CN102633297A - Preparation method of general-purpose multi-metal sulfide nano-material - Google Patents
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Abstract
The invention discloses a preparation method of a general-purpose multi-metal sulfide nano-material. The preparation method comprises the following steps of: taking two or more different metal diethyldithiocarbamates, or two or more different metal phenanthroline diethyldithiocarbamates, or the combination of the metal diethyldithiocarbamates and the metal phenanthroline diethyldithiocarbamates as reaction predecessors, performing co-thermal decomposition in a mixed solution of surfactants with different coordination properties, and performing nucleation and growth so as to prepare a high-quality multi-metal sulfide nano-material by one step. The multi-metal sulfide prepared by the preparation method disclosed by the invention has the advantages of pure phase state, adjustable composition, uniform and controllable appearance and size, high yield, low toxicity or no toxicity, better dispersivity in a non-polar organic solvent, easiness in control of reaction conditions, mild preparation conditions, simple operation, good repeatability and capability of realizing large-scale production.
Description
Technical field
The invention belongs to technical field of nano material, relate in particular to a kind of preparation method of general multi-element metal sulfide nano-material.
Background technology
Multi-element metal sulfide has performances such as good light, electricity, magnetic, catalysis, is widely used in semi-conductor, biomedicine, photo luminescent devices, solar cell, photolysis water hydrogen, device for non-linear optical, fiber optics communication, lubricant, magneto-optical recorder material etc.Along with the green sustainability requirement to the energy, solar cell and photolysis water hydrogen are the focuses of current energy research.Some I-III-VI
2The ternary semiconductor nano material has tempting prospect at solar cell and photovoltaic applications field.Along with the research and the application of multi-element metal sulfide are day by day extensive, emerged the preparation method of a collection of multi-element metal sulfide nano-material.
For example: Du Weimin etc. have applied for " monodisperse ternary chalkogenide AgInS
2The preparation method " 200710040756.9) and " monodisperse ternary chalkogenide CuInS (number of patent application:
2The preparation method " (number of patent application: 200710040757.3) patent, this two invention are to adopt chemical solution method that each metal-salt, sulphur source and alkylamine are scattered in to carry out solvent heat treatment in the solvent to obtain each two kinds of monodispersed ternary sulfide nanocrystalline.Chen Wentong has applied for that (number of patent application: patent 200910151022.7), this invention adopt solid reaction process to prepare M " Novel Chalcogenides semiconductor material "
3Q
2X
2(M=Zn, Cd, Hg; Q=S, Se, Te; X=Cl, Br, I) serial chalcogen compound semiconductor material, but this method needs vacuum-sealing also to need various complex apparatus, and the high production cycle length of temperature of reaction etc.Chen Jun etc. have applied for " ZnIn
2S
4Nano material and compound method thereof and application " (number of patent application: patent 200610013827.1); this invention is that employing solvent thermal/hydrothermal method selection zinc salt, indium salt and organic sulfide are that raw material carries out solvent thermal/hydro-thermal reaction; but this method requires high pressure, problems such as long reaction time and not environmental protection of raw material.Liu Qiangchun, Dai Jianming etc. have applied for " a kind of wurtzite structure CuInS
2Solvent process for thermosynthesizing " (number of patent application: patent 200910116920.9), this invention are that to adopt the muriate and the thiocarbamide of copper and indium be raw material, in thanomin, carry out the CuInS that solvent heat treatment obtains wurtzite
2Metastable phase, but this method needs HTHP, and preparation cycle is long, and pattern is wayward etc.Mi Liwei, Shen Changyu etc. have applied for " the binary sulfide Cu with flower-like structure
XZn
1-XS particulate and preparation method thereof " 200910227295.5), " binary sulfide Pb (number of patent application: with flower-like structure
XZn
1-XS particulate and preparation method thereof " 200910227294.0), " binary sulfide Cd (number of patent application: with flower-like structure
XZn
1-XS particulate and preparation method thereof " (number of patent application: 200910227296.X), " binary sulfide Ag with flower-like structure
XZn
1-XS particulate and preparation method thereof " (number of patent application: patent 200910227297.4), this series of patents are to adopt ion exchange method, and this method is the ZnS particulate that makes flower-like structure earlier; the soluble salt that adds lead, cadmium, copper and silver then carries out IX and obtains; the appearance of this method all depends on the pattern of ZnS, and the pattern of whole ternary sulfide is wayward, and needs two-step approach; more loaded down with trivial details, and size is wayward etc.Han Tukui; The king orders Thailand etc. and has applied for " zincblende lattce structure and wurtzite structure CuInS quantum dot and preparation method thereof " (number of patent application: patent 200910251728.0); This invention is to adopt solvent thermal reaction reconciliation statement surface-active agent to synthesize the copper indium sulphur quantum dot of zink sulphide and wurtzite structure; It is HTHP that but this method requires reaction conditions, and condition is harsh, and appearance and size is wayward.Product phase purity is low, yields poorly.Zhou Jicheng; Li Shaowen etc. have applied for " yellow copper structure CIS powdered material and liquid phase preparation process thereof " (number of patent application: patent 201110094854.7); It is carrier that existing machine mixed solvent or organic single solvent are adopted in this invention, under normal pressure, synthesizes yellow copper ore CIS powder with the liquid-phase reflux method.This method reaction times is longer, and pattern is easy-regulating not, and particle is bigger.Comprehensive above-mentioned multiple preparation method exists that preparation condition is harsh relatively, product phase purity is lower, and size and valence state are difficult to problems such as control.
Summary of the invention
Seeing that the deficiency of the existence of above-mentioned prior art; The objective of the invention is to propose a kind of general I-III-VI family and the preparation method of II-IV-VI family multi-element metal sulfide nano-material; So that the general preparation method of the higher multi-element metal sulfide of a kind of large-scale production and quality to be provided, further promote the application of multi-element metal sulfide.The general formula of I-III-VI family and II-IV-VI family multi-element metal sulfide nano-material is M
xN
yQ
zS
t(M, N, Q are Ag, Cu, Pb, Zn, In, Bi, Cd, Sb, W, Mn, Fe, Sn, Ni, Ti, Hg, Mo, Cr, any three kinds of elements among the Co; X>=1; Y>=1; Z>=0; T is the numerical value of being confirmed by the value of the valence state of the element except sulphur in the general formula and x, y, z).
The object of the invention; To be achieved through following technical scheme: a kind of preparation method of general multi-element metal sulfide nano-material; Wherein: adopt two or more different metallic N,N-Diethyldithiocarbamic Acid; Perhaps two or more different metallic phenanthroline N,N-Diethyldithiocarbamic Acid; Perhaps the combination of metal N,N-Diethyldithiocarbamic Acid and metal phenanthroline N,N-Diethyldithiocarbamic Acid is carried out common thermolysis as pre-reaction material in having the tensio-active agent mixing solutions of different coordination characteristics, and nucleation, growth; One step made that phase is pure, thing is mutually controlled, the multi-element metal sulfide nano-material of pattern and size adjustable, and its step is following:
Step 1: the mol ratio of pre-reaction material according to metal constituent element in the multi-element metal sulfidic material composition is dissolved in the tensio-active agent mixing solutions with different coordination characteristics,, kept 10 minutes ~ 20 minutes 120 ℃ and following vacuumizing;
Step 2: under protection of inert gas, the resulting solution of step 1 is warming up to more than 180 ℃, more than 5 minutes;
Step 3: after the solution that step 2 is obtained naturally cools to room temperature, add polar organic solvent, after centrifugal, washing and drying, obtain the multi-element metal sulfide nano-material.
Preferably; The preparation method of above-mentioned a kind of general multi-element metal sulfide nano-material, wherein: the metallic element in the said pre-reaction material comprises any one among silver-colored Ag, plumbous Pb, copper Cu, cadmium Cd, bismuth Bi, iron Fe, cobalt Co, nickel, tungsten W, molybdenum Mo, zinc Zn, tin Sn, antimony Sb, titanium Ti, manganese Mn, indium In, chromium Cr and the mercury Hg.
Preferably, the preparation method of above-mentioned a kind of general multi-element metal sulfide nano-material, wherein: said tensio-active agent comprises any one the perhaps multiple combination in chain alkyl acid, alkylamine, long-chain alcohol, long-chain mercaptan and the ether.
The present invention adopts two or more different metallic N,N-Diethyldithiocarbamic Acid; Perhaps two or more different metallic phenanthroline N,N-Diethyldithiocarbamic Acid; The combination of perhaps above-mentioned two kinds of salt is as pre-reaction material; In having the tensio-active agent mixing solutions of different coordination characteristics, carry out common thermolysis by certain stoichiometric ratio; Through be total to the control of thermal decomposition process and solvent composition to the pre-reaction material ratio and in high boiling surfactivity mixed solvent, regulate nanocrystal nucleation and process of growth, a step makes the multi-element metal sulfide nano crystal material.The multi-element metal sulfide phase that makes thus is pure, it is adjustable to form, pattern and size homogeneous are controlled, and productive rate is high, and toxicity is low or nontoxic; Dispersiveness in non-polar organic solvent is better, easily-controlled reaction conditions, and preparation condition is gentle; Simple to operate, good reproducibility can scale operation.
For the preparation method who makes a kind of general multi-element metal sulfide nano-material of the present invention is easier to understand the practicality of its substantive distinguishing features and institute's tool thereof, below constipation close accompanying drawing the specific embodiment of the invention done further to specify.But following description and explanation about embodiment do not constitute any limitation protection domain of the present invention.
Description of drawings
The AgInS of Fig. 1 for making through the embodiment of the invention 1
2The transmission electron microscope photo of nano material.
Fig. 2 is AgInS among Fig. 1
2The XRD figure of nano material.
The Cu of Fig. 3 for making through the embodiment of the invention 2
12Sb
4S
13The transmission electron microscope photo of nano material.
The AgBiS of Fig. 4 for making through the embodiment of the invention 2
2The transmission electron microscope photo of nano material.
The AgInS of Fig. 5 for making through the embodiment of the invention 3
2The photoelectric properties figure of nano material.
The Cu of Fig. 6 for making through the embodiment of the invention 4
2ZnSnS
4The transmission electron microscope photo of nano material.
Embodiment
The preparation method of a kind of general multi-element metal sulfide nano-material provided by the invention, utilize N,N-Diethyldithiocarbamic Acid (DDTC) or phenanthroline N,N-Diethyldithiocarbamic Acid (DDTC) (Phen) counterweight metal ions M e (Me is silver-colored Ag
+, plumbous Pb
2+, copper Cu
2+, cadmium Cd
2+, bismuth Bi
3+, iron Fe
3+, cobalt Co
2+, nickel
2+, tungsten W
2+, molybdenum Mo
2+, zinc Zn
2+, tin Sn
4+, antimony Sb
3+, thallium Ti
3+, manganese Mn
3+With mercury Hg
2+) have complex ability preferably, can form stable title complex, and this kind title complex is water insoluble.Therefore can be easy to obtain pure Me (DDTC)
XPerhaps Me (DDTC)
X(Phen) pre-reaction material.The multi-element metal sulfide that high temperature formed after the thermolysis nucleation altogether in the tensio-active agent mixing solutions after two or more this type of pre-reaction material mixed does not dissolve in organic solution; In reactor drum, exist, be prone to realize the separation and the purification of product with the solid form.The product of the present invention's preparation is the multi-element metal sulfide powder.
Divided by concrete steps, preparation feedback precursor at first: the aqueous solution of heavy metallic salt dropwise is added in the aqueous solution that diethyldithiocar bamic acid receives, forms heavy metal Me (DDTC)
XDeposition is filtered then, is washed and dry and obtains pre-reaction material Me (DDTC)
XPressed powder; The aqueous solution of heavy metallic salt dropwise is added in the aqueous solution that the phenanthroline diethyldithiocar bamic acid receives, forms metal M e (DDTC)
X(Phen) deposition is filtered then, is washed and dry and obtains pre-reaction material Me (DDTC)
X(Phen) pressed powder.And then begin to prepare multi-element metal sulfide: with two or more Me (DDTC)
X, perhaps two or more Me (DDTC)
X(Phen), perhaps Me (DDTC)
XAnd Me (DDTC)
X(Phen) blended solid powder; Be dissolved in the tensio-active agent mixed solvent with different coordination characteristics, vacuumize below 120 ℃, and kept 10 minutes～20 minutes; Under protection of inert gas, be warming up to suitable temp (being generally more than 180 ℃) again and keep for some time; Common pyrolysis can at high temperature take place in such mix, and is last, treat that solution naturally cools to room temperature after; Add polar solvent (like ethanol etc.), just after centrifugal, washing and drying, can obtain the multi-element metal sulfide nano-material.
In addition; The prioritization scheme of technique scheme can also comprise: 1. this pre-reaction material is the N,N-Diethyldithiocarbamic Acid of single source form; This pre-reaction material had both contained metallic element; Also contain element sulphur, so can avoid owing to the too high ununiformity that causes the product particle size of partial concn in the reaction process; This kind pre-reaction material can form the solution (under the certain temperature) of clear in the tensio-active agent mixing solutions, can guarantee that like this environmental facies of metallic sulfide nucleation in the organic solvent system are same, makes that the sulfide nano crystal that generates is more even; 2. the optional scope of this tensio-active agent comprises chain alkyl acid, alkylamine, long-chain alcohol, long-chain mercaptan and ether etc.; From practical implementation; Said mixed solvent is that in oleic acid, oleyl amine, stearylamine, octadecylene, cetylamine, the Dodecyl Mercaptan etc. one or more make up allotment in proportion and form; According to the reaction parameter (solvent burden ratio, temperature, time, reactant concn etc.) of pre-reaction material in different ligand solvents, control the coordination characteristic of mixed solvent and between crystalline nucleation and growth, keep certain balance.
Below, introduce preparation process of the present invention in detail through specific embodiment.
Embodiment 1: quadrature phase AgInS
2Synthesizing of nano material.Take by weighing 0.05mmol siliver diethyldithiocarbamate and 0.05mmol diethyldithiocar bamic acid indium as raw material; It is dissolved in Dodecyl Mercaptan and oleic acid (15g: 7g) in the there-necked flask of mixed solvent, vacuumize under the room temperature, kept 10 minutes are housed; Under inert atmosphere, being warming up to 200 ℃ then kept 2 hours; After treating that at last solution naturally cools to room temperature, add an amount of absolute ethyl alcohol, centrifugal, washing and dry; Gained red powder material is dispersed in the polar solvent, confirms that with transmission electron microscope (as shown in Figure 1) and through X-ray diffraction (as shown in Figure 2) gained red powder material is quadrature phase AgInS
2Nano material.
Embodiment 2:Cu
12Sb
4S
13Synthesizing of nano material.Take by weighing 0.05mmol copper diethyl dithiocarbamate and 0.1mmol diethyldithiocar bamic acid antimony as raw material; It is dissolved in Dodecyl Mercaptan and oleyl amine are housed (20mmol: 20mmol) in the there-necked flask of mixed solvent, 120 ℃ vacuumize, and keep 15 minutes; Under inert atmosphere, being warming up to 220 ℃ then kept 0.5 hour; After treating that at last solution naturally cools to room temperature, add an amount of absolute ethyl alcohol, centrifugal, washing and dry; The gained powder mass is dispersed in the polar solvent, confirms that with transmission electron microscope (as shown in Figure 3) and through X-ray diffraction gained red powder material is Cu
12Sb
4S
13Nano material.
Embodiment 3: quadrature phase AgBiS
2Synthesizing of nano material.Take by weighing 0.1mmol siliver diethyldithiocarbamate and 0.1mmol diethyldithiocar bamic acid bismuth as raw material, it is dissolved in stearylamine and octadecylene are housed (20mmol: 20mmol) in the there-necked flask of mixed solvent, 100 ℃ vacuumize; Kept 20 minutes; Under inert atmosphere, be warming up to 240 ℃ then and kept 1 hour, treat that at last solution naturally cools to room temperature after, add and fit the calorimetric absolute ethyl alcohol; Centrifugal, washing and dry; Gained black powder material is dispersed in the polar solvent, with transmission electron microscope (as shown in Figure 4) and through X-ray diffraction, confirms that gained black powder material is quadrature phase AgBiS
2Nano material.As shown in Figure 5, the nano material that obtains has good optical characteristics.
4: six side's phases of embodiment Cu
2ZnSnS
4Synthesizing of nano material.Take by weighing 0.2mmol copper diethyl dithiocarbamate, 0.1mmol zinc diethyldithiocarbamate and 0.1mmol phenanthroline tin diethyldithiocarbamate as raw material; It is dissolved in oleyl amine and Dodecyl Mercaptan (5.4g: 5.4g) in the there-necked flask of mixed solvent are housed; 80 ℃ vacuumize; Kept 20 minutes, and under inert atmosphere, be warming up to 240 ℃ then and kept 5 minutes, treat that at last solution naturally cools to room temperature after; Add and fit the calorimetric absolute ethyl alcohol; Centrifugal, washing and dry, gained black powder material is dispersed in the polar solvent, confirms that with transmission electron microscope (as shown in Figure 6) and through X-ray diffraction gained black powder material is six side's phase Cu
2ZnSnS
4Nano material.
Claims (5)
1. the preparation method of a general multi-element metal sulfide nano-material; It is characterized in that: adopt two or more different metallic N,N-Diethyldithiocarbamic Acid; Perhaps two or more different metallic phenanthroline N,N-Diethyldithiocarbamic Acid; Perhaps the combination of metal N,N-Diethyldithiocarbamic Acid and metal phenanthroline N,N-Diethyldithiocarbamic Acid is carried out common thermolysis as pre-reaction material in having the tensio-active agent mixing solutions of different coordination characteristics, and nucleation, growth; One step made that phase is pure, thing is mutually controlled, the multi-element metal sulfide nano-material of pattern and size adjustable, and its step is following:
Step 1: the mol ratio of pre-reaction material according to metal constituent element in the multi-element metal sulfidic material composition is dissolved in the tensio-active agent mixing solutions with different coordination characteristics,, kept 10 minutes ~ 20 minutes 120 ℃ and following vacuumizing;
Step 2: under protection of inert gas, the resulting solution of step 1 is warming up to more than 180 ℃, reaction is more than 5 minutes;
Step 3: after the solution that step 2 is obtained naturally cools to room temperature, add polar organic solvent, after centrifugal, washing and drying, obtain the multi-element metal sulfide nano-material.
2. the preparation method of a kind of general multi-element metal sulfide nano-material according to claim 1 is characterized in that: the metallic element in the said pre-reaction material comprises any one among silver-colored Ag, plumbous Pb, copper Cu, cadmium Cd, bismuth Bi, iron Fe, cobalt Co, nickel, tungsten W, molybdenum Mo, zinc Zn, tin Sn, antimony Sb, titanium Ti, manganese Mn, indium In, chromium Cr and the mercury Hg.
3. the preparation method of a kind of general multi-element metal sulfide nano-material according to claim 1 is characterized in that: said tensio-active agent comprises any one the perhaps multiple combination in chain alkyl acid, alkylamine, long-chain alcohol, long-chain mercaptan and the ether.
4. the preparation method of a kind of general multi-element metal sulfide nano-material according to claim 3 is characterized in that: said tensio-active agent is any one the perhaps multiple combination in oleic acid, oleyl amine, stearylamine, octadecylene, cetylamine, the Dodecyl Mercaptan.
5. the preparation method of a kind of general multi-element metal sulfide nano-material according to claim 1 is characterized in that: said polar solvent is an absolute ethyl alcohol.
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