CN108585018A - A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres - Google Patents
A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres Download PDFInfo
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- CN108585018A CN108585018A CN201810159337.5A CN201810159337A CN108585018A CN 108585018 A CN108585018 A CN 108585018A CN 201810159337 A CN201810159337 A CN 201810159337A CN 108585018 A CN108585018 A CN 108585018A
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The present invention provides a kind of Cu of the size less than 100nm2O nanosphere preparation methods, belong to nano-metal-oxide preparing technical field.The preparation method belongs to liquid phase reduction, including the alcohol water mixed solution of configuration mantoquita and highly basic, preparation Cu (OH)2Presoma, glucose reduction Cu (OH)2Prepare Cu2O and post-processing.Preparation method provided by the present application, without using any surfactant and repeatability it is good, by the regulation and control of type, solvent volume ratio, reactant concentration, reaction temperature and reaction time to mantoquita, alkali and alcohols solvent, it can prepare that monodispersity is good, Cu of size uniform, regular shape2O nanospheres, the Cu obtained2O nanosphere grain sizes are less than 100nm and configuration of surface is controllable.Preparation method provided by the present application, it is easy to operate, controllability is strong, of low cost, has both solved the disadvantage that nanoscale lower surface activating agent is difficult to thoroughly remove, environment-friendly high-efficiency, demand easy to operate instantly are also met, suitable for industrialized production.
Description
Technical field
The present invention relates to nano-metal-oxide preparing technical fields, and in particular to a kind of size is less than the Cu of 100nm2O
The preparation method of nanosphere.
Background technology
Literature research shows：The performance of material and the size of its microscopic structural units are closely related.Cu2The specific surface area of O
It is sharply increased with the reduction of its crystallite dimension so that nanometer Cu2O produces the special effects not available for its block material,
Such as crystal face effect and dimensional effect.
Currently, nanometer Cu2O is shown in terms of photochemical catalyst, secondary cell, solar cell and gas sensor
General body block Cu2Excellent properties incomparable O.Therefore, size uniform, monodispersity are prepared well and there is nanometer ruler
The pure Cu of degree2O powder has become one of research hotspot of researcher.
However, the nanometer Cu reported at present2It usually requires to introduce organic surface active agent in the preparation process of O particles
(such as polyvinylpyrrolidone, neopelex and cetyl trimethylammonium bromide), these organic molecules are deposited
It will certainly influence Cu2The purity of O final products increases the synthesis cost of material, while the size of product is typically larger than 100nm,
Influence the physical and chemical performance of material.At present about " preparation size is less than the Cu of 100nm under the conditions of additive-free2O nanospheres " are ground
Study carefully still rare document report.
In consideration of it, exploitation one kind can efficiently synthesize, size uniform, monodispersity are good and grain size is less than 100nm
Pure Cu2The method of O nanospheres is particularly important.
Invention content
The problem to be solved in the present invention is existing Cu2It usually requires to introduce organic surface work in the liquid phase synthesis of O powder
Property agent, and particle size is typically larger than 100nm, influences the purity and performance of final product.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of Cu of the size less than 100nm is provided2O
The preparation method of nanosphere.The preparation method comprises the following steps：
(1)：Prepare cupric salt mixed solution
Make solute with water as solvent, cupric salt, prepares cupric salt aqueous solution, make Cu2+Molar concentration be 0.1~
3.0mol/L；
Later, at room temperature, above-mentioned cupric salt aqueous solution is mixed with the alcohols solvent of certain volume, obtained divalent
Mantoquita mixed solution is denoted as solution A；
(2)：Configure alkali mixed solution
Make solute with water as solvent, highly basic, prepares aqueous alkali, OH in the aqueous alkali-With cupric salt aqueous solution
Middle Cu2+Molar ratio be 1~10:1；
Later, at room temperature, above-mentioned aqueous alkali is mixed with the alcohols solvent of certain volume, obtained alkali mixed solution
It is denoted as solution B；
The alcohols solvent is consistent with the alcohols solvent in step (1)；
(3)：Prepare Cu (OH)2Presoma
The solution A that step (1) is configured, is heated to 60~100 DEG C；Then the solution B again configured step (2) is slow
Slowly it is added in solution A, stirring is remained during addition, and keep the temperature 1~15min at 60~100 DEG C；
(4)：Reduction reaction
Glucose powder is disposably added to the Cu (OH) that step (3) is obtained2In presoma, then react 3~
10min is obtained containing Cu2The solidliquid mixture of O precipitations；
Wherein, the ratio between the glucose of addition and the amount of substance of cupric salt in step (1) are 0.5~10:1；
(5)：Post-processing
Contain Cu by what step (4) obtained2The solidliquid mixture centrifuge washing of O precipitations 3~5 times, then by centrifuge washing
Product drying 6 afterwards~for 24 hours, obtain the Cu of pulverulence2O nanospheres.
Further, in the step (1), cupric salt is one kind in copper nitrate, copper acetate, copper sulphate, copper chloride
Or several mixture.
Further, in the step (2), highly basic is sodium hydroxide, potassium hydroxide.
Preferably, OH in the aqueous alkali-Molar concentration and cupric salt aqueous solution in Cu2+The ratio between molar concentration
It is 1~10:1.
Further, the alcohols solvent in the step (1) and (2) is the one or more of ethyl alcohol, ethylene glycol, glycerine
Mixture.
Preferably, in the step (1), the volume ratio of alcohols solvent and cupric salt aqueous solution is 1~100:1.
Preferably, in the step (2), the volume ratio of alcohols solvent and aqueous alkali is 1~100:1.
Further, in the step (4), the ratio between the amount of substance of the glucose and cupric salt in step (1) of addition
It is 1~6:1.
Further, it in the step (5), is washed respectively with deionized water and absolute ethyl alcohol.
Preferably, in the step (5), the product after centrifuge washing is dry at 50~80 DEG C.
The invention has the advantages and positive effects that：It is equal that size has been synthesized under conditions of unused any surfactant
Even, monodispersity is good, grain size is less than the Cu of 100nm2O nanospheres.Meanwhile preparation method is easy to operate, controllability is strong, cost
It is cheap, the application demand of environment-friendly high-efficiency instantly is met, suitable for industrialized production.Prepared nanometer Cu2O nanosphere powder possesses
Larger specific surface area makes it have general commercialization Cu2The skin effect and dimensional effect that O does not have.
Description of the drawings
Fig. 1 is Cu prepared by embodiment 12Transmission electron microscopy (TEM) figure of O nanospheres.
Fig. 2 is Cu prepared by embodiment 22The TEM of O nanospheres schemes.
Specific implementation mode
In order to better understand the present invention, the present invention is further retouched with reference to specific embodiments and the drawings
It states.
Embodiment 1
A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres, includes the following steps：
(1)：0.0375g copper nitrates and 1mL water are configured to copper nitrate aqueous solution；Then, by above-mentioned copper nitrate aqueous solution
It is mixed with 1mL ethyl alcohol, is denoted as solution A；
(2)：0.008g sodium hydroxides and 1mL water are configured to sodium hydrate aqueous solution；Then, by above-mentioned sodium hydroxide water
Solution is mixed with 25mL ethyl alcohol, is denoted as solution B；
(3)：The solution A that step 1 is configured is heated to 70 DEG C；Then the solution B that step 2 is configured is added dropwise again
Enter into solution A, magnetic agitation is remained during addition, and 3min is kept the temperature at 70 DEG C；
(4)：Quality is disposably added to by the glucose powder of 0.1153g in the mixture that step 3 obtains, so
After react 3min, that is, have solid precipitation object generation；
(5)：Contain Cu by what step 4 obtained2The solidliquid mixture of O precipitations uses deionized water and absolute ethyl alcohol to centrifuge respectively
Then product after centrifuge washing is dried 12h at 60 DEG C, obtains the Cu of pulverulence by washing 4 times2O nanospheres.
The Cu that the present embodiment obtains2O nanosphere powder, TEM figures are as shown in Figure 1, its mean particle size is 60nm.
Embodiment 2
A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres, includes the following steps：
(1)：0.372g copper nitrates and 4mL water are configured to copper nitrate aqueous solution；Then, by above-mentioned copper nitrate aqueous solution with
100mL ethylene glycol mixes, and is denoted as solution A；
(2)：0.6899g potassium hydroxide and 1mL water are configured to potassium hydroxide aqueous solution；Then, by above-mentioned potassium hydroxide
Aqueous solution is mixed with 320mL ethylene glycol, is denoted as solution B；
(3)：The solution A that step 1 is configured is heated to 100 DEG C；Then the solution B that step 2 is configured is added dropwise again
Enter into solution A, magnetic agitation is remained during addition, and 5min is kept the temperature at 100 DEG C；
(4)：Quality is disposably added to by the glucose powder of 2.0011g in the mixture that step 3 obtains, so
After react 10min, that is, have solid precipitation object generation；
(5)：Contain Cu by what step 4 obtained2The solidliquid mixture of O precipitations uses deionized water and absolute ethyl alcohol to centrifuge respectively
Washing 5 times, then by the product after centrifuge washing, drying for 24 hours, obtains the Cu of pulverulence at 50 DEG C2O nanospheres.
The present embodiment obtains Cu2O nanosphere powder, TEM figures are as shown in Fig. 2, its mean particle size is 75nm.
Embodiment 3
A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres, includes the following steps：
(1)：0.4936g copper sulphate and 2mL water are configured to copper sulfate solution；Then, by above-mentioned copper sulfate solution
It is mixed with 110mL glycerine, is denoted as solution A；
(2)：1.1998g sodium hydroxides and 2mL water are configured to sodium hydrate aqueous solution；Then, by above-mentioned sodium hydroxide
Aqueous solution is mixed with 200mL glycerine, is denoted as solution B；
(3)：The solution A that step 1 is configured is heated to 90 DEG C；Then the solution B that step 2 is configured is added dropwise again
Enter into solution A, magnetic agitation is remained during addition, and 15min is kept the temperature at 90 DEG C；
(4)：Quality is disposably added to by the glucose powder of 0.1153g in the mixture that step 3 obtains, so
After react 8min, that is, have solid precipitation object generation；
(5)：Contain Cu by what step 4 obtained2The solidliquid mixture of O precipitations uses deionized water and absolute ethyl alcohol to centrifuge respectively
Then product after centrifuge washing is dried 18h at 80 DEG C, obtains the Cu of pulverulence by washing 3 times2O nanospheres, grain size
Average out to 80nm.
Embodiment 4
A kind of Cu2The liquid phase preparation process of O nanospheres, includes the following steps：
(1)：2.55g copper chlorides and 0.98g copper sulphate are configured to cupric salt aqueous solution with 10mL water；It then, will be upper
State cupric salt aqueous solution with by ethylene glycol, ethyl alcohol with the volume mixture of equivalent at 800mL organic solvents mix, be denoted as solution
A；
(2)：5.054g potassium hydroxide and 10mL water are configured to potassium hydroxide aqueous solution；Then, by above-mentioned potassium hydroxide
Aqueous solution with by ethylene glycol, ethyl alcohol with the volume mixture of equivalent at 10mL organic solvents mix, be denoted as solution B；
(3)：The solution A that step 1 is configured is heated to 60 DEG C；Then the solution B that step 2 is configured is added dropwise again
Enter into solution A, magnetic agitation is remained during addition, and 8min is kept the temperature at 60 DEG C；
(4)：Quality is disposably added to by the glucose powder of 14.6929g in the mixture that step 3 obtains,
Then 5min is reacted, that is, has the generation of solid precipitation object；
(5)：Contain Cu by what step 4 obtained2The solidliquid mixture of O precipitations uses deionized water and absolute ethyl alcohol to centrifuge respectively
Then product after centrifuge washing is dried 7h at 70 DEG C, obtains the Cu of pulverulence by washing 4 times2O nanospheres, grain size
Average out to 70nm.
Embodiment 5
A kind of Cu2The liquid phase preparation process of O nanospheres, includes the following steps：
(1)：0.5618g copper acetates and 1mL water are configured to acetic acid copper liquor；Then, by above-mentioned acetic acid copper liquor
It is mixed with 100mL ethylene glycol, is denoted as solution A；
(2)：0.3591g sodium hydroxides and 1mL water are configured to sodium hydrate aqueous solution；Then, by above-mentioned sodium hydroxide
Aqueous solution is mixed with 50mL ethylene glycol, is denoted as solution B；
(3)：The solution A that step 1 is configured is heated to 80 DEG C；Then the solution B that step 2 is configured is added dropwise again
Enter into solution A, magnetic agitation is remained during addition, and 10min is kept the temperature at 80 DEG C；
(4)：Quality is disposably added to by the glucose powder of 0.9987g in the mixture that step 3 obtains, so
After react 10min, that is, have solid precipitation object generation；
(5)：Contain Cu by what step 4 obtained2The solidliquid mixture of O precipitations uses deionized water and absolute ethyl alcohol to centrifuge respectively
Then product after centrifuge washing is dried 10h at 65 DEG C, obtains the Cu of pulverulence by washing 5 times2O nanospheres, grain size
Average out to 75nm.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
It should not be construed as limiting the practical range of the present invention.It is all according to all the changes and improvements made by the scope of the invention, should all be still
It belongs within this patent covering scope.
Claims (10)
1. a kind of size is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：Include the following steps：
(1)：Prepare cupric salt mixed solution
Make solute with water as solvent, cupric salt, prepares cupric salt aqueous solution, make Cu2+Molar concentration be 0.1~
3.0mol/L；
Later, at room temperature, above-mentioned cupric salt aqueous solution is mixed with the alcohols solvent of certain volume, obtained cupric salt
Mixed solution is denoted as solution A；
(2)：Configure alkali mixed solution
Make solute with water as solvent, highly basic, prepares aqueous alkali, OH in the aqueous alkali-With Cu in cupric salt aqueous solution2+
Molar ratio be 1~10:1；
Later, at room temperature, above-mentioned aqueous alkali is mixed with the alcohols solvent of certain volume, obtained alkali mixed solution is denoted as
Solution B；
The alcohols solvent is consistent with the alcohols solvent in step (1)；
(3)：Prepare Cu (OH)2Presoma
The solution A that step (1) is configured, is heated to 60~100 DEG C；Then the solution B that step (2) is configured slowly is added again
Enter into solution A, stirring is remained during addition, and keep the temperature 1~15min at 60~100 DEG C；
(4)：Reduction reaction
Glucose powder is disposably added to the Cu (OH) that step (3) is obtained2In presoma, 3~10min is then reacted,
It obtains containing Cu2The solidliquid mixture of O precipitations；
Wherein, the ratio between the glucose of addition and the amount of substance of cupric salt in step (1) are 0.5~10:1；
(5)：Post-processing
Contain Cu by what step (4) obtained2The solidliquid mixture centrifuge washing of O precipitations 3~5 times, then by the production after centrifuge washing
Object drying 6~for 24 hours, obtain the Cu of pulverulence2O nanospheres.
2. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The step
Suddenly in (1), cupric salt is the mixture of one or more of copper nitrate, copper acetate, copper sulphate, copper chloride.
3. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The step
Suddenly the highly basic in (2) is sodium hydroxide, potassium hydroxide.
4. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The alkali
OH in aqueous solution-Molar concentration and cupric salt aqueous solution in Cu2+The ratio between molar concentration be 1~10:1.
5. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The step
Suddenly the alcohols solvent in (1) and (2) is one or more of mixtures of ethyl alcohol, ethylene glycol, glycerine.
6. size is less than the Cu of 100nm according to claim 1 or 52The preparation method of O nanospheres, it is characterised in that：Institute
It states in step (1), the volume ratio of alcohols solvent and cupric salt aqueous solution is 1~100:1.
7. size is less than the Cu of 100nm according to claim 1 or 52The preparation method of O nanospheres, it is characterised in that：Institute
It states in step (2), the volume ratio of alcohols solvent and aqueous alkali is 1~100:1.
8. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The step
Suddenly in (4), the ratio between the amount of substance of cupric salt is 1~6 in the glucose and step (1) of addition:1.
9. size according to claim 1 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：The step
Suddenly it in (5), is washed respectively with deionized water and absolute ethyl alcohol.
10. the size according to claim 1 or 9 is less than the Cu of 100nm2The preparation method of O nanospheres, it is characterised in that：Institute
It states in step (5), the product after centrifuge washing is dry at 50~80 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704387A (en) * | 2019-01-17 | 2019-05-03 | 西安理工大学 | 20 hexahedron Cu of one kind2O, which is situated between, sees the preparation method of crystal powder |
| CN111905835A (en) * | 2020-08-28 | 2020-11-10 | 盐城工学院 | Preparation method and application of efficient photo-thermal catalytic material |
| CN112323138A (en) * | 2020-09-09 | 2021-02-05 | 西安理工大学 | Twin crystal-containing nano cuprous oxide powder and preparation method thereof |
| CN114835152A (en) * | 2022-05-14 | 2022-08-02 | 安徽纳洛米特新材料科技股份有限公司 | Method for industrially producing nano cuprous oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109704387A (en) * | 2019-01-17 | 2019-05-03 | 西安理工大学 | 20 hexahedron Cu of one kind2O, which is situated between, sees the preparation method of crystal powder |
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| CN112323138A (en) * | 2020-09-09 | 2021-02-05 | 西安理工大学 | Twin crystal-containing nano cuprous oxide powder and preparation method thereof |
| CN112323138B (en) * | 2020-09-09 | 2021-10-22 | 西安理工大学 | Twin crystal-containing nano cuprous oxide powder and preparation method thereof |
| CN114835152A (en) * | 2022-05-14 | 2022-08-02 | 安徽纳洛米特新材料科技股份有限公司 | Method for industrially producing nano cuprous oxide |
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