CN106298259B - 一种2h相单层二硫化钼纳米片的制备方法 - Google Patents
一种2h相单层二硫化钼纳米片的制备方法 Download PDFInfo
- Publication number
- CN106298259B CN106298259B CN201610698720.9A CN201610698720A CN106298259B CN 106298259 B CN106298259 B CN 106298259B CN 201610698720 A CN201610698720 A CN 201610698720A CN 106298259 B CN106298259 B CN 106298259B
- Authority
- CN
- China
- Prior art keywords
- lithium
- phase
- mos
- centrifuge
- individual layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 42
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000002135 nanosheet Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000013049 sediment Substances 0.000 claims abstract description 10
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 7
- -1 lithium salt compound Chemical class 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 150000003384 small molecules Chemical class 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 230000007062 hydrolysis Effects 0.000 claims abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 2
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 41
- 239000010410 layer Substances 0.000 description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000007789 gas Substances 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical class [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- IQMAMZYAQFTIAU-UHFFFAOYSA-N lithium;sulfanylidenemolybdenum Chemical compound [Li].[Mo]=S IQMAMZYAQFTIAU-UHFFFAOYSA-N 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000001420 photoelectron spectroscopy Methods 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Secondary Cells (AREA)
Abstract
本发明公开了一种2H相单层二硫化钼纳米片的制备方法,具体步骤为:将硫代钼酸铵和锂盐化合物按1:2摩尔比混合研磨,研磨后的混合物在惰性气体保护下于200‑400℃保温1‑10h,冷却至室温得到插锂的2H相硫化钼块体;将插锂的2H相硫化钼块体置于去离子水中,辅助超声水解剥离5‑30min,再将得到的悬浮液置于离心机中,经离心分离去除未剥离的沉淀物后得到2H相单层MoS2纳米片悬浮液;将2H相单层MoS2纳米片悬浮液在离心机上分别用水和乙醇离心洗涤去除可溶性杂质,最后将沉淀物2H相单层MoS2纳米片分散于小分子溶剂中保存,该2H相单层MoS2纳米片的厚度小于1nm。本发明工艺操作简单,反应条件温和,所用试剂价格低廉,绿色环保。
Description
技术领域
本发明属于二硫化钼纳米材料的合成技术领域,具体涉及一种2H相单层二硫化钼纳米片的制备方法。
背景技术
二硫化钼具有典型三明治层状结构,由于其层间相对较弱的范德华力,也可以剥离成单层或少层数的纳米片,被认为是另外一种相当重要的二维纳米片材料,具有独特的物理、化学和电学特性。Radisavljevic等人测试表明单层MoS2的电导率要比块体MoS2提高100个数量级,使得其在电子器件及电子传感器中有着优越的性能(Nat.Nanotechnol.2011,6,147);Mak等人通过计算模拟表明MoS2从块体剥离至单层,由于量子限域效应,其禁带宽度由间接带隙的1.3eV增大为直接带隙的1.8eV,使得光生电子空穴的分离能力提高(Phys.Rev.Lett.2010,105);Hinnemann等人通过密度函公式计算纳米级MoS2的暴露活性边缘的吸附氢吉布斯自由能,发现其边缘有很强的氢吸附能力,并有着金属Pt一样接近零吉布斯自由能的析氢性能,从而推断出单层的MoS2拥有更多的暴露活性边缘,很有希望成为替代Pt作为析氢材料的催化剂(J.Am.Chem.Soc.2005,127,5308)。ChenW.X.等人研究表明,单层MoS2在与碳基材料复合时,有着超高的容量贡献(>1500mAh/g),远远超过其块体材料的理论值(J.Mater.Chem.2011,21,6251)。
二硫化钼存在三种相态,即1T、2H和3R相。其中,1T相是MoS2以一个S-Mo-S单分子层作为最小重复单元堆叠,而2H和3R相是以两个和三个S-Mo-S单分子层作为最小重复单元堆叠。自然界中大部分MoS2是以2H稳定相存在的,1T和3R相属于亚稳态结构,在一定条件下可以转变为2H相。由于单层2H相的MoS2已经失去了双分子层为最小重复单元的特性,因此也被称为1H相。不同相态的MoS2材料所呈现的物理化学特性也不尽相同。例如,2H态MoS2材料展现出禁带宽度为1.3-1.9eV的半导体特性,其通过层数的多少来调节禁带宽度的大小;而1T态的MoS2材料则呈现出金属特性,其优越的导电性在催化水分解制氢以及超级电容领域取得了重要的突破(Advanced Energy Materials,2016,DOI:10.1002/aenm.201502555)。
虽然单层MoS2纳米材料在热、电、光、力学等方面的性质及其在光电子器件领域的潜在应用引起了科研人员的广泛关注。然而,一般的化学、物理法难以制备出纯单层结构的MoS2纳米材料,尤其是不同相态的单层硫化钼剥离制备。目前制备单层MoS2纳米材料的主要有微机械力剥离法、化学气相沉积法、锂离子插层法以及液相超声法等,这些剥离方法不仅操作繁琐,工艺复杂,而且单层MoS2的产量极低,大部分是厚度为1-100nm的少层数MoS2纳米片,而非真正意义上的单层MoS2。除了难以高效率地剥离制备单层MoS2纳米片外,MoS2纳米片只能在诸如二甲基甲酰胺和N-甲基吡咯烷酮等高沸点有机溶剂中剥离和保存,而这些有机溶剂粘度大、沸点很高,在离心收集过程中,单层或少层数MoS2又重新聚集成多层MoS2纳米片,从而限制了单层MoS2纳米片在一些科研或工业领域的探索和应用。
发明内容
本发明解决的技术问题是提供了一种简单、安全、高效且适合规模化生产的2H相单层二硫化钼纳米片的制备方法,该方法是以硫代钼酸铵和锂盐化合物为原料,在一定温度下热处理得到2H相的插锂Li2MoS2块体,插锂Li2MoS2块体在去离子水中水解自行剥离得到单层目标产物。
本发明为解決上述技术问题采用如下技术方案,一种2H相单层二硫化钼纳米片的制备方法,其特征在于具体步骤为:
(1)将硫代钼酸铵和锂盐化合物按1:2摩尔比混合研磨,研磨后的混合物在惰性气体保护下于200-400℃保温1-10h,冷却至室温得到插锂的2H相硫化钼块体;
(2)将插锂的2H相硫化钼块体直接置于去离子水中,辅助超声水解剥离5-30min,再将得到的悬浮液置于离心机中,经离心分离去除未剥离的沉淀物后得到2H相单层MoS2纳米片悬浮液;
(3)将2H相单层MoS2纳米片悬浮液在离心机上分别用水和乙醇离心洗涤去除可溶性杂质,最后将沉淀物2H相单层MoS2纳米片分散于小分子溶剂中保存,该2H相单层MoS2纳米片的厚度小于1nm。
进一步限定,步骤(1)中所述的锂盐化合物为氢氧化锂、氯化锂、醋酸锂、碳酸锂、硫酸锂或硝酸锂中的一种或多种。
进一步限定,步骤(2)中所述的离心机转速为1000r/min,步骤(3)中所述的离心机转速为4000-20000r/min。
进一步限定,步骤(3)中所述的小分子溶剂为水、甲醇、乙醇、异丙醇、丁醇、丙酮、N-甲基吡咯烷酮或N-甲基甲酰胺。
本发明与现有技术相比具有以下优点:
1、本发明以硫代钼酸铵和锂盐化合物为原料,通过简单的温度控制可以合成为插锂的2H相硫化钼块体,插锂的2H相硫化钼块体可以在水中水解自行剥离成2H相单层MoS2纳米片,并且可以在水、乙醇等小分子溶剂中稳定存在;
2、本发明得到的2H相单层MoS2纳米片的厚度小于1nm,而非现有技术中的1-100nm厚度的MoS2纳米片;
3、本发明合成的2H相单层MoS2纳米片可以用于单层硫化钼在光析氢、电催化和储能等领域的研究;
4、本发明工艺操作简单,反应条件温和,所用试剂价格低廉,绿色环保。
附图说明
图1是本发明实施例1制得的2H相单层MoS2的光电子能图谱;
图2是本发明实施例1制得的2H相单层MoS2的原子力显微图谱。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
分别称取0.008mol的氢氧化锂和0.004mol的硫代钼酸铵,在玛瑙研钵中混合研磨1h,将研磨后的混合物置于刚玉坩埚中,放置在管式炉中,通氩气保护,程序升温至400℃,保温1h,然后继续通氩气自然降温至室温,得到插锂的2H相硫化钼(Li2MoS4)块体;将插锂的硫化钼块体置于盛有100mL去离子水的容器中,超声分散10min,分散后的悬浮液在转速为1000r/min的离心机上离心分离沉淀;将去除沉淀后的悬浮液在转速为4000r/min的离心机上分别用水和乙醇离心洗涤3次去除Li2S等可溶性杂质,将洗涤后的沉淀物超声分散在200mL去离子水中,其中2H相单层MoS2的浓度约为0.8mg/mL,经原子力显微镜检测其厚度为0.66nm,X-光电子能谱显示为2H相。
实施例2
分别称取0.008mol的醋酸锂和0.004mol的硫代钼酸铵,在玛瑙研钵中混合研磨1h,将研磨后的混合物置于刚玉坩埚中,放置在管式炉中,通氩气保护,程序升温至200℃,保温10h,然后继续通氩气自然降温至室温,得到插锂的2H相硫化钼(Li2MoS4)块体;将插锂的硫化钼块体置于盛有200mL去离子水的容器中,超声分散10min,分散后的悬浮液在转速为1000r/min的离心机上离心分离沉淀;将去除沉淀后的悬浮液在转速为10000r/min的用离心机上分别用水和乙醇离心洗涤3次去除Li2S等可溶性杂质,将洗涤后的沉淀物超声分散在200mL无水乙醇中,其中2H相单层MoS2的浓度约为1.2mg/mL,经原子力显微镜检测其厚度为0.65nm,X-光电子能谱显示为2H相。
实施例3
分别称取0.008mol的硝酸锂和0.004mol的硫代钼酸铵,在玛瑙研钵中混合研磨1h,将研磨后的混合物置于刚玉坩埚中,放置在管式炉中,通氩气保护,程序升温至300℃,保温5h,然后继续通氩气自然降温至室温,得到插锂的2H相硫化钼(Li2MoS4)块体;将插锂的硫化钼块体置于盛有100mL去离子水的容器中,超声分散5min,分散后的悬浮液在转速为1000r/min的离心机上离心分离沉淀;将去除沉淀后的悬浮液在转速为15000r/min的离心机上分别用水和乙醇离心洗涤3次去除Li2S等可溶性杂质,将洗涤后的沉淀物超声分散在200mL异丙醇中,其中2H相单层MoS2的浓度约为1.3mg/mL,经原子力显微镜检测其厚度为0.62nm,X-光电子能谱显示为2H相。
实施例4
分别称取0.008mol的碳酸锂和0.004mol的硫代钼酸铵,在玛瑙研钵中混合研磨1h,研磨后的将混合物置于刚玉坩埚中,放置在管式炉中,通氩气保护,程序升温至300℃,保温5h,然后继续通氩气自然降温至室温,得到插锂的2H相硫化钼(Li2MoS4)块体;将插锂的硫化钼块体置于盛有100mL去离子水的容器中,超声分散30min,分散后的悬浮液在转速为1000r/min的离心机上离心分离沉淀;将去除沉淀后的悬浮液在转速为20000r/min的离心机分别用水和乙醇离心洗涤3次去除Li2S等可溶性杂质,将洗涤后的沉淀物超声分散在200mL N-甲基吡咯烷酮中,其中2H相单层MoS2的浓度约为1.5mg/mL,经原子力显微镜检测其厚度为0.6nm,X-光电子能谱显示为2H相。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (4)
1.一种2H相单层二硫化钼纳米片的制备方法,其特征在于具体步骤为:
(1)将硫代钼酸铵和锂盐化合物按1:2摩尔比混合研磨,研磨后的混合物在惰性气体保护下于200-400℃保温1-10h,冷却至室温得到插锂的2H相硫化钼块体;
(2)将插锂的2H相硫化钼块体直接置于去离子水中,辅助超声水解剥离5-30min,再将得到的悬浮液置于离心机中,经离心分离去除未剥离的沉淀物后得到2H相单层MoS2纳米片悬浮液;
(3)将2H相单层MoS2纳米片悬浮液在离心机上分别用水和乙醇离心洗涤去除可溶性杂质,最后将沉淀物2H相单层MoS2纳米片分散于小分子溶剂中保存,该2H相单层MoS2纳米片的厚度小于1nm。
2.根据权利要求1所述的2H相单层二硫化钼纳米片的制备方法,其特征在于:步骤(1)中所述的锂盐化合物为氯化锂、醋酸锂、碳酸锂、硫酸锂或硝酸锂中的一种或多种。
3.根据权利要求1所述的2H相单层二硫化钼纳米片的制备方法,其特征在于:步骤(2)中所述的离心机转速为1000r/min,步骤(3)中所述的离心机转速为4000-20000r/min。
4.根据权利要求1所述的2H相单层二硫化钼纳米片的制备方法,其特征在于:步骤(3)中所述的小分子溶剂为水、甲醇、乙醇、异丙醇、丁醇、丙酮、N-甲基吡咯烷酮或N-甲基甲酰胺。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610698720.9A CN106298259B (zh) | 2016-08-22 | 2016-08-22 | 一种2h相单层二硫化钼纳米片的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610698720.9A CN106298259B (zh) | 2016-08-22 | 2016-08-22 | 一种2h相单层二硫化钼纳米片的制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106298259A CN106298259A (zh) | 2017-01-04 |
CN106298259B true CN106298259B (zh) | 2018-03-06 |
Family
ID=57662242
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610698720.9A Expired - Fee Related CN106298259B (zh) | 2016-08-22 | 2016-08-22 | 一种2h相单层二硫化钼纳米片的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106298259B (zh) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109273543B (zh) * | 2018-10-29 | 2020-05-19 | 华中科技大学 | 硫族化合物膜上涂覆纳米颗粒的晶体管及制备方法与应用 |
CN109589801A (zh) * | 2018-12-21 | 2019-04-09 | 清华-伯克利深圳学院筹备办公室 | 一种抗菌膜、及其制备方法和用途 |
CN115986125B (zh) * | 2023-03-15 | 2023-06-02 | 中国华能集团清洁能源技术研究院有限公司 | 一种二维过渡金属硫化物催化剂及基于其的锂硫电池 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101857273A (zh) * | 2010-05-26 | 2010-10-13 | 上海大学 | 纳米级片状二硫化钼的制备方法 |
CN102723463A (zh) * | 2012-06-08 | 2012-10-10 | 浙江大学 | 一种锂离子电池单层MoS2/石墨烯复合电极的制备方法 |
CN104934602A (zh) * | 2015-06-19 | 2015-09-23 | 上海交通大学 | 一种二硫化钼/碳复合材料及其制备方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20160093491A1 (en) * | 2014-09-29 | 2016-03-31 | University Of North Texas | LARGE SCALE AND THICKNESS-MODULATED MoS2 NANOSHEETS |
-
2016
- 2016-08-22 CN CN201610698720.9A patent/CN106298259B/zh not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101857273A (zh) * | 2010-05-26 | 2010-10-13 | 上海大学 | 纳米级片状二硫化钼的制备方法 |
CN102723463A (zh) * | 2012-06-08 | 2012-10-10 | 浙江大学 | 一种锂离子电池单层MoS2/石墨烯复合电极的制备方法 |
CN104934602A (zh) * | 2015-06-19 | 2015-09-23 | 上海交通大学 | 一种二硫化钼/碳复合材料及其制备方法 |
Non-Patent Citations (1)
Title |
---|
二硫化钼纳米片(管)及其复合物的制备和性能研究;刘文宏;《合肥工业大学博士学位论文》;20150301;第1-7页 * |
Also Published As
Publication number | Publication date |
---|---|
CN106298259A (zh) | 2017-01-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106241878B (zh) | 一种1t相单层二硫化钼纳米片的制备方法 | |
CN106257609B (zh) | 一种制备单层1t相二硫化钼/石墨烯复合材料的方法 | |
Zou et al. | Crystal-plane-dependent metal oxide-support interaction in CeO2/g-C3N4 for photocatalytic hydrogen evolution | |
Huang et al. | Recent progress of TMD nanomaterials: phase transitions and applications | |
Halim et al. | Transparent conductive two-dimensional titanium carbide epitaxial thin films | |
Hemanth et al. | Recent advances in 2D MXenes for enhanced cation intercalation in energy harvesting applications: a review | |
Fang et al. | 2 D MXene‐based energy storage materials: interfacial structure design and functionalization | |
Tran et al. | Unusual synthesis of safflower-shaped TiO2/Ti3C2 heterostructures initiated from two-dimensional Ti3C2 MXene | |
Ghidiu et al. | Ion-exchange and cation solvation reactions in Ti3C2 MXene | |
Ellefson et al. | Synthesis and applications of molybdenum (IV) oxide | |
Naguib et al. | Synthesis of two-dimensional materials by selective extraction | |
CN106335925B (zh) | 一种制备单层2h相二硫化钼/石墨烯复合材料的方法 | |
CN106495221B (zh) | 一种单层二硫化钼纳米片的制备方法 | |
Liu et al. | Mild fabrication of SiC/C nanosheets with prolonged cycling stability as supercapacitor | |
CN108658122A (zh) | 一种二维金属碳氮化物衍生纳米材料及其制备方法 | |
CN106298259B (zh) | 一种2h相单层二硫化钼纳米片的制备方法 | |
Zaretski et al. | Metal-assisted exfoliation (MAE): green, roll-to-roll compatible method for transferring graphene to flexible substrates | |
Numan et al. | Microwave-assisted rapid MAX phase etching and delamination: A paradigm shift in MXene synthesis | |
CN106517335B (zh) | 一种单层二硫化钨纳米片的制备方法 | |
CN105016331B (zh) | 一种石墨烯微片‑金刚石复合物的合成方法 | |
CN106384811A (zh) | 一种蓝磷/过渡金属二硫化物异质结阳极材料及制备方法 | |
Wang et al. | Solution synthesis of ZnO nanotubes via a template-free hydrothermal route | |
CN106335927B (zh) | 一种2h相单层二硫化钨纳米片的制备方法 | |
CN106315678B (zh) | 一种1t相单层二硫化钨纳米片的制备方法 | |
CN106229155B (zh) | 一种制备单层2h相二硫化钼/微纳米碳复合材料的方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180306 Termination date: 20210822 |