CN105923625B - 一种石墨烯负载均匀单一氧化物量子点的制备方法 - Google Patents
一种石墨烯负载均匀单一氧化物量子点的制备方法 Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 45
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 235000011089 carbon dioxide Nutrition 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
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- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 239000006184 cosolvent Substances 0.000 claims abstract description 4
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 12
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- 239000000908 ammonium hydroxide Substances 0.000 abstract description 6
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
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- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/308—Thermal decomposition of nitrates
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
本发明公开了一种石墨烯负载均匀单一氧化物量子点的制备方法,将石墨烯均匀分散在助溶剂中;然后加入金属盐,使金属离子吸附在石墨烯的表面;再加入干冰,然后放入高压反应釜中,加热搅拌反应后得到前驱体,将前驱体在惰性气氛中煅烧后即得石墨烯负载均匀单一氧化物量子点的复合材料。本发明采用干冰为膨胀剂,加热后干冰迅速膨胀并在高压反应釜中形成高压,从而形成超临界二氧化碳膨胀体系,二氧化碳溶解在少量的结晶水中形成的碳酸根离子参与了前驱体的形成,不需要氨水、氢氧化钠、氢氧化钾等沉淀剂或者用于均匀分散的表面活性剂,无需洗涤等复杂的后处理,同时限制了颗粒的结晶以及粒径的增大。
Description
技术领域
本发明属于石墨烯复合材料的制备技术领域,具体涉及到在超临界二氧化碳膨胀体系中石墨烯负载均匀单一氧化物量子点的制备方法。
背景技术
2004年,曼切斯特大学的Andre Geim教授研究团队利用一种机械剥离的方法获得了单原子层厚度的石墨烯,并且测量了它们的物理性质-霍尔效应。因此,他们获得了2010年诺贝尔物理学奖。石墨烯良好的性能和应用前景引起了科研领域和应用领域的高度关注。
石墨烯负载氧化物是石墨烯复合材料中众多的研究领域之一,在上述复合物中,石墨烯由于具有高的导电性、比表面积和良好的化学稳定性以及机械性能,使得到的复合材料整体的导电性、机械加工性能得到了较大的提高。目前,关于制备石墨烯氧化物复合材料的研究报道很多,上述复合材料在超级电容器、锂离子电池、光催化等领域都已经展现出了良好的应用前景。
目前制备石墨烯负载金属氧化物复合材料的方法主要有水热法、溶剂热法、共沉淀法。水热法和共沉淀法中大多使用氨水、氢氧化钠、氢氧化钾等沉淀剂或者用于均匀分散的表面活性剂,这些试剂的使用带来了后处理繁琐的洗涤步骤,浪费了大量的水资源,另外大多耗时较长。此外,由于反应体系中水的作用,负载的氧化物纳米粒子大多存在负载不均匀或者负载效率低。溶剂热法中,大多使用有毒、有害的有机溶剂,在合成过程中需要格外注意使用的安全问题以及给环境带来的污染问题。例如申请专利CN103553031A中描述的制备还原氧化石墨烯/二氧化铈纳米颗粒复合物的方法中,需要加入油酸、乙二胺、甲苯都有机溶剂,反应时间需要12小时以上,并且后续的洗涤需要消耗乙醇以及去离子水。申请专利CN10066292A中描述的石墨烯/稀土氧化物纳米复合材料、制备方法及其应用中,需要加入氨水作为沉淀剂,并且需要后续的洗涤步骤,需要消耗乙醇以及去离子水。申请专利CN102716734A描述了一种氧化铈/氧化石墨烯纳米复合材料的制备方法中,需要使用尿素和醋酸钠作为缓慢沉淀剂,无机盐的去除也需要后续繁琐的洗涤步骤。申请专利CN102631913A中描述的一种石墨烯负载二氧化铈纳米立方复合物的制备方法中,需要使用氨水作为沉淀剂,反应时间需要12小时以上,并且后续需要繁琐的洗涤步骤。
发明内容
本发明的目的是针对现有的制备石墨烯负载氧化物复合材料的制备方法中所存在的对设备的要求高、反应耗时长,需要使用沉淀剂、表面活性剂、有毒有害有机溶剂以及氧化物纳米粒子粒径大、在石墨烯表面分布不均匀等不足之处,提供了一种石墨烯负载均匀单一氧化物量子点的制备方法。
为实现上述目的,本发明的技术方案为:
一种石墨烯负载均匀单一氧化物量子点的制备方法,将石墨烯溶均匀分散在助溶剂中;然后加入金属盐,使金属离子吸附在石墨烯的表面;再加入干冰,然后放入高压反应釜中,加热搅拌反应后得到前驱体,将前驱体在惰性气氛中煅烧后即得石墨烯负载均匀单一氧化物量子点的复合材料。
本发明采用干冰为膨胀剂,加热后干冰迅速膨胀并在高压反应釜中形成高压,从而形成超临界二氧化碳膨胀体系,二氧化碳溶解在少量的结晶水中形成的碳酸根离子参与了前驱体的形成,不需要氨水、氢氧化钠、氢氧化钾等沉淀剂或者用于均匀分散的表面活性剂,无需洗涤等复杂的后处理,同时得到的前驱体为无定形结构,限制了颗粒的结晶以及粒径的增大,从而得到的氧化物纳米颗粒的粒径小于10纳米的氧化物量子点。
本发明直接加入干冰为膨胀剂,无需使用其他设备形成超临界二氧化碳膨胀体系,从而降低了对设备的要求。
优选的,具体步骤如下:
(1)将石墨烯加入到助溶剂中,超声至溶液分散均匀并且呈半透明的亮褐色;
(2)加入金属硝酸盐搅拌,使得金属离子吸附在石墨烯表面;
(3)加入干冰形成混合物;
(4)将步骤(3)得到的混合物放入高压反应釜中,加热搅拌反应;
(5)将反应后的溶液冷却、离心、干燥得到无定形结构的前驱体,将前驱体在惰性气氛中煅烧,得到石墨烯负载均匀单一氧化物量子点的复合材料。
进一步优选的,所述石墨烯为石墨片层结构。
进一步优选的,所述石墨烯为还原石墨烯或石墨烯氧化物。
进一步优选的,步骤(1)所述的助溶剂为沸点低于100℃的有机溶剂。
更进一步优选的,所述有机溶剂为甲醇、乙醇、丙醇或乙腈。这些溶剂对环境影响较小,有利于保护环境。
进一步优选的,所述硝酸盐为硝酸铝、硝酸镍、硝酸钴、硝酸铁、硝酸锰、硝酸锌、硝酸铜、硝酸铅或稀土硝酸盐。
进一步优选的,所述步骤(4)的加热温度为150-200℃,反应时间为0.5-2小时。
进一步优选的,所述步骤(5)的煅烧温度为400-500℃。
进一步优选的,所述干冰的加入量与高压反应釜的容积比为1:20,g:mL。该条件下,形成的石墨烯负载的氧化物量子点更均匀单一。
一种上述制备方法制备的石墨烯负载均匀单一氧化物量子点的复合材料。
一种上述复合材料在催化领域、光领域、电领域或磁领域中的应用。
本发明的有益技术效果为:
1.本发明可以简单、快速制备出石墨烯负载均匀单一氧化物量子点的复合材料。
2.本发明对设备要求低、操作简单、反应速度快、不使用氨水、氢氧化钠、氢氧化钾等沉淀剂或者用于均匀分散的表面活性剂,无需洗涤等复杂的后处理步骤以及得到的氧化物纳米粒子粒径小、负载率高、表面高度分散均匀。
3.本发明制备出的石墨烯负载氧化物复合材料在催化和光电磁等领域具有很大的应用前景。
附图说明
图1为实施例1制备的石墨烯负载二氧化铈复合材料的高倍透射电子显微镜照片。
具体实施方式
下面结构附图及具体实施例对本发明作进一步说明。
实施例1
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸铈搅拌,使得铈离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在400℃下煅烧,得到还原石墨烯负载氧化铈量子点的复合材料(如图1所示)。
实施例2
将20毫克石墨烯氧化物分散在10毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.4克金属硝酸镍搅拌,使得镍离子吸附在石墨烯氧化物表面。在上述溶液中再加入2.5克干冰,将上述混合物放在50毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在450℃下煅烧,得到还原石墨烯负载氧化镍量子点的复合材料。
实施例3
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸铁搅拌,使得铁离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在500℃下煅烧,得到还原石墨烯负载三氧化二铁量子点的复合材料。
实施例4
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸镧搅拌,使得镧离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在500℃下煅烧,得到还原石墨烯负载氧化镧量子点的复合材料。
实施例5
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸铝搅拌,使得铝离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在500℃下煅烧,得到还原石墨烯负载氧化铝量子点的复合材料。
实施例6
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸钴搅拌,使得钴离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在500℃下煅烧,得到还原石墨烯负载氧化亚钴量子点的复合材料。
实施例7
将40毫克石墨烯氧化物分散在20毫升乙醇中,超声1小时至溶液分散均匀并且呈半透明的亮褐色,加入0.8克硝酸锌搅拌,使得锌离子吸附在石墨烯氧化物表面。在上述溶液中再加入5克干冰,将上述混合物放在100毫升高压反应釜中,在200℃加热反应2小时,同时搅拌;将反应后的溶液冷却、离心、干燥,在惰性气氛中在500℃下煅烧,得到还原石墨烯负载氧化锌量子点的复合材料。
上述虽然结合附图对本发明的具体实施方式进行了描述,但并非对发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围内。
Claims (1)
1.一种石墨烯负载均匀单一氧化物量子点的制备方法,其特征是,具体步骤如下:
(1)将石墨烯加入到助溶剂中,超声至溶液分散均匀并且呈半透明的亮褐色;
(2)加入金属硝酸盐搅拌,使得金属离子吸附在石墨烯表面;
(3)加入干冰形成混合物;
(4)将步骤(3)得到的混合物放入高压反应釜中,加热搅拌反应;
(5)将反应后的溶液冷却、离心、干燥得到无定形结构的前驱体,将前驱体在惰性气氛中煅烧,得到石墨烯负载均匀单一氧化物量子点的复合材料;
所述干冰的加入量与高压反应釜的容积比为1:20g/mL ;
所述石墨烯为石墨片层结构;所述石墨烯为还原石墨烯或石墨烯氧化物;所述硝酸盐为硝酸铝、硝酸镍、硝酸钴、硝酸铁、硝酸锰、硝酸锌、硝酸铅或稀土硝酸盐;
所述步骤(4)的加热温度为150-200℃,反应时间为0.5-2小时;
所述步骤(5)的煅烧温度为400-500℃。
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