凝膠體系中有機(jī)分子和沸石分子篩的晶體生長(zhǎng)與結(jié)構(gòu)研究.pdf

1、摘要與傳統(tǒng)的材料制備方法相比，溶膠凝膠法具有許多獨(dú)特的性質(zhì)，如可以使原料變得高度均勻，并可在較低的溫度下完成整個(gè)制備過(guò)程。因此，墮鑒：塑壁技術(shù)已被廣泛應(yīng)用于制備各種類型和形狀的材料。本文用溶膠一凝膠法，分別在采而的溶膠一凝膠體系中制備了激光染料羅丹明旦凼墮＆皇昌、ac平面擇優(yōu)生長(zhǎng)的ZSM一5晶體和纖維狀磷酸鋁晶體。品a^搴圳參／(1)羅丹明B內(nèi)酯的單晶生長(zhǎng)及結(jié)構(gòu)測(cè)定f、在硅酸凝膠中，羅丹明B從兩性離子形態(tài)(zwitterion)轉(zhuǎn)變成內(nèi)

2、酯形態(tài)(1actone，以下簡(jiǎn)稱為RBL)，并以此凝膠為介質(zhì)，生長(zhǎng)出了尺寸大于lmm的RBL的單晶。同時(shí)考察了合成條件對(duì)單晶生長(zhǎng)的影響，發(fā)現(xiàn)凝膠是生長(zhǎng)RBL完美單晶的良好的介質(zhì)：甘油的加入改變體系的粘度，使得到的晶體更趨于完美。分別在293K和120K下解析出了RBL的晶體結(jié)構(gòu)。RBL晶體屬單斜晶系，在293K時(shí)的晶胞參數(shù)為：a=16559A，b=15657A，C=19381A，p=loo10。z=8。晶胞中每個(gè)不對(duì)稱單元含有兩個(gè)獨(dú)立的

3、RBL分子(分子1和2)，這兩個(gè)分子的主平面在293K和120K下分別相交成423。和416。。常溫下分子2的一個(gè)乙基處于無(wú)序狀態(tài)(disordered，溫度因子較高)，在120K下成功地定出了這個(gè)乙基的兩種取向，出現(xiàn)的幾率分別為71％和29％。(2)復(fù)合模板劑導(dǎo)向ZSM一5晶體沿dc平面的擇優(yōu)生長(zhǎng)在摩爾組成為10Si020050H?！甔Rl(1一x)R204NaF‘40H20(0乙胺正丁胺，即選用正丙胺作為Rl，樣品的擇優(yōu)取向程度最高

4、。從樣品的SEM照片可以看出，AbstractMaterialswithvariousshapes，suchasfilms，fibers，monoliths，powders，composites，andporousmedia，CanbedirectlyderivedfromthegelstateThemostsuccessfulapplicationsarethosethatutilizethepotentialadvantagesof

5、sol。gelprocessingsuchaspurityhomogeneityandcontrolledporositycombinedwiththeabilitytOformshapedobjectsatlowtemperaturesInthispapersinglecrystalgrowthofthelactoneformofrhodamineB，preferentialgrowthofZSM一5crystals，andthepr

6、eparationoffibrousaluminophosphatesynthesizedfromdifferentgelreactantaredescribedInsilicagel，thesinglecrystalsofthelactoneformofrhodamineB(RBL)weregrownonthenucleusderivedfromthezwitterionformTheeffectsofthesynthesiscond

7、itionsoncrystalgrowthwerefullyinvestigatedItwasfoundthatsilicagelwastheabsolutelyessentialmediumforthecrystalgrowthofRBLMoreovertheviscosityofthemediumincreasedgraduallywithincreasingthecontentofglyceroladdedintothereact

8、ant，leadingtothegrowthoftheperfectsinglecrystalsuptomillimetersizesThefirstdetailedcrystalstructuredeterminationofRBLat293KispresentedaswellRBLcrystallizesinamonoclinicsystem，spacegroupP2I／nwitha=16559A，b=15657A，C=19381A

9、，∥=10010。，Z=8AnasymmetricunitconsistsoftwoindependentlactonemoleculesThemajorcentralplanesofthesetwomoleculesareinclinedtOeachotheratallangleof423。Asynchrotron—radiationstudyofRBLsinglecrystalat120Kshowsthatmolecule2hasa

10、statisticallydisorderedethylgroupwitll71％inoneorientationand29％inasecondorientationZSM5Canbesynthesizedfromthesolgelsystemwithmolarcompositionof10Si02‘O05OH一‘XR1’(1一x)R2‘04NaF‘40H20(Oxs1)，whereR1=EtNH2，n—PrNH2Orn—BuNH2，R