CN102925141A - Preparation of water-soluble CdS:Ag doped nano-crystalline through microwave method - Google Patents
Preparation of water-soluble CdS:Ag doped nano-crystalline through microwave method Download PDFInfo
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- CN102925141A CN102925141A CN 201210410745 CN201210410745A CN102925141A CN 102925141 A CN102925141 A CN 102925141A CN 201210410745 CN201210410745 CN 201210410745 CN 201210410745 A CN201210410745 A CN 201210410745A CN 102925141 A CN102925141 A CN 102925141A
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Abstract
The invention discloses a method and device for synthesizing a CdS:Ag doped nano-crystalline material in the chemical industry fields and aims to provide a preparation method, which is environment-friendly, simple, easy, low in energy consumption and free from injury of operators. The method comprises the following steps of: preparing a cadmium source, a doped cadmium source and a sulphur source; mixing the doped cadmium source with the sulphur source; and promoting growth of doped CdS:Ag nano-crystalline through microwave. Doped CdS:Ag nano-crystalline nucleus in a precursor rapidly grows under the action of microwave; doped CdS:Ag nano-crystalline solutions of different fluorescent wavelengths are obtained within different action times; the solutions are clear and transparent; the fluorescence emission spectrum coverage range is wide; the quantum efficiency is high; the powdered CdS:Ag doped nano-crystalline material is obtained after freeze-drying; and the CdS:Ag doped nano-crystalline material has better chemical stability and light stability.
Description
Technical field
The invention belongs to a kind of aqueous phase preparation method of doping type CdS:Ag semiconductor nanocrystal materials, particularly the fluorescent emission wavelength covers preparation method and the synthesizer of the CdS:Ag nanocrystal of whole visible region.
Background technology
Cadmium Sulfide (CdS) is a kind of semiconductor material of important quantum yield occurred frequently.In recent years, be that stablizer is studied in the synthetic nanocrystalline beginning of high-quality CdS of water with sulfhydryl compound, recently research finds that CdS is a kind of extremely promising semiconductor material aspect opto-electronic conversion.But adopt the stable nanocrystalline fluorescent emission peak position of CdS of sulfhydryl compound mainly to concentrate on 420 ~ 510 nm, be difficult to expand to whole visibility region.Therefore limited the nanocrystalline development of CdS.
Can change the nanocrystalline photoluminescent property of CdS by doping techniques, but the method generally is confined to the organic synthesis field, mainly be with manganese and copper metal ion be entrained in CdS nanocrystalline in, although changed to a certain extent the nanocrystalline emission peak positions of CdS, but variable range is very narrow, generally is no more than 20 nm.And the method for organic phase doping, complex process, conditional request is harsh, and toxicity is very large, and is large to operator's health hazardness, is difficult to synthesize in large quantity, can't realize industrialization.The water doping techniques can't change the nanocrystalline photoluminescent property of CdS at present, and major cause is surface metal ion, for example: cupric ion, with sulfhydryl compound generation redox reaction, have a strong impact on the stability of solution, thereby cause fluorescence decay, and do not have suitable method to improve.Key in herein background technology and describe paragraph.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency that overcomes background technology, by microwave technology at the nanocrystalline middle doping Ag of CdS
+, changing the nanocrystalline photoluminescent property of CdS, major technique comprises: stable, the microwave generator of even microwave, Ag are provided
+Doping-sequence and position, and the selection of stablizer are realized synthetic fast.To operator's health substantially without the method for synthetic CdS:Ag nanocrystalline material of harm.
The present invention adopts following technical scheme to be achieved in the method for synthetic CdS:Ag nanocrystalline material.It comprises the step of following order: 1) water miscible cadmium salt, sulfhydryl compound and water are put into three-necked flask, at room temperature magnetic stirring apparatus stirs,, transfer to alkalescence, the pH value is set(ting)value, obtains stable cadmium source; 2) in 100 mL water, add 5 mL, 0.01 molL
-1Ag
+, after the dissolving, add 1.25 μ L thiohydracrylic acids fully, pour in the constant pressure funnel that is installed in the three-necked flask upper right side after mixing; 3) with 0.2 molL
-1Na
2S solution 1 mL puts into and is installed in three-necked flask upper left side funnel, is stable sulphur source solution; 4) open the right side discharge gate, lentamente silver-colored source solution is dropped to completely, close the right side discharge gate, cadmium source solution obtains mixing under the normal temperature; 5) open the discharge gate of control funnel switch, under magnetic agitation, slowly drip sulphur source solution, be controlled at about 5 minutes and dropwise, close discharge gate, after continuing to stir half an hour, the nanocrystalline precursor water solution of CdS:Ag obtains mixing; 6) Doped nanocrystal solution is transferred in the quartzy microwave reaction pipe, heat-up time and temperature are set, under microwave action, the CdS:Ag nanocrystal solution obtains mixing; 7) adopt freeze drying technology to remove unreacted presoma, obtain the pressed powder of CdS:Ag nanocrystalline material.
Described in the technical scheme: the cadmium salt in the solution is water miscible salt, can select cadmium nitrate, Cadmium chloride fine powder, cadmium acetate or cadmium perchlorate, dispersion agent can be selected thiohydracrylic acid, Thiovanic acid or halfcystine, cadmium salt and dispersion agent mol ratio are 1:2 ~ 5, the cadmium salt that in water, dissolves and dispersion agent, transfer to alkalescence, the pH value is 9 ~ 13, obtains stable cadmium source; The Ag that mixes
+Can select silver nitrate solution, add simultaneously thiohydracrylic acid, form title complex, after mix in the cadmium source, form the cadmium source solution that mixes; The sulphur source is for containing S
2-The aqueous solution, can select sodium sulphite, potassium sulphide or hydrogen sulfide; The nanocrystalline presoma of CdS:Ag is that sulphur source and doping cadmium source are mixed equably under agitation condition and obtain, and add-on is Cd in molar ratio
2+: S
2-=3 ~ 5:1, this forerunner's liquid solution is the dopen Nano nucleus, for the growth that doping CdS:Ag is nanocrystalline is supplied raw materials; In the case of necessary, if when the gas in the three-necked flask makes air pressure be higher than normal atmosphere, can reduce pressure by discharge valve, guarantee that rate of addition is stable.It is 100 ℃ that the microwave temperature is set, and be 20 ~ 100 minutes heat-up time.When size is set in nanocrystalline the growing into of CdS:Ag, show its distinctive fluorescent characteristic, characterize by fluorescence analyser; Adopt freeze drying technology to remove unreacted presoma, freeze-drying time was controlled in 12 hours, and the doping CdS:Ag nanocrystalline material after the freeze-drying is placed in the vacuum drier, and room temperature is placed and got final product.
Beneficial effect of the present invention:
1) method of this synthesizing blender CdS:Ag nanocrystalline material and conventional production methods contrast, present method preparation cost is low, good reproducibility, toxicity are low, and a kind of method of practicality is provided for the commercialization of product;
2) this synthetic method is compared with traditional method, and speed is faster, efficient is higher, energy consumption is lower;
Doping CdS:Ag nanocrystal solution clarification after synthetic, transparent has good photoluminescent property, and room temperature is placed, can continued growth, easily preservation.
Description of drawings
Fig. 1 is the synthesizer of the synthetic nanocrystalline precursor solution of CdS:Ag:
Preparation facilities figure, wherein: 1. three-necked flask, with the there-necked flask of magnetic agitation, 2. constant pressure funnel, 3. discharge gate, 4. airway.
Specific implementation method
Below in conjunction with drawings and Examples the present invention is described in further detail, rather than will be with this limitation of the present invention.
Consult Fig. 1, described synthesizer is comprehensive parts, it comprises the magnetic stirring apparatus that is placed on the worktable, be placed on the three-necked flask in the magnetic stirring apparatus cavity, be installed in the constant pressure funnel of both sides, three-necked flask top, the discharge gate that install the airway of plug-in mounting and funnel bottom directly over the constant pressure funnel.Wherein: when discharge valve was opened, the gas that assurance three-necked flask internal reaction produces was discharged smoothly and is reduced pressure, and also can add materials, and when discharge valve cuts out, can prevent that air from entering; The speed that drips silver ion solution can be controlled by control right side discharge gate opening degree in cadmium source in the constant pressure funnel, when the right side discharge gate is closed, can prevent that air from entering; Rate of addition can be controlled by control discharge gate opening degree in sulphur source in the funnel, when discharge gate is closed, can prevent that air from entering.
Embodiment one:
1) preparation cadmium source
Get 100 mL water and put into three-necked flask, dissolve again 29 mg CdCl
22.5H
2O and 25 μ L Thiovanic acids are transferred pH to 9 with NaOH in water, form stable cadmium metal complex compound, and cadmium salt and dispersion agent mol ratio are 1:2.5.
2) preparation doping cadmium source
In 100 mL water, add 5 mL, 0.01 molL
-1Ag
+, after the dissolving, add 1.25 μ L thiohydracrylic acids fully, mix, pour in the constant pressure funnel that is installed in the three-necked flask upper right side, for subsequent use;
3) preparation sulphur source
Take by weighing 156 mg Na
2The S solid is dissolved in the 10 mL water, gets 1 mL Na
2S solution is poured in the constant pressure funnel of three-necked flask upper left side;
4) open right side discharge gate on the constant pressure funnel, lentamente with Ag
+Solution is added drop-wise in the solution of cadmium source, and dripping quantity is Cd in molar ratio
2+: Ag
+=10:1 closes the right side discharge gate, and cadmium source solution obtains mixing;
5) open left side discharge gate on the constant pressure funnel, lentamente with Na
2S solution is added drop-wise in the solution of doping cadmium source, stirs after 30 minutes, closes the left side discharge gate, and the nanocrystalline presoma of CdS:Ag obtains mixing;
6) microwave heating temperature being set is 100 ℃, be 30 minutes heat-up time, precursor solution is poured in the crystal reaction tube, treat the microwave stopped heating, take out crystal reaction tube, after being down to room temperature, adopt fluorescence analyser to characterize its photoluminescent property, the CdS:Ag nanocrystal solution that to obtain a kind of fluorescent emission wavelength be 540 nm;
7) adopt Freeze Drying Equipment to carry out frozen dried doping CdS:Ag nanocrystal solution, the time of freeze-drying was controlled within 12 hours, and lyophilized powder is placed in the vacuum drier, preserves under the room temperature.
Embodiment two:
1) preparation cadmium source
Get 100 mL water and put into three-necked flask, dissolve again 290 mg CdCl
22.5H
2O and 250 μ L Thiovanic acids are transferred pH to 9 with NaOH in water, form stable cadmium metal complex compound, and cadmium salt and dispersion agent mol ratio are 1:2.5;
2) preparation doping cadmium source
In 100 mL water, add 5 mL, 0.1 molL
-1Ag
+, after the dissolving, add 12.5 μ m MPA fully, mix, pour in the constant pressure funnel that is installed in the three-necked flask upper right side, for subsequent use;
3) preparation sulphur source
Take by weighing 1.56 g Na
2The S solid is dissolved in the 10 mL water, gets 1 mL Na
2S solution is poured in the constant pressure funnel of three-necked flask upper left side;
4) open right side discharge gate on the constant pressure funnel, lentamente with Ag
+Solution is added drop-wise in the solution of cadmium source, and dripping quantity is Cd in molar ratio
2+: Ag
+=10:1 closes the right side discharge gate, and cadmium source solution obtains mixing;
5) open left side discharge gate on the constant pressure funnel, lentamente with Na
2S solution is added drop-wise in the solution of doping cadmium source, stirs after 30 minutes, closes the left side discharge gate, and the nanocrystalline presoma of CdS:Ag obtains mixing;
6) microwave heating temperature being set is 100 ℃, be 30 minutes heat-up time, precursor solution is poured in the crystal reaction tube, treat the microwave stopped heating, take out crystal reaction tube, after being down to room temperature, adopt fluorescence analyser to characterize its photoluminescent property, the CdS:Ag nanocrystal solution that to obtain a kind of fluorescent emission wavelength be 540 nm;
7) adopt Freeze Drying Equipment to carry out frozen dried doping CdS:Ag nanocrystal solution, the time of freeze-drying was controlled within 12 hours, and lyophilized powder is placed in the vacuum drier, preserves under the room temperature.
Embodiment three:
1) preparation cadmium source
Get 100 mL water and put into three-necked flask, dissolve again 29 mg CdCl
22.5H
2O and 25 μ L Thiovanic acids are transferred pH to 9 with NaOH in water, form stable cadmium metal complex compound, and cadmium salt and dispersion agent mol ratio are 1:2.5, lead to into high-purity argon gas by the airway that inserts directly over the constant pressure funnel, slough the oxygen that contains in the solution;
2) preparation doping cadmium source
In 100 mL water, add 5 mL, 0.01 molL
-1Ag
+, after the dissolving, pour in the constant pressure funnel that is installed in the three-necked flask upper right side fully, lead to into high-purity argon gas by the airway that inserts directly over the constant pressure funnel, slough the oxygen that contains in the solution, add 12.5 μ L thiohydracrylic acids, mix, for subsequent use;
3) preparation sulphur source:
Take by weighing 156 mg Na
2The S solid is dissolved in the 10 mL water, gets 1 mL Na
2S solution is poured in the constant pressure funnel of three-necked flask upper left side, beats the material valve of starting discharging a little, can slough airborne oxygen in the constant pressure funnel;
4) open right side discharge gate on the constant pressure funnel, lentamente with Ag
+Solution is added drop-wise in the solution of cadmium source, and dripping quantity is Cd in molar ratio
2+: Ag
+=10:1 closes the right side discharge gate, and cadmium source solution obtains mixing;
5) open left side discharge gate on the constant pressure funnel, lentamente with Na
2S solution is added drop-wise in the solution of doping cadmium source, stirs after 30 minutes, closes the left side discharge gate, and the nanocrystalline presoma of CdS:Ag obtains mixing;
6) microwave heating temperature being set is 100 ℃, be 90 minutes heat-up time, precursor solution is poured in the crystal reaction tube, treat the microwave stopped heating, take out crystal reaction tube, after being down to room temperature, adopt fluorescence analyser to characterize its photoluminescent property, the CdS:Ag nanocrystal solution that to obtain a kind of fluorescent emission wavelength be 600 nm;
7) adopt Freeze Drying Equipment to carry out frozen dried doping CdS:Ag nanocrystal solution, the time of freeze-drying was controlled within 12 hours, and lyophilized powder is placed in the vacuum drier, preserves under the room temperature.
Cadmium salt is water miscible salt, in the process in preparation cadmium source, except the Cadmium chloride fine powder that the present embodiment adopts, can also adopt cadmium nitrate, cadmium acetate, cadmium perchlorate, dispersion agent is except the Thiovanic acid that the present embodiment adopts, can also adopt thiohydracrylic acid, halfcystine, they all are the compounds that has a sulfydryl, can both play stable effect to solution, if increasing embodiment, only need to change the title of dispersion agent, other is without any need for change.So, adopt cadmium salt and the dispersion agent of lifting according to the step of above-described embodiment, can obtain the multiple varigrained CdS:Ag nanocrystal solution that has, repeat no more herein.
Claims (8)
1. preparation method who utilizes microwave technology to prepare water-soluble CdS:Ag dopen Nano crystal, step is divided into: preparation cadmium source, preparation doping cadmium source, preparation sulphur source, microwave promotes the growth of CdS:Ag dopen Nano crystal, namely can obtain different colours CdS:Ag dopen Nano crystalloid solution in the different timed intervals, it is characterized in that, the method of synthetic CdS:Ag dopen Nano crystal material in turn includes the following steps: with water miscible cadmium salt, dispersion agent and water are put into three-necked flask, the cadmium salt that in water, dissolves and dispersion agent, transfer to alkalescence, the pH value is set(ting)value, obtains stable cadmium source; Water miscible silver salt, dispersion agent are dissolved in the water Ag of preparation lower concentration
+Solution is put into the upper right side constant pressure funnel, slowly is added drop-wise in the three-necked flask by constant pressure funnel, under magnetic agitation, evenly mixes, and obtains stable doping cadmium source; Na as the sulphur source
2S solution is poured in the upper left constant pressure funnel of three-necked flask; Under magnetic agitation, open the left side discharge gate, drip lentamente the sulphur source, mix, obtain the precursor solution of CdS:Ag dopen Nano crystal under the normal temperature; Precursor solution is poured in the quartzy microwave reaction pipe, microwave temperature and action time are set, the different timed intervals can obtain different colours CdS:Ag dopen Nano crystalloid solution; Adopt freeze drying technology to remove unreacted presoma, obtain Powdered CdS:Ag dopen Nano crystal material, be placed under the interior room temperature of vacuum drier and can keep.
2. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, adopt Na
2S or H
2S is as the sulphur source, prevents oxidizedly with the protection of argon gas, guarantees S in the solution of sulphur source
2-Concentration be 0.2 ~ 2 mol/L.
3. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, cadmium salt is water miscible salt, can select cadmium nitrate, Cadmium chloride fine powder, cadmium acetate or cadmium perchlorate; Dispersion agent can be selected thiohydracrylic acid, Thiovanic acid or halfcystine; The mol ratio of cadmium salt and dispersion agent is 1:2.5 ~ 5; The cadmium salt that dissolves in water and dispersion agent transfer to alkalescence, and the pH value is 9 ~ 13, obtain stable cadmium source.
4. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, adopt silver nitrate solution, the required Ag that mixes is provided
+, and and dispersant, be evenly dispersed in the solution of cadmium source, form stable doping cadmium source.
5. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, sulphur source solution is added in the solution of doping cadmium source lentamente, evenly mix and obtain precursor solution.
6. dripping quantity is Cd in molar ratio
2+: Na
2S=3 ~ 5:1 where necessary, if when pressure of the inside of a bottle is higher than normal atmosphere, can pass through the discharge valve exhaust decompression, guarantees that rate of addition is stable.
7. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, under microwave action, CdS:Ag Doped nanocrystal bulk-growth is when setting size, show its distinctive fluorescent characteristic, microwave action time and temperature all can affect the photoluminescent property of CdS:Ag dopen Nano crystal, namely by control microwave temperature and time, can control the photoluminescent property of CdS:Ag dopen Nano crystal, the dopen Nano crystalloid solution can directly use, and can preserve more than 3 months at ambient temperature.
8. according to the method for synthetic CdS:Ag dopen Nano crystal material claimed in claim 1, it is characterized in that, adopt Freeze Drying Equipment to remove unreacted presoma, freeze-drying time was controlled within 12 hours, obtain pulverous CdS:Ag dopen Nano crystal material, be placed in the vacuum drier under the room temperature, can preserve more than at least one year.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316693A (en) * | 2013-07-03 | 2013-09-25 | 西北师范大学 | Photocatalyst Cd/CdS containing catalyst promoter Cd as well as preparation method and application of photocatalyst Cd/CdS in photocatalysis hydrogen production reaction |
| CN105460903A (en) * | 2015-09-22 | 2016-04-06 | 苏州星烁纳米科技有限公司 | Nanocrystal preparation method, nanocrystal, and preparation and preservation apparatus of gas solution |
| CN105838357A (en) * | 2014-12-23 | 2016-08-10 | 南京化工职业技术学院 | Preparation method of zinc and silver co-doped cadmium sulfide quantum dots |
-
2012
- 2012-10-25 CN CN 201210410745 patent/CN102925141A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316693A (en) * | 2013-07-03 | 2013-09-25 | 西北师范大学 | Photocatalyst Cd/CdS containing catalyst promoter Cd as well as preparation method and application of photocatalyst Cd/CdS in photocatalysis hydrogen production reaction |
| CN105838357A (en) * | 2014-12-23 | 2016-08-10 | 南京化工职业技术学院 | Preparation method of zinc and silver co-doped cadmium sulfide quantum dots |
| CN105460903A (en) * | 2015-09-22 | 2016-04-06 | 苏州星烁纳米科技有限公司 | Nanocrystal preparation method, nanocrystal, and preparation and preservation apparatus of gas solution |
| US10519038B2 (en) | 2015-09-22 | 2019-12-31 | Suzhou Xingshuo Nanotech Co., Ltd. | Nanocrystal preparation method, nanocrystals, and apparatus for preparing and storing dissolved gas |
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Application publication date: 20130213 |