CN102452681A - Porous hollow copper oxide nano fiber and preparation method thereof - Google Patents
Porous hollow copper oxide nano fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a porous hollow copper oxide nano fiber and a preparation method thereof. The method comprises the following steps: 1) dissolving a copper salt and a polymer into ethanol so as to obtain a spinning solution; 2) carrying out electrostatic spinning on the spinning solution obtained in the step 1), and then sintering after electrostatic spinning is finished, so as to obtain the porous hollow copper oxide nano fiber. Compared with the traditional template method and coaxial electrostatic spinning method, the method disclosed by the invention is simple and practicable, and low in cost, and the obtained material is novel in structure and has an important potential application in the fields of preparations of catalysts, gas sensors or semiconductors and the like.
Description
Technical field
The invention belongs to field of nano material preparation, relate to a kind of porous hollow nanofiber and preparation method thereof, be specifically related to a kind of porous hollow cupric oxide nano fiber and preparation method thereof.
Background technology
One-dimensional metal oxide nano-material is because structure is special, and chemical property is excellent, at transmitter, and photoelectricity, aspects such as catalyzer are widely used, and its preparation gets most of the attention with performance study always.Cupric oxide is a kind of as MOX; Show unique character at aspects such as catalysis, desulfurization, sterilizations; Simultaneous oxidation copper nanofiber is an one dimension intrinsic p-type, semiconductor material, has narrower bandwidth (1.2eV), at field-effect transistor(FET); There is wide purposes aspects such as opto-electronic conversion, therefore become the focus of research.The method of traditional preparation process cupric oxide nano fiber comprises: method of electrostatic spinning (H.Wu, D.D.Lin, W.Pan, Applied Physics Letters 2006; 89:133125), template (C.T.Hsieth, J.M.Chen, H.H.Lin; H. C.Shih, Applied Physics Letters 2003,82:3316), heat deposition method (W.Wang; Z.Liu, Y.Liu, C.Xu, C.Zheng; G.Wang, Applied Physics A-Materials Science & Processing, 2003,76:417) etc.In these methods, method of electrostatic spinning is simple and convenient, and the cupric oxide nano fiber of acquisition reaches several microns, so become the typical method of preparation one dimension copper oxide nano material.In recent years, in order to increase the metal oxide nano fiber specific surface area to improve its original performance, people are often through following method design and preparation hollow metal oxidate nano fiber: (1) template: with the fiber-like material is template; Through electroless plating; Sintering obtains hollow nanofiber (R.A.Caruso, J.H.Schattka, A.Greiner then; Advanced Materials2001,13:1577); (2) coaxial electrostatic spinning method: through spinning nozzle is carried out coaxial design, spinning obtains having the nanofiber of nucleocapsid structure, and final sintering obtains hollow nanofiber (D.Li, Y.N.Xia, Nano Letters, 2004,4,933).Though these two kinds of methods can both obtain the hollow nanofiber, the former needs multistep, and the latter need carry out special and accurate design to device for spinning, therefore still has certain limitation.In addition, the preparation of relevant porous hollow cupric oxide nano fiber also rarely has report.
Summary of the invention
The purpose of this invention is to provide a kind of porous hollow cupric oxide nano fiber and preparation method thereof.
The method for preparing porous hollow cupric oxide nano fiber provided by the invention comprises the steps:
1) mantoquita and polymkeric substance are dissolved in the ethanol, obtain spinning solution;
2) said step 1) gained spinning solution is carried out electrostatic spinning, carry out sintering again after said electrostatic spinning step finishes, obtain said porous hollow cupric oxide nano fiber.
In the step 1) of aforesaid method, said mantoquita is selected from least a in a Glacial acetic acid copper and the hydration neutralized verdigris, a preferred hydration neutralized verdigris; Said polymkeric substance is selected from least a in PVP K120, vinyl pyrrolidone-vinyl acetate copolymer and PVP K120-Vinyl Acetate Copolymer ester blend, preferably polyethylene base pyrrolidone; Wherein, the relative molecular weight of said Vinylpyrrolidone polymer is 100,000-500,000, preferred 360,000; The weight-average molecular weight of said vinyl pyrrolidone-vinyl acetate copolymer is 45,000-70, and 000, preferred 50,000, in said PVP K120-Vinyl Acetate Copolymer ester blend; The relative molecular weight of PVP K120 is 100,000-500,000, preferred 360,000; The weight-average molecular weight of PVA is 100,000-500,000, preferred 170,000.In vinyl pyrrolidone-vinyl acetate copolymer; The mass ratio of vinyl pyrrolidone and vinyl acetate can be 6: 4; In the blend that PVP K120 and PVA are formed, the mass ratio of PVP K120 and PVA can be 9: 1.
Said organic solvent is an ethanol.The mass ratio of said polymkeric substance and said mantoquita is 2-8: 1, preferred 4: 1-6: 1; In the said spinning solution, the mass percentage concentration of said polymkeric substance is 5-20%, specifically can be 9-11%, 11-15%, 5-11% or 11-20%, preferred 9%-15%.
Said step 2) in the electrostatic spinning step, voltage is 10-20KV, preferred 10-15KV; The flow velocity of spinning solution is 0.1-0.01ml/min, preferred 0.02-0.05ml/min; The internal diameter of spray silk syringe needle is the 0.5-1.0 millimeter, preferred 0.6-0.8 millimeter; The spacing of spray silk syringe needle and dash receiver is 10-20 centimetre, preferred 10-15 centimetre; In the said sintering step, temperature is 450-550 ℃, preferred 500-550 ℃; Time is 2-10 hour; Specifically can be 2-3 hour, 3-5 hour, 5-10 hour or 2-5 hour, preferred 2-5 hour, heat-up rate was 5 ℃/min-15 ℃/min; Specifically can be 5 ℃/min-6.7 ℃/min, 6.7 ℃/min-10 ℃/min or 6.7 ℃/min-15 ℃/min, preferred 5 ℃/min-10 ℃/min.
Prepare gained porous hollow cupric oxide nano fiber according to the method described above, also belong to protection scope of the present invention.
The diameter of this porous hollow cupric oxide nano fiber is the 50-1200 nanometer, preferred 100-400 nanometer, and specific surface area is 8-20m
2/ g.
In addition, the application of the porous hollow cupric oxide nano fiber that the invention described above provides in preparation catalyzer, gas sensor or semiconducter device also belongs to protection scope of the present invention.
The present invention prepares porous hollow cupric oxide nano fiber through simple method.Compare traditional template and coaxial electrostatic spinning method, this method is simple, need not carry out special design to electrostatic spinning apparatus, need not multistep and handles, and with low cost, the material structure of acquisition is special, novelty.Hollow porous copper oxide nanofiber provided by the invention all has important potential application in fields such as preparation catalyzer, gas sensor or semiconducter device.
Description of drawings
Fig. 1 is the embodiment of the invention 1 step 2) stereoscan photograph of electrostatic spinning step gained nano fiber non-woven fabric.
Fig. 2 is the stereoscan photograph of the embodiment of the invention 1 gained porous hollow cupric oxide nano fiber.
Fig. 3 is the XRD analysis figure of the embodiment of the invention 1 gained porous hollow cupric oxide nano fiber.
Fig. 4 is the transmission electron microscope photo of the embodiment of the invention 1 gained porous hollow cupric oxide nano fiber.
Fig. 5 is the stereoscan photograph of the embodiment of the invention 2 gained porous hollow cupric oxide nano fibers.
Fig. 6 is the transmission electron microscope photo of the embodiment of the invention 2 gained porous hollow cupric oxide nano fibers.
Fig. 7 is the stereoscan photograph of the embodiment of the invention 3 gained porous hollow cupric oxide nano fibers.
Fig. 8 is the transmission electron microscope photo of the embodiment of the invention 3 gained porous hollow cupric oxide nano fibers.
Fig. 9 is the stereoscan photograph of the embodiment of the invention 4 gained porous hollow cupric oxide nano fibers.
Figure 10 is the transmission electron microscope photo of the embodiment of the invention 4 gained porous hollow cupric oxide nano fibers.
Figure 11 is the stereoscan photograph of the embodiment of the invention 5 gained porous hollow cupric oxide nano fibers.
Figure 12 is the transmission electron microscope photo of the embodiment of the invention 5 gained porous hollow cupric oxide nano fibers.
Figure 13 is the stereoscan photograph of the embodiment of the invention 6 gained porous hollow cupric oxide nano fibers.
Figure 14 is the transmission electron microscope photo of the embodiment of the invention 6 gained porous hollow cupric oxide nano fibers.
Figure 15 is the stereoscan photograph of the embodiment of the invention 7 gained porous hollow cupric oxide nano fibers.
Figure 16 is the transmission electron microscope photo of the embodiment of the invention 7 gained porous hollow cupric oxide nano fibers.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but the present invention is not limited to following examples.Method is ordinary method if no special instructions described in the following embodiment, and said compound all obtains from open commercial sources purchase if no special instructions.The molecular weight of used PVP K120 (Mr) is 360,000 among the following embodiment, and PIN is K90, all available from Fluka company.Weight-average molecular weight (the M of vinyl pyrrolidone-vinyl acetate copolymer
w) be 50,000, PIN is CAS25086-89-9, and all available from Aladdin reagent ltd, in this multipolymer, the mass ratio of vinyl pyrrolidone and vinyl acetate is 6: 4.In the blend that PVP K120 and PVA are formed, the molecular weight (M of PVP K120
r) be 360,000, the weight-average molecular weight (M of PVA
w) being 170,000, the mass ratio of PVP K120 and PVA is 9: 1, and the PIN of this blend is CAS:9003-20-7, all available from Acros Organics company.
In the X-ray diffraction test (XRD), used instrument is Japanese Rigaku D/max 2500 powder diffractometers, the copper target, and WV 40kV, working current 200mA. scanning (2 θ) scope is 3 °～80 °, sweep velocity is 8 °/min.In the nitrogen adsorption specific surface area test of porous hollow cupric oxide nano fiber, used instrument is Micromertics ASAP2020M, and testing method is for testing 100 ℃ of degassings sample after 10 hours.
Embodiment 1
1) a hydration neutralized verdigris is dissolved in the ethanol, ultrasonic to dissolving fully.Add molecular weight (M then
r) be 360,000 PVP K120 mixings, obtain spinning solution.
In this spinning solution, the mass ratio of PVP K120 and neutralized verdigris is 4: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 9%.
2) with step 1) gained spinning solution electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 6.7 ℃/min be raised to 500 ℃, 500 ℃ of sintering 2 hours, obtain porous hollow cupric oxide nano fiber.Wherein, the condition of electrostatic spinning is: voltage is 10KV; The spinning solution flow velocity is 0.02ml/min; The internal diameter of spray silk syringe needle is that the spacing of 0.8mm spray silk syringe needle and dash receiver is 13cm.
Fig. 1 is a step 2) stereoscan photograph of electrostatic spinning step gained nano fiber non-woven fabric.Fig. 2 is the stereoscan photograph of present embodiment gained porous hollow cupric oxide nano fiber.Fig. 3 is the XRD analysis figure of present embodiment gained porous hollow cupric oxide nano fiber.Fig. 4 is the transmission electron microscope photo of present embodiment gained porous hollow cupric oxide nano fiber.XRD figure shown in Figure 3 and cupric oxide standard spectrogram are compared, confirm that it is the oblique system cupric oxide that this embodiment prepares the gained nanofiber.This nanofiber diameter is 50nm-150nm, and it is 20m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 2
1) will not have the hydration neutralized verdigris and be dissolved in the ethanol, ultrasonic to dissolving fully, add molecular weight (M then
r) be 360,000 PVP K120 mixings, obtain spinning solution.
In this spinning solution, the mass ratio of PVP K120 and neutralized verdigris is 2: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 15%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 10 ℃/min be raised to 500 ℃, 500 ℃ of sintering 3 hours, obtain porous hollow cupric oxide nano fiber.Wherein, the electrostatic spinning condition is: voltage is 10KV; The spinning solution flow velocity is 0.05ml/min; The internal diameter of spray silk syringe needle is 0.8mm; The spacing of spray silk syringe needle and dash receiver is 13cm.
Fig. 5 and Fig. 6 are respectively the stereoscan photograph and the transmission electron microscope photos of gained porous hollow cupric oxide nano fiber.This nanofiber diameter is 150-300nm, and it is 13m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 3
1) will not have the hydration neutralized verdigris and be dissolved in the ethanol, ultrasonic to dissolving fully.Add weight-average molecular weight (M then
w) be the multipolymer mixing of vinyl pyrrolidone-vinyl acetate of 50,000, obtain spinning solution.
In this spinning solution, the mass ratio of multipolymer and neutralized verdigris is 8: 1, and the mass percentage concentration of this multipolymer in spinning solution is 15%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 5 ℃/min be raised to 450 ℃, 450 ℃ of sintering 5 hours, obtain porous hollow cupric oxide nano fiber.Wherein, the electrostatic spinning condition is: voltage is 10KV; The spinning solution flow velocity is 0.02ml/min; The internal diameter of spray silk syringe needle is 0.5mm; The spacing of spray silk syringe needle and dash receiver is 13cm.
Fig. 7 and Fig. 8 are respectively the stereoscan photograph and the transmission electron microscope photos of gained porous hollow cupric oxide nano fiber.This nanofiber diameter is 300-500nm, and it is 11m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 4
1) a hydration neutralized verdigris is dissolved in the ethanol, ultrasonic to dissolving fully.Add molecular weight (M then
r) be 360,000 PVP K120 and weight-average molecular weight (M
w) be the blend mixing of 170,000 PVA (mass ratio of two kinds of polymkeric substance is 9: 1), obtain spinning solution.
In this spinning solution, the mass ratio of polymkeric substance and neutralized verdigris is 4: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 20%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 6.7 ℃/min be raised to 550 ℃, 550 ℃ of sintering 2 hours, obtain porous hollow cupric oxide nano fiber.Wherein, the electrostatic spinning condition is: voltage is 20KV; The spinning solution flow velocity is 0.02ml/min; The internal diameter of spray silk syringe needle is 1.0mm; The spacing of spray silk syringe needle and dash receiver is 20cm.
Fig. 9 and Figure 10 are respectively the stereoscan photograph and the transmission electron microscope photos of gained porous hollow cupric oxide nano fiber.The diameter of this nanofiber is 300-1200nm, and it is 8m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 5
1) Glacial acetic acid copper is dissolved in the ethanol, ultrasonic to dissolving fully, add molecular weight (M then
r) be 360,000 PVP K120 mixings, obtain spinning solution.
In this spinning solution, the mass ratio of PVP K120 and neutralized verdigris is 6: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 5%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, the back that finishes is raised to 450 ℃ of sintering 5 hours with the heat-up rate of 6.7 ℃/min in retort furnace, obtains porous hollow cupric oxide nano fiber.Wherein, spinning condition is: voltage is 10KV; The spinning solution flow velocity is 0.02ml/min; The internal diameter of spray silk syringe needle is 0.6mm; The spacing of spray silk syringe needle and dash receiver is 13cm.
Figure 11 and Figure 12 are respectively the stereoscan photograph and the transmission electron microscope photos of gained porous hollow cupric oxide nano fiber.The diameter of this nanofiber is 100nm-300nm, and it is 12m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 6
1) Glacial acetic acid copper is dissolved in the ethanol, ultrasonic to dissolving fully, add molecular weight (M then
r) be 360,000 PVP K120 mixings, obtain spinning solution.
In this spinning solution, the mass ratio of PVP K120 and neutralized verdigris is 4: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 11%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 15 ℃/min be raised to 500 ℃, 500 ℃ of sintering 3 hours, obtain porous hollow cupric oxide nano fiber.Wherein, spinning condition is: voltage is 10KV; The spinning solution flow velocity is 0.01ml/min; The internal diameter of spray silk syringe needle is 1.0mm; The spacing of spray silk syringe needle and dash receiver is 10cm.
Figure 13 and Figure 14 are respectively the stereoscan photograph and the transmission electron microscope photos of gained porous hollow cupric oxide nano fiber.The diameter of this nanofiber is 100nm-300nm, and it is 13m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Embodiment 7
1) a hydration neutralized verdigris is dissolved in the ethanol, ultrasonic to dissolving fully, add molecular weight (M then
r) be 360,000 PVP K120 mixings, obtain spinning solution.
In this spinning solution, the mass ratio of PVP K120 and neutralized verdigris is 4: 1, and the mass percentage concentration of this polymkeric substance in spinning solution is 11%.
2) step 1) gained spinning solution is carried out electrostatic spinning under the voltage electrostatic field, after finishing again in retort furnace the heat-up rate with 5 ℃/min be raised to 500 ℃, 500 ℃ of sintering 2 hours, obtain porous hollow cupric oxide nano fiber.Wherein, the electrostatic spinning condition is: voltage is 15KV; The spinning solution flow velocity is 0.1ml/min; The internal diameter of spray silk syringe needle is 1.0mm; The spacing of spray silk syringe needle and dash receiver is 15cm.
Figure 15 and Figure 16 are respectively the stereoscan photograph and the transmission electron microscope photos of the porous hollow cupric oxide nano fiber of gained.The diameter of this nanofiber is 100nm-300nm, and it is 12m that the test of nitrogen adsorption specific surface area obtains this porous hollow cupric oxide nano fiber specific surface area
2/ g.
Claims (9)
1. a method for preparing porous hollow cupric oxide nano fiber comprises the steps:
1) mantoquita and polymkeric substance are dissolved in the ethanol, obtain spinning solution;
2) said step 1) gained spinning solution is carried out electrostatic spinning, carry out sintering again after said electrostatic spinning step finishes, obtain said porous hollow cupric oxide nano fiber.
2. method according to claim 1 is characterized in that: in the said step 1), said mantoquita is selected from least a in a Glacial acetic acid copper and the hydration neutralized verdigris, a preferred hydration neutralized verdigris;
Said polymkeric substance is selected from least a in PVP K120, vinyl pyrrolidone-vinyl acetate copolymer and PVP K120-Vinyl Acetate Copolymer ester blend, preferably polyethylene base pyrrolidone; The relative molecular weight of said Vinylpyrrolidone polymer is 100,000-500, and 000, preferred 360,000, the weight-average molecular weight of said vinyl pyrrolidone-vinyl acetate copolymer is 45; 000-70,000, preferred 50,000, in said PVP K120-Vinyl Acetate Copolymer ester blend; The relative molecular weight of PVP K120 is 100,000-500,000, preferred 360,000; The weight-average molecular weight of PVA is 100,000-500,000, preferred 170,000.
3. method according to claim 1 and 2 is characterized in that: in the said step 1), the mass ratio of said polymkeric substance and said mantoquita is 2-8: 1, preferred 4: 1-6: 1; In the said spinning solution, the mass percentage concentration of said polymkeric substance is 5-20%, preferred 9%-15%.
4. according to the arbitrary described method of claim 1-3, it is characterized in that: said step 2) in the electrostatic spinning step, voltage is 10-20KV, preferred 10-15KV; The flow velocity of spinning solution is 0.1-0.01ml/min, preferred 0.02-0.05ml/min; The internal diameter of spray silk syringe needle is the 0.5-1.0 millimeter, preferred 0.6-0.8 millimeter; The spacing of spray silk syringe needle and dash receiver is 10-20 centimetre, preferred 10-15 centimetre.
5. according to the arbitrary described method of claim 1-4, it is characterized in that: said step 2) in the sintering step, temperature is 450-550 ℃; Preferred 500-550 ℃, the time is 2-10 hour, preferred 2-5 hour; Heat-up rate is 5 ℃/min-15 ℃/min, preferred 5 ℃/min-10 ℃/min.
6. the arbitrary said method of claim 1-5 prepares gained porous hollow cupric oxide nano fiber.
7. nanofiber according to claim 6 is characterized in that: the diameter of said porous hollow cupric oxide nano fiber is the 50-1200 nanometer, preferred 100-400 nanometer.
8. according to claim 6 or 7 described nanofibers, it is characterized in that: said porous hollow cupric oxide nano fiber specific surface area is 8-20m
2/ g.
9. the application of the arbitrary said porous hollow cupric oxide nano fiber of claim 6-8 in preparation catalyzer, gas sensor or semiconducter device.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776603A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Method for preparing porous hollow nano-alumina fiber by static spinning |
| CN103408054A (en) * | 2013-06-09 | 2013-11-27 | 燕山大学 | Preparation method of hierarchical zeolite structural copper oxide |
| CN103979599A (en) * | 2014-05-16 | 2014-08-13 | 齐鲁工业大学 | Method for preparing two-component oxide nanobelt |
| CN106498560A (en) * | 2016-11-10 | 2017-03-15 | 合肥铭志环境技术有限责任公司 | A kind of cotton fiber/electrostatic spinning nano fiber composite air-sensitive material and preparation method thereof |
| CN106835318A (en) * | 2017-02-20 | 2017-06-13 | 南通市中和化纤有限公司 | The cellular porous MnO of high magnification2Composite nano fiber |
| CN107140605A (en) * | 2017-06-29 | 2017-09-08 | 东北师范大学 | A kind of porous oxide and preparation method thereof |
| CN107555466A (en) * | 2017-09-21 | 2018-01-09 | 华中农业大学 | A kind of preparation method of copper oxide nano fiber |
| CN109399691A (en) * | 2018-12-04 | 2019-03-01 | 江苏理工学院 | A kind of Cu-CuO/ carbon nano-fiber composite material and preparation method thereof |
| CN109686497A (en) * | 2018-12-18 | 2019-04-26 | 太原理工大学 | The method for preparing copper nanometer grid transparent electrode based on vapour phase reduction copper oxide |
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| CN102776603A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Method for preparing porous hollow nano-alumina fiber by static spinning |
| CN103408054A (en) * | 2013-06-09 | 2013-11-27 | 燕山大学 | Preparation method of hierarchical zeolite structural copper oxide |
| CN103979599A (en) * | 2014-05-16 | 2014-08-13 | 齐鲁工业大学 | Method for preparing two-component oxide nanobelt |
| CN103979599B (en) * | 2014-05-16 | 2016-02-10 | 齐鲁工业大学 | A kind of preparation method of bi component oxide nano belt |
| CN106498560A (en) * | 2016-11-10 | 2017-03-15 | 合肥铭志环境技术有限责任公司 | A kind of cotton fiber/electrostatic spinning nano fiber composite air-sensitive material and preparation method thereof |
| CN106835318A (en) * | 2017-02-20 | 2017-06-13 | 南通市中和化纤有限公司 | The cellular porous MnO of high magnification2Composite nano fiber |
| CN107140605A (en) * | 2017-06-29 | 2017-09-08 | 东北师范大学 | A kind of porous oxide and preparation method thereof |
| CN107555466A (en) * | 2017-09-21 | 2018-01-09 | 华中农业大学 | A kind of preparation method of copper oxide nano fiber |
| CN109399691A (en) * | 2018-12-04 | 2019-03-01 | 江苏理工学院 | A kind of Cu-CuO/ carbon nano-fiber composite material and preparation method thereof |
| CN109686497A (en) * | 2018-12-18 | 2019-04-26 | 太原理工大学 | The method for preparing copper nanometer grid transparent electrode based on vapour phase reduction copper oxide |
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Application publication date: 20120516 |