CN1556041A - Temperature and pressure controlled microwave synthesis method of high quantum yield cadmium tellurate quantum point - Google Patents
Temperature and pressure controlled microwave synthesis method of high quantum yield cadmium tellurate quantum point Download PDFInfo
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- CN1556041A CN1556041A CNA2004100156815A CN200410015681A CN1556041A CN 1556041 A CN1556041 A CN 1556041A CN A2004100156815 A CNA2004100156815 A CN A2004100156815A CN 200410015681 A CN200410015681 A CN 200410015681A CN 1556041 A CN1556041 A CN 1556041A
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- cadmium
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- telluride
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Abstract
A microwave synthesis process for preparing the CdTe with high quantum yield by controlling temp and pressure includes mixing the salt (or oxide) of Cd with carbonylated compound, adding sodium(or potassium) hydride telluride to obtain the precurser solution of CdTe, putting it in teflon container, sealing, and reacting in microwave reactor while controlling temp and pressure. The resultant CdTe features high water solubility, stability and fluorescent quantum yield, and adjustable emission spectrum.
Description
Technical field
The present invention relates to the process for temperature-control pressure-control microwave synthesis of a kind of high quantum production rate cadmium telluride (CdTe) quantum dot, be with cadmium salt (or its oxide compound, oxyhydroxide) and sodium hydrogen telluride (or hydrogen telluride potassium, the tellurium powder) is raw material, utilize temperature control, pressure control microwave-assisted synthesis to prepare the CdTe quantum dot, belong to nano material preparation technology and bioanalysis detection technique field.
Background technology
Quantum dot (quantum dots) claims semiconductor nanocrystal again, is the elementary composition nano particle of a kind of IIB-VIA of having or IIIB-VA family, and CdTe belongs to wherein a kind of.This material is compared with organic fluorescent dye, has unique photoluminescent property, and wide as excitation wavelength range, emission wavelength ranges is narrow, and the Stocks displacement is big, the quantum yield height, and fluorescence lifetime is long, characteristics such as be difficult for photodissociation or drift.Fluorescence quantum is linked to each other with biomacromolecule, constitute biological fluorescent labeling, at immunoassay, genetic analysis, the living body fluorescent imaging, clinical diagnosis, fields such as drug screening are with a wide range of applications.The organic synthesis of the synthetic mainly employing of CdTe at present method (Murray C.B., et.al., J.Am.Chem.Soc., 1993,115,8706-8715.), the product that this method obtains (CdTe) quantum yield height, emmission spectrum narrow range.But the required reagent of this method costs an arm and a leg, and toxicity is big, synthesis condition harshness (needing 300 celsius temperatures), and explosive, particularly its product C dTe is water insoluble, has limited its application greatly.Studies show that recently the water method also can be used for the synthetic of CdTe quantum dot, the product good water solubility that this method obtains easily is connected with biomacromolecule.But the heating in water bath of the synthetic generally employing of water at present (Rogach A.L., et.al., J.Phys.Chem., 1999,103,3065-3069.) or High Temperature High Pressure heating means (Zhang H, et.al., Advanced Materials, 2003,15 (20): 1712-1715.), required time of this method is long, and the quantum yield of product is lower.
Summary of the invention
The objective of the invention is to defective at present water and organic synthesis method, a kind of process for temperature-control pressure-control microwave synthesis of high quantum production rate cadmium telluride quantum dot is provided, has that resultant velocity is fast, synthesis condition is gentle, a product good water solubility, advantage that quantum yield is high.
For achieving the above object, the present invention is a raw material with cadmium salt (or the oxide compound of cadmium, oxyhydroxide) and sodium hydrogen telluride (or hydrogen telluride potassium, tellurium powder), utilizes temperature-control pressure-control microwave heating in the aqueous solution, rapidly synthetic CdTe fluorescence quantum, its quantum yield can reach 60%.
Method of the present invention specifically comprises the steps:
1, the preparation of sodium hydrogen telluride (or hydrogen telluride potassium):
With mol ratio 1: 4 to 4: 1 sodium borohydride (NaBH
4) or POTASSIUM BOROHYDRIDE (KBH
4) and tellurium powder (Te) place water, reaction generates sodium hydrogen telluride (NaHTe) or hydrogen telluride potassium (KHTe) under 0-50 degree centigrade temperature.
2, the synthetic CdTe quantum dot of microwave:
With water is solvent, with concentration is that the cadmium salt of 0.0001～0.1 mol or oxide compound, the oxyhydroxide of cadmium mix with water-soluble sulfhydryl compound, the pH value of regulator solution is to 3-12, the mol ratio of the oxide compound of cadmium salt or cadmium, oxyhydroxide and water-soluble sulfhydryl compound is 1: 5 to 5: 1, inject NaHTe or hydrogen telluride potassium (KHTe) then, the mol ratio of the oxide compound of cadmium salt or cadmium, oxyhydroxide and NaHTe (or KHTe) is 10: 1 to 1: 4, under 0-100 degree centigrade temperature, stirred 1-10 minute, obtain the CdTe precursor solution.This solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate the CdTe fluorescence quantum.Microwave heating condition is: microwave oscillation frequency 300MHZ～3000MHZ, microwave power 50W～1000W, 1 minute～10 hours heat-up time, 50～250 degrees centigrade of Heating temperatures.
Oxide compound, the oxyhydroxide of cadmium salt of the present invention or cadmium comprise: cadmium nitrate, Cadmium oxide, cadmium perchlorate, cadmium chlorate, cadmium acetate, Cadmium Sulphate, cadmium iodate, cadmium hydroxide, Cadmium chloride fine powder, cadmium iodide, cadmium bromide, cadmium carbonate, etc.; Water miscible sulfhydryl compound comprises: Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, halfcystine, Gelucystine, thioglycerin, mercaptoethanol, mercaprol, 2,3-dimercapto-1-propyl alcohol, two-thiohydracrylic acid etc.
Method of the present invention is simple to operate, mild condition, and cost is low.Synthetic product CdTe has water-soluble and good stability, the fluorescence quantum yield height, and emmission spectrum is adjustable, easily with characteristics such as biomacromolecule are connected.
Embodiment
Below by several specific embodiments technical scheme of the present invention is further described.
Embodiment 1
(1). the sodium hydrogen telluride preparation
With 0.8 gram NaBH
4Solid and 1.32 gram Te powder are put in the little flask, add 20 ml waters., after 8 hours solution is taken out in reaction under 25 degrees centigrade, standby.
(2). microwave synthesizes the CdTe quantum dot
With water is solvent, with 20 mmoles/rise CdCl
2With 20 mmoles/rising thiohydracrylic acid (MPA) equal-volume ratio mixes, and regulates pH value to 11.Inject NaHTe solution to concentration then and be 1 mmole/liter, stirred 5 minutes down at 25 degrees centigrade, obtain the CdTe precursor solution.This solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, heat, obtain fluorescence quantum by following condition.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ
Microwave power: 400W,
Heat-up time: 4 hours
Heating temperature: 70 degrees centigrade.
Embodiment 2
(1). the preparation of hydrogen telluride potassium
With 0.9 gram KBH
4Solid and 1.32 gram Te powder are put in the little flask, add 20 ml waters., after 8 hours solution is taken out in reaction under 25 degrees centigrade, standby.
(2). microwave synthesizes the CdTe quantum dot
With water is solvent, with 8 mmoles/rise CdCl
2With 12 mmoles/rising MPA equal-volume ratio mixes, and regulates pH value to 6.Inject then KHTe to concentration be 0.4 mmole/liter, stirred 10 minutes, obtain the CdTe precursor solution.This solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, heat, obtain fluorescence quantum by following condition.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ
Microwave power: 600W
Heat-up time: 2 hours,
Heating temperature: 160 degrees centigrade.
Embodiment 3
(1). the sodium hydrogen telluride preparation is identical with example 1.
(2). microwave synthesizes the CdTe quantum dot
With water is solvent, with 1.2 mmoles/rise CdCl
2With 1 mmole/rising MPA equal-volume ratio mixes, and regulates pH value to 9.Inject then NaHTe to concentration be 0.2 mmole/liter, stirred 5 minutes down at 25 degrees centigrade, obtain the CdTe precursor solution.This solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, heat, obtain fluorescence quantum by following condition.
Microwave heating condition is:
Microwave oscillation frequency: 2450MHZ
Microwave power: 600W,
Heat-up time: 0.5 hour
Heating temperature: 180 degrees centigrade.
Claims (2)
1, a kind of process for temperature-control pressure-control microwave synthesis of high quantum production rate cadmium telluride quantum dot is characterized in that comprising the steps:
1) preparation of sodium hydrogen telluride or hydrogen telluride potassium: the sodium borohydride NaBH that with mol ratio is 1: 4 to 4: 1
4Or POTASSIUM BOROHYDRIDE KBH
4Te places water with the tellurium powder, and reaction generates sodium hydrogen telluride NaHTe or hydrogen telluride potassium KHTe under 0-50 degree centigrade temperature;
2) the synthetic cadmium telluride CdTe quantum dot of microwave: with water is solvent, with concentration is the cadmium salt of 0.0001～0.1 mol or the oxide compound of cadmium, oxyhydroxide mixes with water-soluble sulfhydryl compound, pH value to 3～12 of regulator solution, the oxide compound of cadmium salt or cadmium, the mol ratio of oxyhydroxide and water-soluble sulfhydryl compound is 1: 5 to 5: 1, inject NaHTe or KHTe then, the oxide compound of cadmium salt or cadmium, the mol ratio of oxyhydroxide and NaHTe or KHTe is 10: 1 to 1: 4, under 0～100 degree centigrade temperature, stirred 1～10 minute, obtain the CdTe precursor solution, this solution is placed airtight polytetrafluoroethyltank tank, but in the microwave reactor of temperature controllable and pressure control, react, generate the CdTe fluorescence quantum, microwave heating condition is: microwave oscillation frequency 300MHZ～3000MHZ, microwave power 50W～1000W, 1 minute～10 hours heat-up time, 50～250 degrees centigrade of Heating temperatures.
2, the process for temperature-control pressure-control microwave synthesis of high quantum production rate cadmium telluride quantum dot as claimed in claim 1, the oxide compound that it is characterized in that described cadmium salt or cadmium, oxyhydroxide comprises: cadmium nitrate, Cadmium oxide, cadmium perchlorate, cadmium chlorate, cadmium acetate, Cadmium Sulphate, cadmium iodate, cadmium hydroxide, Cadmium chloride fine powder, cadmium iodide, cadmium bromide, cadmium carbonate, described water miscible sulfhydryl compound comprises Thiovanic acid, thiohydracrylic acid, the sulfydryl butyric acid, thioglycolate salt, mercapto propionate, the sulfydryl butyrates, halfcystine, Gelucystine, thioglycerin, mercaptoethanol, mercaprol, 2,3-dimercapto-1-propyl alcohol, two-thiohydracrylic acid.
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| CN 200410015681 CN1234600C (en) | 2004-01-08 | 2004-01-08 | Temperature and pressure controlled microwave synthesis method of high quantum yield cadmium tellurate quantum point |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306003C (en) * | 2005-04-28 | 2007-03-21 | 复旦大学 | Process for preparing water soluble CdTe/CdS nuclear/shell type quantum point by microwave radiation reaction |
| CN1328351C (en) * | 2005-09-23 | 2007-07-25 | 上海大学 | Method for preparing II-VI family fluorescent mark semiconductor quantum point MX |
| EP1908134A1 (en) * | 2005-07-11 | 2008-04-09 | National Research Council Of Canada | Hybrid nanocomposite semiconductor material and method of producing inorganic semiconductor therefor |
| CN101250403B (en) * | 2008-02-28 | 2010-06-23 | 上海交通大学 | Method for synthesizing water-soluble long-chain mercapto compound coated cadmium telluride quantum dot |
| CN102887489A (en) * | 2012-10-26 | 2013-01-23 | 苏州大学 | Method for preparing water-solubility near-infrared cadmium telluride quantum dots through microwave radiation |
-
2004
- 2004-01-08 CN CN 200410015681 patent/CN1234600C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306003C (en) * | 2005-04-28 | 2007-03-21 | 复旦大学 | Process for preparing water soluble CdTe/CdS nuclear/shell type quantum point by microwave radiation reaction |
| EP1908134A1 (en) * | 2005-07-11 | 2008-04-09 | National Research Council Of Canada | Hybrid nanocomposite semiconductor material and method of producing inorganic semiconductor therefor |
| EP1908134A4 (en) * | 2005-07-11 | 2011-06-01 | Ca Nat Research Council | Hybrid nanocomposite semiconductor material and method of producing inorganic semiconductor therefor |
| CN1328351C (en) * | 2005-09-23 | 2007-07-25 | 上海大学 | Method for preparing II-VI family fluorescent mark semiconductor quantum point MX |
| CN101250403B (en) * | 2008-02-28 | 2010-06-23 | 上海交通大学 | Method for synthesizing water-soluble long-chain mercapto compound coated cadmium telluride quantum dot |
| CN102887489A (en) * | 2012-10-26 | 2013-01-23 | 苏州大学 | Method for preparing water-solubility near-infrared cadmium telluride quantum dots through microwave radiation |
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