Powder X 使用说明详解

006 18.04 3.712 3.731 3.721 3.725 3.724 3.727 008 25.43 3.762 3.730 3.735 3.731 3.729 0010 32.96 3.712 3.711 3.714

从以上计算可以证明我们的零点漂移计算方法是比较精确的，而且也证明了我们的误 差估计公式的正确性。经过零点校正，我们可以求得该Bi2201单晶的晶格常数：

hkl 004 006 008 0010 0012 0014 0016 0020

2q ( ) 14.46 21.76 29.15 36.68 44.36 52.27 60.45 77.99 d( ) 6.12073 4.08090 3.06090 2.44802 2.04039 1.74870 1.53017 1.22414 c( ) 24.4829 24.4854 24.4872 24.4802 24.4847 24.4818 24.4827 24.4828

从上表可以看出，经过零点漂移校正，尽管实验中衍射角测定范围较小(q<40度),但 晶格参数的相对误差已接近1×10－4。 经过长时间使用，发现我们的零点漂移校正公式非常实用。最近对电化学方法掺氧LaCu O4

+d的超导样品和郑东宁博士从英国带回的(Gd,Pb)Mo6S8样品的衍射数据都是经过零点 漂移校正以后才得出准确的晶格参数。

3.5.3未知晶体结构时零点漂移的校正

一个未知结构的Pr-Li-Ni-O体系的化合物，其衍射数据如下： 2Thetad(A)HeightAreaFWHMLine pair

14.286.19717112.22009.70.20001 17.085.18708429.06041.30.31032 18.524.78688372.010660.00.6195 25.243.5255715109.075974.70.1253 28.643.114297281.034662.70.12191 32.462.7559824664.0138512.00.1394 34.382.6063417423.0116272.00.15572 37.462.398812091.021900.00.2293 43.722.068755809.029656.00.1322 45.242.0027213188.065306.70.1207 49.321.846169258.046973.30.1215 56.121.637513232.019993.30.1484 56.441.628992025.012366.70.1371 57.241.608115062.025429.30.1157 59.061.562821342.07269.30.12411 60.201.535927466.044300.00.1356 67.901.379273203.019152.00.1325 70.061.341942043.010786.70.1243 72.241.306711986.014645.30.17062 77.801.22663642.05049.30.1604 78.781.213813255.020288.00.1393

......

使用原始数据用TREOR90程序未能指标化，经分析推测可能存在严重的零点漂移，使 用d值比例接近1：2：4的17.08 ,34.38 和72.24 的衍射线对，利用零点漂移校正公 式进行计算，得到零点漂移值为0.16 ,然后对衍射数据进行零点漂移校正，所得数据 用TREOR90成功地进行了指标化，得到品质因数M(20)=29,F(20)=19的结果，确定该化 合物为四方晶系，a=5.237,c=12.536，并进而解出了该化合物的晶体结构。

3.6指标化

利用3.5.1中经零点校正后的Si粉的衍射数据，可以编辑指标化输入控制文件如下：

Si粉的衍射数据指标化输入控制文件内容 si6

28.4371000 47.291493 56.107291 69.11559 76.35692 88.004103 94.92264 106.68033 114.05964 127.50844 136.85324

KH=4, KK=4, KL=4, KS=12, THS=0, OS1=0, MONO=0, SHORT=1, MERIT=10, NIX=1, IDIV=1,

WAVE=1.5405981, VOL=1000, CEM=25, D1=0.0002, SSQTL=0.05, CHOICE=3, TRIC=0, END*

利用以上指标化输入控制文件进行指标化得到的指标化结果如下：

VBVERSIONBYCHENGDONGBASEDONTREOR90 si6

28.4370001000 47.291000493 56.107000291 69.11500059 76.35600092 88.004000103 94.92200064 106.68000033 114.05900064 127.50800044 136.85300024

LINENUMBER=7SHOULDNOTBEINCLUDEDINTHETREOR BASELINESETS.SINESQUARETHETAFORTHISLINE=9 TIMESSINESQUARETHETAFORLINENUMBER=1

LINENUMBER=7WILLBESKIPPEDINTHETRIALPHASE. LINENUMBER=8SHOULDNOTBEINCLUDEDINTHETREOR BASELINESETS.SINESQUARETHETAFORTHISLINE=4 TIMESSINESQUARETHETAFORLINENUMBER=2

LINENUMBER=8WILLBESKIPPEDINTHETRIALPHASE. STOPLIMITS

FIGUREOFMERITREQUIRED=10

MAXNUMBEROFUNINDEXEDLINESINFIGUREOFMERITTEST=1 THE7FIRSTLINESADJUSTEDBYTHEIRHIGHERORDERS

CUBIC,TETRAGONAL,HEXAGONALANDORTHOROMBICSYMMETRY MAXCELLEDGE=25.0MAXCELLVOLUME=1000.0

D1=0.000200SSQTL=0.050000D2=0.000400WAVE=1.540598 NUMBEROFLINESWITHSQLESSTHAN0.327NOTEQUALTO9 NUMBEROFTESTLINES=4IQREQUIRED=1

**CUBICTEST*********************MAX.VOLUME=1000 SELECTEDBASELINES(1)(2)

BASELINEONE.(HKL)-MAX444MAXH+K+L=12 THISMAYBETHESOLUTION!!!

THEREFINEMENTOFTHECELLWILLNOWBEREPEATED THREECYCLESMORE.---GOODLUCK! CYCLERESULTS

0.0201100.0000000.0000000.0000000.0000000.000000 0.0201100.0000000.0000000.0000000.0000000.000000 0.0201100.0000000.0000000.0000000.0000000.000000 NUMBEROFSINGLEINDEXEDLINES=11

TOTALNUMBEROFLINES=11

A=5.4319280.000062AALFA=90.0000000.000000DEG. B=5.4319280.000062ABETA=90.0000000.000000DEG. C=5.4319280.000062AGAMMA=90.0000000.000000DEG. UNITCELLVOLUME=160.27

HKLSST-OBSSST-CALCDELTA2TH-OBS2TH-CALCD-OBSFREEPARAM. 1110.0603220.060330-0.00000828.43528.4373.13631000 2200.1608780.160879-0.00000147.29347.2941.9205493 3110.2211780.221209-0.00003156.10756.1111.6379291 4000.3217530.321759-0.00000669.11569.1161.358059 3310.3820560.382089-0.00003376.35676.3601.246292 4220.4825850.482638-0.00005388.00488.0101.1088103 5110.5429000.542968-0.00006994.92294.9301.045464 4400.6435130.643518-0.000005106.680106.6810.960233 5310.7038390.703848-0.000009114.059114.0600.918264 6200.8044360.8043970.000039127.508127.5020.858844 5330.8648010.8647270.000073136.853136.8410.828324 NUMBEROFOBS.LINES=11 NUMBEROFCALC.LINES=11 M(11)=297AV.EPS=0.0000297 F11=56.(0.004050,49)

MCF.J.APPL.CRYST.1(1968)108 FCF.J.APPL.CRYST.12(1979)60 0LINESAREUNINDEXED.

ANYCOMMONFACTORINTHEQUADRATICFORMS?? CHECKCONVERGENCEINTHEREFINEMENT (EV.USEPROGRAMPIRUMORPURUM) endsubOFINDEXINGCALCULATIONS SETKS=0TOCHECKTHESOLUTION..... ANDRUNTREORONCEMORE.

IFYOUWANTTOLOOKFORABETTERSOLUTIONYOU

MAYTRYTOINCREASETHEPARAMETERMERITABOVE297 ....ORPERHAPSTHISWASTHEBESTSOLUTION...

3.7由晶格参数计算衍射位置(dhkl)

以下给出利用PowderX程序中的dhkl功能计算得出的石英从10度到140度之间的衍射位

置和晶面间距(使用铜靶Ka1辐射)：

SampleNameSiO2(Quartz)

Crystalsystem:HexagonalLatticeType:P Radiation:CuWaveLength:1.540598

LatticeParameter:a=4.9133b=4.9133c=5.4053 LatticeParameter:Alpha=90Beta=90Gama=120