionRietveldrefinement把所創(chuàng)建的group都刪除(點(diǎn)選橢球后刪除)，重建晶體。Rietveldrefinement把所創(chuàng)建的group都RietveldrefinementRietveldrefinementRietveldrefinementRwp=57.26%RietveldrefinementRwp=57.26%RietveldrefinementRietveldrefinementStructureSolutionRwp=54.22%StructureSolutionRwp=54.22%RietveldrefinementRietveldrefinementRietveldrefinementRwp=53.57%RietveldrefinementRwp=53.57%RietveldrefinementRietveldrefinement不斷精修，可使Rwp變小，最終結(jié)果為：Rietveldrefinement不斷精修，可使Rwp變小，最終結(jié)果為：RietveldreStructureSolutionSi的位置O的位置StructureSolutionSi的位置O的位置由石英晶體的XRD圖解析出該晶體的結(jié)構(gòu)唐家業(yè)SA08014019由石英晶體的XRD圖唐家業(yè)主要內(nèi)容IndexingPawleyfittingStructuresolutionRietveldrefinement主要內(nèi)容Indexing

INDEXING導(dǎo)入實(shí)驗(yàn)數(shù)據(jù)File/Import/Examples/Reflex/ExperimentalData/Bruker/Quartz.raw文件。如下圖所示：INDEXING導(dǎo)入實(shí)驗(yàn)數(shù)據(jù)File/Import

INDEXING將導(dǎo)入的石英衍射譜，去背底，平滑，剝離Ka2產(chǎn)生的衍射峰。具體操作如下：INDEXING將導(dǎo)入的石英衍射譜，去背底，平滑，剝離

INDEXINGINDEXING

INDEXING

Quartz(BackgroundRemoved)(Smoothed)(Stripped)圖如下：INDEXINGQuartz(Ba

INDEXING打開ReflexPowderIndexing對(duì)話框，利用粉末衍射譜中的峰位確定晶系和估計(jì)晶格常數(shù)。操作步驟如下：INDEXING打開ReflexPowder

INDEXINGINDEXING

INDEXING得到的晶胞如下：INDEXING得到的晶胞如下：Pawleyfitting打開PowderRefinement對(duì)話框。選擇Setup條目并點(diǎn)擊Convergencequality右側(cè)的More...按鈕，打開RefinementConvergence

Options窗口。將Numberofcycles值從2改為5，點(diǎn)擊OK。

Convergencequality選項(xiàng)提供了一種快捷的，單擊選擇所有參數(shù)設(shè)置的方法，它控制著模擬的速度和精確度。Pawleyfitting打開PowderRPawleyfitting

U,V,W,NA,NB和ZeroPointLineShift。將AsymmetryCorrection從None改成-Baldinozzi，允許P1,P2,P3和P4參數(shù)的精修。20個(gè)背底系數(shù)的精修在默認(rèn)狀態(tài)下都處于打開狀態(tài)。PawleyfittingU,V,W,Pawleyfitting調(diào)節(jié)好相應(yīng)的參數(shù)后，點(diǎn)擊Refine.Pawleyfitting調(diào)節(jié)好相應(yīng)的參數(shù)后，點(diǎn)擊RefiPawleyfittingPawleyfittingPawleyfitting初步得到結(jié)果Rwp=2.90%，在誤差范圍內(nèi)。Pawleyfitting初步得到結(jié)果Rwp=2.90%，Pawleyfitting將得到的結(jié)果尋找空間群為P4/NBMPawleyfitting將得到的結(jié)果尋找空間群為P4/NPawleyfitting對(duì)得到的結(jié)果再次精修，得到結(jié)果Rwp=2.83%，誤差減小。Pawleyfitting對(duì)得到的結(jié)果再次精修，得到結(jié)果RStructureSolution嘗試往晶胞中添加原子。步驟：BuildCrystalsRebuildCrystal

OptionstabIgnorespecialpositionsRebuildStructureSolution嘗試往晶胞中添加原子。步StructureSolution添加原子：畫出Si原子，拷貝后黏貼到empty_cell_P6.xsd一次，同時(shí)畫出O原子，拷貝后黏貼到empty_cell_P6.xsd兩次StructureSolution添加原子StructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionStructureSolutionRietveldrefinement把所創(chuàng)建的group都刪除(點(diǎn)選橢球后刪除)，重建晶體。Rietveldrefinement把所創(chuàng)建的group都RietveldrefinementRietveldrefinementRietveldrefinementRwp=57.26%RietveldrefinementRwp=57.26%RietveldrefinementRietveldrefinementStructureSolutionRwp=54.22%StructureSolutionRwp=54.22%RietveldrefinementRietveld