CN104916743A - Thermal evaporation method for preparing stoichiometric CdS thin film by using quantum dots as precursors - Google Patents
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- 239000002243 precursor Substances 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 title abstract description 3
- 239000000758 substrate Substances 0.000 claims abstract description 57
- 238000001704 evaporation Methods 0.000 claims abstract description 23
- 230000008020 evaporation Effects 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 15
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- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 claims description 9
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- 229910052793 cadmium Inorganic materials 0.000 description 1
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- 238000001755 magnetron sputter deposition Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
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Abstract
The invention discloses a thermal evaporation method for preparing a stoichiometric CdS thin film by using quantum dots as precursors. The thermal evaporation method comprises the following steps: putting a substrate after being washed on a sample holder (Emitech, K950X) of a thermal evaporimeter vacuum chamber; putting 0.1-0.3 g of the precursors with proper sizes in a W basket to close the chamber; pumping the chamber to be vacuum at 1.0*10<-3> to 1.0*10<-5> mbar under room temperature, and controlling the evaporation velocity by adjusting the current passing through the W basket; firstly, enabling the current to be slowly increased from 0 A to 6-10 A, and then waiting until the W basket becomes red; then, further enabling the current to be increased to 13-20 A and maintaining for 5-10 s, and finally enabling the current to be reduced to 0 A to complete the whole evaporation process. The thermal evaporation method has the advantages that a single-source thermal evaporation technology is adopted, and the complex control problem for each evaporation source in a multiple thermal evaporation technology is avoided; CdS QDS rich in element Cd are taken as precursors, the preparation method of the quantum dots is a room-temperature co-precipitation method, the method is simple, low in consumption and easy to operate, and the yield is extremely high.
Description
Technical field
The invention belongs to material chemistry technical field, particularly relating to a kind of quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film.
Background technology
Day by day in short supply along with the energy, the development and utilization of new forms of energy has become the study hotspot problem of people.Solar energy is a kind of cleaning and inexhaustible new forms of energy.Solar cell is a kind of device of direct applied solar energy.CdS is a kind of common semi-conducting material, and it has the wide direct band gap of about 2.4 eV.Wider band gap can allow most of visible ray to pass through, photoconductive effect and high electron affinity, makes CdS become a kind of Window layer and buffer layer material preferably in photoelectric device.
At present, different technology is usually used to prepare the CdS film with better crystallinity and balanced stoichiometric proportion.These technologies of preparing mainly comprise chemical bath deposition (CBD) method, spray pyrolysis method, chemical vapour deposition technique (CVD), electrochemical deposition method, magnetron sputtering method, physical vaporous deposition and thermal evaporation.In these technologies of preparing, thermal evaporation and the method based on solution have simple operation, low cost and other advantages and be applicable to can repeat on a large scale to prepare even CdS film.In above-mentioned two kinds of preparation methods, the technology of preparing based on solution is usually inevitably introduced some specific impurity and is entered film.Such as, from the compound of reaction solution or from the hydrogeneous of presoma or oxygen containing compound etc.Although thermal evaporation techniques can fundamentally avoid above-mentioned impurity, have different saturated vapour pressures between the component due to presoma, this just results through, and traditional thermal evaporation techniques still acquires a certain degree of difficulty to the semiconductive thin film obtaining near-stoichiometric.Such as, in CdS compound, the saturated vapor pressure of the saturated steam pressure ratio element S of Elements C d is little.Therefore, under room temperature substrate, adopt business CdS powder to carry out thermal evaporation as presoma and prepare CdS film, this can cause prepared CdS film to lack Cd element usually.But the performance of semiconductor device is often closely related with the stoichiometry of film, there is balanced stoichiometric CdS film and be more suitable for photovoltaic application.In addition, room temperature substrate is prepared film a lot of application, and when with organic film being such as substrate making corresponding device, organic substance can not resist high temperature.In addition, when also heating existing device for during various photoelectric device evaporation apex electrode.
In order on room temperature substrate, thermal evaporation has balanced stoichiometric CdS film, we can take several scheme.The first, application flash evaporation technology.It is by the presoma of powdery is transported to heat porcelain boat on carry out rapid evaporation, this with regard to need some extra plant equipment to disperse presoma.Another kind of scheme is application multi-source coevaporation technology.It is the temperature by adjusting each evaporation source, and replace CdS compound to control the stoichiometry of CdS film as presoma by Elements C d and element S, therefore this evaporation technique needs more equipment accurately to control the temperature of each evaporation source.In fact, low-temperature substrate builds rich Cd Elements C dS compound as single source presoma to evaporate CdS film be the most easily strategy.But obtain the presoma being rich in Cd element, existing method needs to adopt powdery CdS, and CdS powder need be heated in the hydrogen stream of 800 DEG C, and this just turn increases the complexity of preparation process.
Existing preparation method's existing defects, needs to improve.
Summary of the invention
The problem that the present invention will overcome is in CdS compound, because large than Cd element of the vapour pressure of S element, on room temperature substrate, if with the CdS powder of commercialization for precursor, the content of the CdS film prepared of application conventional thermal evaporation often S element is high and cause the stoichiometric proportion of film unbalance.Wherein, commercial CdS powder is the CdS body material that comparatively balances of stoichiometric proportion often.Replace CdS powder as presoma using the CdS quantum dot (QDs) synthesizing rich Cd element the invention provides a kind of simple method, on room temperature substrate, CdS film is prepared in thermal evaporation.In addition, CdS QDs is gathered into block does not need extra instrument to disperse, and more weak this of CdS QDs interaction being gathered into block will accelerate thermal evaporation process in itself.These are different from the situation of flash distillation or traditional thermal evaporation, and flash distillation or traditional thermal evaporation need the CdS powder of dispersion as presoma, and our presoma used does not need to carry out dispersion treatment.In the present invention, application CdS QDs is presoma, by one list source thermal evaporation process, and the stoichiometry of the CdS film prepared by effectively having recovered.
Problem to be solved by this invention is: provide a kind of with the CdS QDS of rich element Cd for precursor, on room temperature substrate, original position prepares the thermal evaporation of the CdS film of near-stoichiometric.
the present invention to the technical scheme that the problem that will solve is taked is:
Quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, and on room temperature substrate, the CdS quantum dot (QDs) applying rich Cd element is precursor material, is prepared the CdS film of near-stoichiometric by thermal evaporation original position.First, on the specimen holder substrate after cleaning being placed on thermal evaporation instrument vacuum chamber (Emitech, K950X).The presoma of suitable dimension, 0.1-0.3 g, is placed in W basket and closes this room.At room temperature, this room is pumped into 1.0 × 10
-3-1.0 × 10
-5the vacuum of mbar, controls evaporation rate by the electric current adjusted through W basket.First, electric current is slowly increased to 6-10 A from 0 A, then waits for until W basket becomes red.Then, electric current increases to 13-20 A further and keeps 5-10 s, and finally, reducing electric current is that 0 A is to complete whole evaporation process.
On room temperature substrate, the CdS quantum dot (QDs) applying rich Cd element is precursor material, is prepared the CdS film of near-stoichiometric by thermal evaporation original position.(Emitech, K950X) on the specimen holder that the substrate after cleaning is placed on thermal evaporation instrument vacuum chamber.The presoma of suitable dimension, 0.1-0.3 g, is placed in W basket and closes this room.At room temperature, this room is pumped into 1.0 × 10
-3-1.0 × 10
-5the vacuum of mbar, controls evaporation rate by the electric current adjusted through W basket.First, electric current is slowly increased to 6-10 A from 0 A, then waits for until W basket becomes red.Then, electric current increases to 13-20 A further and keeps 5-10 s, and finally, reducing electric current is that 0 A is to complete whole evaporation process.
Process of heating or lower the temperature is not carried out in the environment that substrate is put in room temperature.Wherein, it is especially particularly applicable to the substrate of those non-refractories in an experiment that substrate refers to tin indium oxide (ITO) electro-conductive glass, various metal pool sheet or any required backing material, such as organic substrate.
CdS QDs as the rich Cd element of thermal evaporation process presoma is application Co deposited synthesis, under room temperature and electromagnetic agitation, by nitric acid every Cd (NO3) the 24H2O aqueous solution (75 mL, 0.1-1 M) constantly instill in the vulcanized sodium Na2S aqueous solution (75 mL, 0.1-1 M).React and be just precipitated out immediately once, orange CdS QDs.After question response completes, the product centrifuge of precipitation is assisted centrifugal down and rinses up hill and dale with deionization (DI) water.Finally, the product-collecting of precipitation to a centrifuge tube, at 80-100
oCtemperature under dry 4-10 H-shaped become a bulk of faint yellow solid, subsequently faint yellow solid is divided into many fritters, prepare carry out subsequently thermal evaporation experiment.
Oil stain on substrate surface and dust is tentatively removed with the deionized water containing liquid detergent, this process ultrasonic auxiliary under carry out 10-50 minute after, by washed with de-ionized water and the deionized water ultrasonic cleaning 2-20 minute renewed again after ultrasonic 2-20 minute, circulation like this 1-5 time, then, this substrate is at ammoniacal liquor (NH3H2O), in the mixed solution of hydrogen peroxide (H2O2) and deionized water, volume ratio is 1:2:5, being heated to 80 oC-100 oC boils to not having bubble to produce, remove the organic contaminations that all are residual, afterwards, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes-30 minutes 10 minutes-30 minutes, circulation like this 3-5 time, finally, dry 3 hours-8 hours of 50-100oC in an oven.
of the present inventionthe CdS QDS of rich element Cd is that precursor refers to: the stoichiometry of (1) CdS quantum dot is unbalance; (2) in the majority with the content of Cd element; (3) preparation method of this quantum dot is room temperature coprecipitation, and method is simple, low consumption, easy to operate and productive rate is very high.
of the present inventionthermal evaporation CdS film refers to: (1) adopts single source technology; (2) with the commercial CdS powder that block CdS QDS is traditional for source substitutes, (3), without the need to any dispersing apparatus, further simplify preparation process, reduce preparation process.
of the present inventionroom temperature substrate refers in environment that substrate is put in room temperature and does not carry out process of heating or lower the temperature.Wherein, it is especially particularly applicable to the substrate of those non-refractories in an experiment that substrate refers to tin indium oxide (ITO) electro-conductive glass, various metal pool sheet or any required backing material, such as organic substrate.
of the present inventioncdS QDs as the rich Cd element of thermal evaporation process presoma is application Co deposited synthesis, it is characterized in that, under room temperature and electromagnetic agitation, by nitric acid every Cd (NO3) the 24H2O aqueous solution (75 mL, 0.1-1 M) constantly instill in the vulcanized sodium Na2S aqueous solution (75 mL, 0.1-1 M).React and be just precipitated out immediately once, orange CdS QDs.After question response completes, the product centrifuge of precipitation is assisted centrifugal down and rinses up hill and dale with deionization (DI) water.Finally, the product-collecting of precipitation to a centrifuge tube, at 80-100
oCtemperature under dry 4-10 H-shaped become a bulk of faint yellow solid, subsequently faint yellow solid is divided into many fritters, prepare carry out subsequently thermal evaporation experiment.
of the present inventionthe clean method of substrate, it is characterized in that, oil stain on substrate surface and dust is tentatively removed with the deionized water containing liquid detergent, this process ultrasonic auxiliary under carry out 10-50 minute after, by washed with de-ionized water and the deionized water ultrasonic cleaning 2-20 minute renewed again after ultrasonic 2-20 minute, circulation like this 1-5 time, then, this substrate is at ammoniacal liquor (NH3H2O), in the mixed solution of hydrogen peroxide (H2O2) and deionized water, volume ratio is 1:2:5, being heated to 80 oC-100 oC boils to not having bubble to produce, remove the organic contaminations that all are residual, afterwards, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes-30 minutes 10 minutes-30 minutes, circulation like this 3-5 time, finally, dry 3 hours-8 hours of 50-100oC in an oven.
beneficial effect of the present invention:
1, the present invention adopts single source thermal evaporation techniques, avoids the complicated problem to each evaporation source in polynary thermal evaporation techniques.
2, the present invention adopts the CdS QDS of rich element Cd to be precursor, and the preparation method of this quantum dot is room temperature coprecipitation, and method is simple, low consumption, easy to operate and productive rate is very high.Further, CdS QDs be gathered into block and in block the interphase interaction of CdS QDs more weak be conducive to Rapid Thermal evaporation but do not need extra instrument to disperse, therefore, further simplify preparation process, reduce preparation process.
3, the present invention carries out thermal evaporation on room temperature ito glass substrate, can be applied to a variety of occasion, is such as substrate or evaporation device termination electrode etc. with organic substance.
The present invention has great importance to the research carrying out CdS film base photoelectric device.
Accompanying drawing explanation
In Fig. 1, embodiment thermal evaporation prepare the apparatus structure schematic diagram of CdS film and CdS film, CdS QDS precursor dry before and pictorial diagram after drying.
Field emission microscope photo (FE-SEM) illustration of the CdS film prepared in Fig. 2, embodiment is the FE-SEM of this film compared with high-amplification-factor.
The X ray electron diffraction pattern (EDX) of precursor CdS QDs and corresponding CdS film in Fig. 3, embodiment.
Be Optical Electro-Chemistry (PEC) the battery structure schematic diagram built of base and the photoinduced carrier transport schematic diagram of transient state with CdS film in Fig. 4, embodiment.
The density of photocurrent of the CdS film base PEC battery device prepared in Fig. 5, embodiment and the ITO Conducting Glass of sky changes (I-t) curve in time.
Embodiment
For the ease of understanding the present invention, below in conjunction with the drawings and specific embodiments, the present invention will be described in more detail.Preferred embodiment of the present invention is given in accompanying drawing.But the present invention can realize in many different forms, is not limited to the embodiment described by this specification.On the contrary, provide the object of these embodiments be make the understanding of disclosure of the present invention more comprehensively thorough.
Unless otherwise defined, all technology of using of this specification and scientific terminology are identical with belonging to the implication that those skilled in the art of the present invention understand usually.The object of term used in the description of the invention in this specification just in order to describe specific embodiment is not for limiting the present invention.The term "and/or" that this specification uses comprises arbitrary and all combinations of one or more relevant Listed Items.
Below in conjunction with accompanying drawing and example, the present invention is further described.
Quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, and on room temperature substrate, the CdS quantum dot (QDs) applying rich Cd element is precursor material, is prepared the CdS film of near-stoichiometric by thermal evaporation original position.First, on the specimen holder substrate after cleaning being placed on thermal evaporation instrument vacuum chamber (Emitech, K950X).The presoma of suitable dimension, 0.1-0.3 g, is placed in W basket and closes this room.At room temperature, this room is pumped into 1.0 × 10
-3-1.0 × 10
-5the vacuum of mbar, controls evaporation rate by the electric current adjusted through W basket.First, electric current is slowly increased to 6-10 A from 0 A, then waits for until W basket becomes red.Then, electric current increases to 13-20 A further and keeps 5-10 s, and finally, reducing electric current is that 0 A is to complete whole evaporation process.
On room temperature substrate, the CdS quantum dot (QDs) applying rich Cd element is precursor material, is prepared the CdS film of near-stoichiometric by thermal evaporation original position.(Emitech, K950X) on the specimen holder that the substrate after cleaning is placed on thermal evaporation instrument vacuum chamber.The presoma of suitable dimension, 0.1-0.3 g, is placed in W basket and closes this room.At room temperature, this room is pumped into 1.0 × 10
-3-1.0 × 10
-5the vacuum of mbar, controls evaporation rate by the electric current adjusted through W basket.First, electric current is slowly increased to 6-10 A from 0 A, then waits for until W basket becomes red.Then, electric current increases to 13-20 A further and keeps 5-10 s, and finally, reducing electric current is that 0 A is to complete whole evaporation process.
Process of heating or lower the temperature is not carried out in the environment that substrate is put in room temperature.Wherein, it is especially particularly applicable to the substrate of those non-refractories in an experiment that substrate refers to tin indium oxide (ITO) electro-conductive glass, various metal pool sheet or any required backing material, such as organic substrate.
CdS QDs as the rich Cd element of thermal evaporation process presoma is application Co deposited synthesis, under room temperature and electromagnetic agitation, by nitric acid every Cd (NO3) the 24H2O aqueous solution (75 mL, 0.1-1 M) constantly instill in the vulcanized sodium Na2S aqueous solution (75 mL, 0.1-1 M).React and be just precipitated out immediately once, orange CdS QDs.After question response completes, the product centrifuge of precipitation is assisted centrifugal down and rinses up hill and dale with deionization (DI) water.Finally, the product-collecting of precipitation to a centrifuge tube, at 80-100
oCtemperature under dry 4-10 H-shaped become a bulk of faint yellow solid, subsequently faint yellow solid is divided into many fritters, prepare carry out subsequently thermal evaporation experiment.
Oil stain on substrate surface and dust is tentatively removed with the deionized water containing liquid detergent, this process ultrasonic auxiliary under carry out 10-50 minute after, by washed with de-ionized water and the deionized water ultrasonic cleaning 2-20 minute renewed again after ultrasonic 2-20 minute, circulation like this 1-5 time, then, this substrate is at ammoniacal liquor (NH3H2O), in the mixed solution of hydrogen peroxide (H2O2) and deionized water, volume ratio is 1:2:5, being heated to 80 oC-100 oC boils to not having bubble to produce, remove the organic contaminations that all are residual, afterwards, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes-30 minutes 10 minutes-30 minutes, circulation like this 3-5 time, finally, dry 3 hours-8 hours of 50-100oC in an oven.
Composition graphs 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5 do further explaination to the present invention,
In Fig. 1, embodiment thermal evaporation prepare the apparatus structure schematic diagram of CdS film and CdS film, CdS QDS precursor dry before and pictorial diagram after drying.
As can be seen from the pictorial diagram 1 of sample, the CdS film prepared by us is yellow transparent.And the stickup experiment of adhesive tape shows that this CdS film shows fabulous characterization of adsorption to ITO substrate.
Field emission microscope photo (FE-SEM) illustration of the CdS film prepared in Fig. 2, embodiment is the FE-SEM of this film compared with high-amplification-factor.
In fig. 2, fine and close CdS film surface is dispersed with a large amount of CdS nanometer rods equably.Can see further from illustration, diameter about 50 nm of this CdS nanometer rods, length are more than 200 nm, and they are overlapped, intersect and tightly packed.
The X ray electron diffraction pattern (EDX) of precursor CdS QDs and corresponding CdS film in Fig. 3, embodiment.
By EDX result, in CdS QDs, the atomic ratio of Elements C d and S is about 1.13:1, and the atomic ratio of CdS film interior element Cd and S is then about 1.03:1.As can be seen here, in CdS film, the content of Elements C d reduces and very close with the stoichiometric proportion of CdS compound, reaches our expected results.
Be Optical Electro-Chemistry (PEC) the battery structure schematic diagram built of base and the photoinduced carrier transport schematic diagram of transient state with CdS film in Fig. 4, embodiment.
The density of photocurrent of the CdS film base PEC battery device prepared in Fig. 5, embodiment and the ITO Conducting Glass of sky changes (I-t) curve in time.
(Fig. 5 a) raises with the photogenerated current density of empty ito glass substrate (Fig. 5 b) this PEC battery under light illumination instantaneously, and stop illumination then reducing immediately, this illustrates that this CdS film and ito glass substrate all have N-type conductive characteristic.Unlike, under the sensitization of CdS film, the photoelectric respone of ito glass substrate significantly strengthens, and this illustrates, CdS film has good sensibilization to ITO Conducting Glass, is a kind of effective photo cathode material.
embodiment
1, preparation:
(1) solution is configured: the nitric acid of 75 mL, 0.125 M is every Cd (NO3) the 24H2O aqueous solution and the vulcanized sodium Na2S aqueous solution.
(2) substrate is cleaned: selective oxidation indium tin (ITO) electro-conductive glass is as substrate.First, with the oil stain tentatively removed containing the washed with de-ionized water electroconductive ITO/glass substrate of liquid detergent on substrate surface and dust.This process ultrasonic auxiliary under carry out 30 minutes after, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes 10 minutes, so circulation 3 times.Then, this substrate is at ammoniacal liquor (NH3H2O), and in the mixed solution of hydrogen peroxide (H2O2) and deionized water, volume ratio is 1:2:5,80 oC, boils and do not remove all residual organic contaminations to having bubble to produce.Afterwards, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes 10 minutes, so circulation 3 times.Finally, dry 3 hours of 80 oC in an oven.
2, reactions steps:
(1) CdS QDs is synthesized
With the presoma of Co deposited synthesis CdS QDs as thermal evaporation process.Detailed process is as follows: under room temperature and electromagnetic agitation, by nitric acid in Cd (NO3) the 24H2O aqueous solution (75 mL, 0.125 M) constantly the instillation vulcanized sodium Na2S aqueous solution (75 mL, 0.125 M).React and be just precipitated out immediately once, orange CdS QDs.After question response completes, the product centrifuge of precipitation is assisted centrifugal down and rinses up hill and dale with deionization (DI) water.Finally, the product-collecting of precipitation to a centrifuge tube, 80
oat the temperature of C, dry 4 H-shapeds become a bulk of faint yellow solid, subsequently faint yellow solid are divided into many fritters and are placed on the thermal evaporation experiment carried out in tungsten (W) basket subsequently.
(2) thermal evaporation CdS film
Ito glass substrate after clean is placed on (Emitech, K950X) on the specimen holder of vacuum chamber.The presoma of suitable dimension, about 0.13 g, is placed in W basket and closes this room.In order to prepare CdS film by thermal evaporation, at room temperature, this room is pumped into 1.0 × 10
-3the vacuum of mbar, controls evaporation rate by the electric current adjusted through W basket.First, electric current is slowly increased to 6 A from 0 A, then waits for until W basket becomes red.Then, electric current increases to 13 A further and keeps 5 s, be secondly reduce electric current be that 0 A is to complete whole evaporation process.
3, sign and performance study: the CdS film of the yellow transparent prepared in ITO electro-conductive glass original position is taken out, crystal structure (XRD is carried out to it, Fig. 1), surface topography (FE-SEM, Fig. 2), stoichiometry (EDX, Fig. 3) and photoelectrochemical behaviour carry out characterizing (PEC battery, Fig. 4 and transient photocurrents response, Fig. 5).
The present invention has great importance to the exploitation of CdS film base photoelectric device and research.
It should be noted that, above-mentioned each technical characteristic continues combination mutually, is formed not in above-named various embodiment, is all considered as the scope that specification of the present invention is recorded; Further, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection range that all should belong to claims of the present invention.
Claims (4)
1. a quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, it is characterized in that, on room temperature substrate, the CdS quantum dot (QDs) applying rich Cd element is precursor material, the CdS film of near-stoichiometric is prepared by thermal evaporation original position, (Emitech on the specimen holder that the substrate after cleaning is placed on thermal evaporation instrument vacuum chamber, K950X), the presoma of suitable dimension, 0.1-0.3 g, be placed in W basket and close this room, at room temperature, this room is pumped into 1.0 × 10
-3-1.0 × 10
-5the vacuum of mbar, evaporation rate is controlled by the electric current adjusted through W basket, first, electric current is slowly increased to 6-10 A from 0 A, then wait for that then, electric current increases to 13-20 A further and keeps 5-10 s until W basket becomes red, finally, reducing electric current is that 0 A is to complete whole evaporation process.
2. a kind of quantum dot according to claim 1 is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, it is characterized in that, process of heating or lower the temperature is not carried out in the environment that substrate is put in room temperature, wherein, it is especially particularly applicable to the substrate of those non-refractories in an experiment that substrate refers to tin indium oxide (ITO) electro-conductive glass, various metal pool sheet or any required backing material, such as organic substrate.
3. a kind of quantum dot according to claim 1 is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, it is characterized in that, CdS QDs as the rich Cd element of thermal evaporation process presoma is application Co deposited synthesis, under room temperature and electromagnetic agitation, by nitric acid every Cd (NO3) the 24H2O aqueous solution (75 mL, 0.1-1 M) constantly instill the vulcanized sodium Na2S aqueous solution (75 mL, 0.1-1 M) in, react once, orange CdS QDs has just been precipitated out immediately, after question response completes, the product centrifuge of precipitation is assisted centrifugal down and rinses up hill and dale with deionization (DI) water, finally, the product-collecting of precipitation to a centrifuge tube, at 80-100
oCtemperature under dry 4-10 H-shaped become a bulk of faint yellow solid, subsequently faint yellow solid is divided into many fritters, prepare carry out subsequently thermal evaporation experiment.
4. a kind of quantum dot as requested described in 1 is the thermal evaporation that forerunner prepares near-stoichiometric CdS film, it is characterized in that, oil stain on substrate surface and dust is tentatively removed with the deionized water containing liquid detergent, this process ultrasonic auxiliary under carry out 10-50 minute after, by washed with de-ionized water and the deionized water ultrasonic cleaning 2-20 minute renewed again after ultrasonic 2-20 minute, circulation like this 1-5 time, then, this substrate is at ammoniacal liquor (NH3H2O), in the mixed solution of hydrogen peroxide (H2O2) and deionized water, volume ratio is 1:2:5, being heated to 80 oC-100 oC boils to not having bubble to produce, remove the organic contaminations that all are residual, afterwards, by washed with de-ionized water and the deionized water ultrasonic cleaning that renews again after ultrasonic 10 minutes-30 minutes 10 minutes-30 minutes, circulation like this 3-5 time, finally, dry 3 hours-8 hours of 50-100oC in an oven.
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| CN103736500A (en) * | 2013-12-23 | 2014-04-23 | 清华大学 | Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof |
| CN103882514A (en) * | 2014-02-28 | 2014-06-25 | 湖南大学 | Semiconductor CdS/CdSSe heterojunction nanowire and preparation method thereof |
| CN105177499A (en) * | 2015-05-22 | 2015-12-23 | 许昌学院 | Thermal evaporation method for preparation of near-stoichiometric CdS film with quantum dot as precursor |
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| CN103736500A (en) * | 2013-12-23 | 2014-04-23 | 清华大学 | Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof |
| CN103882514A (en) * | 2014-02-28 | 2014-06-25 | 湖南大学 | Semiconductor CdS/CdSSe heterojunction nanowire and preparation method thereof |
| CN105177499A (en) * | 2015-05-22 | 2015-12-23 | 许昌学院 | Thermal evaporation method for preparation of near-stoichiometric CdS film with quantum dot as precursor |
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