CN104445098B - A kind of AgInSe2Nanocrystalline and preparation method thereof - Google Patents
A kind of AgInSe2Nanocrystalline and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of AgInSe2Nanocrystalline and preparation method thereof, prepare AgInSe by the isothermal reaction method of 3～20 hours at the precursor solution that silver nitrate, indium chloride and/or four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide are mixed and stirred for be obtained after uniformly carry out in autoclave 160～220 DEG C2Nanocrystalline, this AgInSe2Nanocrystalline be space group is Pna21Metastable state rhombic system, water soluble。The raw material simple cheap that the preparation method of the present invention uses, process is simple and direct, and synthesis cycle is short, reproducible, and environmental protection, the AgInSe thus prepared2Nanocrystalline can be scattered in aqueous phase preferably, in the fields such as biomedical and aqueous phase photocatalysis, there is application advantage。
Description
Technical field
The present invention relates to a kind of nanocrystalline with nanocrystalline preparation method, particularly to a kind of AgInSe2Nanocrystalline preparation method and corresponding AgInSe2Nanocrystalline。
Background technology
I-III-VI2Race's semiconductor nano has the character of many excellences, such as toxicity is low, the absorption coefficient of light is big, band gap is narrow, emission wavelength is in character such as near infrared regions, therefore show tempting application prospect in technical fields such as solaode, light emitting diode, biological fluorescent labelling, visible light photocatalysis, cause strong concern。As I-III-VI2A member important in race's semiconductor nano, AgInSe2The nanocrystalline energy gap with about 1.24eV, is conducive to the applications well in fields such as biological fluorescent labelling, photocatalysis, solaodes, but for want of effective general synthetic method, it focuses primarily upon the research of block and film morphology。Until 2006, seminar (the MengT.Ng of Vittal, ChrisB.Boothroyd, JagadeseJ.Vittal, J.Am.Chem.Soc., 2006,128:7118-7119.) method by thermally decomposing previously prepared unit predecessor in the mixed solvent of oleyl amine and lauryl mercaptan, is prepared for the good AgInSe of quality2Nanocrystalline。Hereafter, some additive methods are also found successively for AgInSe2Nanocrystalline synthesis is (such as (a) DingshengWang, WenZheng, ChenhuiHao, QingPeng, YadongLi, Chem.Commun., 2008,2556 2558；(b) TianyuBai, ChunguangLi, FeifeiLi, LanZhao, ZhaoruiWang, HeHuang, CailingChen, YuHan, ZhanShi, ShouhuaFeng, Nanoscale, 2014,6,6782 6789；(c) LiWang, PengzhanYing, YuanDeng, HongZhou, ZhengliangDu, JiaolinCui, RSCAdv., 2014, 4, 33897 33904 are reported), but above synthetic method still has many weak points, first, these synthetic methods are all comparatively laborious, and not environmentally, what use mostly is toxic solvent (such as oleyl amine, tri-n-octyl phosphine etc.), secondly these synthetic methods single predecessor needing preparation complicated more, operating process is complicated, in addition, what these synthetic methods prepared nanocrystalline is oil solubility nanometer crystalline substance, nonpolar organic solvent can only be dispersed in, such as normal hexane, among toluene equal solvent, and nanocrystalline ought be applied to biological fluorescent labelling, during the field such as photocatalytic degradation of dye or photocatalysis hydrogen production, what can be dispersed in aqueous phase nanocrystalline is clearly better selection, namely wish that what use nanocrystalline has water solublity。
Summary of the invention
Based on the defect of prior art, it is within the contemplation of the invention that prepare water miscible AgInSe by the preparation method that a kind of process is simple, easy and simple to handle2Nanocrystalline。
First the present invention discloses a kind of AgInSe2Nanocrystalline preparation method, comprises the following steps:
1) preparation of precursor solution
To be mixed and stirred for uniformly, namely obtaining precursor solution as the silver nitrate of raw material, indium chloride and/or four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide；
2) nanocrystalline chemical combination
By by step 1) precursor solution that obtains puts in autoclave, and by reacted solution centrifugal and collect solid after isothermal reaction 3～20 hours at 160～220 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
In above-mentioned preparation method, silver nitrate, indium chloride and/or four chloride hydrate indiums, selenium dioxide respectively product AgInSe2The source of nanocrystalline middle Ag element, In element and Se element, it is AgInSe that the ratio of its amount of substance can form chemical formula after meeting chemical combination2Product, selectivity adjustment under premise that simultaneously Se element is suitably excessive, if amount of substance is Ag:In:Se=1:1:(2～8)；The polyvinylpyrrolidone used as protective agent can interact to control the carrying out reacted with Ag ion, In ion etc. on the one hand, and making product is do not contain Ag2Se、AgIn5Se8Deng the pure AgInSe that the form of impurity is regular2Nanocrystalline；On the other hand, it is water miscible macromolecule, and in nanocrystalline chemical combination, it can be adsorbed on nanocrystal surface by chemical action, makes nanocrystalline being dispersed in water；Consumption as the dimethylformamide of solvent use can selectivity adjustment under the premise fully dissolved；Step 2) described in centrifugal, its parameter can selectivity adjustment under as far as possible many premises being settled out solid, the solvent being used for washing solid can select water and ethanol。
In above-mentioned preparation method, raw material described in preferably: step 1) is silver nitrate, four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide, wherein silver nitrate, four water indium chloride, selenium dioxide, polyvinylpyrrolidone mass ratio be 30～37:53～64:60～110:200～2000。
In above-mentioned preparation method, it is preferred that step 1) described in raw material also include oleic acid, and the volume ratio of oleic acid and dimethylformamide is 0:1～6:1。
In above-mentioned preparation method, when oleic acid is different from the volume ratio of dimethylformamide, corresponding product AgInSe2Nanocrystalline form is different from size, as when the volume ratio of oleic acid Yu dimethylformamide is 5:2, obtained the graininess AgInSe that diameter is about 60nm2Nanocrystalline, and when the volume ratio of oleic acid Yu dimethylformamide is 1:6, obtain the AgInSe of the Tinea Ranae shape that length is about 200～1200nm2Nanocrystalline。
In above-mentioned preparation method, it is preferred that in described precursor solution, the concentration of silver nitrate is 0.00285mol L-1～0.0228mol L-1。
In above-mentioned preparation method, it being preferably: step 2): will by step 1) precursor solution that obtains adds in autoclave, by reacted solution centrifugal and collect solid after isothermal reaction 3～12 hours at 200 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
In above-mentioned preparation method, it being preferably: step 2): by by step 1) precursor solution that obtains puts in autoclave, by reacted solution centrifugal and collect solid after isothermal reaction 12 hours at 180 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
In above-mentioned preparation method, it being preferably: step 2): by by step 1) precursor solution that obtains puts in autoclave, at 220 DEG C, reacted solution centrifugal was collected solid after 12 hours by isothermal reaction, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
In above preferred embodiment, reaction temperature produces various sizes of nanocrystalline from the different meetings of time accordingly, and nanocrystalline crystallinity can be produced certain impact by it simultaneously, thus affecting its application in light absorption with photoluminescent property further。
In above-mentioned preparation method, it is preferred that after described precursor solution adds described autoclave, its filling proportion in autoclave is 70%～90%。
In above-mentioned preparation method, it is preferred that the inner lining material of described autoclave is tetrafluoroethene。
The present invention further discloses a kind of AgInSe2Nanocrystalline, it prepares according to the optimal way of above-mentioned preparation method Yu this preparation method, and its chemical formula is AgInSe2, it is space group is Pna21Metastable state rhombic system, water soluble。
This water solublity AgInSe disclosed by the invention2Nanocrystalline it is usable in the multiple fields such as biological fluorescent labelling and aqueous phase photocatalysis。
The method have the advantages that
1) preparation method of the present invention is by selecting suitable reaction system and corresponding synthetic method to prepare water solublity AgInSe2Nanocrystalline, it is synthesized by airtight reactor, relies on the self-generated pressure of high temperature and precursor solution and the reaction that carries out, efficiently utilizes coordinating between reaction system with synthetic method；
2) present invention prepares AgInSe2The raw material simple cheap that nanocrystalline method uses, technical process is simple and direct, and synthesis cycle is short, reproducible, and environmental protection；
3) AgInSe that the present invention prepares2Nanocrystalline can being dispersed in aqueous phase preferably and form stable system, it can save, in the application such as the biomedicine in later stage and photocatalysis, the step that ligand exchange is modified, has application advantage。
Accompanying drawing explanation
Fig. 1 is the AgInSe of the embodiment of the present invention 1 preparation2Nanocrystalline XRD spectra；
Fig. 2 is the AgInSe of the embodiment of the present invention 1 preparation2Nanocrystalline SEM picture；
Fig. 3 is the AgInSe of the embodiment of the present invention 1 preparation2Nanocrystalline EDX spectrogram；
Fig. 4 is the AgInSe that the embodiment of the present invention 5 prepares2Nanocrystalline SEM picture。
Detailed description of the invention
1) preparation of precursor solution
To be mixed and stirred for uniformly, namely obtaining precursor solution as the silver nitrate of raw material, indium chloride and/or four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide；
3) nanocrystalline chemical combination
By by step 1) precursor solution that obtains puts in autoclave, and by reacted solution centrifugal and collect solid after isothermal reaction 3～20 hours at 160～220 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline；
Step 1) in select four chloride hydrate indiums time, mass ratio between raw material is silver nitrate: four water indium chloride: selenium dioxide: polyvinylpyrrolidone=30～37:53～64:60～110:200～2000, certainly, during selective chlorination indium, its consumption can be converted by above mass ratio。In step 1) raw material in can also add oleic acid mixing and stirring in the lump, the oleic acid of addition and the volume ratio of dimethylformamide are 0:1～6:1。
Step 2) liner of the preferred tetrafluoroethene of autoclave that uses, precursor solution filling proportion wherein preferably 70%～90%。
Above-mentioned raw materials all can buied on the market, it is also possible to prepares voluntarily during preparation, and device therefor can be bought voluntarily, it is also possible to according to preparation principle provided by the invention, uses the miscellaneous equipment with similar functions to replace。
Below in conjunction with embodiments of the invention, the invention will be further elaborated。
Embodiment 1
First 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1g polyvinylpyrrolidone (PVP) are joined formation mixed liquor in 25mL oleic acid and 10mL dimethylformamide, above-mentioned mixed liquor is stirred 40 minutes, forms precursor solution；This precursor solution being joined 50mL using tetrafluoroethene as the autoclave of liner afterwards, reactor sealing be placed in temperature programmed control baking oven and react, reaction temperature is 200 DEG C, and the response time is 12 hours。After reaction terminates, after question response still naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing collecting reaction product, and it uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble, it is carried out XRD figure spectrum test, can be seen that this AgInSe by the XRD style obtained2Nanocrystalline for metastable orthorhombic crystal structure, it is carried out EDX spectrogram test, being appreciated that in prepared product the mol ratio of Ag:In:Se by this spectrogram is 1:1:1.91, it is carried out SEM test, it is possible to learn preparation-obtained AgInSe2The nanocrystalline graininess for diameter about 60nm。
Embodiment 2
First 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 0.5gPVP are joined in 25mL oleic acid and 10mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 3
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 2gPVP join in 25mL oleic acid and 10mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 4
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 0mL oleic acid and 35mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 5
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 5mL oleic acid and 30mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble, it is carried out SEM test, it is possible to learn prepared product AgInSe2The nanocrystalline Tinea Ranae shape for length 200～1200nm。
Embodiment 6
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 15mL oleic acid and 20mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 7
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 25mL oleic acid and 10mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 200 DEG C, and the response time is 3 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 8
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 25mL oleic acid and 10mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 180 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, open reactor, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Embodiment 9
First by 34mg silver nitrate, 60mg tetra-chloride hydrate indium, 88.8mg selenium dioxide and 1gPVP join in 25mL oleic acid and 10mL dimethylformamide, stir 40 minutes, form precursor solution；Precursor solution joins in the autoclave that 50mL tetrafluoroethene is liner afterwards。Sealing kettle is placed in temperature programmed control baking oven and reacts, and sets reaction temperature as 220 DEG C, and the response time is 12 hours。
After reaction terminates, band reactor naturally cools to room temperature, take out tetrafluoroethene liner, thereafter it is centrifuged reactant liquor processing with collecting reaction product, and product uses deionized water, ethanol etc. clean successively, is centrifuged for several times, finally in vacuum drying oven, 60 DEG C of insulations dry for 4 hours, can obtain AgInSe2Nanocrystalline, its water soluble。
Although the present invention has been described in detail above in conjunction with the embodiments, but, it will be appreciated by those skilled in the art that under the premise without departing from present inventive concept, within the scope of the claims, it is also possible to above-described embodiment is carried out and more or change etc.。
Claims (8)
1. an AgInSe2Nanocrystalline preparation method, it is characterised in that: comprise the following steps:
1) preparation of precursor solution
To be mixed and stirred for uniformly, namely obtaining precursor solution as the silver nitrate of raw material, indium chloride and/or four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide；
2) nanocrystalline chemical combination
By by step 1) precursor solution that obtains puts in autoclave, and by reacted solution centrifugal and collect solid after isothermal reaction 3～20 hours at 160～220 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
2. AgInSe according to claim 12Nanocrystalline preparation method, it is characterized in that: step 1) described in raw material be silver nitrate, four chloride hydrate indiums, selenium dioxide, polyvinylpyrrolidone and dimethylformamide, wherein silver nitrate, four water indium chloride, selenium dioxide, polyvinylpyrrolidone mass ratio be 30～37:53～64:60～110:200～2000。
3. AgInSe according to claim 12Nanocrystalline preparation method, it is characterised in that: described step 1) described in raw material also include oleic acid, the volume ratio of described oleic acid and described dimethylformamide is 0:1～6:1。
4. AgInSe according to claim 12Nanocrystalline preparation method, it is characterized in that: described step 2) be: will by step 1) precursor solution that obtains adds in autoclave, by reacted solution centrifugal and collect solid after isothermal reaction 3～12 hours at 200 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
5. AgInSe according to claim 12Nanocrystalline preparation method, it is characterized in that: described step 2) be: by by step 1) precursor solution that obtains puts in autoclave, by reacted solution centrifugal and collect solid after isothermal reaction 12 hours at 180 DEG C, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
6. AgInSe according to claim 12Nanocrystalline preparation method, it is characterized in that: described step 2) be: by by step 1) precursor solution that obtains puts in autoclave, at 220 DEG C, reacted solution centrifugal was collected solid after 12 hours by isothermal reaction, gained solid is used solvent wash, drying, namely obtains AgInSe2Nanocrystalline。
7. AgInSe according to claim 12Nanocrystalline preparation method, it is characterised in that: after described precursor solution adds described autoclave, its filling proportion in autoclave is 70%～90%。
8. AgInSe according to claim 12Nanocrystalline preparation method, it is characterised in that: the inner lining material of described autoclave is tetrafluoroethene。
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| CN110429148B (en) * | 2019-07-31 | 2020-04-07 | 南京倍格电子科技有限公司 | Selenide nanorod, preparation method thereof and photoelectric detector prepared from selenide nanorod |
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