CN103289683A - Preparation method of CdS quantum dot nanometer composite film cladded by SiO2 - Google Patents
Preparation method of CdS quantum dot nanometer composite film cladded by SiO2 Download PDFInfo
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- CN103289683A CN103289683A CN2013101672459A CN201310167245A CN103289683A CN 103289683 A CN103289683 A CN 103289683A CN 2013101672459 A CN2013101672459 A CN 2013101672459A CN 201310167245 A CN201310167245 A CN 201310167245A CN 103289683 A CN103289683 A CN 103289683A
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Abstract
The invention relates to a preparation method of a CdS quantum dot nanometer composite film cladded by SiO2 through a sol gelation process, belonging to the technical field of preparation of semiconductor nanometer composite films. The cladded CdS quantum dot has excellent dispersity and the light emitting efficiency and corrosion resistance are improved. The preparation method specifically comprises the steps of: utilizing cadmium nitrate, sodium sulfide and TGA (thioglycollic acid) as main raw materials to prepare a high-concentration CdS quantum dot solution through a chemical water bath method; utilizing TEOS (tetraethyl orthosilicate), absolute ethyl alcohol, concentrated hydrochloric acid and deionized water as raw materials to prepare SiO2 sol; and then, mixing the sole with the quantum dot according to a certain mol ratio, spin coating to obtain the CdS quantum dot nanometer composite film cladded by SiO2; and drying the film sample, putting the film sample in a tubular annealing furnace, and annealing the film sample in N2 atmosphere to obtain the CdS quantum dot nanometer composite film cladded by SiO2. The CdS nanometer granules are compounded with other substrates to beneficially improve the photoelectric property of CdS and expand the application field of a CdS material.
Description
Technical field
The present invention relates to a kind of Prepared by Sol Gel Method SiO that utilizes
2The method of the CdS quantum dot nano laminated film that coats belongs to the semiconductor nanometer compound film preparing technical field.
Background technology
Sol-gel method is a kind of nanometer grain preparation method commonly used, mainly is used in the earliest in pottery and the glasswork.But, after utilizing these class methods to make nano particle both at home and abroad, it is received publicity again.Sol-gel method mainly comprises several aspects, at first precursor (being metal-salt or inorganic salt) is dissolved in the solvent (organic solvent or water); Solute is hydrolyzed in solvent or alcoholysis forms colloidal sol gradually; Colloidal sol forms gel through polycondensation then; At last gel is heat-treated (dry, roasting), thereby make nano particle.
CdS is a kind of typical II-VI family semi-conductor, and its energy gap is 2.42 eV, has wideer energy gap.The CdS quantum dot is a kind of important semi-conductor nano particles then, has good optical performance and surface modificability, can be widely used in the fields such as light emitting devices, laser, biological detection and analysis of fluorescence labeling.But under the optical excitation condition since photo-generated carrier easily compound its quantum yield that makes is lower, and the photoresponse of CdS is limited in scope, and limited it in the application of photocatalysis field.Because SiO
2The surface has the silicon hydroxyl, thereby it is suitable for the finishing of material, SiO very much
2After being coated on outside the nano material, both can having made material have good dispersiveness and prevent its reunion, and also can make nanoparticle have better erosion resistance, coated Si O
2The luminous efficiency of back CdS also can be greatly improved.
The CdS quantum dot has wideer absorbing wavelength band, higher emissive porwer and light stability preferably, not only can control emission and absorbing wavelength by regulating self size, to satisfy different solar cells to the absorption of light, and because its absorption spectrum and emission spectrum are overlapping less, enough Stokes shifts being arranged to reduce the heavily absorption of light beam, increased the incident light subnumber, is a kind of more satisfactory fluorescence luminescent material.SiO
2Has very high transmissivity, very low scattered power, SiO
2Be coated on the CdS quantum dot effect that play the protection quantum dot, improves luminous efficiency.CdS quantum dot nano laminated film is as the nano compound film of economical and efficient, at photocatalyst material, and photoelectric device, the aspects such as conversion layer as under the fluorescent solar condensing apparatus also have wide practical use.Have very high transmitance, the photoexcitation peak value of laminated film and its absorption peak exist a Stokes displacement energy to improve the spectrum efficiency of conversion, improve the assimilated efficiency of solar cell.Under the situation that does not change device material and structure, convert solar spectrum to frequency range that existing device has higher absorption, when improving battery conversion efficiency, can effectively reduce production costs.Introduce nano material, utilize its higher photochemical stability, reach the purpose of accurate spectral conversion.
At present, the preparation method of CdS quantum dot nano film mainly is the chemical bath method.There is not patent definitely to put down in writing and uses sol-gel method, preparation SiO
2The report of the CdS quantum dot nano laminated film that coats.
Summary of the invention
The purpose of this invention is to provide a kind of SiO
2The preparation method of the CdS quantum dot nano laminated film that coats.For this reason, use cadmium nitrate, sodium sulphite, tetraethoxy (TEOS), dehydrated alcohol and thioglycolic acid (TGA) they are main raw material, and a kind of sol-gel method is provided, preparation SiO
2The CdS quantum dot nano laminated film that coats, it has following technological process and step:
1) SiO
2Colloidal sol: in reactor, at first use TEOS, dehydrated alcohol, concentrated hydrochloric acid, deionized water are raw material, with TEOS and dehydrated alcohol certain volume ratio, namely mix with volume ratio=1:1, carry out magnetic agitation under the normal temperature; In addition, dripping concentrated hydrochloric acid in deionized water, regulate the pH value of requirement that this solution reaches, is 2 ~ 5, and volume ratio (being above-mentioned TEOS and dehydrated alcohol) the same volume ratio of tool with this deionized water hydrochloric acid soln and TEOS is 1:1; The mixed system for the treatment of dehydrated alcohol and TEOS stirs certain hour, after being 30min, reactor is put into the heated water bath magnetic stirrer, under certain temperature, general temperature is set at 50 ~ 70 ℃, drips the deionized water hydrochloric acid soln of above-mentioned preparation while stirring, stir the some time, after 2 ~ 8 hours, reaction finishes, SiO
2Colloidal sol is stand-by;
2) CdS quantum dot solution preparation: in another reactor, with cadmium nitrate, sodium sulphite, TGA is main raw material, takes by weighing cadmium nitrate and sodium sulphite that mol ratio is 1:1 ~ 1:8, is dissolved in respectively in the deionized water, it is stirred again, and solute is fully dissolved; Add a certain amount of TGA in cadmium nitrate solution, adopt both certain mol proportions, its mol ratio is that following scope is TGA:Cd
2+=1.5:1 ~ 3:1; After adding TGA, the cadmium nitrate solution of clarification becomes oyster white rapidly originally, slowly drips strong aqua to this solution again and becomes again till the clarification; With TGA, the mixed system at reactor of cadmium nitrate and ammoniacal liquor is put into the water-bath magnetic stirring apparatus, drips sodium sulfide solution under the constant temperature while stirring, and wherein design temperature is 50 ~ 70 ℃, and reaction system is variable color gradually, by the initial faint yellow glassy yellow that becomes.Water-bath for some time, the time is controlled at 20min ~ 60min, and CdS quantum dot concentration is 0.1mol/L; The high concentrations of Cd S quantum dot solution of preparation, place normal temperature 24 h after, adopt acetone and deionized water carries out repeatedly centrifugal to it and clean;
3) CdS quantum dot nano laminated film processed: the CdS quantum dot with obtaining after the above-mentioned eccentric cleaning process, be dissolved in the small quantity of deionized water, according to different Cd:Si mol ratios, add last 1) prepared SiO
2Colloidal sol, and carry out magnetic agitation, the time is 1h; At last, by spin-coating method, by with per minute rotation more than or equal under 700 rotary speeds, can be under 700～2000rpm, the colloidal sol of reaction gained is clean on glass what handled, carry out the whirl coating film forming; The film sample that makes is put into loft drier, and regularly dry, the time is 10min, sends in the tubular type annealing furnace, at N again
2Carry out the annealing of timing constant temperature under the middle protection, temperature is 100 ℃ ~ 200 ℃, and annealing time is 10min ~ 100min, can obtain SiO
2The CdS quantum dot nano laminated film that coats.
Conclude the present invention, i.e. SiO
2The preparation of the CdS quantum dot nano laminated film that coats at first is to be equipped with the CdS quantum dot with the chemical bath legal system, its again with SiO
2Colloidal sol is according to certain C d:Si mixed in molar ratio, and behind the one-tenth mixed sols, spin-coating film is dried and obtained SiO
2The CdS quantum dot nano laminated film that coats, and to preparation SiO
2The CdS quantum dot nano laminated film that coats has carried out sign and the performance analysis of pattern.
Description of drawings
The atomic force microscope figure of Fig. 1 CdS quantum dot nano laminated film.
The X-ray diffractogram of Fig. 2 CdS quantum dot nano film.
The UV, visible light light transmission rate collection of illustrative plates of CdS quantum dot nano laminated film under the different Cd:Si mol ratio of Fig. 3 condition.
Embodiment
Embodiment
1, the cleaning of glass substrate:
Simple glass is carried out surface cleaning processing work, put into the Triton aqueous solution, acetone soln, raw spirit solution and deionized water successively each ultrasonic 15 minutes, then glass substrate is dried.
2, SiO
2The preparation of colloidal sol:
With TEOS, dehydrated alcohol, concentrated hydrochloric acid, deionized water are raw material, and TEOS and dehydrated alcohol with the mixed of volume ratio=1:1, are carried out magnetic agitation at normal temperatures; In addition, in deionized water, drip concentrated hydrochloric acid, regulate this hydrochloric acid soln pH value and be 2-3, after treating the mixed system stirring 30min of dehydrated alcohol and TEOS, its mixed system is put into the heating in water bath magnetic stirrer, and temperature is 50 ℃, drips the hydrochloric acid soln of above-mentioned preparation while stirring, stir after 2 hours, reaction finishes stand-by;
3, the chemical bath legal system is equipped with high concentrations of Cd S quantum dot solution:
With cadmium nitrate, sodium sulphite, TGA is main raw material, takes by weighing cadmium nitrate and sodium sulphite that mol ratio is 1:2, is dissolved in the deionized water respectively, and it is stirred, and makes it abundant dissolving; In cadmium nitrate solution, add a certain amount of TGA, adopting both mol ratios is TGA:Cd
2+=1.5:1.Slowly drip strong aqua, become clarification to this solution till; With TGA, the mixed system of cadmium nitrate and ammoniacal liquor is put into the heating in water bath magnetic stirring apparatus, and temperature is 60 ℃, drips sodium sulfide solution while stirring; Water-bath time 30min.With the CdS quantum dot solution for preparing, place normal temperature 24h after, adopt acetone and deionized water carries out repeatedly centrifugal to it and clean.
4, revolve glue and make laminated film:
According to Cd:Si mol ratio 1:8, with the SiO of CdS quantum dot for preparation before adding
2Carry out magnetic agitation 1H in the colloidal sol.By spin-coating method the colloidal sol that reacts gained is carried out the whirl coating film forming under the 900r/min condition.The film sample that makes is put into the dry 10min of loft drier, send into then in the tubular type annealing furnace, at N
2In anneal, temperature is 100 ℃, annealing time is 30min, can obtain SiO
2The CdS quantum dot nano laminated film that coats.
5, laminated film characterizes: preparation SiO
2The CdS quantum dot nano laminated film that coats, (AFM) observes its pattern with atomic force microscope, and the reflection laminated film is more smooth; X-ray diffractogram (XRD) characterizes, and SiO is described
2And the CdS phase structure exists simultaneously; Under different Cd:Si mol ratio 1:1～1:300 condition, UV, visible light light transmission rate to CdS quantum dot nano laminated film, carried out performance analysis, its UV, visible light light transmission rate (Fig. 3) also increases successively, when wavelength〉during 300nm, light transmission rate is corresponding successively respectively, from nearly 30% to being higher than 80%, for the fluorescent solar condensing apparatus transmitance high as far as possible to visible light wave range, when Si:Cd mol ratio ratio is about below 25, it is 60% comparatively appropriate when above that the whole transmitance of CdS quantum dot nano laminated film has reached.
CdS quantum dot nano laminated film, it is as the nano compound film of economical and efficient, and at photocatalyst material, photoelectric device etc. aspect has a wide range of applications.Simultaneously, preparation method's of the present invention success, the characteristics of this nano compound film preparation work due to: be equipped with CdS quantum dot method maturation, simple as the chemical bath legal system, the CdS quantum dot size of preparation is unified; The CdS quantum dot nano laminated film of Prepared by Sol Gel Method, surperficial SiO
2The CdS even particle distribution that coats, the phenomenon that film surface was tied and was adsorbed in the macromolecular mass coacervation does not appear in the granular size homogeneous; The surface particle of this laminated film, it is comparatively tight to arrange, and formed film surface is more smooth; SiO
2Adhering to of the CdS quantum dot nano laminated film that coats and substrate is powerful higher, and higher transmittance and good optical performance are arranged; This technical equipment is simple, easy handling, good reproducibility.
Claims (5)
1. SiO
2The preparation method of the CdS quantum dot nano laminated film that coats is characterized in that being equipped with CdS quantum dot, SiO then with the chemical bath legal system
2Colloidal sol mixes with the CdS quantum dot, and the colloidal sol spin-coating film obtains SiO
2The CdS quantum dot nano laminated film that coats, it has following technological process and step:
1) SiO
2Colloidal sol: in reactor, at first use the TEOS(tetraethoxy), dehydrated alcohol, concentrated hydrochloric acid, deionized water are raw material, with TEOS and dehydrated alcohol with certain volume than mixing, carry out magnetic agitation under the normal temperature; In addition, dripping concentrated hydrochloric acid in deionized water, regulate this solution and reach requirement pH value, is above-mentioned TEOS and dehydrated alcohol with this deionized water hydrochloric acid soln and TEOS() the same volume ratio of tool; After the mixed system for the treatment of dehydrated alcohol and TEOS regularly stirs, reactor is put into the heated water bath magnetic stirrer, under constant temperature, drip the deionized water hydrochloric acid soln of above-mentioned preparation while stirring, stirred some hours, become SiO
2Colloidal sol is stand-by;
2) CdS quantum dot solution preparation: in another reactor, with cadmium nitrate, sodium sulphite, TGA is main raw material, takes by weighing cadmium nitrate and sodium sulphite that mol ratio is 1:1 ~ 1:8, is dissolved in respectively in the deionized water, it is stirred again, and solute is fully dissolved; In cadmium nitrate solution, add a certain amount of TGA, adopt both certain mol proportions, add TGA again after, the cadmium nitrate solution of clarification becomes oyster white rapidly originally, slowly drips strong aqua to this solution again and becomes again till the clarification; With TGA, the mixed system at reactor of cadmium nitrate and ammoniacal liquor is put into the water-bath magnetic stirring apparatus, drips sodium sulfide solution under the constant temperature while stirring, and reaction system is variable color gradually, by the initial faint yellow glassy yellow that becomes.Water-bath for some time, obtaining CdS quantum dot concentration is 0.1mol/L; Be placed in the normal temperature behind 24 h, adopt acetone and deionized water carries out repeatedly centrifugal to it and clean;
3) CdS quantum dot nano laminated film processed: the CdS quantum dot with obtaining after the above-mentioned eccentric cleaning process, be dissolved in the small quantity of deionized water, according to different Cd:Si mol ratios, add last 1) prepared SiO
2Colloidal sol, and carry out magnetic agitation, the time is 1h, again by with the per minute rotation more than or equal under 700 rotary speeds, will be to the colloidal sol of reaction gained, clean on glass what handled, carry out the whirl coating film forming; After the film sample drying, be fed in N
2The tubular type annealing furnace of middle protection is annealed under the timing constant temperature, can obtain SiO
2The CdS quantum dot nano laminated film that coats.
2. according to the preparation SiO described in the claim 1
2The method of the CdS quantum dot nano laminated film that coats is characterized in that preparing SiO
2During colloidal sol, TEOS and dehydrated alcohol with the mixed of volume ratio=1:1, are carried out magnetic agitation.Drip concentrated hydrochloric acid in deionized water, regulating this hydrochloric acid soln pH value is 2 ~ 5, and the volume ratio of deionized water and TEOS is similarly 1:1.After treating the mixed system stirring 30min of dehydrated alcohol and TEOS, put into the heated water bath magnetic stirrer, design temperature is 50 ~ 70 ℃, drips above-mentioned aqueous hydrochloric acid, stirs 2 ~ 8 hours.
3. according to the preparation SiO described in the claim 1
2The method of the CdS quantum dot nano laminated film that coats is characterized in that adopting the preparation of high concentrations of Cd S quantum dot solution, and the cadmium nitrate that takes by weighing earlier and sodium sulphite mol ratio are 1:1 ~ 1:8.In cadmium nitrate solution, add a certain amount of TGA, adopt both mol ratio TGA:Cd
2+=1.5:1 ~ 3:1.With TGA, the mixed system of cadmium nitrate and ammoniacal liquor is put into the heating in water bath magnetic stirring apparatus, and design temperature is 50 ~ 70 ℃, and the reaction times is 20min ~ 60min.
4. according to the preparation SiO described in the claim 1
2The method of the CdS quantum dot nano laminated film that coats is characterized in that CdS quantum dot and SiO
2What colloidal sol mixed can be according to different Cd:Si mol ratios, and the magnetic agitation time is 1h, spin-coating method to the colloidal sol of reaction gained under 700r/min ~ 2000r/min condition, clean whirl coating film forming on glass, sample is put into the dry 10min of loft drier, at N
2In anneal, temperature is 100 ℃ ~ 200 ℃, annealing time is 10min ~ 100min.
5. according to claim 1, the preparation SiO described in 4
2The method of the CdS quantum dot nano laminated film that coats is characterized in that CdS quantum dot and SiO
2The Cd:Si mol ratio that colloidal sol mixes can be at 1:1 ~ 1:300 category, and its UV, visible light light transmission rate also increases successively, when wavelength〉during 300nm, light transmission rate is corresponding successively respectively, from nearly 30% to being higher than 80%, for the fluorescent solar condensing apparatus transmitance high as far as possible to visible light wave range, when Si:Cd mol ratio ratio is about below 25, it is 60% comparatively appropriate when above that the whole transmitance of CdS quantum dot nano laminated film has reached.
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| 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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| CN105177499B (en) * | 2015-05-22 | 2018-02-06 | 许昌学院 | A kind of quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film |
| 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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Application publication date: 20130911 |