【纳米二硫化钼制备方法分析8500字】

纳米二硫化钼制备方法分析目录TOC\o"1-3"\h\u32321纳米二硫化钼制备方法分析 160801.1“自下而上”合成法 1302601.2“自上而下”剥离法 5113761.3模板法制备纳米二硫化钼 7二硫化钼类似于石墨的层状结构使其可以被剥离成单层或少层数的类石墨烯纳米片，层内的强化学键保证了纳米片的稳定性。与体相材料相比，纳米尺寸的MoS2显示出一些独特的物理、化学和电子学特性，如增大的比表面积、极高的荧光量子效率、增强的荷电迁移率、增大的能带带隙等ADDINEN.CITE<EndNote><Cite><Author>Di</Author><Year>2017</Year><RecNum>26</RecNum><DisplayText><stylefont="微软雅黑">（</style>Dietal.,2017<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>26</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615179054">26</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>JunDi</author><author>JiexiangXia</author><author>HuamingLi</author><author>ZhengLiu</author></authors></contributors><titles><title>Freestandingatomically-thintwo-dimensionalmaterialsbeyondgraphenemeetingphotocatalysis:Opportunitiesandchallenges</title><secondary-title>NanoEnergy</secondary-title></titles><periodical><full-title>NanoEnergy</full-title></periodical><pages>79-91</pages><volume>35</volume><dates><year>2017</year></dates><urls></urls></record></Cite></EndNote>（Dietal.,2017）。目前，单层或少层纳米结构已经成为层状材料发展的主要方向之一，如何快速、高效、简便、低耗地制备大面积、结构完善、具有单原子层厚度的二维纳米片结构，也是目前研究的热点与前沿。目前典型的纳米MoS2制备方法可以归为两大类：“自下而上”合成法和“自上而下”剥离法ADDINEN.CITEADDINEN.CITE.DATA（Wangetal.,2017）（图1.3）。图1.3纳米MoS2制备方法示意图ADDINEN.CITEADDINEN.CITE.DATA（Wangetal.,2017）Fig1.3SchematicillustrationofthepreparationmethodsofMoS2ADDINEN.CITEADDINEN.CITE.DATA(Wangetal.,2017)1.1“自下而上”合成法1.1.1水热/溶剂热法水热/溶剂热法是指在密闭反应器中将溶液加热到一定温度，从而在反应体系中产生高压环境，进行无机合成与材料制备的一种方法。水热反应过程以水作为反应介质，高温下在密闭容器中达到饱和蒸气压，形成一定的压力。反应过程产生的压力不仅取决于反应温度，还受到反应物量和浓度等因素影响。通过控制这一系列条件可以控制反应的进行，进而控制产物的形貌、大小和性能。目前已经能通过溶剂热法合成多种形貌的MoS2ADDINEN.CITE<EndNote><Cite><Author>Ye</Author><Year>2007</Year><RecNum>27</RecNum><DisplayText><stylefont="微软雅黑">（</style>Yeetal.,2007<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>27</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615179282">27</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>LinaYe</author><author>WenGuo</author><author>YeYang</author><author>YongfangDu</author><author>YiXie</author></authors></contributors><titles><title>DirectingthearchitectureofvariousMoS2hierarchicalhollowcagesthroughthecontrollablesynthesisofsurfactant/molybdatecompositeprecursors</title><secondary-title>ChemistryofMaterials</secondary-title></titles><periodical><full-title>ChemistryofMaterials</full-title></periodical><pages>6331-6337</pages><volume>19</volume><number>25</number><dates><year>2007</year></dates><urls></urls></record></Cite></EndNote>（Yeetal.,2007）。Sen等ADDINEN.CITE<EndNote><Cite><Author>Sen</Author><Year>2013</Year><RecNum>28</RecNum><DisplayText><stylefont="微软雅黑">（</style>Senetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>28</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615179295">28</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Sen,U.K.</author><author>Mitra,S.</author></authors></contributors><auth-address>ElectrochemicalEnergyLaboratory,DepartmentofEnergyScienceandEngineering,IndianInstituteofTechnology,Bombay,Mumbai-400076,India.</auth-address><titles><title>High-rateandhigh-energy-densitylithium-ionbatteryanodecontaining2DMoS2nanowallandcellulosebinder</title><secondary-title>ACSAppliedMaterials&Interfaces</secondary-title></titles><periodical><full-title>ACSAppliedMaterials&Interfaces</full-title></periodical><pages>1240-7</pages><volume>5</volume><number>4</number><dates><year>2013</year><pub-dates><date>Feb</date></pub-dates></dates><isbn>1944-8252(Electronic) 1944-8244(Linking)</isbn><accession-num>23360622</accession-num><urls><related-urls><url>/pubmed/23360622</url></related-urls></urls><electronic-resource-num>10.1021/am3022015</electronic-resource-num></record></Cite></EndNote>（Senetal.,2013）利用溶剂热反应得到球花状MoS2，每个花瓣微球都是由许多MoS2纳米片蜷曲堆叠自组装形成的，对其生长过程进行研究，发现花瓣微球的形成主要包括成核、延展、自组装等多个连续过程，由于MoS2纳米片边缘悬挂了很多不饱和键，能量较高，为降低表面能，纳米片会自动弯曲蜷缩成球花状（图1.4）。在反应体系中加入一定量的添加剂，能够有效调控产物形貌。Lin等ADDINEN.CITE<EndNote><Cite><Author>Lin</Author><Year>2010</Year><RecNum>30</RecNum><DisplayText><stylefont="微软雅黑">（</style>Linetal.,2010<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>30</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615184278">30</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Lin,Hongtao</author><author>Chen,Xiaoya</author><author>Li,Hongling</author><author>Yang,Min</author><author>Qi,Yanxing</author></authors></contributors><titles><title>HydrothermalsynthesisandcharacterizationofMoS2nanorods</title><secondary-title>MaterialsLetters</secondary-title></titles><periodical><full-title>MaterialsLetters</full-title></periodical><pages>1748-1750</pages><volume>64</volume><number>15</number><dates><year>2010</year></dates><isbn>0167577X</isbn><urls></urls><electronic-resource-num>10.1016/j.matlet.2010.04.032</electronic-resource-num></record></Cite></EndNote>（Linetal.,2010）以钼酸钠和硫脲为反应物，硅钨酸为添加剂，在220℃水热反应24h制备了长度400-500nm，直径20-50nm的均匀纳米棒，研究发现硅钨酸的存在对于纳米棒的形成至关重要，在反应过程中可能作为牺牲模板诱导MoS2的定向生长，同时WO42-进入MoS2层间扩大层间距。不同的有机溶剂也可以代替水作为反应介质，由于溶剂的性质不同，例如极性、粘度和柔和度等等，溶剂对于前体在反应中溶解性和传输行为有着重要的影响。如Hwang等ADDINEN.CITE<EndNote><Cite><Author>Hwang</Author><Year>2011</Year><RecNum>31</RecNum><DisplayText><stylefont="微软雅黑">（</style>Hwangetal.,2011<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>31</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615184291">31</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Hwang,H.</author><author>Kim,H.</author><author>Cho,J.</author></authors></contributors><auth-address>InterdisciplinarySchoolofGreenEnergy,UlsanNationalInstituteofScienceandTechnology(UNIST),Ulsan689-798,Korea.</auth-address><titles><title>MoS2nanoplatesconsistingofdisorderedgraphene-likelayersforhighratelithiumbatteryanodematerials</title><secondary-title>NanoLetters</secondary-title></titles><periodical><full-title>NanoLetters</full-title></periodical><pages>4826-30</pages><volume>11</volume><number>11</number><keywords><keyword>Disulfides/*chemistry</keyword><keyword>*ElectricPowerSupplies</keyword><keyword>Electrodes</keyword><keyword>EquipmentDesign</keyword><keyword>EquipmentFailureAnalysis</keyword><keyword>Graphite/*chemistry</keyword><keyword>Lithium/*chemistry</keyword><keyword>Molybdenum/*chemistry</keyword><keyword>Nanostructures/*chemistry/ultrastructure</keyword><keyword>Nanotechnology/*instrumentation</keyword><keyword>ParticleSize</keyword><keyword>Titanium/*chemistry</keyword></keywords><dates><year>2011</year><pub-dates><date>Nov9</date></pub-dates></dates><isbn>1530-6992(Electronic) 1530-6984(Linking)</isbn><accession-num>21958327</accession-num><urls><related-urls><url>/pubmed/21958327</url></related-urls></urls><electronic-resource-num>10.1021/nl202675f</electronic-resource-num></record></Cite></EndNote>（Hwangetal.,2011）以Mo(CO)6和硫粉为反应原料，在二甲苯溶液中250℃溶剂热反应24h，制备出了无定形MoS2纳米片，其层间距扩大至0.69nm。Jing等ADDINEN.CITE<EndNote><Cite><Author>Jing</Author><Year>2019</Year><RecNum>32</RecNum><DisplayText><stylefont="微软雅黑">（</style>Jingetal.,2019<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>32</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615184430">32</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Jing,Laiying</author><author>Lian,Gang</author><author>Wang,Junru</author><author>Zhao,Mingwen</author><author>Liu,Xizheng</author><author>Wang,Qilong</author><author>Cui,Deliang</author><author>Wong,Ching-Ping</author></authors></contributors><titles><title>Porous-hollownanorodsconstructedfromalternateintercalationofcarbonandMoS2monolayersforlithiumandsodiumstorage</title><secondary-title>NanoResearch</secondary-title></titles><periodical><full-title>NanoResearch</full-title></periodical><pages>1912-1920</pages><volume>12</volume><number>8</number><dates><year>2019</year></dates><isbn>1998-0124 1998-0000</isbn><urls></urls><electronic-resource-num>10.1007/s12274-019-2458-9</electronic-resource-num></record></Cite></EndNote>（Jingetal.,2019）以乙酰丙酮钼和硫粉为原料，采用有机胺辅助溶剂热法得到了一种由垂直于管方向的薄层纳米片自组装形成的新型MoS2基多孔管状结构（图1.5），其中作为自组装单元的纳米片是通过MoS2和非连续的氮掺杂单分子层碳交替插层构成的，由于单层碳的插入使得相邻MoS2的层间距从0.62nm扩展到0.96nm。水热/溶剂热法适用于原位合成MoS2纳米材料，产物具有形态可控、纯度高、粒度分布均匀等优点，但是产物结晶程度不高，结构稳定性差，宏量制备寡层MoS2纳米片有困难。图1.4球花状MoS2自组装过程示意图ADDINEN.CITE<EndNote><Cite><Author>Sen</Author><Year>2013</Year><RecNum>28</RecNum><DisplayText><stylefont="微软雅黑">（</style>Senetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>28</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615179295">28</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Sen,U.K.</author><author>Mitra,S.</author></authors></contributors><auth-address>ElectrochemicalEnergyLaboratory,DepartmentofEnergyScienceandEngineering,IndianInstituteofTechnology,Bombay,Mumbai-400076,India.</auth-address><titles><title>High-rateandhigh-energy-densitylithium-ionbatteryanodecontaining2DMoS2nanowallandcellulosebinder</title><secondary-title>ACSAppliedMaterials&Interfaces</secondary-title></titles><periodical><full-title>ACSAppliedMaterials&Interfaces</full-title></periodical><pages>1240-7</pages><volume>5</volume><number>4</number><dates><year>2013</year><pub-dates><date>Feb</date></pub-dates></dates><isbn>1944-8252(Electronic) 1944-8244(Linking)</isbn><accession-num>23360622</accession-num><urls><related-urls><url>/pubmed/23360622</url></related-urls></urls><electronic-resource-num>10.1021/am3022015</electronic-resource-num></record></Cite></EndNote>（Senetal.,2013）Fig1.4SchematicrepresentationforthegrowthmechanismofcauliflowerlikeMoS2ADDINEN.CITE<EndNote><Cite><Author>Sen</Author><Year>2013</Year><RecNum>28</RecNum><DisplayText><stylefont="微软雅黑">（</style>Senetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>28</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615179295">28</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Sen,U.K.</author><author>Mitra,S.</author></authors></contributors><auth-address>ElectrochemicalEnergyLaboratory,DepartmentofEnergyScienceandEngineering,IndianInstituteofTechnology,Bombay,Mumbai-400076,India.</auth-address><titles><title>High-rateandhigh-energy-densitylithium-ionbatteryanodecontaining2DMoS2nanowallandcellulosebinder</title><secondary-title>ACSAppliedMaterials&Interfaces</secondary-title></titles><periodical><full-title>ACSAppliedMaterials&Interfaces</full-title></periodical><pages>1240-7</pages><volume>5</volume><number>4</number><dates><year>2013</year><pub-dates><date>Feb</date></pub-dates></dates><isbn>1944-8252(Electronic) 1944-8244(Linking)</isbn><accession-num>23360622</accession-num><urls><related-urls><url>/pubmed/23360622</url></related-urls></urls><electronic-resource-num>10.1021/am3022015</electronic-resource-num></record></Cite></EndNote>(Senetal.,2013)图1.5中空管状超结构MoS2/C制备过程示意图ADDINEN.CITE<EndNote><Cite><Author>Jing</Author><Year>2019</Year><RecNum>32</RecNum><DisplayText><stylefont="微软雅黑">（</style>Jingetal.,2019<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>32</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615184430">32</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Jing,Laiying</author><author>Lian,Gang</author><author>Wang,Junru</author><author>Zhao,Mingwen</author><author>Liu,Xizheng</author><author>Wang,Qilong</author><author>Cui,Deliang</author><author>Wong,Ching-Ping</author></authors></contributors><titles><title>Porous-hollownanorodsconstructedfromalternateintercalationofcarbonandMoS2monolayersforlithiumandsodiumstorage</title><secondary-title>NanoResearch</secondary-title></titles><periodical><full-title>NanoResearch</full-title></periodical><pages>1912-1920</pages><volume>12</volume><number>8</number><dates><year>2019</year></dates><isbn>1998-0124 1998-0000</isbn><urls></urls><electronic-resource-num>10.1007/s12274-019-2458-9</electronic-resource-num></record></Cite></EndNote>（Jingetal.,2019）Fig1.5SchematicillustrationoftheformationprocessofMoS2/CtubularsuperstructureADDINEN.CITE<EndNote><Cite><Author>Jing</Author><Year>2019</Year><RecNum>32</RecNum><DisplayText><stylefont="微软雅黑">（</style>Jingetal.,2019<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>32</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615184430">32</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Jing,Laiying</author><author>Lian,Gang</author><author>Wang,Junru</author><author>Zhao,Mingwen</author><author>Liu,Xizheng</author><author>Wang,Qilong</author><author>Cui,Deliang</author><author>Wong,Ching-Ping</author></authors></contributors><titles><title>Porous-hollownanorodsconstructedfromalternateintercalationofcarbonandMoS2monolayersforlithiumandsodiumstorage</title><secondary-title>NanoResearch</secondary-title></titles><periodical><full-title>NanoResearch</full-title></periodical><pages>1912-1920</pages><volume>12</volume><number>8</number><dates><year>2019</year></dates><isbn>1998-0124 1998-0000</isbn><urls></urls><electronic-resource-num>10.1007/s12274-019-2458-9</electronic-resource-num></record></Cite></EndNote>(Jingetal.,2019)1.1.2热分解法热分解法是通过在一定温度下分解硫代钼酸盐或富硫硫钼化合物，使得Mo周围的S原子与Mo发生局部重新组合形成MoS2。由于前驱体中含有S、Mo两种元素，反应过程中无需添加其它硫源或者钼源，且反应无需任何反应中介，直接热解即可获得MoS2。Wang等ADDINEN.CITE<EndNote><Cite><Author>Wang</Author><Year>1998</Year><RecNum>34</RecNum><DisplayText><stylefont="微软雅黑">（</style>Wangetal.,1998<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>34</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615188586">34</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>H.W.Wang</author><author>P.Skeldon</author><author>G.E.Thompson</author></authors></contributors><titles><title>Thermogravimetric-differentialthermalanalysisofthesolid-statedecompositionofammoniumtetrathiomolybdateduringheatinginargon</title><secondary-title>JournalofMaterialsScience</secondary-title></titles><periodical><full-title>JournalofMaterialsScience</full-title></periodical><pages>3079—3083</pages><volume>33</volume><dates><year>1998</year></dates><urls></urls></record></Cite></EndNote>（Wangetal.,1998）研究发现(NH4)2MoS4在氩气气氛下加热到230-260℃时就会分解形成MoS2，其具体分解过程如图1.6所示。Liu等ADDINEN.CITEADDINEN.CITE.DATA（Liuetal.,2012）将(NH4)2MoS4的DMF溶液在蓝宝石或SiO2/Si晶片上分别以500℃（Ar-H2气氛）、1000℃（Ar-S气氛）两步热解制得了寡层MoS2薄膜（图1.7），蓝宝石衬底上生长的MoS2薄膜厚度为三层，结晶程度高，相比之下，在SiO2/Si衬底上生长的MoS2层晶粒尺寸不均匀，甚至出现非晶态结构。Hu等ADDINEN.CITE<EndNote><Cite><Author>Hu</Author><Year>2007</Year><RecNum>36</RecNum><DisplayText><stylefont="微软雅黑">（</style>Huetal.,2007<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>36</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615207015">36</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Hu,KunHong</author><author>Hu,XianGuo</author><author>Sun,XiaoJun</author><author>Jing,HeFeng</author><author>Zhan,Song</author></authors></contributors><titles><title>Synthesisandcharacterizationofnanosizemolybdenumdisulfideparticlesbyquickhomogeneousprecipitationmethod</title><secondary-title>KeyEngineeringMaterials</secondary-title></titles><periodical><full-title>KeyEngineeringMaterials</full-title></periodical><pages>2107-2110</pages><volume>353-358</volume><dates><year>2007</year></dates><isbn>1662-9795</isbn><urls></urls><electronic-resource-num>10.4028//KEM.353-358.2107</electronic-resource-num></record></Cite></EndNote>（Huetal.,2007）利用快速均匀沉淀法制备了MoS3无定型纳米颗粒，其平均尺寸达到40nm，再在氢气气氛下780℃煅烧热解得到具有良好结晶度的MoS2纳米球富勒烯纳米颗粒。利用热分解法可制备较大面积的MoS2薄膜，但是在热分解过程中放出大量H2S、NH3等有害气体，并且所得MoS2片尺寸较小，厚度均匀性难控制。图1.6四硫代钼酸铵（ATT）的热解过程ADDINEN.CITE<EndNote><Cite><Author>Wang</Author><Year>1998</Year><RecNum>34</RecNum><DisplayText><stylefont="微软雅黑">（</style>Wangetal.,1998<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>34</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615188586">34</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>H.W.Wang</author><author>P.Skeldon</author><author>G.E.Thompson</author></authors></contributors><titles><title>Thermogravimetric-differentialthermalanalysisofthesolid-statedecompositionofammoniumtetrathiomolybdateduringheatinginargon</title><secondary-title>JournalofMaterialsScience</secondary-title></titles><periodical><full-title>JournalofMaterialsScience</full-title></periodical><pages>3079—3083</pages><volume>33</volume><dates><year>1998</year></dates><urls></urls></record></Cite></EndNote>（Wangetal.,1998）Fig1.6DecompositionsequencesofATTsolidsADDINEN.CITE<EndNote><Cite><Author>Wang</Author><Year>1998</Year><RecNum>34</RecNum><DisplayText><stylefont="微软雅黑">（</style>Wangetal.,1998<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>34</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615188586">34</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>H.W.Wang</author><author>P.Skeldon</author><author>G.E.Thompson</author></authors></contributors><titles><title>Thermogravimetric-differentialthermalanalysisofthesolid-statedecompositionofammoniumtetrathiomolybdateduringheatinginargon</title><secondary-title>JournalofMaterialsScience</secondary-title></titles><periodical><full-title>JournalofMaterialsScience</full-title></periodical><pages>3079—3083</pages><volume>33</volume><dates><year>1998</year></dates><urls></urls></record></Cite></EndNote>(Wangetal.,1998)图1.7两步热解制备MoS2薄膜过程示意图ADDINEN.CITEADDINEN.CITE.DATA（Liuetal.,2012）Fig1.7Schematicillustrationofthetwo-stepthermolysisprocessforthesynthesisofMoS2thinlayersoninsulatingsubstratesADDINEN.CITEADDINEN.CITE.DATA(Liuetal.,2012)1.1.3化学气相沉积法化学气相沉积法（Chemicalvapordeposition，CVD）是利用一种或几种气相化合物或单质在衬底表面上进行化学反应生成薄膜的方法。由于CVD法得到的MoS2纯度高、残余应力小、结晶度好，并且能实现形貌、厚度、尺寸大小的可控制备，目前已经成为制备高质量层状MoS2的有效方法。Kong等ADDINEN.CITE<EndNote><Cite><Author>Kong</Author><Year>2013</Year><RecNum>38</RecNum><DisplayText><stylefont="微软雅黑">（</style>Kongetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>38</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615212434">38</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Kong,D.</author><author>Wang,H.</author><author>Cha,J.J.</author><author>Pasta,M.</author><author>Koski,K.J.</author><author>Yao,J.</author><author>Cui,Y.</author></authors></contributors><auth-address>DepartmentofMaterialsScienceandEngineering,StanfordUniversity,Stanford,California94305,UnitedStates.</auth-address><titles><title>SynthesisofMoS2andMoSe2filmswithverticallyalignedlayers</title><secondary-title>NanoLetters</secondary-title></titles><periodical><full-title>NanoLetters</full-title></periodical><pages>1341-7</pages><volume>13</volume><number>3</number><dates><year>2013</year><pub-dates><date>Mar13</date></pub-dates></dates><isbn>1530-6992(Electronic) 1530-6984(Linking)</isbn><accession-num>23387444</accession-num><urls><related-urls><url>/pubmed/23387444</url></related-urls></urls><electronic-resource-num>10.1021/nl400258t</electronic-resource-num></record></Cite></EndNote>（Kongetal.,2013）首先在基底上沉积一层5nm厚的Mo金属薄膜，然后在硫气氛中550℃快速硫化制备了竖直排列的MoS2层，这一过程主要受动力学驱动，在高温条件下，金属薄膜转化成金属硫化物的速度要远快于S扩散速度，因而限制了平面生长过程，纳米片沿着垂直基底方向生长（图1.8a）。Lin等ADDINEN.CITE<EndNote><Cite><Author>Lin</Author><Year>2012</Year><RecNum>39</RecNum><DisplayText><stylefont="微软雅黑">（</style>Linetal.,2012<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>39</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615213788">39</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Lin,Y.C.</author><author>Zhang,W.</author><author>Huang,J.K.</author><author>Liu,K.K.</author><author>Lee,Y.H.</author><author>Liang,C.T.</author><author>Chu,C.W.</author><author>Li,L.J.</author></authors></contributors><auth-address>InstituteofAtomicandMolecularSciences,AcademiaSinica,Taipei,10617,Taiwan.</auth-address><titles><title>Wafer-scaleMoS2thinlayerspreparedbyMoO3sulfurization</title><secondary-title>Nanoscale</secondary-title></titles><periodical><full-title>Nanoscale</full-title></periodical><pages>6637-41</pages><volume>4</volume><number>20</number><dates><year>2012</year><pub-dates><date>Oct21</date></pub-dates></dates><isbn>2040-3372(Electronic) 2040-3364(Linking)</isbn><accession-num>22983609</accession-num><urls><related-urls><url>/pubmed/22983609</url></related-urls></urls><electronic-resource-num>10.1039/c2nr31833d</electronic-resource-num></record></Cite></EndNote>（Linetal.,2012）首先通过热蒸发法在蓝宝石衬底上沉积了一定厚度的MoO3薄膜，然后在H2/Ar混合气氛中500℃加热1h，使之还原为MoO2，最后在含硫气氛下1000℃煅烧30min形成MoS2薄膜，厚度约为1.9nm。Wang等ADDINEN.CITE<EndNote><Cite><Author>Wang</Author><Year>2013</Year><RecNum>40</RecNum><DisplayText><stylefont="微软雅黑">（</style>Wangetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>40</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615218115">40</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Wang,X.</author><author>Feng,H.</author><author>Wu,Y.</author><author>Jiao,L.</author></authors></contributors><auth-address>KeyLabofOrganicOptoelectronics&MolecularEngineering,DepartmentofChemistry,TsinghuaUniversity,Beijing100084,China.</auth-address><titles><title>ControlledsynthesisofhighlycrystallineMoS2flakesbychemicalvapordeposition</title><secondary-title>JournaloftheAmericanChemicalSociety</secondary-title></titles><periodical><full-title>JournaloftheAmericanChemicalSociety</full-title></periodical><pages>5304-7</pages><volume>135</volume><number>14</number><dates><year>2013</year><pub-dates><date>Apr10</date></pub-dates></dates><isbn>1520-5126(Electronic) 0002-7863(Linking)</isbn><accession-num>23489053</accession-num><urls><related-urls><url>/pubmed/23489053</url></related-urls></urls><electronic-resource-num>10.1021/ja4013485</electronic-resource-num></record></Cite></EndNote>（Wangetal.,2013）在含硫气氛下650~850℃加热蒸发MoO3，二者在SiO2/Si基底上发生反应生长出菱形的MoO2，再进一步高温硫化处理（850~950℃），则在MoO2表面生长薄层MoS2。MoS2的形成限制了S原子的扩散速率，因而可以通过控制硫化条件控制MoS2层的厚度，尺寸大小则由MoO2晶粒大小决定，得到的MoS2晶体尺寸可达10μm，并具有很高的结晶度（图1.8b）。利用化学气相沉积法能够制备高质量的MoS2片层，但是这种方法设备复杂且难以量产，而且大面积、连续、均匀单层薄膜的制备仍是一个难题，同时，实验过程会产生大量有毒废气，S与Mo蒸汽的利用率也不高。(a)(b)图1.8（a）垂直衬底生长的MoS2薄膜的结构示意图及微观形貌ADDINEN.CITE<EndNote><Cite><Author>Kong</Author><Year>2013</Year><RecNum>38</RecNum><DisplayText><stylefont="微软雅黑">（</style>Kongetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>38</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615212434">38</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Kong,D.</author><author>Wang,H.</author><author>Cha,J.J.</author><author>Pasta,M.</author><author>Koski,K.J.</author><author>Yao,J.</author><author>Cui,Y.</author></authors></contributors><auth-address>DepartmentofMaterialsScienceandEngineering,StanfordUniversity,Stanford,California94305,UnitedStates.</auth-address><titles><title>SynthesisofMoS2andMoSe2filmswithverticallyalignedlayers</title><secondary-title>NanoLetters</secondary-title></titles><periodical><full-title>NanoLetters</full-title></periodical><pages>1341-7</pages><volume>13</volume><number>3</number><dates><year>2013</year><pub-dates><date>Mar13</date></pub-dates></dates><isbn>1530-6992(Electronic) 1530-6984(Linking)</isbn><accession-num>23387444</accession-num><urls><related-urls><url>/pubmed/23387444</url></related-urls></urls><electronic-resource-num>10.1021/nl400258t</electronic-resource-num></record></Cite></EndNote>（Kongetal.,2013）；（b）MoS2合成和剥离示意图以及制备的MoS2/MoO2片和分散的MoS2片的光学图像ADDINEN.CITE<EndNote><Cite><Author>Wang</Author><Year>2013</Year><RecNum>40</RecNum><DisplayText><stylefont="微软雅黑">（</style>Wangetal.,2013<stylefont="微软雅黑">）</style></DisplayText><record><rec-number>40</rec-number><foreign-keys><keyapp="EN"db-id="ts2setpavsxtr1edt23vd9apdedsp92ffazv"timestamp="1615218115">40</key><keyapp="ENWeb"db-id="">0</key></foreign-keys><ref-typename="JournalArticle">17</ref-type><contributors><authors><author>Wang,X.</author><author>Feng,H.</author><author>Wu,Y.</author><author>Jiao,L.</author></authors></contributors><auth-address>KeyLabofOrganicOptoelectronics&MolecularEngineering,Department