CN101348275A - Preparation of polyhedral cuprous oxide nano particle - Google Patents
Preparation of polyhedral cuprous oxide nano particle Download PDFInfo
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- CN101348275A CN101348275A CNA2008102222044A CN200810222204A CN101348275A CN 101348275 A CN101348275 A CN 101348275A CN A2008102222044 A CNA2008102222044 A CN A2008102222044A CN 200810222204 A CN200810222204 A CN 200810222204A CN 101348275 A CN101348275 A CN 101348275A
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Abstract
The invention provides a method for preparing polyhedral cuprous oxide nanometer granules. The method adopts a chemical solution method to prepare polyhedral cuprous oxide nanometer granules comprising cubes, chamfered cubes, cubic octahedrons, chamfered octahedrons or octahedral series. The method comprises the following concrete steps: copper salt is dissolved in water and stirred at a temperature between 50 and 60 DEG C; polyvinyl pyrrolidone, strong base solution and ascorbic acid solution are orderly added, stirred at a constant temperature between 50 and 60 DEG C and kept for 1 to 3 hours; after the reaction is over, the centrifugation is carried out; and a large amount of the deionized water is used for washing, and the cuprous oxide nanometer granules can be obtained after vacuum drying. By regulating the adding amount of the polyvinyl pyrrolidone, the polyhedral cuprous oxide nanometer granules comprising the cubes, the chamfered cubes, the cubic octahedrons, the chamfered octahedrons or the octahedral series are obtained. The method has the advantages of moderate condition, simple operation, low cost, high yield, controllable shape, and so on.
Description
Technical field
The present invention relates to a kind of preparation method of polyhedral cuprous oxide nano particle, be specifically related to adopt the chemical solution method preparation to comprise the method for cubes, top rake cubes, cuboctahedron, top rake octahedron, octahedra shape series cuprous oxide nano particle.Belong to the inorganic compound semiconductor technical field of material.
Background technology
Nano material is because the singularity of its structure as big specific surface and a series of new effect (small-size effect, interfacial effect, quantum effect and quantum tunneling effect etc.), has caused people's great attention thereby have unique physics, chemical property.Red copper oxide is good P-type semiconductor, can be applied to fields such as solar energy converting, microelectronics, magnetic storage, catalysis, air-sensitive.Size reaches after the nano level, because of its bigger specific surface area and good Surface Physical Chemistry character make it at aspects such as solar cell, microelectronic device, gas catalysis, gas sensors many very potential application be arranged.
The preparation of cuprous nano material is one of hot fields of research always.The domestic and international at present control to its nanotopography has many researchs reports.Patterns such as the nano wire of Red copper oxide, nano whisker, nanometer ball, nanometer flower, micro-nano cubic block existing relevant research report or patent.As being in the patent of CN1759965 at publication number, Li Yadong group has synthesized accurate monodispersed Nano balls of cuprous oxide, the Murphy of U.S. University of South Carolina, C.J. etc. successfully prepare the cuprous nano cubic block in international periodical Nano Lett..Though the existing report of polyhedral cuprous oxide micro-/ nano crystal, in being the patent of ZL 200510135861.1, the patent No. utilize electrochemical deposition to prepare the Red copper oxide micro-/ nano crystal of controllable shapes as the Zheng Lan of Xiamen University sweet-smelling grass etc., the Siegfried of U.S. Purdue University, M.J have reported also that in international periodical J.Am.Chem.Soc. Red copper oxide micro-/ nano crystalline is synthetic.But owing to all be to adopt electrochemical production, substrate need be anticipated, and can only grow on substrate, makes that its condition is comparatively complicated, synthetic wayward, cost is high, be unfavorable for scale operation.And use the serial polyhedral cuprous oxide nano particle of simple chemical solution method one-step synthesis size and pattern homogeneous at home and abroad there is no report.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, utilize polyvinylpyrrolidone as modifier, a kind of preparation method of simple to operate, temperature of reaction is gentle, cost the is low polyhedral cuprous oxide nano particle that comprises cubes, top rake cubes, cuboctahedron, top rake octahedron, octahedra shape series is provided.
One of purpose of the present invention is to provide a kind of method that adopts chemical solution method to prepare polyhedral cuprous oxide nano particle, it comprises step: polyvinylpyrrolidone is joined in the copper salt solution, under 50～60 ℃, stir, drip strong alkali aqueous solution, after continuing to stir 0.5h, drip aqueous ascorbic acid, at 50～60 ℃ of following restir 1～3h.
In preparation method of the present invention, the molar ratio of polyvinylpyrrolidone and mantoquita is 0.001～32.Preferably, the molar ratio of polyvinylpyrrolidone and mantoquita is 0.001～2; 3～6; 9～20; 23～27; 29～32.
In preparation method of the present invention, the mantoquita in copper salt solution, strong base solution, the ascorbic acid solution: highly basic: the mol ratio of xitix is 0.08: 1: 0.3～0.12: 4: 0.7.Preferably, mantoquita: highly basic: the mol ratio of xitix is 1: 30: 6; 0.8: 10: 3; 1.2: 40: 7.
In preparation method of the present invention, described highly basic is selected from sodium hydroxide or potassium hydroxide.
In preparation method of the present invention, described mantoquita is selected from neutralized verdigris, copper sulfate, cupric nitrate or cupric chloride.
In preparation method of the present invention, can after finishing, reaction carry out centrifugation to resulting product, use a large amount of deionized water wash, then vacuum-drying.
Another object of the present invention is to provide the preparation method according to the application to prepare polyhedral cuprous oxide nano particle, the shape of wherein said nano particle can be cubic, top rake cubic, cuboctahedron shape, the octahedra shape of top rake or octahedra shape, polyhedral cuprous oxide nano particle length of side average out to 650～800nm.
Another object of the present invention also is to provide the purposes of polyvinylpyrrolidone in the preparation polyhedral cuprous oxide nano particle, and the molar ratio of wherein said polyvinylpyrrolidone and mantoquita is 0.001～32.
In this article, if not explanation especially, the solution that is adopted all prepares under normal condition, such as what at room temperature substance dissolves is prepared in the aqueous solution.
A particularly preferred embodiment of the present invention is:
1. prepare the strong alkali aqueous solution that concentration is 1.0～4.0mol/l;
2. prepare the aqueous ascorbic acid that concentration is 0.3～0.7mol/l;
3. preparing concentration is 8 * 10
-3～12 * 10
-3The copper salt solution of mol/l;
4. polyhedral cuprous oxide nano particle is synthetic: a certain amount of polyvinylpyrrolidone is joined in 3. the copper salt solution, under 50～60 ℃, stir, dropwise drip strong alkali aqueous solution, after continuing to stir 0.5h, dropwise drip aqueous ascorbic acid, under 50～60 ℃, then stir 1～3h, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain serial polyhedral cuprous oxide nano particle, the wherein copper salt solution that is adopted after the vacuum-drying, strong base solution, mantoquita in the ascorbic acid solution: highly basic: the mol ratio of xitix is 0.08: 1: 0.3～0.12: 4: 0.7.
In the present invention, if not explanation especially, the device that is adopted, instrument, equipment, material, technology, method, step, preparation condition etc. all are that this area routine adopts or those of ordinary skills can easily obtain according to the conventional technology that adopts in this area.
Than other chemical process of the preparation cuprous oxide nano particle of available technology adopting, the present invention has following advantage:
1. adopt polyvinylpyrrolidone as modifier, synthetic method is easy to control, polyhedral cuprous oxide nano particle size that obtains and pattern homogeneous, and have the advantage of environmental protection,
2. because the chemical solution method temperature of reaction that adopts is low, the highlyest be no more than 60 ℃, mild condition, simple to operate;
3. the solution of the present invention productive rate height, shape can be regulated and control as required, and cost is low.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the embodiment of the invention 1 resulting cubic cuprous oxide nano particle.
Fig. 2 is the stereoscan photograph of the embodiment of the invention 1 resulting cubic cuprous oxide nano particle.
Fig. 3 is the stereoscan photograph of the embodiment of the invention 2 resulting top rake cubic cuprous oxide nano particles.
Fig. 4 is the stereoscan photograph of the embodiment of the invention 3 resulting cuboctahedron shape cuprous oxide nano particles.
Fig. 5 is the stereoscan photograph of the octahedra shape cuprous oxide nano particle of the embodiment of the invention 4 resulting top rakes.
Fig. 6 is the stereoscan photograph of the embodiment of the invention 5 resulting octahedra shape cuprous oxide nano particles.
Embodiment
Specifically describe the preparation method of polyhedral cuprous oxide nano particle of the present invention below in conjunction with drawings and Examples, but should be appreciated that these embodiment only are used to set forth the present invention, and also limit protection scope of the present invention never in any form.
Embodiment 1:
1. the preparation of strong alkali aqueous solution: the 1.2g dissolution of sodium hydroxide in 10ml water, is stirred under the room temperature and makes sodium hydroxide fully dissolving in water, obtain the aqueous solution of sodium hydroxide, the concentration of aqueous sodium hydroxide solution is 3.0mol/l.
2. the preparation of aqueous ascorbic acid: the 1.057g dissolution of ascorbic acid in 10ml water, is stirred under the room temperature and makes xitix fully dissolving in water, obtain the aqueous solution of xitix, the concentration of aqueous ascorbic acid is 0.6mol/l.
3. the preparation of copper salt solution: in the flask of a 250ml, the 0.171g cupric chloride is dissolved in the 100ml water, stirring at room makes cupric chloride fully dissolving in water, obtains the aqueous solution of cupric chloride, and the concentration of copper chloride solution is 10 * 10
-3Mol/l.
4. in flask, add the 0.011g polyvinylpyrrolidone, under 55 ℃, in flask, dropwise drip the aqueous sodium hydroxide solution of 10ml in 1. while stirring, after continuing to stir 0.5h, dropwise drip the aqueous ascorbic acid of 10ml in 2., then stir 3h under 50 ℃, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain cuprous oxide nano particle after the vacuum-drying.X-ray diffraction spectrogram such as Fig. 1 of resultant cuprous oxide nano particle, prepared as seen from Figure 1 nano cuprous oxide are the simple cubic crystal formation.Resultant nano cuprous oxide stereoscan photograph such as Fig. 2, prepared as seen from Figure 2 nano cuprous oxide are cubic, and the average length of side of particle is about 800nm.
Embodiment 2:
1. with the 0.4g dissolution of sodium hydroxide in 10ml water, stirring at room makes sodium hydroxide fully dissolving in water, obtains the aqueous solution of sodium hydroxide, the concentration of aqueous sodium hydroxide solution is 1.0mol/l.
2. with the 0.528g dissolution of ascorbic acid in 10ml water, stirring at room makes xitix fully dissolving in water, obtains the aqueous solution of xitix, the concentration of aqueous ascorbic acid is 0.3mol/l.
3. in the flask of a 250ml, 0.20g copper sulfate is dissolved in the 100ml water, stirs under the room temperature and make copper sulfate fully dissolving in water, obtain the aqueous solution of copper sulfate, the concentration of copper sulfate solution is 8 * 10
-3Mol/l.
4. in flask, add the 0.556g polyvinylpyrrolidone, under 55 ℃, stir, dropwise drip the aqueous sodium hydroxide solution of 10ml in 1., after continuing to stir 0.5h, dropwise drip the aqueous ascorbic acid of 10ml in 2., then stir 3h under 55 ℃, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain cuprous oxide nano particle after the vacuum-drying.Resultant nano cuprous oxide stereoscan photograph such as Fig. 3, prepared as seen from Figure 3 nano cuprous oxide are the top rake cubic, and the average length of side of particle is about 800nm.
Embodiment 3:
1. with the 1.6g dissolution of sodium hydroxide in 10ml water, stirring at room makes sodium hydroxide fully dissolving in water, obtains the aqueous solution of sodium hydroxide, the concentration of aqueous sodium hydroxide solution is 4.0mol/l.
2. with the 1.233g dissolution of ascorbic acid in 10ml water, stirring at room makes xitix fully dissolving in water, obtains the aqueous solution of xitix, the concentration of aqueous ascorbic acid is 0.7mol/l.
3. in the flask of a 250ml, the 0.239g neutralized verdigris is dissolved in the 100ml water, stirring at room makes neutralized verdigris fully dissolving in water, obtains the aqueous solution of neutralized verdigris, and the concentration of the neutralized verdigris aqueous solution is 12 * 10
-3Mol/l.
4. in flask, add the 1.111g polyvinylpyrrolidone, under 55 ℃, stir, dropwise drip the aqueous sodium hydroxide solution of 10ml in 1., after continuing to stir 0.5h, dropwise drip the aqueous ascorbic acid of 10ml in 2., then stir 3h under 55 ℃, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain cuprous oxide nano particle after the vacuum-drying.Resultant nano cuprous oxide stereoscan photograph such as Fig. 4, prepared as seen from Figure 4 nano cuprous oxide are the cuboctahedron shape, and the average length of side of particle is about 650nm.
Embodiment 4:
1. with the 1.2g dissolution of sodium hydroxide in 10ml water, stirring at room makes sodium hydroxide fully dissolving in water, obtains the aqueous solution of sodium hydroxide, the concentration of aqueous sodium hydroxide solution is 3.0mol/l.
2. with the 1.057g dissolution of ascorbic acid in 10ml water, stirring at room makes xitix fully dissolving in water, obtains the aqueous solution of xitix, the concentration of aqueous ascorbic acid is 0.6mol/l.
3. in the flask of a 250ml, the 0.241g cupric nitrate is dissolved in the 100ml water, stirring at room makes cupric nitrate fully dissolving in water, obtains the aqueous solution of cupric nitrate, and the concentration of copper nitrate aqueous solution is 10 * 10
-3Mol/l.
4. in flask, add the 2.775g polyvinylpyrrolidone, under 55 ℃, stir, dropwise drip the aqueous sodium hydroxide solution of 10ml in 1., after continuing to stir 0.5h, dropwise drip the aqueous ascorbic acid of 10ml in 2., then stir 2h under 60 ℃, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain cuprous oxide nano particle after the vacuum-drying.Resultant nano cuprous oxide stereoscan photograph such as Fig. 5, prepared as seen from Figure 5 nano cuprous oxide are the octahedra shape of top rake, and the average length of side of particle is about 800nm.
Embodiment 5:
1. 1.68g potassium hydroxide is dissolved in the 10ml water, stirring at room makes potassium hydroxide fully dissolving in water, obtains the aqueous solution of potassium hydroxide, and the concentration of potassium hydroxide aqueous solution is 3.0mol/l.
2. with the 1.057g dissolution of ascorbic acid in 10ml water, stirring at room makes xitix fully dissolving in water, obtains the aqueous solution of xitix, the concentration of aqueous ascorbic acid is 0.6mol/l.
3. in the flask of a 250ml, the 0.171g cupric chloride is dissolved in the 100ml water, stirring at room makes cupric chloride fully dissolving in water, obtains the aqueous solution of cupric chloride, and the concentration of copper chloride solution is 10 * 10
-3Mol/l.
4. in flask, add the 3.33g polyvinylpyrrolidone, under 55 ℃, stir, dropwise drip the potassium hydroxide aqueous solution of 10ml in 1., after continuing to stir 0.5h, dropwise drip the aqueous ascorbic acid of 10ml in 2., then stir 1h under 55 ℃, reaction finishes the back centrifugation, use a large amount of deionized water wash, can obtain cuprous oxide nano particle after the vacuum-drying.Resultant nano cuprous oxide stereoscan photograph such as Fig. 6, prepared as seen from Figure 6 nano cuprous oxide are octahedra shape, and the average length of side of particle is about 800nm.
Claims (10)
1. the preparation method of polyhedral cuprous oxide nano particle, it comprises step: polyvinylpyrrolidone is joined in the copper salt solution, stir under 50～60 ℃, drip strong alkali aqueous solution, after continuing to stir 0.5h, drip aqueous ascorbic acid, at 50～60 ℃ of following restir 1～3h.
2. the preparation method of the polyhedral cuprous oxide nano particle of claim 1, wherein the molar ratio of polyvinylpyrrolidone and mantoquita is 0.001～32.
3. the preparation method of claim 1 or 2 polyhedral cuprous oxide nano particle, the wherein mantoquita in copper salt solution, strong base solution, the ascorbic acid solution: highly basic: the mol ratio of xitix is 0.08: 1: 0.3～0.12: 4: 0.7.
4. the preparation method of claim 1 or 2 polyhedral cuprous oxide nano particle, wherein the mol ratio of polyvinylpyrrolidone and mantoquita is selected from 0.001～2 respectively; 3～6; 9～20; 23～27; 29～32.
5, the preparation method of claim 1 or 2 polyhedral cuprous oxide nano particle, wherein said highly basic is selected from sodium hydroxide or potassium hydroxide.
6, the preparation method of claim 1 or 2 polyhedral cuprous oxide nano particle, wherein said mantoquita is selected from neutralized verdigris, copper sulfate, cupric nitrate or cupric chloride.
7, the polyhedral cuprous oxide nano particle for preparing according to each method in the aforesaid right requirement, its length of side average out to 650～800nm.
8, the polyhedral cuprous oxide nano particle of claim 7, wherein said nano particle be shaped as octahedra shape of cubic, top rake cubic, cuboctahedron shape, top rake or octahedra shape.
9, the purposes of polyvinylpyrrolidone in the preparation polyhedral cuprous oxide nano particle is characterized in that: polyvinylpyrrolidone is joined in the copper salt solution, obtain difform cuprous oxide nano particle.
10, the purposes of polyvinylpyrrolidone as claimed in claim 9 in the preparation polyhedral cuprous oxide nano particle, the molar ratio of wherein said polyvinylpyrrolidone and mantoquita is 0.001～32.
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