CN101016461A - Method of synthesizing near-infrared CdHgTe and CdHgTe/CdS fluorescence quantum points - Google Patents
Method of synthesizing near-infrared CdHgTe and CdHgTe/CdS fluorescence quantum points Download PDFInfo
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Abstract
The invention discloses a synthetic method of near-infrared CdHgTe and CdHgTe/CdS fluorescence quantum point, which comprises the following steps: choosing water as dissolvent; choosing cadmium salt, mercuric salt and sodium hydride telluride as reacting forerunner body; choosing sulfhydryl group compound as stabilizer; synthesizing CdHgTe quantum point through heating directly with luminous position at 600-900 nanometer, quantum yield at 10-30% and half-peak width of sending peak at 40-70 nanometer; injecting into cadmium salt, sulfide and sulfhydryl group compound; heating; getting CdHgTe/CdS core-shell quantum point with fluorescence spectrum red shift at 10-20 nanometer. This invention possesses simple steps, warm condition and high quantum yield, which can be used to cell image formation and tissue image formation widely.
Description
Technical field
The present invention relates to the synthetic method of a kind of near infrared CdHgTe and CdHgTe/CdS fluorescence quantum, belong to nano material preparation technology and bioanalysis detection technique field.
Background technology
(700-900 nanometer) has less absorption and autofluorescence in the near-infrared region owing to organism, so near infrared light has penetrance and higher sensitivity preferably in biological tissue, has wide practical use on cell imaging and imaging of tissue.Yet traditional near infrared fluorescent dye is synthetic to cost an arm and a leg, and easily photobleaching brings inconvenience to practical application.At present, advantages such as fluorescence quantum owing to have widely excites, narrow emission, quantum yield height and good light stability have caused people's extensive concern.People begin near infrared fluorescence quantum point, as InAs/ZnS, and InAs
xP
1-x/ ZnSe, CdTe/CdS Type-II quantum dot is applied to study the distribution of sentinel lymph node, fields such as lesion detection.
At present, synthetic near-infrared quantum dots mainly adopts the organo-metallic method, and it is many to react required step, and the condition harshness needs anhydrous, anaerobic, high temperature, used reagent cost an arm and a leg and toxicity big, have in addition explosive.This has brought many difficulties for synthetic near-infrared quantum dots, has limited application greatly.People such as Rogach adopt Thiovanic acid in the aqueous solution be stablizer, and earlier synthetic CdTe quantum dot adds Hg more gradually
2+, Cd
2+And H
2Te forms CdTe/CdHgTe alloy quantum dot (PHYSICA STATUS SOLIDI B-BASICRESEARCH 224 (1): 153-158).Though the quantum dot emission peak that this method makes is positioned at the near-infrared region, peak shape is too wide, can not obtain narrow and symmetric fluorescent emission.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of novel method at synthetic CdHgTe of aqueous phase and CdHgTe/CdS fluorescence quantum is proposed, simple, the mild condition of this method steps, synthetic CdHgTe and CdHgTe/CdS fluorescence quantum luminous position in the near-infrared region, the quantum yield height, emmission spectrum is narrow and adjustable.
For achieving the above object, the present invention is solvent with water, with cadmium salt, mercury salt and sodium hydrogen telluride is the reaction precursor body, with the thiol compound is stablizer, by heating directly synthetic CdHgTe quantum dot, light emitting region is in the 600-900 nanometer, quantum yield 10-30%, emission peak peak width at half height 40-70 nanometer.In the CdHgTe quantum dot, inject cadmium salt, sulfide and sulfhydryl compound then, obtain the CdHgTe/CdS core-shell quanta dots by heating, fluorescence spectrum red shift 10-20 nanometer, light stability is improved.
Method of the present invention specifically may further comprise the steps:
1, the preparation of sodium hydrogen telluride
Tellurium powder, sodium borohydride and ultrapure water be placed in the flask react.Wherein, the mol ratio of tellurium powder and sodium borohydride is 1: 4 to 4: 1.Through 5-12 hour reaction, the tellurium powder of black faded away, and the Sodium Tetraborate precipitation of white appears in drag.The careful supernatant liquid with in the flask is transferred in the flask that is equipped with in the ultrapure water that removed gas, prepares sodium hydrogen telluride solution.
2. the water of near infrared CdHgTe quantum dot is synthetic
With water is solvent, with concentration is that the water-soluble cadmium salt of 0.00001-0.1 mol, mercury salt and sulfhydryl compound mix, adjusting pH is 7.0-12.0, and wherein the mol ratio of cadmium salt and mercury salt is 1: 50 to 1: 5, and the mol ratio of cadmium salt and mercury salt total amount and sulfhydryl compound is 1: 5 to 2: 1.Then, inject sodium hydrogen telluride solution, the mol ratio of cadmium salt and mercury salt total amount and sodium hydrogen telluride is 10: 1 to 1: 4, obtains the CdHgTe precursor solution.Get 10-60 milliliter CdHgTe precursor solution and put into microwave reactor, the conditioned reaction temperature is 80-140 degree centigrade, and the reaction times is 5 minutes-10 hours, obtains CdHgTe alloy quantum dot solution, and wherein the light emitting region of near-infrared quantum dots is in the 600-900 nanometer.
3.CdHgTe/CdS the preparation of core-shell quanta dots
Cadmium salt, sulfide and sulfhydryl compound are mixed, and regulator solution pH value prepares the CdS presoma at 7.0-12.0, and wherein the mol ratio of cadmium salt and sulfide is 1: 1 to 2: 1, and the mol ratio of cadmium salt and sulfhydryl compound is 1: 1 to 1: 5.The CdS presoma that obtains is injected in the CdHgTe alloy quantum dot solution, in the control CdS presoma in the amount of S and the CdHgTe quantum dot mol ratio of the amount of Te be 2: 1 to 1: 10.The solution that makes heated 30-120 minute down at 80-100 degree centigrade, obtained the CdHgTe/CdS nuclear shell structure quantum point.
The described cadmium salt of present method comprises cadmium nitrate, cadmium perchlorate, cadmium chlorate, cadmium acetate, Cadmium Sulphate, cadmium iodate, Cadmium chloride fine powder, cadmium iodide, cadmium bromide, cadmium carbonate, etc.
Described mercury salt comprises mercuric perchlorate, mercuric chlorate, mercuric acetate, mercury chloride, Mercury pernitrate, etc.
Described sulfide comprises sodium sulphite, potassium sulphide, sulfuration ammonia, thiocarbamide, and thioacetamide, etc.
Described 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.
The inventive method step is simple, mild condition, synthetic CdHgTe and CdHgTe/CdS quantum dot light emitting position in the near-infrared region, the quantum yield height, emmission spectrum is narrow and adjustable, on cell imaging and imaging of tissue, have wide practical use.
Embodiment
Below by several specific embodiments technical scheme of the present invention is further described.
Embodiment 1
1. the preparation of sodium hydrogen telluride
80 milligrams of tellurium powder, 80 milligrams of sodium borohydrides and 2 ml waters are placed in one 10 milliliters the little flask, the little flask mouth of reaction is inserted a minute hand head, so that the hydrogen that release reaction produces simultaneously immediately with the soft rubber ball sealing on soft rubber ball.At room temperature reacted 8 hours, the tellurium powder of black fades away, and the Sodium Tetraborate precipitation of white appears in drag.The careful supernatant liquid with in the flask is transferred in 100 ml flasks that are equipped with in the ultrapure water that removed gas, prepare 6.25 mmoles/liter sodium hydrogen telluride solution.
2. the water of near infrared CdHgTe quantum dot is synthetic
0.125 mmole Cadmium chloride fine powder and 0.025 mmole mercury chloride are dissolved in 90 milliliters of ultrapure waters, add 0.625 mmole thiohydracrylic acid and regulate pH value to 9.0, inject 6.25 mmoles/liter 10 milliliters of NaHTe solution, at this moment obtain the CdHgTe precursor solution, it is orange-yellow that solution is.This precursor solution is put into the microwave reactor reaction, heated 30 minutes down, obtain fluorescence emission peak in 700 nanometers, the near infrared CdHgTe quantum dot of quantum yield 20% at 120 degrees centigrade.
3.CdHgTe/CdS the preparation of core-shell quanta dots
0.125 mmole Cadmium chloride fine powder, 0.125 mmole sodium sulphite and 0.125 mmole thiohydracrylic acid are dissolved in 10 ml waters, regulate pH value to 9.0, the CdS presoma that obtains is injected the CdHgTe quantum dot solution that reaction obtains, heated 60 minutes down at 80 degrees centigrade, obtain the CdHgTe/CdS core-shell quanta dots, fluorescent emission peak position red shift 10 nanometers, quantum yield changes little.
Embodiment 2
1. the preparation of sodium hydrogen telluride
0.4g tellurium powder, 0.3g sodium borohydride and 10 ml waters are placed in one 25 milliliters the little flask, the little flask mouth of reaction is inserted a minute hand head, so that the hydrogen that release reaction produces simultaneously immediately with the soft rubber ball sealing on soft rubber ball.At room temperature reacted 12 hours, the tellurium powder of black fades away, and the Sodium Tetraborate precipitation of white appears in drag.The careful supernatant liquid with in the flask is transferred in 100 ml flasks that are equipped with in the ultrapure water that removed gas, prepares the hydrogen telluride potassium solution of 0.0313 mol.
2. the water of near infrared CdHgTe quantum dot is synthetic
6.25 mmole cadmium perchlorates, 3.13 mmole mercuric perchlorates and 28 mmole Thiovanic acids are dissolved in 90 milliliters of ultrapure waters, the pH value of regulating this solution is 11.0, and inject 10 milliliters in the hydrogen telluride potassium of 0.0313 mol prepare, and at this moment obtaining the CdHgTe precursor solution, it is orange-yellow that solution is.This precursor solution is placed in the microwave reactor reacts,, obtain fluorescence emission peak in 800 nanometers, the near infrared CdHgTe quantum dot of quantum yield 15% 130 degrees centigrade of heating 30 minutes down.
3.CdHgTe/CdS the preparation of core-shell quanta dots
1.25 mmole cadmium perchlorates, 0.625 mmole thioacetamide and 1.25 mmole Thiovanic acids are dissolved in 10 milliliters of ultrapure waters, regulating the pH value is 11.0, the CdS presoma that obtains is injected the CdHgTe quantum dot solution that reaction obtains, heated 30 minutes down at 100 degrees centigrade, obtain the CdHgTe/CdS core-shell quanta dots.
Embodiment 3
1. the preparation of sodium hydrogen telluride
0.64g tellurium powder, 0.64g sodium borohydride and 20 ml waters are placed in one 25 milliliters the little flask, the little flask mouth of reaction is inserted a minute hand head, so that the hydrogen that release reaction produces simultaneously immediately with the soft rubber ball sealing on soft rubber ball.At room temperature reacted 12 hours, the tellurium powder of black fades away, and the Sodium Tetraborate precipitation of white appears in drag.The careful supernatant liquid with in the flask is transferred in 100 ml flasks that are equipped with in the ultrapure water that removed gas, prepares the sodium hydrogen telluride solution of 0.05 mol.
2. the water of near infrared CdHgTe quantum dot is synthetic
2.5 mmole cadmium acetates, 2.5 mmole mercuric acetates and 10 mmole thiohydracrylic acids are dissolved in 90 milliliters of ultrapure waters, the pH value of regulating this solution is about 7.0, and inject 10 milliliters of the sodium hydrogen telluride solution of 0.05 mol prepare, and at this moment obtaining the CdHgTe precursor solution, it is orange-yellow that solution is.This precursor solution is placed in the microwave reactor reacts,, obtain fluorescence emission peak in 850 nanometers, the near infrared CdHgTe quantum dot of quantum yield 10% 150 degrees centigrade of heating 30 minutes down.
3.CdHgTe/CdS the preparation of core-shell quanta dots
10 mmole cadmium acetates, 10 mmole thiocarbamides and 20 mmole thiohydracrylic acids are dissolved in 20 milliliters of ultrapure waters, regulating the pH value is about 7.0, the CdS presoma that obtains is injected the CdHgTe quantum dot solution that reaction obtains, heated 60 minutes down at 100 degrees centigrade, obtain the CdHgTe/CdS core-shell quanta dots.
Claims (3)
1, a kind of synthetic method of near infrared CdHgTe fluorescence quantum is characterized in that comprising the steps:
(1) preparation of sodium hydrogen telluride: tellurium powder, sodium borohydride and ultrapure water be placed in the flask react, wherein the mol ratio of tellurium powder and sodium borohydride is 1: 4 to 4: 1, react after 5-12 hour, the tellurium powder of black fades away, the Sodium Tetraborate precipitation of white appears in drag, supernatant liquid in the flask is transferred in the flask that is equipped with in the ultrapure water that removed gas, prepares sodium hydrogen telluride solution;
(2) water of near infrared CdHgTe quantum dot is synthetic: with water is solvent, with concentration is that the water-soluble cadmium salt of 0.00001-0.1 mol, mercury salt and sulfhydryl compound mix, adjusting pH is 7.0-12.0, wherein the mol ratio of cadmium salt and mercury salt is 1: 50 to 1: 5, and the mol ratio of cadmium salt and mercury salt total amount and sulfhydryl compound is 1: 5 to 2: 1.Then, the sodium hydrogen telluride solution that injection prepares, the mol ratio of cadmium salt and mercury salt total amount and sodium hydrogen telluride is 10: 1 to 1: 4, obtain the CdHgTe precursor solution, get 10-60 milliliter CdHgTe precursor solution and put into microwave reactor, the conditioned reaction temperature is 80-140 degree centigrade, and the reaction times is 5 minutes-10 hours, obtain CdHgTe alloy quantum dot solution, wherein the light emitting region of near-infrared quantum dots is in the 600-900 nanometer.
2, a kind of synthetic method of near infrared CdHgTe/CdS fluorescence quantum is characterized in that comprising the steps:
(1) preparation of sodium hydrogen telluride: tellurium powder, sodium borohydride and ultrapure water be placed in the flask react, wherein the mol ratio of tellurium powder and sodium borohydride is 1: 4 to 4: 1, react after 5-12 hour, the tellurium powder of black fades away, the Sodium Tetraborate precipitation of white appears in drag, supernatant liquid in the flask is transferred in the flask that is equipped with in the ultrapure water that removed gas, prepares sodium hydrogen telluride solution;
(2) water of near infrared CdHgTe quantum dot is synthetic: with water is solvent, with concentration is that the water-soluble cadmium salt of 0.00001-0.1 mol, mercury salt and sulfhydryl compound mix, adjusting pH is 7.0-12.0, wherein the mol ratio of cadmium salt and mercury salt is 1: 50 to 1: 5, and the mol ratio of cadmium salt and mercury salt total amount and sulfhydryl compound is 1: 5 to 2: 1.Then, the sodium hydrogen telluride solution that injection prepares, the mol ratio of cadmium salt and mercury salt total amount and sodium hydrogen telluride is 10: 1 to 1: 4, obtain the CdHgTe precursor solution, get 10-60 milliliter CdHgTe precursor solution and put into microwave reactor, the conditioned reaction temperature is 80-140 degree centigrade, and the reaction times is 5 minutes-10 hours, obtain CdHgTe alloy quantum dot solution, wherein the light emitting region of near-infrared quantum dots is in the 600-900 nanometer;
(3) preparation of CdHgTe/CdS core-shell quanta dots: cadmium salt, sulfide and sulfhydryl compound are mixed, regulator solution pH value is at 7.0-12.0, prepare the CdS presoma, wherein the mol ratio of cadmium salt and sulfide is 1: 1 to 2: 1, and the mol ratio of cadmium salt and sulfhydryl compound is 1: 1 to 1: 5; The CdS presoma that obtains is injected in the CdHgTe alloy quantum dot solution, in the control CdS presoma in the amount of S and the CdHgTe quantum dot mol ratio of the amount of Te be 2: 1 to 1: 10, the solution that makes heated 30-120 minute down at 80-100 degree centigrade, obtained the CdHgTe/CdS nuclear shell structure quantum point.
3, according to the synthetic method of the fluorescence quantum of claim 1 or 2, it is characterized in that described cadmium salt is cadmium nitrate, cadmium perchlorate, cadmium chlorate, cadmium acetate, Cadmium Sulphate, cadmium iodate, Cadmium chloride fine powder, cadmium iodide, cadmium bromide or cadmium carbonate; Described mercury salt is mercuric perchlorate, mercuric chlorate, mercuric acetate, mercury chloride or Mercury pernitrate; Described sulfide comprises sodium sulphite, potassium sulphide, sulfuration ammonia, thiocarbamide or thioacetamide; Described sulfhydryl compound is Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, halfcystine, Gelucystine, thioglycerin, mercaptoethanol, mercaprol, 2,3-dimercapto-1-propyl alcohol or two-thiohydracrylic acid.
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