CN1239396C - Synthesis method of cadmium sulfide nano rod - Google Patents
Synthesis method of cadmium sulfide nano rod Download PDFInfo
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- CN1239396C CN1239396C CN 200410010619 CN200410010619A CN1239396C CN 1239396 C CN1239396 C CN 1239396C CN 200410010619 CN200410010619 CN 200410010619 CN 200410010619 A CN200410010619 A CN 200410010619A CN 1239396 C CN1239396 C CN 1239396C
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Abstract
本发明属于模板法合成半导体纳米棒的方法。本发明以三甲基十六烷基溴化胺的胶束水溶液为模板，采用氯化镉和硫代乙酰胺为原料，利用硫代乙酰胺在该体系环境内不与氯化镉反应的特点，首先使其与氯化镉在胶束溶液中充分混合，然后在逐滴加入与反应物同摩尔数的氢氧化钠溶液的条件下使硫代乙酰胺释放出的硫离子与氯化镉反应成核并逐渐生长成棒。这些纳米棒可在紫外灯下发蓝光。The invention belongs to a method for synthesizing semiconductor nanorods by a template method. The present invention uses the micellar aqueous solution of trimethylhexadecylamine bromide as a template, adopts cadmium chloride and thioacetamide as raw materials, and utilizes the characteristic that thioacetamide does not react with cadmium chloride in the system environment , first make it fully mixed with cadmium chloride in the micellar solution, and then make the sulfur ion released from thioacetamide react with cadmium chloride under the condition of adding dropwise a sodium hydroxide solution with the same molar number as the reactant Nucleate and gradually grow into rods. These nanorods glow blue under ultraviolet light.
Description
Technical field
The invention belongs to the method for template synthesized semiconductor nanometer rod.
Background technology
Studies show that in recent years, nano material have the character that is different from bulk material, and these character depend on the size and the pattern of nano material.So, the synthetic focus that becomes present research of the nano material of different-shape and size.The one dimension semiconductor nano material is paid close attention to owing to have the potential application prospect in the development of nano-device.As important semiconductor material, unidimensional CdS nano material can have important use in fields such as solar cell, nonlinear optics and opto-electronic devices.And in the development of nano-device and catalytic field, may have different purposes based on the nano material of the different-shape of nanometer rod, so more and more cause people's attention.For example, the research group of A.P.Alivisatos has synthesized the CdSe nanocrystalline (J.Am.Chem.Soc.2000,122,12700) of tear drop shape, arrow-shaped and four arm clavates by the thermolysis of organometallics presoma; The thermolysis by single presoma in the presence of single tensio-active agent of J.Cheon research group has obtained multi-arm CdS (J.Am.Chem.Soc.2001,123,5150) and MnS (J.Am.Chem.Soc.2002,124,615) nano material respectively; Recently, the research group of D.Zhao has also obtained the CdS nanometer rod (Adv.Mater.2002,14,1537) of multi-arm by solvent thermal process.And above-mentioned these methods or cost are higher, or security is relatively poor, all are unfavorable for the protection of industrial production and environment.Up to the present, the rarely found report of method for preparing multi-arm CdS nanometer rod under the room temperature.
Summary of the invention
The synthetic method that the purpose of this invention is to provide a kind of cadmium sulfide nano-stick.
The main process of the present invention is that preparation earlier contains the trimethylammonium hexadecyl amine bromide micellar aqueous solution of Cadmium chloride fine powder and trimethylammonium hexadecyl amine bromide micellar aqueous solution that same molar ratio contains the sulfo-ethanamide as two stock solution, and with the two equal-volume together with micro-hexanaphthene thorough mixing under ultrasonication, under ultrasonication, dropwise add and the sodium hydroxide solution of reactant then, can generate the yellow product that contains single armed and multi-arm cadmium sulfide nano-stick with mole number.It is raw material that the present invention adopts Cadmium chloride fine powder and thioacetamide, utilize thioacetamide in this system environment not with the characteristics of Cadmium chloride fine powder reaction, at first make itself and Cadmium chloride fine powder thorough mixing in micellar solution, then dropwise add with the condition of reactant with the sodium hydroxide solution of mole number under thioacetamide is discharged sulfonium ion also grow into rod gradually with Cadmium chloride fine powder reaction nucleation.Concerning the CdS crystal, (00 1) face of hexagonal structure is more a lot of than the fast growth of other face, and approximately fast 100 times, and also much active than (111) face of cubic structure; In addition, Cadmium Sulfide is easy to generate the nucleus of cubic structure at a lower temperature, so, induce down at the rod-shaped micelle of certain orientation, (00 1) face of hexagonal structure in case on (111) of cubic structure nucleus face, grown, the CdS nanometer rod will form rapidly along [00 1] direction, is the multi-arm nanometer rod at center thereby formed with the nucleus of cubic structure.
Characteristics of the present invention are at room temperature just can obtain the different multi-arm cadmium sulfide nano-stick of aspect ratio by the quantity that changes hexanaphthene.At first preparation contains the micellar aqueous solution of 0.06-1.0M trimethylammonium hexadecyl amine bromide, this solution of 20ml of respectively getting with volumetric molar concentration is respectively charged into two containers of A, B, and add 0.114-0.32g Cadmium chloride fine powder and 0.038-0.11g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.025-0.07M Cadmium chloride fine powder and contain the storing solution B of 0.025-0.07M thioacetamide.Mix with 0.2 or 0.3ml hexanaphthene with the 2ml storing solution B of volumetric molar concentration with 2ml storing solution A with A, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.04-0.11ml (at least 5 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, get yellow colloidal solution, add methyl alcohol and get final product to such an extent that yellow CdS nanometer rod precipitates.The synthetic method of this controllable size helps can selecting as required the CdS nanometer rod of different size in the development of the nano-device in future.
Embodiment
Embodiment 1:
At first preparation contains the micellar aqueous solution 100ml of 0.06M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.114g Cadmium chloride fine powder and 0.038g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.025M Cadmium chloride fine powder and contain the storing solution B of 0.025M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.2ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.04ml that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 41nm, aspect ratio are 8 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 2:
At first preparation contains the micellar aqueous solution 100ml of 0.08M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.114g Cadmium chloride fine powder and 0.038g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.025M Cadmium chloride fine powder and contain the storing solution B of 0.025M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.2ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.04ml (needs 5 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 45nm, aspect ratio are 7 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 3:
At first preparation contains the micellar aqueous solution 100ml of 0.08M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.114g Cadmium chloride fine powder and 0.038g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.025M Cadmium chloride fine powder and contain the storing solution B of 0.025M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.3ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.04ml (needs 5 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 35nm, aspect ratio are 25 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 4:
At first preparation contains the micellar aqueous solution 100ml of 0.08M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.228g Cadmium chloride fine powder and 0.075g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.05M Cadmium chloride fine powder and contain the storing solution B of 0.05M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.3ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.08ml (needs 10 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 33nm, aspect ratio are 27 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 5:
At first preparation contains the micellar aqueous solution 100ml of 0.10M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.114g Cadmium chloride fine powder and 0.038g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.025M Cadmium chloride fine powder and contain the storing solution B of 0.025M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.2ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.04ml (needs 5 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 40nm, aspect ratio are 7 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 6:
At first preparation contains the micellar aqueous solution 100ml of 0.10M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.32g Cadmium chloride fine powder and 0.11g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.07M Cadmium chloride fine powder and contain the storing solution B of 0.07M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.2ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.11ml (needs 20 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 40nm, aspect ratio are 12 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
Embodiment 7:
At first preparation contains the micellar aqueous solution 100ml of 0.10M trimethylammonium hexadecyl amine bromide, respectively get this solution of 20ml and be respectively charged into two containers of A, B, and add 0.32g Cadmium chloride fine powder and 0.11g thioacetamide respectively at A, B two containers, make the storing solution A that contains the 0.07M Cadmium chloride fine powder and contain the storing solution B of 0.07M thioacetamide.2ml storing solution A and 2ml storing solution B are mixed with the 0.3ml hexanaphthene, and ultrasonic concussion down 10 minutes, the sodium hydroxide 0.11ml (needs 20 minutes) that under the ultrasonication that continues, dropwise adds 1.25M then, finish the back and continue ultrasonication 10 minutes, yellow colloidal solution, add methyl alcohol get final product yellow mercury oxide.This is precipitated as mean diameter is that 42nm, aspect ratio are 40 the single armed and the mixture of multi-arm CdS nanometer rod.This sedimentary toluene solution blue light-emitting under ultraviolet lamp.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| ITMI20051502A1 (en) | 2005-07-29 | 2007-01-30 | Getters Spa | GETTER SYSTEMS INCLUDING ONE OR MORE DEPOSITS OF GETTER MATERIAL AND A LAYER OF MATERIAL FOR H02O TRANSPORT |
| CN100347088C (en) * | 2005-09-02 | 2007-11-07 | 清华大学 | Wurtzite structure cadmium sulfide nanowire synthesis method |
| CN100336729C (en) * | 2006-07-03 | 2007-09-12 | 天津大学 | Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same |
| CN100497163C (en) * | 2007-06-21 | 2009-06-10 | 重庆大学 | Compound alkali metal hydrate dissolvent synthesis method for metallic sulfide nano crystal material |
| CN102275870B (en) * | 2010-06-12 | 2014-03-12 | 国家纳米科学中心 | Water-soluble cadmium sulfide nanorod and nanometer heterostructure as well as preparation methods thereof |
| CN101994156B (en) * | 2010-12-09 | 2012-10-10 | 东北林业大学 | Preparation method of magnetic element-doped CdS nanorods |
| CN102145915B (en) * | 2011-03-04 | 2012-08-29 | 北京化工大学 | Method for synthetizing ZnS/CdS nano rod by controlling oxygen content in thermal process of solvent |
| CN102849692B (en) * | 2012-09-29 | 2014-08-13 | 浙江东晶光电科技有限公司 | Preparation method of high oriented tungsten biselenide nanowire |
| CN103803637B (en) * | 2014-01-27 | 2016-05-11 | 湖北大学 | A kind of preparation method of CdS quantum dot |
| CN106698500A (en) * | 2015-11-16 | 2017-05-24 | 天津大学 | Cadmium sulfide ultrathin nanometer flaky material preparation method and application thereof |
| CN110975890B (en) * | 2019-12-24 | 2021-11-02 | 福州大学 | A method for preparing Mo-doped CdS photocatalyst by cation replacement method |
| CN113877610B (en) * | 2021-10-20 | 2022-09-20 | 广西北投环保水务集团有限公司 | CdS quantum dot modified bismuth-based composite material and preparation method and application thereof |
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Effective date of registration: 20170323 Address after: Changzhou City, Jiangsu province Hehai road 213000 No. 9 Patentee after: Changzhou Institute of Energy Storage Materials & Devices Address before: 130022 Changchun people's street, Jilin, No. 5625 Patentee before: Changchun Institue of Applied Chemistry, Chinese Academy of Sciences |
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