CN104876257B - A kind of preparation method of water solublity cadmiumsulfide quantum dot - Google Patents
A kind of preparation method of water solublity cadmiumsulfide quantum dot Download PDFInfo
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Abstract
The invention discloses the preparation method of a kind of water solublity cadmiumsulfide quantum dot, comprise the following steps: cadmium salt and sulfur-containing compound are dissolved in organic solvent respectively as cadmium source and sulfur source, the mixing under conditions of ultrasonic or stirring of cadmium source and sulfur source is carried out reaction and forms presoma；The presoma formed is added high purity water, the aqueous solution containing surfactant or the aqueous solution containing protein, then said mixture is prepared water solublity cadmiumsulfide quantum dot in 4 80 DEG C of reaction 8 24h.The present invention is compared with the preparation method of existing cadmiumsulfide quantum dot, and the preparation method of the present invention is the most controlled, reaction condition is gentle, cheaper starting materials is easy to get, environmentally friendly and prepared product has good fluorescence.
Description
Technical field
The invention belongs to the synthesis technical field of inorganic functional material cadmium sulfide, be specifically related to the preparation method of a kind of water solublity cadmiumsulfide quantum dot.
Background technology
Quantum dot, can be described as again nanocrystalline, and particle diameter is typically in the range of between 1-10nm, and owing to electronics and hole are by quantum confinement, continuous print band structure becomes the discrete energy levels structure with molecular characterization, can launch fluorescence after being excited.Due to quantum size effect, skin effect, 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 solaode, luminescent device and optical bio labellings.Cadmiumsulfide quantum dot is a kind of common quantum dot, there is the PhotoelectrochemicalProperties Properties of uniqueness, it is widely used in photoelectrochemical cell and energy storage device, has a wide range of applications in many fields such as luminescence generated by light, electroluminescent, sensor, material of infrared window and photocatalysis.At present, the method of synthesizing cadmium sulfide quantum dot mainly has electrochemical method, hot injecting method, ion exchange and hydro-thermal method etc., these synthetic method major parts need the device of high temperature and complexity, complex operation step and apply to aspect biology and need to be converted into water-soluble quantum dot.At present, the method for synthesizing water-solubility cadmiumsulfide quantum dot is little, and its reason is: the quantum dot that (1) synthesizes is unstable, the most easily reunites；(2) crystallinity is bad, limits its application；(3) productivity is relatively low, is difficult to apply in commercial production.Therefore, synthesizing water-solubility cadmiumsulfide quantum dot is faced with huge challenge, is also the focus studied in recent years.
Summary of the invention
Present invention solves the technical problem that the preparation method that there is provided a kind of water solublity cadmiumsulfide quantum dot, this preparation method uses a kind of new proportioning raw materials to prepare the stable and preferable cadmiumsulfide quantum dot of water solublity, and prepared water solublity cadmiumsulfide quantum dot has the strongest fluorescence property.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of preparation method of water solublity cadmiumsulfide quantum dot, it is characterized in that comprising the following steps: cadmium salt and sulfur-containing compound are dissolved in organic solvent as cadmium source and sulfur source by (1) respectively, the mixing under conditions of ultrasonic or stirring of cadmium source and sulfur source is carried out reaction and forms presoma, wherein cadmium salt is Caddy (Cleary), cadmium nitrate or cadmium acetate, sulfur-containing compound is thioacetamide or thiourea, and organic solvent is methanol, ethanol or propanol；null(2) presoma step (1) formed adds high purity water、Aqueous solution containing surfactant or the aqueous solution containing protein，Wherein surfactant is dodecyl sodium sulfate、DBSA、Sodium hexadecyl sulfate、Dioctyl succinate disulfonate acid、Cetylpyridinium chloride、Brocide、Potassium stearate、Potassium oleate、Potassium laurate or Polyethylene Glycol，Protein is bovine serum albumin，Presoma and high purity water、The volume ratio of the aqueous solution containing surfactant or the aqueous solution containing protein is 1:0.5-2，Then said mixture is reacted 8-24h in 4-80 DEG C，It is centrifugal that reaction terminates to be placed in centrifuge the centrifugation rate with 13000r/min，Alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water，Obtain water solublity cadmiumsulfide quantum dot after drying.
Limits further the mol ratio of cadmium salt and sulfur-containing compound as 0.58:1.
Limit further the mass concentration of aqueous solution of surfactant as 1-4g/L.
Limit further the mass concentration of aqueous solution of protein as 1-4g/L.
The outstanding advantages of the present invention is to have employed raw material cheap and easy to get, utilizes presoma to be hydrolyzed under different temperature and times from high purity water reaction, controlled prepared different crystalline types, different size, can the cadmiumsulfide quantum dot of stable existence.Compared with the preparation method of existing cadmiumsulfide quantum dot, the preparation method of the present invention is the most controlled, reaction condition is gentle, cheaper starting materials is easy to get, environmentally friendly and prepared product has good fluorescence.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the water solublity cadmiumsulfide quantum dot that the embodiment of the present invention 1 prepares, and Fig. 2 is the transmission electron microscope picture of the water solublity cadmiumsulfide quantum dot that the embodiment of the present invention 1 prepares.
Detailed description of the invention
Being described in further details the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all technology realized based on foregoing of the present invention belong to the scope of the present invention.
Embodiment 1
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
From figure 1 it appears that the crystalline types of the water solublity cadmiumsulfide quantum dot of this method synthesis is amorphous.From figure 2 it can be seen that the cadmiumsulfide quantum dot particle diameter of this method synthesis is the least, less than 5nm, and size is homogeneous, good dispersion.
Embodiment 2
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, stirring 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 24h in 4 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 3
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, stirring 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 80 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 4
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 600mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 5
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 150mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 6
(1) in 200mL dehydrated alcohol, 3.808g cadmium nitrate is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added in thioacetyl amine aqueous solution by cadmium nitrate solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 7
(1) in 200mL dehydrated alcohol, 2.846g cadmium acetate is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium acetate solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 8
(1) adding 2.820g Caddy (Cleary) in 200mL dehydrated alcohol, stirring, to being completely dissolved, adds 1.623g thiourea in 200mL dehydrated alcohol, and cadmium chloride solution, to being completely dissolved, is slowly added in thiourea solution by stirring, and ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 9
(1) adding 2.820g Caddy (Cleary) in 200mL methanol, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL methanol, and cadmium chloride solution, to being completely dissolved, is slowly added in thioacetyl amine aqueous solution by stirring, and ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 10
(1) adding 2.820g Caddy (Cleary) in 200mL propanol, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL propanol, and cadmium chloride solution, to being completely dissolved, is slowly added in thioacetyl amine aqueous solution by stirring, and ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL high purity water is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 11
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL sodium dodecyl sulfate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 12
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL dodecylbenzene sodium sulfonate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 13
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL sodium hexadecyl sulfate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 14
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL dioctyl succinate disulfonate acid solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 15
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL cetylpyridinium chloride solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 16
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL brocide solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 17
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL potassium stearate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 18
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL potassium oleate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 19
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL potassium laurate solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 20
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL polyglycol solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 21
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL bovine serum albumin solution (1g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment 22
(1) in 200mL dehydrated alcohol, 2.820g Caddy (Cleary) is added, stirring, to being completely dissolved, adds 1.602g thioacetamide in 200mL dehydrated alcohol, and stirring is to being completely dissolved, being slowly added to by cadmium chloride solution in thioacetyl amine aqueous solution, ultrasonic 10min forms presoma；
(2) 300mL presoma is taken, 300mL sodium dodecyl sulfate solution (4g/L) is added under conditions of stirring, both mixture are reacted 8h in 40 DEG C, reaction is centrifuged with the centrifugation rate of 13000r/min after terminating, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; under the scope without departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements each fall within the scope of protection of the invention.
Claims (3)
1. the preparation method of a water solublity cadmiumsulfide quantum dot, it is characterized in that comprising the following steps: cadmium salt and sulfur-containing compound are dissolved in organic solvent as cadmium source and sulfur source by (1) respectively, the mixing under conditions of ultrasonic or stirring of cadmium source and sulfur source is carried out reaction and forms presoma, wherein cadmium salt is Caddy (Cleary), cadmium nitrate or cadmium acetate, sulfur-containing compound is thioacetamide or thiourea, and organic solvent is methanol, ethanol or propanol；(2) presoma step (1) formed adds high purity water or the aqueous solution containing protein, wherein protein is bovine serum albumin, presoma is 1:0.5-2 with the volume ratio of high purity water or the aqueous solution containing protein, then said mixture is reacted 8-24h in 4-80 DEG C, it is centrifugal that reaction terminates to be placed in centrifuge the centrifugation rate with 13000r/min, alternately washing three times of the product dehydrated alcohol of centrifugal gained and high purity water, obtain water solublity cadmiumsulfide quantum dot after drying.
The preparation method of water solublity cadmiumsulfide quantum dot the most according to claim 1, it is characterised in that: described cadmium salt is 0.58:1 with the mol ratio of sulfur-containing compound.
The preparation method of water solublity cadmiumsulfide quantum dot the most according to claim 1, it is characterised in that: the mass concentration of the described aqueous solution containing protein is 1-4g/L.
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| CN109100340B (en) * | 2018-08-23 | 2020-10-16 | 浙江理工大学 | Preparation method of implantable sensor modified by cadmium sulfide quantum dots |
| CN110184048A (en) * | 2019-06-19 | 2019-08-30 | 岭南师范学院 | A kind of preparation method of cadmiumsulfide quantum dot |
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