CN105776316A - Universal synthesis method for nanocrystals - Google Patents
Universal synthesis method for nanocrystals Download PDFInfo
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- CN105776316A CN105776316A CN201410775513.XA CN201410775513A CN105776316A CN 105776316 A CN105776316 A CN 105776316A CN 201410775513 A CN201410775513 A CN 201410775513A CN 105776316 A CN105776316 A CN 105776316A
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Abstract
The invention discloses a universal synthesis method for nanocrystals. The method comprises the steps: firstly, mixing a metal source with a water/pyridine mixed solvent so as to obtain a metal source solution, wherein the metal source is selected from zinc acetate, copper acetate, lead acetate, silver acetate, nickel acetate, cadmium acetate, ferric acetate, magnesium acetate or barium acetate, and the concentration of the metal source solution is 1mol/L to 5mol/L; then, mixing a nonmetal source with water so as to obtain a nonmetal source solution, wherein the nonmetal source is sodium sulfide or potassium hydroxide, and the concentration of the nonmetal source solution is 1mol/L to 5mol/L; and finally, adding the nonmetal source solution into the metal source solution, carrying out a reaction for 2 to 20 hours at the temperature of 60 DEG C to 100 DEG C, and carrying out centrifugal separation, thereby obtaining the nanocrystals. According to the universal synthesis method for the nanocrystals, pyridine serves as a ligand; the universal synthesis method has the characteristics that the reaction conditions are mild, the preparation process and product morphology are controllable, and the universality is high; and the prepared nanocrystals have hydrophilicity and have lipophilicity after ligand exchange, so that the field of application of the nanocrystals is enlarged.
Description
Technical field
The present invention relates to field of nano material preparation, be specifically related to a kind of nanocrystalline universal synthesis method.
Background technology
Comparing block materials, nano material has three big features: (1) quantum size effect；(2) skin effect；(3) macro quanta tunnel effect.These features make nano material show make new advances optics, electricity, catalysis, fluorescence, mechanical property so that nano material is widely used in electronics, catalytic chemistry, pharmacy, magnetizing mediums etc..
The preparation method of nano material can be divided into three major types: vapor phase method, liquid phase method and high-energy ball milling method.Applying more is first two method, but vapor phase method equipment needed thereby is complicated, and preparation cost is higher, it is impossible to complete mass-produced requirement；On the contrary, liquid phase method equipment needed thereby is simple, has had mass-produced potentiality.
At present, Liquid preparation methods nano material can be divided into:
(1) sol-gel process: what sol-gel process obtained is the nano material of solid, this limit to a certain extent nano material some field application [Zhang Wanzhong, Li Wanxiong. nano materials research summarize, Agricultural College of Hubei Prov.'s journal, 2003,23 (5): 397-340]；
(2) sedimentation method: the advantage of the sedimentation method is that course of reaction is simple, and cost is low, it is simple to industrialized production, but the material particle size of preparation is wayward, and granular size is uneven so that the nano material application in the field such as electricity, optics is restricted；
(3) hydro-thermal and solvent-thermal method: hydro-thermal and solvent thermal are using the solvent in the high temperature in autoclave, reaction under high pressure environment as reaction medium, because equipment needed thereby is complicated, [Wu Jinqiao cannot be produced equally in a large number, Wang Yukun. the preparation technique of liquid phase of nano material and progress thereof, Xi'an shiyou University's journal, 2002,17 (3): 31-36]；
(4) microemulsion method: microemulsion method experimental provision is simple, energy consumption is low, processing ease, and the nano-powder grain diameter of synthesis is little, particle size distribution range is little and is easily controlled, surface activity is high, and monodispersity is good, not easily reunites, there is industrial production prospect [ShinodaK, FribergS.ColloidInterfaceScience, 1977,4:281-287]；
(5) high temperature injection method: high temperature injection method can obtain high nanocrystalline of size uniformity, degree of crystallinity, but most high temperature injection reactions are amplification quantity to produce mostly, and gained is nanocrystalline is wrapped up by sterically hindered big organic molecule, need to carry out ligand exchange could apply in some field；
(6) other method.
All there is respective drawback in above-mentioned preparation method, and cannot be common to multiple nanocrystalline preparation, therefore, invents simple and highly versatile the multiple nanocrystalline preparation method of a kind of method and has important practical significance.
Summary of the invention
The present invention provides a kind of nanocrystalline universal synthesis method, with pyridine for part, having that reaction condition gentleness, preparation process and product morphology be controlled and the feature of highly versatile, what prepare nanocrystalline has hydrophilic, there is lipophile after ligand exchange, extend nanocrystalline application.
A kind of nanocrystalline universal synthesis method, comprises the steps:
(1) source metal is mixed with water/pyridine mixed solvent, obtain source metal solution；
Described source metal is metal acetate salt, and the concentration of described source metal solution is 1～5mol/L；
(2) non-metal source is mixed with water, obtain non-metal source solution；
Described non-metal source is sodium sulfide or potassium hydroxide, and the concentration of described non-metal source solution is 1～5mol/L；
(3) described non-metal source solution is added in source metal solution, at 60～100 DEG C, react 2～20h, be centrifugally separating to obtain described nanocrystalline.
The present invention is with water and pyridine mixed liquor for solvent, and select specific non-metal source and source metal coupling, under the effect of pyridine (pyridine is as part and solvent dual role), it is achieved the synchronous growth of source metal and non-metal source, it is thus achieved that highly purified nanocrystalline.The use of mixed solution simultaneously is conducive to reaction to carry out in a mild condition, it is no longer necessary to solvent thermal and condition of high voltage necessary to hydro-thermal method.This point is the maximum difference of the method and hydro-thermal method, even if both use similar raw material system.Can be understood as the use of smaller ligand and instead of the necessary harsh reaction condition of additive method to a certain extent.
As preferably, in step (1), in described source metal solution, the volume ratio of water and pyridine is 1:1～5.
As preferably, in step (3), the volume ratio of described non-metal source solution and source metal solution is 1:1～5.
In the present invention, with the stability of complex that formed with pyridine for principle, choose source metal.Based on this, it is preferred that, the concentration of described source metal solution is 1.25mol/L.
In reaction system, using water as reaction dissolvent, pyridine makes the nano-crystalline granule of final preparation have hydrophilic/lipophilic as part, according to source metal different solubility in a solvent, suitably regulate the ratio of water and pyridine in source metal solution, it is preferred that, in described source metal solution, the volume ratio of water and pyridine is 1:3.
In the present invention, the homogeneity of the nanocrystalline particle diameter of preparation is had considerable influence by non-metal source concentration, and considers the ability providing sulfur or oxygen, it is preferred that, the concentration of described non-metal source solution is 1.67mol/L.
As preferably, in step (3), it is 1min～4h that non-metal source solution is added drop-wise to the time in source metal solution.
Under the effect of pyridine, aqueous solvent matches with specific non-metal source and source metal, it is possible to achieve the synchronous growth of source metal and non-metal source, it is thus achieved that highly purified nanocrystalline.Most preferably:
In step (1), the concentration of described source metal solution is 1.25mol/L；In described source metal solution, the volume ratio of water and pyridine is 1:3；
In step (2), the concentration of described non-metal source solution is 1.67mol/L；
In step (3), it is 5～60min that non-metal source solution is added drop-wise to the time in source metal solution.
Compared with prior art, the invention have the advantages that
The invention discloses the universal method of a kind of smaller ligand synthesizing nanocrystalline, comparing sol-gel process, what this method obtained nanocrystalline has a hydrophilic, can carry out simple ligand exchange simultaneously, thus obtaining oil loving nanocrystalline, extend nanocrystalline application；Comparing the sedimentation method, the use of smaller ligand makes material particle size be easily controlled；Compare hydro-thermal method and solvent-thermal method, this method equipment requirements is simple；Comparing high temperature injection method, smaller ligand synthetic method, yield is more, and part is sterically hindered little.In a word, the method for smaller ligand synthesizing nanocrystalline has the potentiality of industrialized production.
Accompanying drawing explanation
Fig. 1 is the sign of the ZnO nano crystalline substance of embodiment 1 synthesis, and (a) TEM schemes, (b) XRD figure；Fig. 2 is the sign nanocrystalline for CuO of the 2-in-1 one-tenth of embodiment, and (a) TEM schemes, (b) XRD figure, (c) ligand exchange figure；
Fig. 3 is the sign nanocrystalline for CdS of embodiment 3 synthesis, and (a) TEM schemes, (b) XRD figure；
Fig. 4 is the Cd (OH) of embodiment 4 synthesis2Nanocrystalline XRD figure；
Fig. 5 is the Ni (OH) of embodiment 5 synthesis2Nanocrystalline XRD figure；
Fig. 6 is the Ag of embodiment 6 synthesis2The XRD figure that S is nanocrystalline；
Fig. 7 is the XRD figure nanocrystalline for PbS of embodiment 7 synthesis.
Detailed description of the invention
In order to be more fully understood that the present invention, the solution of the present invention is expanded on further below in conjunction with embodiment, but present disclosure is not limited solely to the following examples.
The synthesis that embodiment 1ZnO is nanocrystalline
0.05mol zinc acetate is dissolved in 10mL water and 30mL pyridine mixed solvent；Meanwhile, 0.05mol potassium hydroxide is dissolved in 30mL water；Then, being instilled by potassium hydroxide solution in zinc acetate solution, 20min drips off；Finally reactant liquor is warming up to 80 DEG C, reacts 2h.With acetone, Zinc oxide nanoparticle is precipitated, be centrifuged and obtain white solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure Zinc oxide nanoparticle, its transmission electron microscope picture and XRD figure are as shown in Figure 1.
The synthesis that embodiment 2CuO is nanocrystalline
0.05mol Schweinfurt green is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol potassium hydroxide, instill in Schweinfurt green solution, 20min drips off, and reacts 2h.With acetone, nano copper sulfate particle is avaled, be centrifuged and obtain dark brown solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure copper oxide nanometer particle, its transmission electron microscope picture and XRD figure are as shown in Figure 2.
The synthesis that embodiment 3CdS is nanocrystalline
0.05mol cadmium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol sodium sulfide, instill in cadmium acetate solution, 20min drips off, and reacts 2h.With acetone, cadmium sulfide nanoparticles is avaled, be centrifuged and obtain orange/yellow solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure cadmium sulfide nanoparticles, its transmission electron microscope picture and XRD figure are as shown in Figure 3.
Embodiment 4Cd (OH)2Nanocrystalline synthesis
0.05mol cadmium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol potassium hydroxide, instill in cadmium acetate solution, 20min drips off, and reacts 2h.With acetone, Cadmium hydrate. nanoparticle precipitate is got off, be centrifuged and obtain white solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure Cadmium hydrate. nano-particle, its XRD figure is as shown in Figure 4.
Embodiment 5Ni (OH)2Nanocrystalline synthesis
0.05mol nickel acetate is dissolved in 10mL water and 30mL pyridine mixed solvent；Meanwhile, 0.05mol potassium hydroxide is dissolved in 30mL water；Then, being instilled by potassium hydroxide aqueous solution in nickel acetate solution, 20min drips off；Finally mixed liquor is warming up to 80 DEG C, reacts 2h.With acetone, nickel hydroxide nano particle precipitation is got off, be centrifuged and obtain cyan solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure nickel hydroxide nano granule, its XRD figure is as shown in Figure 5.
Embodiment 6Ag2The synthesis that S is nanocrystalline
0.05mol silver acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, is warming up to 75 DEG C when lucifuge；Meanwhile, being dissolved in 30mL water by 0.025mol sodium sulfide, instill in silver acetate solution, 10min drips off, and reacts 30min.With acetone, silver sulfide nano particle is precipitated, be centrifuged and obtain black solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure silver sulfide nano particle, its XRD figure is as shown in Figure 6.
The synthesis that embodiment 7PbS is nanocrystalline
0.05mol lead acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol sodium sulfide, instill in lead acetate solution, 20min drips off, and reacts 2h.With acetone, lead sulfide nanoparticles is precipitated, be centrifuged and obtain black solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure lead sulfide nanoparticles, its XRD figure is as shown in Figure 7.
The synthesis that embodiment 8MgS is nanocrystalline
0.05mol magnesium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, 0.05mol sodium sulfide being dissolved in 30mL water, instill magnesium acetate solution, 20min drips off, and reacts 2h.With acetone, magnesium sulfide nano-particle is avaled, be centrifuged and obtain brown solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain brown magnesium sulfide nano-particle.
The synthesis that embodiment 9BaS is nanocrystalline
0.05mol barium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol sodium sulfide, instill in barium acetate solution, 20min drips off, and reacts 2h.With acetone, barium sulfide nanoparticle precipitate is got off, be centrifuged and obtain white solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain white barium sulfide nano-particle.
Embodiment 10Mg (OH)2Nanocrystalline synthesis
0.05mol magnesium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol potassium hydroxide, instill in magnesium acetate solution, 20min drips off, and reacts 2h.With acetone, magnesium hydroxide nanoparticles is precipitated, be centrifuged and obtain white solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure magnesium hydroxide nanoparticles.
Embodiment 11Ba (OH)2Nanocrystalline synthesis
0.05mol barium acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol potassium hydroxide, instill in barium acetate solution, 20min drips off, and reacts 2h.With acetone, barium hydroxide nanoparticle precipitate is got off, be centrifuged and obtain white solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure barium hydroxide nano-particle.
Embodiment 12Fe (OH)3Nanocrystalline synthesis
0.05mol iron acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, then heats to 80 DEG C；Meanwhile, being dissolved in 30mL water by 0.05mol potassium hydroxide, instill in iron acetate solution, 20min drips off, and reacts 2h.With acetone, hydrated ferric oxide. nanoparticle precipitate is got off, be centrifuged and obtain red brown solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure hydrated ferric oxide. nano-particle.
Embodiment 13Ag2The synthesis that O is nanocrystalline
0.05mol silver acetate is dissolved in 10mL water and in 30mL pyridine mixed solvent, is warming up to 75 DEG C when lucifuge；Meanwhile, being dissolved in 30mL water by 0.025mol potassium hydroxide, instill in silver acetate solution, 10min drips off, and reacts 30min.With acetone, silver oxide nano-particle is avaled, be centrifuged and obtain black solid.Add 30mL water, ultrasonic 10min；Add 30mL acetone, centrifugal, obtain pure silver oxide nano-particle.
Comparative example 1
Being not added with pyridine, other step is identical with embodiment 1, and the product prepared easily is reunited, bad dispersion, it is impossible to form the nano-particle of size uniformity.
Comparative example 2
Replacing zinc acetate with zinc nitrate, other condition, step are identical with embodiment 1, in the product prepared, and nano-particle yardstick heterogeneity, it is impossible to obtain the homogeneous phase being obtained by reacting with zinc acetate, not easily disperse in the solution simultaneously.
Claims (8)
1. universal synthesis method one kind nanocrystalline, it is characterised in that comprise the steps:
(1) source metal is mixed with water/pyridine mixed solvent, obtain source metal solution；
Described source metal is metal acetate salt, and the concentration of described source metal solution is 1～5mol/L；
(2) non-metal source is mixed with water, obtain non-metal source solution；
Described non-metal source is sodium sulfide or potassium hydroxide, and the concentration of described non-metal source solution is 1～5mol/L；
(3) described non-metal source solution is added in source metal solution, at 60～100 DEG C, react 2～20h, be centrifugally separating to obtain described nanocrystalline.
2. nanocrystalline universal synthesis method according to claim 1, it is characterised in that in step (1), in described source metal solution, the volume ratio of water and pyridine is 1:1～5.
3. nanocrystalline universal synthesis method according to claim 1 and 2, it is characterised in that in step (1), the concentration of described source metal solution is 1.25mol/L.
4. the volume ratio of nanocrystalline universal synthesis method according to claim 3, it is characterised in that in described source metal solution, water and pyridine is 1:3.
5. nanocrystalline universal synthesis method according to claim 4, it is characterised in that in step (2), the concentration of described non-metal source solution is 1.67mol/L.
6. the volume ratio of universal synthesis method nanocrystalline according to claim 1 or 5, it is characterised in that in step (3), described non-metal source solution and source metal solution is 1:1～5.
7. the volume ratio of nanocrystalline universal synthesis method according to claim 6, it is characterised in that in step (3), described non-metal source solution and source metal solution is 3:4.
8. nanocrystalline universal synthesis method according to claim 1, it is characterised in that in step (3), it is 1min～4h that non-metal source solution is added drop-wise to the time in source metal solution.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767816A (en) * | 2010-01-12 | 2010-07-07 | 浙江大学 | Method for preparing monodisperse CdS nanocrystal |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multilayer alpha-Ni(OH)2 or NiO nanocrystal by microwave solvothermal method |
| US20120088845A1 (en) * | 2010-04-23 | 2012-04-12 | Gonen Williams Zehra Serpil | Synthesis, capping and dispersion of nanocrystals |
| CN104071827A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Method for synthesizing ordered laminar nanometer zinc oxide by using sodium dodecyl sulfate as template |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767816A (en) * | 2010-01-12 | 2010-07-07 | 浙江大学 | Method for preparing monodisperse CdS nanocrystal |
| US20120088845A1 (en) * | 2010-04-23 | 2012-04-12 | Gonen Williams Zehra Serpil | Synthesis, capping and dispersion of nanocrystals |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multilayer alpha-Ni(OH)2 or NiO nanocrystal by microwave solvothermal method |
| CN104071827A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Method for synthesizing ordered laminar nanometer zinc oxide by using sodium dodecyl sulfate as template |
Non-Patent Citations (2)
| Title |
|---|
| JUN LI等: "Manipulating surface ligands of Copper Sulfide nanocrystals: Synthesis,characterization, and application to organic solar cells", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| PANDENG LI等: "Solvents Induced ZnO Nanoparticles Aggregation Associated with Their Interfacial Effect on Organic Solar Cells", 《APPL. MATER. INTERFACES》 * |
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Application publication date: 20160720 |