CN106006715A - Method for preparing nano zinc oxide by using liquid diaphragm discharge plasma - Google Patents
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Abstract
The invention provides a method for preparing nano zinc oxide by using liquid diaphragm discharge plasma. The method produces the nano zinc oxide by using zinc plates as an anode and a cathode and Na2SO4 solution as electrolyte, irradiating the zinc plate of the anode with liquid diaphragm discharge plasma, and electrochemically sacrificing the zinc plate of the anode. By using the principle of radiation chemistry, transient high temperature and local high pressure are produced in liquid with light and shock wave, and high-activity particles are also produced to initiate chemical reactions, enabling the reactions such as oxidation, reduction, decomposition and hydrolysis to prepare nanoparticles; the nano zinc oxide synthesized herein has good dispersity, low aggregating degree and uniform particle size distribution and has a promising application prospect in terms of catalysis, optics, magnetics, mechanics and the like; products are easy to separate, high in purity and free of pollution; in addition, the method has the advantages of mild conditions, controllable process, simple equipment, good operation convenience, low cost and the like and is applicable to industrial production.
Description
Technical field
The present invention relates to the preparation method of a kind of nano zine oxide, particularly relate to one and utilize liquid phase barrier film plasma discharging
Body prepares the method for nano zine oxide, belongs to the preparation field of inorganic nano material.
Background technology
Nano-ZnO be particle size be the ultrafine dust of 1 ~ 100 nm, it has the dimensional effect of nano material, quantum tunnel
Channel effect, skin effect.Nano-ZnO has wide forbidden band (3.7 eV) and big exciton binding energy (6 eV), is that one has
Quasiconductor and piezoelectric property and thus produce the material of various peculiar property.Nano-ZnO is as a kind of novel function nano
Material, compared with traditional Z nO material, has the advantages such as chemism is higher, product granularity is nanoscale, specific surface area is bigger,
The specificity more incomparable than general ZnO product is shown at the aspect such as optical, electrical, magnetic, chemistry, physics, photocatalysis, sensitivity
Can, can be widely used for ultraviolet screener, fluorophor, cosmetics, effective catalyst, chemical sensor, image recording material, magnetic
Material, piezoelectric device, solaode and medicine and other fields, show tempting application prospect.Thus, the system of nano-ZnO
Preparation Method has become the focus of research both at home and abroad.
The method that current report the most in succession prepares nano zine oxide mainly has: chemical vapor infiltration, sol-gel process, electricity
Chemical method, hydrothermal synthesis method, microemulsion method, spray pyrolysis, the ultrasonic radiation sedimentation method, alcoholysis method, thermal decomposition method etc., use these
Method can prepare multiple micro/nano structure ZnO such as having tubulose, flower-shaped, bar-shaped, lamellar, wire, banding and pyreniform.
The feature of this kind of method is first to prepare presoma in the solution, and then the presoma multi-step such as drying, roasting again obtains corresponding
Nano-oxide.Have also needs to complicated valuable special equipment；Some costs of material are expensive, complex process；Some temperature
Higher, the response time is long, and process is difficult to control to, and productivity is low；Have is seriously polluted, is difficult to the shortcomings such as popularization.
Electrochemical synthesis is the method for the most wide variety of a kind of nano materials, and it has reaction condition temperature
With, process control, environmental protection, and it is prone to the advantages such as automatization.Electrochemistry anodic oxidation is prepared nano-ZnO and is typically used two
Electrode system, negative electrode is platinum electrode or graphite electrode, and anode is zine plate, the aqueous solution of electrolyte many employings fluoride ion or other
Organic solvent.When applying certain voltage at the two poles of the earth, zine plate is oxidized to form nano zine oxide.Such as: the HF-such as Meng Alan
C2H5OH-H2O mixed solution as electrolyte prepare zinc oxide nanowire (Chinese Journal of Inorganic Chemistry, 2005,21 (4):
583-587), Nabeen etc. prepare zinc oxide nano mitron using the mixed solution of sodium sulfide and ammonium fluoride as electrolyte
(Electrochemistry Communications, 2013, 34(34): 9-13).The introducing of fluorion can prepare shape
The nano-ZnO that looks are good, be evenly distributed, but after reaction, the fluorinion concentration in electrolyte is higher, easily causes fluoride pollution.
Liquid phase barrier film glow discharge, discharges also known as under electric discharge under water or liquid, is a kind of novel generation non-equilibrium plasma
The electrochemical method of body.During general electrolytic, anode inserted in narrow meshed quartz test tube and apply hundreds of volt voltage
After, in aperture, aqueous water is breakdown, produces ultraviolet light, shock wave, radiation and high activity particle such as HO, H, O, HO2With
H2O2, these active particles can cause many chemical reactions, as organic wastewater degraded, prepare high-performance polymer, material surface
Modify.But, the research preparing nano-ZnO with liquid phase barrier film discharge plasma technique yet there are no document report.
Summary of the invention
Present invention aims to existing Nano-class zinc oxide preparation process complexity, condition is harsh, pollute environment etc.
Defect, it is provided that a kind of new method convenient, fast, greenization synthesis nano-ZnO utilizes liquid phase barrier film discharge plasma
Prepare nano zine oxide.
One, the preparation of nano zine oxide
The present invention utilizes the method that liquid phase barrier film discharge plasma prepares nano zine oxide, is with zinc metal sheet as anode and negative electrode,
With Na2SO4Solution (concentration is 1 ~ 4 g/L) is electrolyte, utilizes the zinc metal sheet of liquid phase barrier film discharge plasma radiation anode, and
Nano zine oxide is prepared by the zinc metal sheet of electrochemistry sacrificial anode.It is specifically completed by following device and technique:
Discharge in water plasma device: include reactor and interior electrolyte thereof, inserts the negative electrode zinc metal sheet in electrolyte and stone
Ying Guan, and anode zinc metal sheet is placed in quartz ampoule, and on quartz ampoule, bottom distance quartz ampoule, at 0.8 ~ 1.2 cm, open a diameter
Being the aperture 6 of 0.5 ~ 1.0 mm, make anode and cathode electrolyte be connected by this aperture, the aura that aperture 6 sends simultaneously just radiates
To the center of anode zinc metal sheet 5, it is 1.5 ~ 3.0 cm that anode and cathode zinc metal sheet inserts the degree of depth of electrolyte.
Anode and cathode zinc metal sheet need to be carried out by following technique: by first at acetone after high-purity zinc metal sheet liquid honing, polishing
Middle ultrasonic cleaning 10 min, then in the NaOH aqueous solution of 0.3 mol/L, soak 30 min, then with distilled water wash, remove
The oils and fats on zinc metal sheet surface and other organic pollutions.
Preparation technology: utilize liquid phase barrier film plasma discharging body device (Fig. 1), the voltage applied in anode and cathode 550 ~
750 V, electric current is when 90 ~ 200 mA, and aperture two ends produce aura, form stable discharge in water plasma；Anode zinc metal sheet
Be sacrificed and solution become white；After continuous discharge 1 ~ 4 h, ultrasonic 10 ~ 20 min, (rotating speed is 5000 ~ 10000 in centrifugation
R/min), precipitate with deionized water is washed, and is dried 36 ~ 48 h, obtains nano oxidized in thermostatic drying chamber at 40 ~ 60 DEG C
Zinc.
For the uniformity of solution, in course of reaction, electrolyte is carried out continuously stirred by the speed with 80 ~ 150 r/min；
The temperature of electrolyte controls at 20 ~ 35 DEG C.
Two, the sign of product nano zinc oxide
Below by the preparation principle of the current-voltage curve analytic explanation present invention, and spread out by infrared spectrum, x-ray powder
Penetrate, structure and the pattern of material are characterized by scanning electron microscope.
1, current-voltage curve
With LW100J2 DC current regulator power supply (voltage 0 ~ 1000 V, the electric current 0 ~ 1 of Shanghai Li You Electrical Appliances Co., Ltd
A) different voltage, current are measured.Fig. 2 be 2 g/L sodium sulfate be electrolyte, by the different voltage of regulation, the liquid of drafting
The current-voltage curve of phase barrier film discharge plasma.As shown in Figure 2, whole discharge process is divided into four sections: 0 ~ 250 V section, electricity
Stream voltage is the most linear, and general electrolytic occurs；250 ~ 450 V sections, raise with voltage, and current fluctuation rises；450~550
V section, electric current is relatively stable, has discontinuous spark to produce；550 V gradually strengthen with the increase aura of voltage later.But due to electricity
Pressing through height, energy consumption is relatively big, and aura is excessive to the infringement of quartz ampoule aperture too by force.Therefore the present invention mainly select voltage be 550 ~
The glow discharge of about 750 V is tested.It is 550-750 V owing to preparing the voltage range of nano-ZnO, produces in this range
Blaze light, forms plasma, is not common electrolytic process thereby through current-voltage curve analytic explanation discharge process,
But glow discharging process.
2, infrared test
With DIGILAB FTS 3000 FT-IR type infrared spectrometer at 400 ~ 4000 cm-1Scope characterizes the structure of nano-ZnO.
Fig. 3 is the infrared spectrogram of prepared sample.34420 cm-1With 1637 cm-1Place is flexible the shaking of physical absorption water-OH key
Move and bending vibration characteristic absorption peak, 520 ~ 419 cm-1In the range of the absworption peak that occurs be the stronger Zn-of ZnO lattice vibration
O vibration performance absworption peak, through compareing with standard oxidation zinc ultrared spectrum, this peak occurs in that certain Red Shift Phenomena.This is due to grain
The reduction of sub-size and the impact of skin effect, cause absorption intensity to significantly increase, and obvious red shift occurs.
3, XRD test
With Rigaku D/max-2400 type X-ray powder diffractometer (radiation source is CuK α, 40 kV, 150 mA, λ=
0.15406 nm) white powder product is tested.Fig. 4 is the XRD figure spectrum of nano zine oxide.As seen from Figure 4,2θ
There are 7 diffraction maximums in the range of=10 ~ 90 °, lay respectively at 31.7,34.5,36.2,47.6,56.7,62.8,68.1 °, Jing Guoyu
Standard spectrogram JCPDS (No. 36-1451) standard card compares, and these 7 peaks correspond respectively to hexagonal wurtzite structure ZnO's
(100), (002), (101), (102), (110), (103), the diffraction maximum of (112) crystal face.May thereby determine that, obtain receives
Rice ZnO is the ZnO crystal with hexagonal wurtzite structure.From Fig. 4 it can also be seen that these 7 diffraction maximums have obviously
Diffracted intensity, illustrates that the crystallization degree of product is preferable.And in XRD collection of illustrative plates, do not observe Zn and other impurity diffraction maximums,
Illustrate that the purity of product is the highest.It addition, diffraction peaks broadening is obvious, this is one of the characteristic of nanoparticle, shows prepared sample
Product particle diameter is less, is in nanometer scale.Assume that made granule is spherical, according to Debye-Scherrer formulaD =kλ /(β
cosθ), (whereink=0.89, λ=0.1542 nm,βFor half width), calculate diameter of particle.By main peak (101) half-peak breadth
Calculate this crystal face a size of 27.3 nm, show that zinc oxide has the least crystallite dimension.
4, sem test
By JSM-6700F type scanning electron microscope, nano zine oxide is scanned, to observe size and the pattern of sample.
Sample metal spraying after 60 DEG C of vacuum drying before observing.Fig. 5 is the scanning electron microscope of nano zine oxide under 570 V discharge voltages.Permissible
Finding out, prepared product, mainly in club shaped structure as Fructus Musae, size uniform, is about 300 ~ 500 nm, diameter 100 ~ 150
nm.And along with the increase (Fig. 6,650 V electric discharge) of voltage, the length of rod-like nano-zinc oxide is gradually reduced, sample gradually by
Multiple cauliflower form transition stretched for core radioactivity with certain point.
5, X-ray energy spectrum (EDS) test
With the composition of JSM-6700F type X-ray energy spectrum (EDS) test nano zine oxide, test result is shown in Fig. 7.EDS analytical table
Bright: the characteristic peak of only Zn and O in sample, atomic fraction is respectively 56% and 43%, close to 1:1, the i.e. atom of lattice Zn Yu O
The ratio of number is 1:1.White powder prepared by explanation is zinc oxide.It addition, EDS has Elements C, Au and Cu in analyzing, this is
Caused by carbon containing in zinc metal sheet, copper target and metal spraying.
In sum, hinge structure of the present invention has the effect that
1, the present invention utilizes radiation chemistry principle, produces instantaneous high-temperature, partial high pressure along with luminous, impact at liquid internal
The microeffects such as ripple, promote to aoxidize, reduce, decompose and the carrying out of the reaction such as hydrolysis prepares nanoparticle, create for chemical reaction
Make a unique condition；
2, the present invention has mild condition (room temperature, it is not necessary to other gas shields), process control (changes parameter such as voltage or electric current
Size, conduction time, concentration of electrolyte etc., it is thus achieved that different structure, the nano-ZnO of different-grain diameter), equipment is simple, operation side
Just, the feature such as low cost, industrialized production can be carried out；
3, product of the present invention is easy to separate, and product purity is high, pollution-free；The nano zine oxide favorable dispersibility of synthesis, reunion journey
Spend less, even particle size distribution, have broad application prospects at aspects such as catalysis, optics, magnetics, mechanics.
Accompanying drawing explanation
Fig. 1 is the device that nano zine oxide is prepared in liquid phase barrier film electric discharge of the present invention.
Fig. 2 is the current-voltage curve of liquid phase barrier film electric discharge.
The infrared spectrum of Nanometer-sized Rods ZnO when Fig. 3 is 570 V.
The XRD spectrum of Nanometer-sized Rods ZnO when Fig. 4 is 570 V.
Nanometer-sized Rods ZnO SEM pattern under different amplification, (a) × 30000 when Fig. 5 is 570 V； (b)
×50000。
Nanometer cauliflower form zinc oxide SEM pattern under different amplification, (a) × 30000 when Fig. 6 is 650 V；(b)
×50000。
The EDS spectrum of Nanometer-sized Rods ZnO when Fig. 7 is 570 V.
Detailed description of the invention
The method that the present invention is prepared nano zine oxide below in conjunction with specific embodiment is further described.
Embodiment 1
(1) process of anode and cathode zinc metal sheet: take high-purity zinc metal sheet of 4 mm × 1, mm × 15 mm, first exists after liquid honing, polishing
Ultrasonic cleaning 10 min in acetone, then in the NaOH aqueous solution of 0.3 mol/L, soak 30 min, then with distilled water wash,
Remove oils and fats and other organic pollutions on zinc metal sheet surface.
(2) liquid phase barrier film plasma discharging body device: take the reactor 1 of 250 mL temperature-controllable, adds 150 mL 2g/L
Metabisulfite solution is as electrolyte 2；Electrolyte inserts the negative electrode zinc metal sheet 3 of 4 mm × 1, mm × 15 mm and a diameter of 1.5 cm
Quartz ampoule 4；The anode zinc metal sheet 5 of above-mentioned process is placed in quartz ampoule 4；A diameter is opened at 1 cm bottom distance quartz test tube
It is the aperture 6 of 0.5 mm, makes anode and cathode electrolyte be connected by aperture 6；It is 1.5 cm that anode and cathode inserts the degree of depth of solution, the least
The aura that hole 6 sends just is radiated the center of anode zinc metal sheet 5.
(3) preparation of nano zine oxide: the voltage controlling two interpolars is 570 V, and electric current controls at 90 mA, produces in aperture
Blaze light, forms stable glow discharge plasma；In discharge process, anode zinc metal sheet constantly consumes, and solution becomes milky.
For the uniformity of solution, with 100 r/min, solution is carried out continuously stirred.After continuous discharge 2 h, obtain white zinc oxide turbid
Liquid；With the rotating speed centrifugation of 10000 r/min after ultrasonic disperse 30 min, product with distilled water wash for several times to remove electricity
Solve matter sodium sulfate, then with absolute ethanol washing for several times, centrifugal, 50 DEG C are dried under vacuum to constant weight, grind, i.e. obtain rod-like nano oxygen
Changing zinc, scanning electron microscope result is shown in that Fig. 5, EDS spectrogram is shown in Fig. 7.
Embodiment 2
(1) process of anode and cathode zinc metal sheet: the size of anode and cathode zinc metal sheet is 5 mm × 1, mm × 15 mm, the same embodiment of processing mode
1。
(2) liquid phase barrier film plasma discharging body device: with embodiment 1.
(3) preparation of nano zine oxide: the voltage controlling two interpolars is 650 V, it is 110 mA that electric current controls, and produces in aperture
Blaze light, forms stable glow discharge plasma；In discharge process, anode zinc metal sheet constantly consumes, and solution becomes milky.
For the uniformity of solution, with 110 r/min, solution is carried out continuously stirred.After continuous discharge 2 h, obtain white zinc oxide turbid
Liquid；With the rotating speed centrifugation of 10000 r/min after ultrasonic disperse 30 min, product with distilled water wash for several times to remove electricity
Solve matter sodium sulfate, then with absolute ethanol washing for several times, centrifugal, 60 DEG C are dried under vacuum to constant weight, grind, i.e. obtain rod-like nano oxygen
Changing zinc, scanning electron microscope result is shown in Fig. 6.
Embodiment 3
(1) process of anode and cathode zinc metal sheet: the size of anode and cathode zinc metal sheet is 6 mm × 1, mm × 15 mm, the same embodiment of processing mode
1。
(2) discharge in water plasma device: with embodiment 1.
(3) preparation of nano zine oxide: the voltage controlling two interpolars is 700 V, and electric current controls at 130 mA, produces in aperture
Blaze light, forms stable glow discharge plasma；In discharge process, anode zinc metal sheet constantly consumes, and solution becomes milky.
For the uniformity of solution, with 130 r/min, solution is carried out continuously stirred.After continuous discharge 2 h, obtain white zinc oxide turbid
Liquid；With the rotating speed centrifugation of 10000 r/min after ultrasonic disperse 30 min, product with distilled water wash for several times to remove electricity
Solve matter sodium sulfate, then with absolute ethanol washing for several times, centrifugal, 50 DEG C are dried under vacuum to constant weight, grind, i.e. obtain rod-like nano oxygen
Change zinc.According to Debye-Scherrer formulaD =kλ /(β cosθ) calculate this crystal face a size of 23.5 nm.
Claims (9)
1. utilize the method that liquid phase barrier film discharge plasma prepares nano zine oxide, be with zinc metal sheet as anode and negative electrode, with
Na2SO4Solution is electrolyte, utilizes the zinc metal sheet of liquid phase barrier film discharge plasma radiation anode, and by electrochemistry sacrificial anode
Zinc metal sheet prepare nano zine oxide.
Utilize the method that discharge in water plasma prepares nano zine oxide the most as claimed in claim 1, it is characterised in that: be by
Following device and technique complete:
Discharge in water plasma device: include reaction vessel (1) and interior electrolyte (2) thereof, inserts the negative electrode in electrolyte
Zinc metal sheet (3) and quartz ampoule (4), anode zinc metal sheet (5) is placed in quartz ampoule (4), and on quartz ampoule bottom distance quartz ampoule 0.8 ~
Open the aperture (6) of a diameter of 0.5 ~ 1.0 mm at 1.2 cm, make anode and cathode electrolyte be connected by this aperture, aperture simultaneously
(6) aura sent just is radiated the center of anode zinc metal sheet (5)；
Preparation technology: utilize liquid phase barrier film plasma discharging body device, anode and cathode apply voltage at 550 ~ 750 V, electric current
When 90 ~ 200 mA, aperture two ends produce aura, form stable discharge in water plasma；Anode zinc metal sheet is sacrificed and molten
Liquid becomes white；After continuous discharge 1 ~ 4 h, ultrasonic 10 ~ 20 min, centrifugation, precipitate with deionized water is washed, and is dried,
To nano zine oxide.
Utilize the method that discharge in water plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that: quartz
A diameter of 0.5 ~ 1.0 mm of aperture on pipe；It is 1.5 ~ 3.0 cm that anode and cathode zinc metal sheet inserts the degree of depth of electrolyte.
Utilize the method that liquid phase barrier film discharge plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that:
In course of reaction, with the speed of 80 ~ 150 r/min, electrolyte is carried out continuously stirred.
Utilize the method that liquid phase barrier film discharge plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that:
The temperature of electrolyte controls at 20 ~ 35 DEG C.
Utilize the method that liquid phase barrier film discharge plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that:
Electrolyte Na2SO4The concentration of solution is 1 ~ 4 g/L.
Utilize the method that discharge in water plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that: described
Being dried is in thermostatic drying chamber, is dried 36 ~ 48 h at 40 ~ 60 DEG C.
Utilize the method that discharge in water plasma prepares nano zine oxide the most as claimed in claim 2, it is characterised in that: described
The rotating speed of centrifugation is 5000 ~ 10000 r/min.
Utilize the method that discharge in water plasma prepares nano zine oxide the most as claimed in claim 1 or 2, it is characterised in that:
Anode zinc metal sheet need to be carried out processing by following technique: by the most ultrasonic after high-purity zinc metal sheet liquid honing, polishing
Clean 10 min, then in the NaOH aqueous solution of 0.3 mol/L, soak 30 min, then with distilled water wash, remove zinc metal sheet table
The oils and fats in face and other organic pollutions.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673058A (en) * | 2017-01-23 | 2017-05-17 | 上海朗研光电科技有限公司 | Preparation method of titanium dioxide nano-particles based on nano gold solution glow discharge |
| CN107541745A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | A kind of method for preparing nano-cobaltic-cobaltous oxide using liquid barrier film discharge plasma |
| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
| CN107620085A (en) * | 2017-09-13 | 2018-01-23 | 西北师范大学 | A kind of method that hexagonal phase nanometer h molybdenum trioxides are prepared using liquid phase cathode glow discharging plasma |
| CN108044125A (en) * | 2017-09-14 | 2018-05-18 | 白银有色集团股份有限公司 | A kind of method for preparing Ag nano particles using liquid membrane discharge plasma |
| CN111235588A (en) * | 2020-01-17 | 2020-06-05 | 西北师范大学 | Method for preparing nano zinc oxide by liquid cathode glow discharge plasma |
| CN111822727A (en) * | 2020-06-28 | 2020-10-27 | 合肥百诺金科技股份有限公司 | Method for synthesizing metal nano-particles by liquid-phase discharge of rough electrode surface structure |
| CN114016048A (en) * | 2021-12-16 | 2022-02-08 | 西北师范大学 | Zn (OH) with micro-nano structure2And a controllable preparation method of ZnO |
| CN114232003A (en) * | 2021-12-16 | 2022-03-25 | 西北师范大学 | Cu preparation by utilizing cathode glow discharge electrolytic plasma technology2Method for producing O nanoparticles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498051A (en) * | 2009-01-16 | 2009-08-05 | 北京大学 | Preparation of zinc oxide nano-wire array |
| CN103628107A (en) * | 2012-08-27 | 2014-03-12 | 北京低碳清洁能源研究所 | Electrodeposition method for preparing ZnO nanostructure |
| CN104229868A (en) * | 2014-09-17 | 2014-12-24 | 上海大学 | Preparation method of zinc oxide nano tree structure |
-
2016
- 2016-05-20 CN CN201610338565.XA patent/CN106006715B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498051A (en) * | 2009-01-16 | 2009-08-05 | 北京大学 | Preparation of zinc oxide nano-wire array |
| CN103628107A (en) * | 2012-08-27 | 2014-03-12 | 北京低碳清洁能源研究所 | Electrodeposition method for preparing ZnO nanostructure |
| CN104229868A (en) * | 2014-09-17 | 2014-12-24 | 上海大学 | Preparation method of zinc oxide nano tree structure |
Non-Patent Citations (2)
| Title |
|---|
| L.S. CHUAH等: "Nanoporous ZnO prepared by electrochemical anodization deposition", 《PROC. OF SPIE》 * |
| 刘永军等: "液相隔膜辉光放电等离子体自由基发射光谱研究", 《光谱学与光谱分析》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106673058B (en) * | 2017-01-23 | 2019-04-16 | 上海朗研光电科技有限公司 | Titania nanoparticles preparation method based on nano metal solution glow discharge |
| CN106673058A (en) * | 2017-01-23 | 2017-05-17 | 上海朗研光电科技有限公司 | Preparation method of titanium dioxide nano-particles based on nano gold solution glow discharge |
| CN107541745B (en) * | 2017-09-13 | 2019-08-02 | 西北师范大学 | A method of nano-cobaltic-cobaltous oxide is prepared using liquid diaphragm discharge plasma |
| CN107620085A (en) * | 2017-09-13 | 2018-01-23 | 西北师范大学 | A kind of method that hexagonal phase nanometer h molybdenum trioxides are prepared using liquid phase cathode glow discharging plasma |
| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
| CN107541745A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | A kind of method for preparing nano-cobaltic-cobaltous oxide using liquid barrier film discharge plasma |
| CN108044125A (en) * | 2017-09-14 | 2018-05-18 | 白银有色集团股份有限公司 | A kind of method for preparing Ag nano particles using liquid membrane discharge plasma |
| CN108044125B (en) * | 2017-09-14 | 2021-03-05 | 白银有色集团股份有限公司 | Method for preparing Ag nano particles by using liquid diaphragm discharge plasma |
| CN111235588A (en) * | 2020-01-17 | 2020-06-05 | 西北师范大学 | Method for preparing nano zinc oxide by liquid cathode glow discharge plasma |
| CN111822727A (en) * | 2020-06-28 | 2020-10-27 | 合肥百诺金科技股份有限公司 | Method for synthesizing metal nano-particles by liquid-phase discharge of rough electrode surface structure |
| CN111822727B (en) * | 2020-06-28 | 2023-11-03 | 合肥百诺金科技股份有限公司 | Method for synthesizing metal nano particles by liquid phase discharge of rough electrode surface structure |
| CN114016048A (en) * | 2021-12-16 | 2022-02-08 | 西北师范大学 | Zn (OH) with micro-nano structure2And a controllable preparation method of ZnO |
| CN114232003A (en) * | 2021-12-16 | 2022-03-25 | 西北师范大学 | Cu preparation by utilizing cathode glow discharge electrolytic plasma technology2Method for producing O nanoparticles |
| CN114232003B (en) * | 2021-12-16 | 2023-09-12 | 西北师范大学 | Cu preparation by utilizing cathode glow discharge electrolysis plasma technology 2 Method of O nanoparticles |
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