CN100443414C - Production of nanometer copper oxide with controllable microstructure - Google Patents
Production of nanometer copper oxide with controllable microstructure Download PDFInfo
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- CN100443414C CN100443414C CNB2005100946315A CN200510094631A CN100443414C CN 100443414 C CN100443414 C CN 100443414C CN B2005100946315 A CNB2005100946315 A CN B2005100946315A CN 200510094631 A CN200510094631 A CN 200510094631A CN 100443414 C CN100443414 C CN 100443414C
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Abstract
The present invention discloses a production method of nanometer copper oxide with a controllable microstructure, which comprises the following steps: step one, cupric nitrate is dissolved in water, and the cupric nitrate and the water are stirred to obtain a cupric nitrate solution; step two, the cupric nitrate solution is violently stirred under temperature of 0 to 100 DEG C; step three, sodium hydroxide solid is once fast added in the cupric nitrate solution under the temperature of 0 to 100 DEG C to carry out a chemical reaction, and the mole ratio of the cupric nitrate and the sodium hydroxide is 1: 2 to 2.5; step four, blue deposition suspension liquid which is generated in the reaction of the step three is heated up, black deposition suspension liquid is generated after the heated blue deposition suspension liquid is stirred and the black deposition suspension liquid is centrifuged, washed and dried to obtain nanometer copper oxide. The present invention has the advantages that the nanometer CuO of different centrifuge shapes is generated below 100 DEG C; the nanometer CuO has the advantages of small grain size, uniform dispersion and no coacervation; the formation of the nanometer CuO of different microstructures has no need of adding stabilizing agents or surface active agents; through changing the adding temperature of precipitant, rod-shaped, filiform and spindle-shaped nanometer CuO of good dispersivity can be obtained.
Description
One technical field
The present invention relates to the preparation method of a kind of preparation of nanomaterials, particularly a kind of nanometer copper oxide with controllable microstructure.
Two background technologies
CuO has unique electricity, magnetic, catalysis characteristics as a kind of broad-spectrum multifunctional inorganic material, is widely used in key areas such as glass, catalyzer, gas sensor, magnetic storage medium and electrode active material.Along with the development of nanoscale science and technology, the preparation of nanometer CuO, characteristic and application thereof also more and more are subjected to people's attention.The chemical constitution that not only depends on material for the performance of nano material, and depend on the factors such as size, microscopic appearance, condition of surface and structure of material, have only the effective control of realization, just might further be applied in the high-tech areas such as microelectronic device the nano material microstructure.Existing preparation method of nano material roughly is divided into vapor phase process, solid phase method and liquid phase method three major types, and the preparation method of common nanometer CuO mainly contains solid phase method, mantoquita thermal decomposition method, ball milled, ultrasonic method and pure hot method etc.People such as Kumar R V are under argon shield; N at 10% water; utilize sonochemical method to synthesize CuO (the Kumar R V of particle diameter in the dinethylformamide system for 6nm; Diamant Y, Gedanken A.Sonochemial synthesis and characterization of nanometer-size Transition metaloxides from metal acetates.Chem.Mater.2000 12 (8): 2301-2305).People such as Hong Z S are with Cu (OAc)
2Be raw material, under 90-180 ℃, obtained ball shaped nano CuO (the HongZ S of particle diameter 3-9nm with the hot method of ethanol, Cao Y, Deng J F.A convenient alcohothermal approach for low temperature synthesis ofCuO nanoparticles.Mater.Lett.2002 52:34-38).
For aforesaid method, although solid phase method operation is simple, the product size distribution of gained is inhomogeneous, and for the regulation and control inconvenience of microstructure.Additive method, higher as product good dispersity in organic solvent system, specific surface area, but productive rate is low, cost is higher, and reaction conditions is very harsh; Preparation cost is lower in aqueous phase system, but the product bad dispersibility, and for the product that obtains different-shape need add stablizer, reacting weight is very little, is unfavorable for suitability for industrialized production.
Three summary of the invention
The object of the present invention is to provide a kind of technology simple, be suitable for suitability for industrialized production, and product has the preparation method of the nanometer copper oxide with controllable microstructure of qualities such as high-specific surface area, homodisperse, particle diameter are little.
The technical scheme that realizes the object of the invention is: a kind of preparation method of nanometer copper oxide with controllable microstructure may further comprise the steps:
The first step, cupric nitrate is soluble in water, stir and be made into copper nitrate solution;
In second step,, and cupric nitrate is fully dissolved with copper nitrate solution violent stirring under 0~100 ℃ temperature;
The 3rd step, sodium hydrate solid is carried out chemical reaction in the copper nitrate solution under the temperature in disposable quick second step of adding, the mol ratio of cupric nitrate and sodium hydroxide is 1: 2~2.5;
In the 4th step, the blueness precipitation suspension that reaction in the 3rd step is generated is warmed up to 95~100 ℃, fully stirs afterreaction and generates black precipitate suspension;
In the 5th step, the black powder that the black precipitate suspension that generates is centrifugal, washing, drying obtain is a nano cupric oxide.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, the copper nitrate solution volumetric molar concentration that is made into is 0.02~0.1molL
-1
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, copper nitrate solution is violent stirring under 95~100 ℃ temperature.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, copper nitrate solution is violent stirring under 80~85 ℃ temperature.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, copper nitrate solution is violent stirring under 60~65 ℃ temperature.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, copper nitrate solution is violent stirring under 20~25 ℃ temperature.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, copper nitrate solution is violent stirring under 2~5 ℃ temperature.
Among the preparation method of nanometer copper oxide with controllable microstructure of the present invention, blueness precipitation suspension is warmed up to 95~100 ℃ fully stirred 0.5~1 hour down.
The present invention compared with prior art, its remarkable advantage is: (1) is simple to operate, the equipment facility, reaction system is a water, cost is low, is suitable for suitability for industrialized production; (2) temperature of reaction is relatively low, and the nanometer CuO of diverse microcosmic appearance all is being lower than 100 ℃ of generations down; (3) the nanometer CuO particle diameter of gained is little, is uniformly dispersed, and does not have reunion substantially; (4) need not to add any stablizer or tensio-active agent in the formation of different microstructure nanometer CuO; (5) simple by changing the adding temperature of precipitation agent, obtained bar-shaped, thread, the fusoid nanometer CuO of good dispersity.
Four description of drawings
Fig. 1 is the preparation method's of a nanometer copper oxide with controllable microstructure of the present invention schematic flow sheet.
Fig. 2 is the rod-like nano CuO transmission electron microscope picture of preparation method's gained when 100 ℃ of reactions of nanometer copper oxide with controllable microstructure of the present invention.
Fig. 3 is the silky nano CuO transmission electron microscope picture of preparation method's gained when 60 ℃ of reactions of nanometer copper oxide with controllable microstructure of the present invention.
Fig. 4 is the spindle shape nanometer CuO transmission electron microscope picture of preparation method's gained when 25 ℃ of reactions of nanometer copper oxide with controllable microstructure of the present invention.
Fig. 5 is the spindle shape nanometer CuO transmission electron microscope picture of preparation method's gained when 2 ℃ of reactions of nanometer copper oxide with controllable microstructure of the present invention.
Five embodiments
Below in conjunction with accompanying drawing the present invention is further described.
In conjunction with Fig. 1, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step, cupric nitrate is soluble in water, and stirring and being made into volumetric molar concentration is 0.02~0.1molL
-1Copper nitrate solution;
In second step,, and cupric nitrate is fully dissolved with copper nitrate solution violent stirring under 0~100 ℃ temperature;
The 3rd step, sodium hydrate solid is carried out chemical reaction in the copper nitrate solution under the temperature in disposable second step of adding, the mol ratio of cupric nitrate and sodium hydroxide is 1: 2~2.5;
In the 4th step, the blueness precipitation suspension that reaction in the 3rd step is generated is warmed up to 95~100 ℃, fully stirs 0.5~1 hour afterreaction and generates black precipitate suspension;
In the 5th step, the black powder that the black precipitate suspension that generates is centrifugal, washing, drying obtain is a nano cupric oxide.
Reaction equation among the preparation method of nanometer copper oxide with controllable microstructure of the present invention is:
Cu(NO
3)
2+2NaOH→Cu(OH)
2+2NaNO
3
Embodiment 1: in conjunction with Fig. 1, Fig. 2, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 1.45g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 100 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 0.5g is above-mentioned 100 ℃, react very violent, and have a large amount of black precipitates to generate immediately;
In the 4th step, above-mentioned black precipitate suspension was descended abundant stirring reactions 0.5~1 hour at 100 ℃;
In the 5th step, the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter, and to be about the bar-shaped CuO of 5nm nanocrystalline.
Embodiment 2: in conjunction with Fig. 1, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 2.9g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 80 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1g is above-mentioned 80 ℃, react more violent, and have a large amount of black precipitates to generate very soon;
The 4th step was warmed up to 99 ℃ with above-mentioned black precipitate suspension, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is the bar-shaped CuO of the about 10nm of diameter.
Embodiment 3: in conjunction with Fig. 1, Fig. 3, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 4.35g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 60 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1.44g is above-mentioned 60 ℃, react more violent, and have a large amount of blueness precipitations to generate very soon;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 98 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline at the thread CuO of 8~40nm that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter.
Embodiment 4: in conjunction with Fig. 1, Fig. 4, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 5.8g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 25 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1.9g is above-mentioned 25 ℃, react more violent, and have a large amount of blueness precipitations to generate very soon;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 97 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is the spindle shape CuO of the about 140nm of diameter.
Embodiment 5: in conjunction with Fig. 1, Fig. 5, the preparation method of nanometer copper oxide with controllable microstructure of the present invention may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 7.2g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
In second step, the copper nitrate solution for preparing is cooled to 2 ℃ under violent stirring;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 2.4g is above-mentioned 2 ℃, there is a large amount of blueness precipitations to generate gradually;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 96 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline at the spindle shape CuO of 100~150nm that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter.
From above embodiment as can be known, the preparation method of nanometer copper oxide with controllable microstructure of the present invention has changed the habit of nanometer CuO crystal grain, thereby has obtained the nanometer CuO product of diverse microcosmic structure by regulating the adding temperature of precipitation agent NaOH.When adding NaOH down for 100 ℃, gained nanometer CuO is the rod-shaped particle of favorable dispersity, and its diameter is about 5nm, and length is 25~40nm, and dispersed fine, uv-vis spectra presents tangible blue shift phenomenon.And when adding NaOH down for 60 ℃, product has become the CuO nano thread, the about 8~40nm of diameter, and length is 200~600nm.And products therefrom is that spindle shape CuO is nanocrystalline after adding NaOH under 25 ℃, the about 140nm of diameter, and length is 400~600nm; Products therefrom is that spindle shape CuO is nanocrystalline after adding NaOH under 2 ℃, and diameter is 100~150nm, and length is 0.6~1.4 μ m.This is much larger than the calculation result of X-ray diffraction, and the aggregate that this fusiform particle may be made up of less crystallite is described.But 2 ℃ down add NaOH after the nanocrystalline length of gained spindle shape CuO obviously elongated.This shows that low temperature has caused the gathering growth of CuO nanocrystal and made its microscopic appearance that very big change arranged.This is because as a kind of material with anisotropic properties, and the CuO crystal has the trend of preferred orientation growth.Add NaOH when at a lower temperature, under the condition that slowly heats up, the Cu (OH) that at first generates in the solution
2Precipitation is along with the rising gradually of temperature, be decomposed into the lower CuO of solubleness gradually, promptly nucleation and growth are not significantly isolated in system, in nucleation process, also have a large amount of solutes to be used for growth in the solution, and the CuO crystal grain that slowly generates is assembled gradually along certain crystal face and is grown up, and nucleation and growth velocity are all very slow in this process, assemble to have generated the bigger fusiform particle of particle diameter.On the contrary, if under comparatively high temps, add NaOH, high temperature impels high speed of reaction, produce the effect that nuclear is given birth in outburst, cause having in a short period of time a large amount of nucleus to generate, the nucleation rate of crystal grain substantially exceeds growth velocity in the solution, and crystal grain has little time to assemble growth, solute in the solution has consumed fully, and particle diameter is less, the rod-shaped particle of distribution uniform thereby generated.
Claims (5)
1, a kind of preparation method of nanometer copper oxide with controllable microstructure is characterized in that may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 1.45g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 100 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 0.5g is above-mentioned 100 ℃, react very violent, and have a large amount of black precipitates to generate immediately;
In the 4th step, above-mentioned black precipitate suspension was descended abundant stirring reactions 0.5~1 hour at 100 ℃;
In the 5th step, it is that the bar-shaped CuO of 5nm is nanocrystalline that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter.
2, a kind of preparation method of nanometer copper oxide with controllable microstructure is characterized in that may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 2.9g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 80 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1g is above-mentioned 80 ℃, react more violent, and have a large amount of black precipitates to generate very soon;
The 4th step was warmed up to 99 ℃ with above-mentioned black precipitate suspension, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is the bar-shaped CuO of diameter 10nm.
3, a kind of preparation method of nanometer copper oxide with controllable microstructure is characterized in that may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 4.35g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 60 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1.44g is above-mentioned 60 ℃, react more violent, and have a large amount of blueness precipitations to generate very soon;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 98 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline at the thread CuO of 8~40nm that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter.
4, a kind of preparation method of nanometer copper oxide with controllable microstructure is characterized in that may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 5.8g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
Second step is with the temperature adjustment to 25 ℃ under violent stirring of the copper nitrate solution for preparing;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 1.9g is above-mentioned 25 ℃, react more violent, and have a large amount of blueness precipitations to generate very soon;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 97 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is the spindle shape CuO of diameter 140nm.
5, a kind of preparation method of nanometer copper oxide with controllable microstructure is characterized in that may further comprise the steps:
The first step: be furnished with in the three-necked flask of mechanical stirring and reflux one, add the water of 7.2g cupric nitrate and 300mL respectively, stirred 10~20 minutes, fully dissolving;
In second step, the copper nitrate solution for preparing is cooled to 2 ℃ under violent stirring;
In the 3rd step, in the copper nitrate solution that the disposable quick adding of the NaOH solid of 2.4g is above-mentioned 2 ℃, there is a large amount of blueness precipitations to generate gradually;
The 4th goes on foot, and above-mentioned blue precipitation suspension is warmed up to 96 ℃, and blue precipitation gradates and is black, abundant then stirring reaction 0.5~1 hour;
In the 5th step, it is nanocrystalline at the spindle shape CuO of 100~150nm that the black powder that the black precipitate suspension after the ageing is centrifugal, washing, drying obtain is diameter.
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CN101407332B (en) * | 2007-10-12 | 2011-04-27 | 新疆大学 | Hydro-thermal synthesis method for cupric oxide nano-rod |
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CN108128795A (en) * | 2018-01-17 | 2018-06-08 | 上海电力学院 | A kind of method nanocrystalline room temperature synthesis CuO |
CN109675516A (en) * | 2019-01-09 | 2019-04-26 | 东南大学 | The method of the calcium copper complex microsphere of porous hollow is prepared based on hydro-thermal reaction |
CN110144479B (en) * | 2019-05-15 | 2020-06-16 | 内蒙古工业大学 | Method for in-situ synthesis of aluminum-based composite material with hierarchical structure |
CN112473667B (en) * | 2020-11-24 | 2022-11-29 | 西安理工大学 | Cu of different morphology and surface + Preparation method of CuO catalyst |
CN113247942B (en) * | 2021-05-13 | 2022-04-26 | 贵州理工学院 | Preparation method and application of nano copper oxide |
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