CN104860345A - Preparation method for water-soluble tin-monosulfide quantum dot - Google Patents
Preparation method for water-soluble tin-monosulfide quantum dot Download PDFInfo
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Abstract
The invention discloses a preparation method for a water-soluble tin-monosulfide quantum dot. The method comprises the following steps: (1) respectively dissolving tin salts and sulfur-containing compounds in an organic solvent so as to obtain a tin source and a sulfur source, mixing the tin source and the sulfur source under an ultrasonic or stirring condition and then carrying out reaction so as to form a precursor; and (2) adding the formed precursor with highly-purified water, an aqueous solution containing a surfactant or an aqueous solution containing protein, and subjecting the above-mentioned mixture to reaction at 4 to 80 DEG C so as to prepare the water-soluble tin-monosulfide quantum dot. The preparation method provided by the invention is simple and controllable and is mild in reaction conditions, cheap and easily-available in raw material and friendly to environment.
Description
Technical field
The invention belongs to the synthesis technical field of inorganic functional material stannous sulfide, be specifically related to a kind of preparation method of water-soluble stannous sulfide quantum dot.
Background technology
Quantum dot, can be described as again nanocrystalline, and particle diameter is generally between 1-10nm, and because electronics and hole are by quantum confinement, continuous print energy band structure becomes the discrete energy levels structure with molecular characterization, can emitting fluorescence after being excited.Due to quantum size effect, surface effects, macro quanta tunnel effect, quantum dot has the incomparable photoelectric characteristic of bulk material and becomes the focus of research.Based on quantum effect, quantum dot is with a wide range of applications in fields such as solar cell, luminescent device and optical bio marks.Stannous sulfide quantum dot has good photoelectric property, is the good material of solar cell device absorption layer.At present, the method of synthesis stannous sulfide quantum dot mainly contains: electrochemical method, hot injecting method, ion exchange method and hydrothermal method etc., these synthetic method major parts need high temperature and complicated apparatus, complex operation step and apply to biology aspect and need be converted into water-soluble quantum dot.At present, the method for synthesizing water-solubility stannous sulfide quantum dot is little, and its reason is: the quantum dot that (1) synthesizes is unstable, easily reunites in the absence of surfactant; (2) crystallinity is bad, limits its application; (3) productive rate is lower, is difficult to be applied in industrial production.Therefore, synthesizing water-solubility stannous sulfide quantum dot is faced with huge challenge, is also the focus studied in recent years.
Summary of the invention
The technical problem that the present invention solves there is provided a kind of preparation method of water-soluble stannous sulfide quantum dot, to have adopted a kind of new proportioning raw materials to prepare stable and water-soluble good stannous sulfide quantum dot for this preparation method, and obtained water-soluble stannous sulfide quantum dot has very strong fluorescence property.
The present invention adopts following technical scheme for solving the problems of the technologies described above, a kind of preparation method of water-soluble stannous sulfide quantum dot, it is characterized in that comprising the following steps: pink salt and sulfocompound are dissolved in organic solvent as Xi Yuan and sulphur source by (1) respectively, by Xi Yuan and sulphur source, mixing under condition that is ultrasonic or that stir is carried out reaction and is formed presoma, wherein pink salt is tin chloride, sulfocompound is thioacetamide or thiocarbamide, and organic solvent is methyl alcohol, ethanol or propyl alcohol, (2) presoma that step (1) is formed is added high purity water, the aqueous solution containing tensio-active agent or the aqueous solution containing protein, wherein tensio-active agent is sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, Sodium palmityl sulfate, dioctyl succinate disulfonate acid, cetylpyridinium chloride, brocide, potassium stearate, potassium oleate, potassium laurate or polyoxyethylene glycol, protein is bovine serum albumin, presoma and high purity water, the volume ratio of the aqueous solution containing tensio-active agent or the aqueous solution containing protein is 1:0.5-2, then said mixture is reacted 0.5-24h in 4-80 DEG C, the centrifugation rate that reaction terminates to be placed on 13000r/min in whizzer is centrifugal, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, water-soluble stannous sulfide quantum dot is obtained after drying.
Further restriction, described pink salt and the mol ratio of sulfocompound are 0.43:1.
Further restriction, the mass concentration of the described aqueous solution containing tensio-active agent is 1-4g/L, and the mass concentration of the described aqueous solution containing protein is 1-4g/L.
Outstanding advantages of the present invention have employed raw material cheap and easy to get, utilize presoma and high purity water to be hydrolyzed under different temperature and times to react, controlled prepare different crystalline types, different size and can the water-soluble stannous sulfide quantum dot of stable existence.Compared with the preparation method of existing stannous sulfide quantum dot, preparation method of the present invention is simply controlled, reaction conditions is gentle, cheaper starting materials is easy to get and environmentally friendly.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram that the embodiment of the present invention 1 obtains sample, and Fig. 2 is the transmission electron microscope picture that the embodiment of the present invention 1 obtains sample.
Embodiment
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
(1) in 150mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
As can be seen from Figure 1, occur without obvious sharp peak, illustrate that the crystalline types of the stannous sulfide quantum dot that present method is synthesized is amorphous.The water-soluble stannous sulfide quantum point grain diameter of gained is very little as seen from Figure 2, is about 10nm.
Embodiment 2
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, stannous chloride solution is slowly added in thioacetyl amine aqueous solution, stir 10min and form presoma;
(2) presoma that 300mL refrigerates in advance is got, the 300mL high purity water refrigerated in advance is added under the condition stirred, by both mixtures in 4 DEG C of reaction 24h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 3
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, stannous chloride solution is slowly added in thioacetyl amine aqueous solution, stir 10min and form presoma;
(2) 300mL presoma is got, 300mL high purity water is added under the condition stirred, by both mixtures in 80 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 4
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 600mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 5
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 150mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 6
(1) in 200mL dehydrated alcohol, add 2.051g tin protochloride, be stirred to and dissolve completely, add 1.623g thiocarbamide, be stirred to and dissolve completely, slowly added in thiourea solution by stannous chloride solution in 200mL dehydrated alcohol, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 7
(1) in 200mL methyl alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL methyl alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 8
(1) in 200mL propyl alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL propyl alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL high purity water is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 9
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL sodium dodecyl sulfate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 10
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL Sodium dodecylbenzene sulfonate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 11
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL Sodium palmityl sulfate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 12
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL dioctyl succinate disulfonate acid solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 13
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL cetylpyridinium chloride solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 14
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL brocide solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 15
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL potassium stearate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 16
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL potassium oleate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 17
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL potassium laurate solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 18
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL polyglycol solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 21
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL bovine serum albumin solution (1g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment 22
(1) in 200mL dehydrated alcohol, 2.051g tin protochloride is added, be stirred to and dissolve completely, in 200mL dehydrated alcohol, add 1.602g thioacetamide, be stirred to and dissolve completely, slowly added by stannous chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma;
(2) 300mL presoma is got, 300mL sodium dodecyl sulfate solution (4g/L) is added under the condition stirred, by both mixtures in 40 DEG C of reaction 0.5h, it is centrifugal with the centrifugation rate of 13000r/min after reaction terminates, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, obtain water-soluble stannous sulfide quantum dot after drying.
Embodiment above describes ultimate principle of the present invention, principal character and advantage; the technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (4)
1. the preparation method of a water-soluble stannous sulfide quantum dot, it is characterized in that comprising the following steps: pink salt and sulfocompound are dissolved in organic solvent as Xi Yuan and sulphur source by (1) respectively, by Xi Yuan and sulphur source, mixing under condition that is ultrasonic or that stir is carried out reaction and is formed presoma, wherein pink salt is tin chloride, sulfocompound is thioacetamide or thiocarbamide, and organic solvent is methyl alcohol, ethanol or propyl alcohol, (2) presoma that step (1) is formed is added high purity water, the aqueous solution containing tensio-active agent or the aqueous solution containing protein, wherein tensio-active agent is sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, Sodium palmityl sulfate, dioctyl succinate disulfonate acid, cetylpyridinium chloride, brocide, potassium stearate, potassium oleate, potassium laurate or polyoxyethylene glycol, protein is bovine serum albumin, presoma and high purity water, the volume ratio of the aqueous solution containing tensio-active agent or the aqueous solution containing protein is 1:0.5-2, then said mixture is reacted 0.5-24h in 4-80 DEG C, the centrifugation rate that reaction terminates to be placed on 13000r/min in whizzer is centrifugal, the product dehydrated alcohol of centrifugal gained and high purity water replace washing three times, water-soluble stannous sulfide quantum dot is obtained after drying.
2. the preparation method of water-soluble stannous sulfide quantum dot according to claim 1, is characterized in that: described pink salt and the mol ratio of sulfocompound are 0.43:1.
3. the preparation method of water-soluble stannous sulfide quantum dot according to claim 1, is characterized in that: the mass concentration of the described aqueous solution containing tensio-active agent is 1-4g/L.
4. the preparation method of water-soluble stannous sulfide quantum dot according to claim 1, is characterized in that: the mass concentration of the described aqueous solution containing protein is 1-4g/L.
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| CN105800674A (en) * | 2016-03-23 | 2016-07-27 | 昆明理工大学 | Preparation method and application of tin sulfide material |
| CN108452302A (en) * | 2018-02-09 | 2018-08-28 | 深圳大学 | A kind of delivery system and preparation method thereof based on stannous sulfide quantum dot |
| CN108478793A (en) * | 2018-02-09 | 2018-09-04 | 深圳大学 | A kind of stannous sulfide nanometer light thermit powder and preparation method thereof |
| CN108821332A (en) * | 2018-07-05 | 2018-11-16 | 苏州影睿光学科技有限公司 | A kind of preparation method of near-infrared stannous sulfide nano particle |
| CN110217814A (en) * | 2019-06-19 | 2019-09-10 | 昆明物理研究所 | A kind of preparation method of indium sulfide nano dot |
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| CN105800674A (en) * | 2016-03-23 | 2016-07-27 | 昆明理工大学 | Preparation method and application of tin sulfide material |
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| CN108478793A (en) * | 2018-02-09 | 2018-09-04 | 深圳大学 | A kind of stannous sulfide nanometer light thermit powder and preparation method thereof |
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| CN108821332A (en) * | 2018-07-05 | 2018-11-16 | 苏州影睿光学科技有限公司 | A kind of preparation method of near-infrared stannous sulfide nano particle |
| CN110217814A (en) * | 2019-06-19 | 2019-09-10 | 昆明物理研究所 | A kind of preparation method of indium sulfide nano dot |
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