取向因子实验报告

X射线测取向因子一、实验目的1、了解和掌握聚合物长丝取向因子的测试；2、掌握X射线测定取向因子的原理和方法；3、熟悉X射线衍射仪。二、实验原理聚合物材料在挤出、注射、压延、吹塑等加工成型过程中，大分子链或链段、微晶必然要表现出不同程度的取向。聚合物取向时在以共价键相连的分子链方向上，单位截面化学键数目明显增加，拉伸强度大大加强；在垂直分子链方向上丁主要由分子链间较弱的范德华力作用，强度可能降低，从而使材料具有各向异性：对材料的物理性质以及使用均有相当大影响。研究聚合物取向度及其过程是很有实际意义的，本文着重阐述用X射线衍射方法测定结晶聚合物材料的取向。取向是指样品在拉伸、压延等作用下分子链产生重排钓现象。在取向态下，结晶聚合物材料择优取向，可分为单轴取向和双轴取向。对于择优取向的表征，一是要确定取向单元，二是要选定参考方向。纤维状单轴取向聚合物，取向单元可取聚合物结晶主轴（分子链轴）或某个晶面法向；参考方向取外力作用方向或称纤维轴方向。双轴取向单元可取一个晶面;参考方向也可取晶体的某个品轴或晶面。结晶聚合物包含有晶区与非晶区，所以取向分为晶区取向、非晶区取向和全取向。研究聚合物取向度的通常方法是X射线衍射法和双折射法，前者可测量微晶晶区的分子链取向，后者可测量整个分子链或链段的取向。非晶区分子链的取向，可由两种方法测定的结果换算得到。整个材料的取向分布函数可以通过X射线衍射极图法得到，此法比较复杂，故不常用。一般采用Hermans提出的取向因子描述晶区分子链轴方向相对于参考方向的取向情况。取向因子大小反映择优取向单元对参考方向平行排列的程度。定义取向因子f为：1f=—（3〈cos2申〉—1）（1）2<Hermans取向模型仅给出了纤维轴与分子链轴间的取向关系。stein进一步发展了Hermans的理论，给出正交晶系晶体三个晶轴与纤维轴间的取向关系。设a、b、c是聚合物微晶的三个晶轴，与OZ轴（拉伸方向）的夹角分别为屮屮屮,则晶轴abc与拉伸方向间的取向关系是：1f-歼（3〈cos2q〉一1）TOC\o"1-5"\h\za2a1f—（3〈cos2q〉—1）⑵b2b1f-片（3〈cos2q〉一1）c2c对于正交晶系｛cos2Q〉+〈COS2Q〉+〈COS2q〉=1abcf+/+f二1abc对于聚丙烯纤维而言，属于正交晶系，只要测定两个面，根据式（2）即可测定出三个面的取向因子。三、实验步骤（一）制样制样要求：纤维在样品架上必须密实、均匀的排列，并且要完全与孔隙相垂直。（二）测试（一一）样品测定：1）开机前的准备和检查将制备好的试样插入衍射仪样品架，盖上顶盖关闭防护罩；开启水龙头，使冷却水流通；X光管窗口应关闭，管电流管电压表指示应在最小位置；接通总电源，接通稳压电源。2）开机操作开启衍射仪总电源，启动循环水泵；待准备灯亮后，接通x光管电源。缓慢升高管电压、管电流至需要值（若为新X光管或停机再用，需预先在低管电压、管电流下〃老化〃后再用）。打开计算机X射线衍射仪应用软件，设置合适的衍射条件及参数，使计数管在设定条件下扫描。3）停机操作测量完毕，缓慢顺序降低管电流、管电压至最小值，关闭X光管电源；取出试样；15分钟后关闭循环水泵，关闭水龙头；关闭衍射仪总电源、稳压电源及

线路总电源。四、实验结果及处理下表是实验结果及处理过程，由此表可得到:I]*Sin©*Cos2①的和为56969.186I/Sin①的和为258526.4I2*SinQ*Cos2Q的和为30318.49I2*Sin①的和为180858.6*Sin①=0.167636因此：（Cos2①）=YI]*Sin©*Cos2①/»]*Sin*Sin①=0.167636（Cos2①b）=»2*Sin3Cos2①/f故：（Cos2①）=1-（Cos2①）-（Cos2①）=0.612002cab进而：f=0.5（3（Cos2①）-1）=0.418004cc弧度IaIbSineCos2e分子1分母1分子2分母200222768301000010.01722747220.017139.67439.68612.59612.620.03523647020.0350.99982.482.524.46924.49930.05224136960.0520.997125.937126.28336.32536.42540.0724197220.070.995167.915168.73650.11850.36350.08725317290.0870.992218.909220.58563.05263.53560.10525067160.1050.989259.079261.94174.02374.8470.12225256890.1220.985303.141307.71182.71983.96680.1425007390.1390.981341.184347.923100.854102.846901560.976394.018403.902109.721112.4731001740.97439.038452.688112.159115.646110.19225447020.1910.964467.732485.404129.068133.944120.20926207840.2080.957521.168544.713155.952162.998130.22725827160.2250.949551.418580.807152.911161.06140.24426857630.2420.941611.529649.542173.779184.581

150.26224757160.2590.933597.652640.559172.896185.309160.27924447670.2760.924622.461673.638195.347211.408170.29723347460.2920.915624.049682.376199.46218.103180.31422277160.3090.905622.451688.161200.124221.25190.33222157290.3260.894644.683721.113212.178237.332200.34920877390.3420.883630.285713.776223.182252.746210.36720487190.3580.872639.667733.917224.571257.659220.38418337190.3750.86590.285686.635231.541269.335230.40118067530.3910.847597.916705.641249.297294.212240.41916817090.4070.835570.603683.705240.665288.368250.43615957190.4230.821553.673674.058249.587303.854260.45414827910.4380.808524.813649.648280.113346.742270.47114167630.4540.794510.348642.833274.997346.385280.48913787980.4690.78504.34646.914292.063374.628290.50612567670.4850.765465.795608.904284.447371.839300.52411957740.50.75448.121597.484290.247386.99310.54111907670.5150.735450.313612.879290.244395.024320.55811397740.530.719434.082603.562294.978410.147330.57610048020.5450.703384.613546.803307.23436.789340.5939777670.5590.687375.495546.317294.784428.89350.61110127950.5740.671389.494580.444305.976455.982360.6289387320.5880.655360.859551.329281.608430.248370.6469267980.6020.638355.445557.267306.312480.236380.6638817770.6160.621336.81542.384297.05478.357390.6819088050.6290.604345.117571.409305.968506.59400.6988937600.6430.587336.846573.995286.677488.507410.7169047530.6560.57337.813593.063281.386494420.7338707670.6690.552321.502582.13283.439513.211430.758488020.6820.535309.344578.321292.564546.95

440.7688127530.6950.517291.88564.049270.672523.065450.7858236790.7070.5290.981581.935240.068480.114460.8038596890.7190.483298.182617.899239.17495.614470.828487320.7310.465288.471620.174249.011535.339480.8388637390.7430.448287.158641.32245.897549.172490.8558487530.7550.43275.472639.98244.611568.284500.8738097220.7660.413256.068619.717228.53553.072510.898377630.7770.396257.627650.457234.85592.95520.9088747490.7880.379261.065688.707223.727590.208530.9258747220.7990.362252.818697.993208.85576.603540.9428457390.8090.346236.198683.606206.568597.851550.969196890.8190.329247.679752.786185.692564.385560.9779307090.8290.313241.107770.99183.811587.776570.9959047290.8390.297224.91758.144181.371611.379581.0129617530.8480.281228.874814.959179.336638.568591.0310047600.8570.265228.304860.58172.82651.435601.04710818020.8660.25234.064936.157173.654694.54611.06511607600.8750.235238.4851014.541156.249664.699621.08212657770.8830.22246.21116.91151.224686.039631.112878370.8910.206236.3751146.706153.726745.76641.11714928890.8990.192257.731340.979153.567799.0156519060.179248.6671392.067139.714782.1316619140.165254.0881535.647143.444866.942671.169182210080.920.153256.0911677.135141.679927.855681.187201910970.9270.14262.7381871.958142.7551017.106691.204232211220.9340.128278.452167.744134.5481047.463701.222250613690.940.117275.5182354.839150.5131286.422711.239276914630.9460.106277.5642618.108146.6511383.276721.257292316100.9510.096265.5182779.905146.2481531.183

731.274308018490.9560.086251.8372945.385151.1841768.187741.292354020530.9610.076258.6023402.829149.9741973.449751.309375224500.9660.067242.843624.116158.5712366.494761.326406426460.970.059230.8553943.243150.3062567.377771.344430730110.9740.051212.4324196.573148.512933.801781.361467533210.9780.043197.7444572.801140.4733248.4791.379481337590.9820.036172.0834724.534134.3993689.907801.396528342330.9850.03156.9545202.702125.7594168.661811.414544844470.9880.024131.7495380.891107.5424392.221821.431572948830.990.019109.9515673.21293.7154835.45831.449590051840.9930.01587.0355855.99276.4725145.332841.466600654300.9950.01165.3175973.07159.0535400.229851.483610457290.9960.00846.2366080.74943.3965707.178861.501613356250.9980.00529.8086118.04127.3395611.28871.518629057570.9990.00317.2346281.36515.7745749.097881.536605556060.9990.0017.3896051.3026.8425602.576891.55360845430101.8636083.0691.6625429.169901.57158915283100589105283911.58858914961101.7845890.1081.5034960.248921.606554146410.9990.0016.7265537.6345.6344638.18931.623528342900.9990.00314.4245275.77311.7134284.131941.641492638980.9980.00523.8784914.01718.8953888.518951.658471834810.9960.00835.6624700.06726.3123467.769961.675434830040.9950.01147.2034324.20432.6122987.559971.693400827430.9930.01559.0363978.14940.4032722.571981.71390623400.990.01974.8663868.01444.8512317.244991.728340021280.9880.02482.1273358.16751.4022101.8181001.745319219090.9850.0394.7343143.53556.6561880.0151011.763293016860.9820.036104.6612876.19760.2251655.04

1.78262714580.9780.043111.0232569.62261.6181426.1551.798247513050.9740.051121.9782411.59564.3161271.5681.815223311770.970.059126.7542166.69966.8111142.0531.833203110680.9660.067131.3641961.82469.0781031.6241.85186510240.9610.076136.1561792.78174.758984.3471.86717699380.9560.085144.5591691.73276.651897.0291.88515268890.9510.095138.5431451.33880.711845.5051.90215028890.9460.106150.4841420.19689.068840.5821.9213327810.940.117146.3751251.69685.825733.9151.93712168270.9340.128145.7551135.25999.128772.0881.95511017770.9270.14143.2161020.853101.07720.4391.97210447530.9210.153146.681961.031105.796693.1571.9910127430.9140.165152.909924.532112.264678.7822.00710087060.9060.179163.13913.583114.256639.8712.0259347740.8990.192161.286839.498133.657695.6872.0428487120.8910.206155.697755.597130.727634.4162.0598307530.8830.22161.49732.87146.509664.8812.0778417160.8750.235172.853735.58147.161626.2492.0948057430.8660.25174.257697.175160.836643.482.1128027290.8570.265182.324687.474165.729624.8982.1298527630.8480.281202.866722.565181.675647.0862.1478706960.8390.297216.402729.673173.122583.7392.1648096830.8290.313209.692670.72177.033566.2572.1828027290.8190.329216.103656.99196.433597.1892.1998097320.8090.345226.093654.526204.573592.2282.2178056960.7990.362232.818642.933201.294555.8782.2347817630.7880.379233.247615.468227.871601.2832.2518377670.7770.396257.587650.506236.044596.1032.2698707630.7660.413275.336666.496241.473584.525102103104105106107108109110111112113114115116117118119120121122123124125126127128129130

2.2868377490.7550.43271.862631.729243.28565.3112.3048097670.7430.448269.156601.241255.183570.0272.3218377360.7310.465284.697612.182250.343538.3112.3398487460.7190.482294.333610.041258.93536.6632.3568567600.7070.5302.621605.325268.682537.4382.3748597290.6950.517308.749596.755262.023506.4432.3919237490.6820.535336.679629.532273.209510.8552.4089347490.6690.552345.131625.017276.77501.2182.4269427120.6560.57351.994618.058266.051467.1522.44310407360.6430.587392.278668.557277.612473.1322.46110327810.6290.604392.233649.517296.836491.5432.47810777090.6160.621411.73663.129271.046436.5452.49611567810.6020.638443.723695.766299.782470.0632.51311997530.5880.654461.265704.826289.685442.6472.53112657220.5740.671486.869725.652277.881414.1662.54813886830.5590.687533.462776.246262.504381.9712.56614397530.5450.703551.265783.827288.466410.1612.58315507260.530.719590.737821.475276.693384.7682.616917320.5150.735639.926871.041277.011377.0562.61818017320.50.75675.405900.62274.512366.0492.63518067630.4850.765669.809875.689282.981369.9622.65319916730.470.78728.749934.855246.333316.0012.6720997490.4540.794756.577953.073269.974340.0912.68820877260.4380.808739.132915.029257.12318.3092.70522507220.4230.821781.132951.054250.656305.1832.72323347260.4070.835792.359949.495246.466295.3442.7423527020.3910.847778.79919.175232.445274.3452.75823897120.3750.86769.453895.115229.322266.7742.77524756860.3580.872773.167887.15214.3245.893131132133134135136137138139140141142143144145146147148149150151152153154155156157158159

2.79224817120.3420.883749.415848.744215.068243.5732.8125197090.3260.8947