CN101397149B - CdS nano rod growth method by catalyst-assisted and vacuum heat evaporation - Google Patents
CdS nano rod growth method by catalyst-assisted and vacuum heat evaporation Download PDFInfo
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- CN101397149B CN101397149B CN2008100729764A CN200810072976A CN101397149B CN 101397149 B CN101397149 B CN 101397149B CN 2008100729764 A CN2008100729764 A CN 2008100729764A CN 200810072976 A CN200810072976 A CN 200810072976A CN 101397149 B CN101397149 B CN 101397149B
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Abstract
The invention discloses a method for growing a CdS nano rod of II-VI semiconductor compound by vacuum and thermal evaporation and assistance by catalysts, and is realized by the following processes: CdS powder and metal Bi powder are mixed evenly as per the proportion of mol ratio of 1 : 0.01 - 1 : 0.35 for preparing the raw material, placed in a resistance heating boat made of molybdenum sheets,and various substrates are placed 3 mm - 3 cm over the boat. After the cavity of the vacuum evaporation furnace of the evaporation sedimentation system which is placed internally reaches the vacuum environment of 2*10<-2>-2*10<-3>Pa, the evaporation furnace is sealed, 100-180A of current is led to the resistance heating boat for 5-15 minutes and then evaporation and sedimentation are proceeded. The nano rod of cadmium sulphide prepared by the invention is crystal-stated hexagonal-phase-structured CdS. The nano bod of cadmium sulphide of the invention is characterized by being applicable to various substrates, large segment area and even feature; and the method of the invention is simple, can be promoted easily and is applicable to a large scale of industrial production.
Description
Technical field
The invention belongs to the nanostructure growth field, being specifically related to a kind of catalyst-assisted and vacuum thermal evaporation growth microscopic appearance is the method for nanometer rod CdS.
Background technology
CdS belongs to II-VI family semiconductor material, equally is the direct gap semi-conductor with other semiconductor materials of this family, and the energy gap under the room temperature is 2.42 electron-volts, belongs to the visible light category.At optoelectronic areas, it is very important a kind of semiconductor material, can be used to make up device for non-linear optical and photodiode.It also is good photolytic activity waveguide and electroluminescent material simultaneously, can be widely used in communication, information storage and fields such as high integrated chemistry or biosensor.In recent years, the development of nano material shows that the material of nanoscale has more excellent character probably, can prepare the better device of performance.In nano material, monodimension nanometer material comprises that nanometer rod, nano wire etc. all have the important techniques application prospect, is one of focus of present material scientific and technical research.In the method for existing numerous growth of one-dimensional nano structures, thermal evaporation is to operate relative simple, cost inexpensive method with chemical Vapor deposition process at present.Thermal oxidation method has generated the CuO nano-wire array with uniform array density in the oxidation of Cu substrate surface in Younan Xia group of the Washington, DC university employing air, consults Nano Lett. the 12nd phase the 2nd volume 1334-1338 page or leaf; China N.S.Xu group of Zhongshan University adopts the direct heat method of evaporation to generate the height MoO good with the diameter homogeneity on (100) Si substrate
3Nano-wire array, and this nano-wire array has good field emission characteristic, consults Appl.Phys.Lett. the 13rd phase the 83rd volume 2653-2655 page or leaf; H.J.Gao group of physics institute of the Chinese Academy of Sciences used diameter to adopt thermal evaporation to generate the tungsten oxide nano with high light photoluminescence character as the tungsten filament of 0.3mm on (111) Si substrate as evaporation source in 2005, consult the 141901st page of the 86th phase of Appl.Phys.Lett..All there are two processes in aforesaid method: (1) thermal evaporation process; (2) oxidising process, therefore this method only is suitable for preparing the nanostructure of metal oxide, can't be applied among the preparation of other non-oxide compound nanostructures.
Chemical Vapor deposition process has a large amount of reports in configuration aspects such as the nanometer rod for preparing material, nano wires.Is raw material as G.X.Wang etc. with the CdSe powder, is carrier gas with the argon gas, and the CdSe nano wire of the various patterns of having grown on gold-plated substrate is consulted the 193115th page of the 88th phase of Appl.Phys.Lett.2006; Z.Q.Wang etc. are raw material with Cd rod and S powder, and nitrogen is carrier gas, and the CdS nano belt of having grown at the bottom of the stainless steel lining that catalyst-free adheres to is consulted the 033102nd page of the 89th phase of Appl.Phys.Lett.2006; R.M.Ma etc. are raw material with the CdS powder, and argon gas is carrier gas, grow the CdS nano wire with network structure on gold-plated (111) Si substrate, consult the 205605th page of the 18th phase of Nanotechnology2007; Soumitra Kar etc. are raw material with the CdS powder, argon gas is carrier gas, on gold-plated Si substrate, various one dimension Nano structures have been grown, comprising nano wire, nano belt, the network structure nanometer line, pearl chain nano wire and nano-wire array are consulted the 4542nd page of the 110th phase of J.Phys.Chem.B2006.In general, chemical vapor deposition growth nanometer rod or line require to transmit grower with gas.
Can see, at present the typical material for preparing nanometer rod with thermal evaporation is a metal oxide, the report that does not prepare cadmium sulfide nano-stick, chemical Vapor deposition process prepares cadmium sulfide nano-stick need introduce reaction gas and carrier gas, wayward, be difficult in and obtain the uniform nanostructure of big area pattern on the multiple substrate.
Summary of the invention
The object of the present invention is to provide a kind of method of catalyst-assisted and vacuum thermal evaporation CdS nano rod growth, this method can obtain the CdS that microscopic appearance is a nanometer rod.
The present invention realizes by following technological process:
With the bismuth metal-powder as catalyzer, high-purity CdS powder (99.5%) is a raw material, for 1:0.35-1:0.01 CdS powder and bismuth metal-powder uniform mixing are placed in the resistive heating boat that molybdenum sheet makes in molar ratio, place 3 millimeters of evaporation source tops to 3 centimeters substrate, when the vacuum tightness of the vacuum-evaporation furnace cavity that includes resistive heating boat and substrate reaches 2 * 10
-2-2 * 10
-3Behind the Pa, preferably 2 * 10
-3The time, airtight cavity, galvanization is found yellow or filemot settling for 100-180A thermal evaporation deposition 5min-15min on substrate, be the CdS nanometer rod.
Wherein, described nanostructure is that length is 1-2 μ m, diameter is that nanometer rod and/or the length of 50-60nm is 3-5 μ m, the diameter maximum is that major part needle-like nanometer rod and/or the length of 500-800nm is 5-10 μ m, and diameter is that nano wire and/or the diameter of 100-200nm is the nano-wire array of 50-300nm.
Further, described substrate is ito glass, silica glass, silicon chip, molybdenum sheet, nickel sheet, sapphire sheet etc.
Further, described vacuum-evaporation stove is the resistance-type heating, and preferred heater is the vapourizing furnace of molybdenum sheet, and more preferably evaporation source directly is positioned on the molybdenum sheet well heater.
The CdS nanometer rod that the present invention prepares is six side's phase CdS of crystalline state, as shown in Figure 1, its surface topography such as Fig. 2, Fig. 3, shown in Figure 4.The present invention directly uses blended Bi and CdS powder to be raw material, evaporation source is separated with the deposition region, has effectively avoided the influence of impurity and other by products, and the CdS nanometer rod of acquisition has that depositional area is big, pattern is more even, characteristics such as good crystallinity.Simultaneously, method of the present invention is simple, is easy to promote, and is suitable for large-scale industrial production.
Description of drawings
The XRD figure spectrum of Fig. 1 embodiment 1 product, ★ represents the diffraction peak of catalyst B i, ● the diffraction peak of expression product C dS, ■ represents the diffraction peak of substrate molybdenum.
The scanning electron microscope picture of Fig. 2 embodiment 1 product.
The scanning electron microscope picture of Fig. 3 embodiment 2 products.
The scanning electron microscope picture of Fig. 4 embodiment 3 products.
Embodiment
Embodiment 1
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal bismuth meal is a catalyzer, after both press the 1mol:0.125mol uniform mixing, powder is placed directly on the molybdenum sheet well heater, places about 5mm place, evaporation source top with another molybdenum sheet as substrate.When vacuum tightness reaches 8 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with 2.5A/ minute electric current increases to behind the 130A electric current to keep 10 minutes gradually.Yellow settling is arranged sinking to the bottom the surface.The surface topography that SEM observes the substrate deposition thing is a major part needle-like nanometer rod, and its stub end is the 500-800nm particle, and the nanometer rod that links to each other with particle diameter is reduced gradually by 300-500nm, and rod is long for 3-5 μ m, as Fig. 2.XRD analysis result shows that the principal phase of product is six side CdS, and catalyzer is six side Bi, as Fig. 1.
Embodiment 2
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.04mol, the powder that obtains is placed directly on the molybdenum sheet well heater, ito glass is that substrate places about 2cn place, evaporation source top.When vacuum tightness reaches 8 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min increases to behind the 130A electric current to keep 15 minutes gradually.At substrate surface yellow settling is arranged.The surface topography that SEM observes the substrate deposition thing is that length is 1-2 μ m, and diameter is the nanometer rod of 50-60nm, as Fig. 3.
Embodiment 3
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.312mol, powder is placed directly on the molybdenum sheet well heater, and silicon chip places about 1cm place, evaporation source top as substrate.When vacuum tightness reaches 8 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min makes electric current increase to 130A gradually to keep 15 minutes.At substrate surface yellow settling is arranged.It is that the length that is evenly distributed is 5-10 μ m that SEM observes sedimental surface topography, and diameter is the nanometer rod of 100-200nm, as Fig. 4.
Embodiment 4
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.08mol, powder is placed directly on the molybdenum sheet well heater, and another molybdenum sheet is that substrate places about 1cm place, evaporation source top.When vacuum tightness reaches 2 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min increases to behind the 130A electric current to keep 10 minutes gradually.The yellow sediment analysis demonstration that obtains on the molybdenum substrate has prepared the CdS nanometer rod.
Embodiment 5
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.125mol, the powder that obtains is placed directly on the molybdenum sheet well heater, another molybdenum sheet is that substrate places about 5mm place, evaporation source top.When vacuum tightness reaches 8 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 15min after making electric current increase to 130A gradually.The yellow sediment analysis demonstration that obtains on the molybdenum sheet has prepared the CdS nanometer rod.
Embodiment 6
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.08mol, the powder that obtains is placed directly on the molybdenum sheet well heater, monocrystalline silicon piece is that substrate places about 1cm place, evaporation source top.When vacuum tightness reaches 2 * 10
-2Behind the Pa, the closed evaporating cavity, advancing the speed with the electric current of 2.5A/min keeps 15min after making electric current increase to 130A gradually.The yellow settling that obtains on the silicon chip is the CdS nanometer rod that the present invention prepares.
Embodiment 7
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.08mol, the powder that obtains is placed directly on the molybdenum sheet well heater, monocrystalline silicon piece is that substrate places about 2cm place, evaporation source top.When vacuum tightness reaches 1.5 * 10
-2Behind the Pa, the closed evaporating cavity, advancing the speed with the electric current of 2.5A/min keeps 15min after making electric current increase to 140A gradually.The tawny settling that obtains on the silicon chip is the nanometer rod that the present invention prepares.
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.125mol, the powder that obtains is placed directly on the molybdenum sheet well heater, sapphire sheet places about 1cm place, evaporation source top as substrate.When vacuum tightness reaches 2 * 10
-2Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 10min after making electric current increase to 130A gradually.The yellow settling that obtains on the sapphire sheet is the nanometer rod that the present invention prepares.
Embodiment 9
Adopting high-purity CdS powder (99.5%) is raw material, the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.18mol, the powder that obtains is placed directly on the molybdenum sheet well heater, monocrystalline silicon piece is that substrate places about 1cm place, evaporation source top.When vacuum tightness reaches 9 * 10
-3Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 10min after making electric current increase to 120A gradually.The yellow settling that obtains on the silicon chip is the nanometer rod that the present invention prepares.
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal bismuth meal is a catalyzer, behind both ratio uniform mixing in 1mol:0.08mol, powder is placed directly on the molybdenum sheet well heater, and monocrystalline silicon piece is that substrate places about 1.5cm place, evaporation source top.When vacuum tightness reaches 2 * 10
-2Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 10min after making electric current increase to 150A gradually.The tawny settling that obtains on the silicon chip is the nanometer rod that the present invention prepares.
Embodiment 11
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal glass putty is a catalyzer, behind both ratio uniform mixing in 1mol:0.08mol, powder is placed directly on the molybdenum sheet well heater, and monocrystalline silicon piece is that substrate places about 1.5cm place, evaporation source top.When vacuum tightness reaches 2 * 10
-2Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 10min after making electric current increase to 150A gradually.The tawny settling that obtains on the silicon chip is the nanometer rod that the present invention prepares.
Embodiment 12
Adopting high-purity CdS powder (99.5%) is raw material, and the high pure metal glass putty is a catalyzer, behind both ratio uniform mixing in 1mol:0.15mol, powder is placed directly on the molybdenum sheet well heater, and monocrystalline silicon piece is that substrate places about 1cm place, evaporation source top.When vacuum tightness reaches 2 * 10
-2Behind the Pa, airtight evaporation cavity, advancing the speed with the electric current of 2.5A/min keeps 10min after making electric current increase to 140A gradually.The tawny settling that obtains on the silicon chip is the nanometer rod that the present invention prepares.
Claims (2)
1. the method for a catalyst-assisted and vacuum thermal evaporation CdS nano rod growth, it is characterized in that realizing: be 1 in molar ratio: 0.35-1: 0.01 ratio by following technological process, it with purity 99.5% CdS powder, being placed on the molybdenum sheet with bismuth meal or glass putty uniform mixing is in the resistive heating boat made of material, substrate is arranged at 3 millimeters of evaporation source tops to 3 centimeters, when the vacuum tightness of the vacuum-evaporation furnace cavity that includes resistive heating boat and substrate reaches 2 * 10
-2-2 * 10
-3Behind the Pa, airtight cavity, galvanization deposits 5 minutes-15 minutes for the 100-180A thermal evaporation, forms yellow or filemot settling on substrate, is the CdS nanometer rod.
2. the method for claim 1 is characterized in that, described substrate is ito glass, silica glass, silicon chip, sapphire, molybdenum sheet or nickel sheet.
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| 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 |
| CN101967681B (en) * | 2010-11-04 | 2014-10-22 | 新疆大学 | Method for growing zinc telluride (ZnTe) sextic symmetric multi-branched hierarchical nano-structure |
| CN101979723B (en) * | 2010-11-23 | 2012-07-04 | 东华大学 | Method for preparing p-type CdS nanowires |
| CN102263036A (en) * | 2011-07-01 | 2011-11-30 | 新疆大学 | Method for preparing CdS/ZnS nanometer wire heterojunction |
| CN102502787B (en) * | 2011-10-20 | 2013-11-20 | 南京大学 | Preparation method of multi-morphology Zn-Cd-S semiconductor nano composite material based on one-step controllable synthesis |
| CN102618269B (en) * | 2012-03-13 | 2016-06-29 | 浙江理工大学 | A kind of preparation method of CdS/Sn heterogeneous structural nano luminescent material |
| CN104659652B (en) * | 2015-02-13 | 2017-11-10 | 湖南大学 | A kind of wavy nanobelt and the nano laser array preparation method based on wavy nanobelt |
| CN104762608B (en) * | 2015-03-05 | 2017-07-25 | 湖南大学 | A kind of preparation method of the controllable horizontal CdS nano-wire arrays of the direction of growth |
| CN113735160B (en) * | 2021-07-30 | 2023-04-11 | 华南师范大学 | CdS branch structure guided and grown by using Sn nanowire as template and catalytic growth method and application thereof |
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