CN109709737A - A kind of production method of novel electrochromic film - Google Patents
A kind of production method of novel electrochromic film Download PDFInfo
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Abstract
The invention belongs to electrochromism inorganic thin film technologies, for the production method of electrochomeric films, steps are as follows: clean transparent conductive material is placed in magnetron sputtering chamber, controls the parameter of sputtering chamber, is controlled and is got through angle between molecular pump and vacuum sputtering chamber；Pre-sputtering processing is carried out to the metal targets of the first tunic growth, opens the sputtering growth process that substrate baffle plate carries out the first tunic, sputtering power and time is controlled, the first tunic is allowed to increase to suitable thickness；The second tunic growth is carried out on the basis of first layer inorganic electrochromic film, pre-sputtering processing is carried out to the metal targets of the second tunic sputtering, control allows the second tunic to increase to suitable thickness.The method that the present invention utilizes magnetron sputtering; in one layer of protective film with electrochromic property of first layer electrochomeric films basis rise or the protective film of good ionic conductivity; to obtain new structural electrochomeric films, the electrochromic property of monofilm electrochomeric films is effectively increased.
Description
Technical field
The present invention relates to electrochromism inorganic thin film material technology of preparing, specially a kind of system of novel electrochromic film
Make method.
Background technique
Since in recent years, the field of these new energy science and technology such as sustainable development and energy saving, environmental protection
Have become the most worth research of current era and most important project.But currently, the life of the mankind is still led with production method
It when universal use is not yet received in various new energy, to be taken based on the non-renewable energy resources such as petroleum, coal, natural gas
The consumption that various measures reduce the energy, which seems, to be even more important.And annual building energy consumption increases year by year, by adopting an effective means
The energy that reduction is lost because of the building appliances such as door, window, which seems, to be even more important, and improves the energy that window is lost, and improves
The thermal insulation property of window, light-proofness are increasingly becoming a new focus concerned by people.
At the same time, the appearance of energy-saving glass, intelligent window allows it is seen that the new hope of an energy-saving and emission-reduction.It is electroluminescent
Intelligent color-changing window may be implemented to outdoor shine in light transmission with absorb etc. optical properties adjustment, with solve due to
The problem of influence of external environment is to energy loss caused by interior.In addition to on the glass of building, these electroluminescent changes
Color material can also be applied to the anti-string rearview mirror of automobile, be occurred with lowering the unexpected of traffic accident, applied to keeping out the wind for automobile
On glass, glass for vehicle window, to lower the loss for leading to interior thermal insulation property because of external irradiation light.Electrochromic material is also
It can be applied to the carry-on object of all types of displays, clothing etc.
Electrochromism refers under the action of extra electric field, the optical properties (reflectivity, transmitance, absorptivity etc.) of material
Occur to stablize and reversible continuity changes, the color of material can be shown as in appearance, reversible company occurs for transparency
Continuous property variation.Inorganic electrochromic material is mostly transition metal oxide or derivatives thereof.Due to inorganic electrochromic material
Caused by light absorption variation is Dual Implantations or extraction due to ion and electronics, in inorganic electrochromic material (such as WO3、
MoO3) in, electrochomeric films have many advantages, such as that coloration efficiency is high, stability is good and ignores blind angle, are widely studied use.But
Existing inorganic electrochromic material is long there are the response time, the problem of deviation occurs after repeatedly carrying out Cyclic voltamogram.
The technology for preparing electrochomeric films at present mainly has following a few classes:
1, chemical vapor deposition
Although the speed of growth of chemical vapour deposition technique film is fast, quality of forming film is good, is easy to control doping, the disadvantage is that setting
It is standby complex, and the temperature requirement needed is higher, and the film to low temperature preparation is simultaneously not suitable for, and the binding force of film is poor,
It is easy to cause and falls off.
2, sol-gel technology
This method is not necessarily to vacuum equipment, and simple process can get the film of ideal thickness and component, usually contain in colloidal sol
There are water and alcohols material, excluding need to be through dry and heat treatment；And during heat treatment, the cracking of film, which is one, to be solved
Certainly the problem of.This theca externa and the adhesive force of substrate are also poor, and film gauge uniformity is difficult to control, and compactness is poor.
3, vacuum evaporation deposits
Vacuum vapour deposition has longer history, studies relatively more thorough under lab, forms the work of many maturations
Skill.This method deposition rate is high, depositional area is big, high production efficiency, and it is laboratory that in addition equipment and operation are also fairly simple
With the technical way for preparing film in industrial production.But, be also the shortcomings that vacuum vapour deposition it is very outstanding, use is this
The film of method preparation has following shortcoming:
1. gather density is small, refractive index is more relatively low than block numerical value.
2. being easy absorption residual gas and steam, optical absorption is big, poor in timeliness.
3. surface, interface out-of-flatness, scattering, surface scattering are big in vivo.
4. stress is high, anisotropy.
5. hardness is low, adhesive force is small, and fastness is poor.
4, pulsed excimer laser valve penetrates deposition (PLD), is the Novel steam ingot technology that developed recently gets up, and has film forming speed
Fast advantage is spent, but the binding force of film layer and substrate is poor, defect is more, and the quality of film vulnerable to pollution, film is bad.
Summary of the invention
In order to solve the problems of prior art, the present invention provides a kind of production side of novel electrochromic film
Method, on transparent conductive material substrate utilize magnetron sputtering method, by the indoor temperature of control chamber, pressure, mix oxygen amount with
And the variable of sputtering, the inorganic electrochromic for first growing one layer of suitable thickness by doped or undoped method on substrate are thin
Film；Then the material system for changing the film that rises again, on the basis of first layer electrochomeric films, rising again one layer has good ion
The TaO of conducting power2Film has electrochromic property TiO2It is thin to obtain the new structural electrochromism of the present invention for film
Film effectively increases the electrochromic property of monofilm electrochomeric films.
In order to reach the goals above, the present invention is the following technical schemes are provided: a kind of production side of novel electrochromic film
Method, comprising the following steps:
Step 1: clean transparent conductive material is placed in magnetron sputtering chamber, and pipeline vacuumizes, and controls sputtering chamber
In total gas flow rate and oxygen and argon gas proportional amount；
Step 2: sputtering chamber temperature being adjusted within the required range, is controlled between molecular pump and vacuum sputtering chamber
Angle is got through, within the required range by gas pressure intensity control in sputtering chamber；
Step 3: pre-sputtering processing being carried out to the required metal targets for carrying out the first tunic growth, for removing original target
Then impurity on material surface opens the sputtering growth process that substrate baffle plate carries out the first tunic, controls sputtering power and sputtering
Time allows the first tunic to increase to suitable thickness；
Step 4: the substrate for the second tunic that will be grown is placed in the same position of substrate with the growth of the first tunic, the
The basis of one layer of inorganic electrochromic film grown carries out the growth of the second tunic；
Step 5: controlling the proportional amount of the total gas flow rate and oxygen and argon gas in second of sputtering chamber, adjust
Chamber temp, and control the indoor gas pressure intensity of chamber；
Step 6: pre-sputtering processing being carried out to the required metal targets for carrying out the second tunic sputtering, for removing original target
Impurity on material surface, then opens the sputtering growth process that substrate baffle plate carries out the second tunic, and sputtering time control is to allowing the
Two tunics increase to suitable thickness；
Second tunic is the protective film of the protective film with electrochromic property or good ionic conductivity.
Preferably, step 3 carries out pre-sputtering processing to the metal tungsten target material that the first tunic is grown, or grows to the first tunic
Metal tungsten target material and Titanium target carry out cosputtering pre-sputtering handle.When the tungsten that step 3 grows the first tunic
When target carries out pre-sputtering processing, sputtering power is controlled between 50w~200w, and sputtering time is between 10min~1h, wanting
The WO of growth3Film thickness monitoring is between 100nm~400nm.When the metal tungsten target material and Titanium that step 3 grows the first tunic
When target carries out the pre-sputtering processing of cosputtering, the sputtering power of metal tungsten target material is controlled in 150w, the sputtering of Titanium target
For power control in 50w, sputtering time is 17min, the WO to be grown3Adulterate TiO2Film film thickness monitoring in 360nm.
The metal targets that second tunic sputters in step 6 are Titanium target or metal tantalum target.Second tunic in step 6
Sputtering growth process, for Titanium target power control in 150w, sputtering time 11min, the TiO to be grown2's
Film thickness monitoring is in 100nm；And metal tantalum target power is controlled in 130w, sputtering time 30min, the TaO to be grown2
Film thickness monitoring in 100nm.
Preferably, pipeline vacuum is evacuated to 1.0x10 in step 1-4Pa~1.0x10-5Pa, total gas flow rate control exist
The proportional amount of 40sccm~100sccm, oxygen and argon gas is controlled 20%~40%；Chamber temp range control in step 2
System is at 30 DEG C~150 DEG C, and gas pressure intensity scope control is in 0.5pa~3pa in sputtering chamber；Total gas flow rate controls in step 5
In 40sccm~100sccm, the control of the proportional amount of oxygen and argon gas 20%~40%, chamber temp control 30 DEG C~
150 DEG C, the indoor gas pressure intensity control of chamber is in 0.5pa~3pa.
Compared with prior art, the invention has the following beneficial effects:
1, the substrate of the electrochomeric films made by the present invention is the ito glass or FTO glass of electrically conducting transparent.Transparent
The method that magnetron sputtering is utilized on conductive material substrate, passes through the indoor temperature of control chamber, pressure, the change for mixing oxygen amount and sputtering
Amount is first become by the inorganic electroluminescence that doped or undoped method grows one layer of suitable thickness (such as 100-350nm) on substrate
Color film；Then change the material system for the film that rises again, on the basis of first layer electrochomeric films, rise again one layer have well from
The TaO of sub- conducting power2Film has weak electrochromic property TiO2Film obtains the new structural electroluminescent change of the present invention
Color film effectively increases the electrochromic property of monofilm electrochomeric films.
2, based on inorganic electrochromic film, by the basis of original electrochomeric films, being superimposed one layer of property
It can stablize, and the film of the associated electrochromic material system of script electrochomeric films performance can be promoted or there is good ion
The protective film of conducting power, by utilizing different inorganic electrochromic materials or the different characteristics with ionic conductivity material
Improve the electrochromic property of single inorganic electrochromic film originally, technique is simple for production, just can in the same chamber
Requirement needed for realizing.
Detailed description of the invention
Fig. 1 is a kind of electricity optically variable films structural schematic diagram made by the method for the present invention；
Fig. 2 is another electricity optically variable films structural schematic diagram made by the method for the present invention；
Fig. 3 is the electricity optically variable films structural schematic diagram that embodiment 1 makes；
Fig. 4 is the electricity optically variable films structural schematic diagram that embodiment 2 makes；
Fig. 5 is the electricity optically variable films structural schematic diagram that embodiment 3 makes.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this.
The present invention utilizes magnetron sputtering using transparent conductive material ito glass or FTO glass as the substrate of electrochomeric films
Method, by the indoor temperature of control magnetron sputtering chamber, pressure, mix the parameters such as oxygen amount and sputtering variable, first led transparent
One layer of inorganic electrochromic film is grown by doped or undoped method on electric material substrate, then in the electroluminescent change of first layer
On the basis of color film, one layer of TaO with good ionic conductivity of growth2Film has electrochromism performance TiO2
Film, to be finally completed the preparation of new structure electrochomeric films of the present invention, as shown in Figure 1.Separately below with different nothings
Machine electrochromism thin-film material is illustrated to implementation process of the invention and is described in detail.
Embodiment 1
Step 1: clean ito glass or FTO glass being placed in magnetron sputtering chamber, pipeline vacuum is evacuated to 1.0x10- 4Pa~1.0x10-5Pa, control the indoor parameter of sputtering chamber, control in sputtering chamber gas gross control 40sccm~
Between 100sccm, such as gas gross controlled as 80sccm, the proportional amount of oxygen and argon gas is controlled 20%~40%
Between, the present embodiment controls the ratio of oxygen and argon gas in 24sccm:56sccm.
Step 2: the indoor temperature device of chamber is opened, the temperature range of sputtering chamber is controlled between 30 DEG C~150 DEG C,
Such as chamber temp is adjusted at 50 DEG C；Control the angle of getting through between molecular pump and vacuum sputtering chamber, the present embodiment control
System makes the indoor pressure of sputtering chamber reach 0.5pa~3pa in 18 ° this angle.The present embodiment can control by force chamber inner pressure
System is in 2pa.
Step 3: opening DC power supply, the required metal tungsten target material for carrying out the first tunic growth is carried out at pre-sputtering
Reason, time of processing is 10~15min, for removing the impurity on original target material surface, then opens substrate baffle plate and carries out the
The sputtering growth process of one tunic, sputtering power are can be controlled between 50w~200w, such as control, in 150w, sputtering time can
It is arranged between 10min~1h, sputtering time can be set as 17min by the present embodiment, the WO to be grown3Plastics thickness control exists
Between 100nm~400nm, the WO that ultimately generates3Film thickness can be this numerical value of 360nm.
Step 4: the substrate for the second tunic that will be grown is placed in the same position of substrate with the growth of the first tunic, the
One layer of WO grown3On the basis of electrochomeric films by way of d.c. sputtering Ti target, the second tunic TiO is carried out2's
Sputtering growth, makes the second tunic TiO2It is covered on the first tunic WO3Surface, as shown in Figure 2.
Step 5: controlling the proportional amount of the gas gross and oxygen and argon gas in second of sputtering chamber, wherein oxygen
The proportional amount of gas and argon gas is controlled in 24sccm:56sccm, then opens temperature device again, and the temperature range of chamber is adjusted
It controls within the scope of suitable temperature, such as by temperature at 50 degrees Celsius.
Step 6: controlling the angle of getting through between molecular pump and vacuum chamber, this angle of the present embodiment control at 18 °
On degree, the indoor pressure of chamber is made to reach 2pa.Then DC power supply is opened, to the required Titanium for carrying out the second tunic growth
Target carries out pre-sputtering processing, and the time of processing is then 10~15min is beaten for removing the impurity on original target material surface
The sputtering growth process that substrate baffle plate carries out the second tunic is opened, power control is in 150w, sputtering time 11min, growing
TiO2Film thickness monitoring 100nm this numerically.
It should be noted that in the present embodiment when second of sputtering growth, the ratio of gas gross, oxygen and argon gas in chamber
The numberical range of the parameters such as content, chamber temp range, chamber pressure, pre-sputtering processing time, sputtering time, sputtering power,
It is essentially identical when being grown with first time sputtering, but the growth thickness different from of film.
Embodiment 2
Numberical range selected by sputtering principle and technological parameter of the present embodiment with embodiment 1 is essentially identical, and institute is different
Mainly metal targets.
Step 1: clean ito glass or FTO glass being placed in magnetron sputtering chamber, pipeline vacuum is evacuated to 1.0x10- 4Pa~1.0x10-5Pa controls the indoor parameter of sputtering chamber, and controlling gas gross in chamber is 80sccm, wherein oxygen with
The ratio of argon gas is controlled in 24sccm:56sccm.
Step 2: opening the indoor temperature device of sputtering chamber, chamber temp is adjusted at 50 DEG C, control molecular pump and true
Angle is got through between empty sputtering chamber, the present embodiment also controls in 18 ° this angle, reaches the indoor pressure of chamber
2pa。
Step 3: opening DC power supply, the required metal tungsten target material for carrying out the first tunic growth is carried out at pre-sputtering
Reason, the processing time is 10~15min, for removing the impurity on original target material surface, then opens substrate baffle plate and carries out first
The sputtering growth process of tunic, power control is in 150w, and the time of sputtering is 17min, the WO to be grown3Film thickness monitoring exists
This numerical value of 360nm.
Step 4: the substrate for the second tunic that will be grown is placed in the same position of substrate with the growth of the first tunic, the
One layer of WO grown3On the basis of electrochomeric films by way of d.c. sputtering Ta target, the second tunic TaO is carried out2's
Sputtering growth, makes the second tunic TaO2It is covered on the first tunic WO3Surface.
Step 5: the proportional amount of the gas gross and oxygen and argon gas in second of sputtering chamber is controlled, wherein comparing
Then example content control opens temperature device again, the temperature of chamber is adjusted in suitable temperature range in 24sccm:56sccm
It is interior, such as temperature is controlled at 50 degrees Celsius.
Step 6: the angle of getting through between molecular pump and vacuum sputtering chamber is controlled, is controlled in 18 ° this angle,
The indoor pressure of sputtering chamber is set to reach 2pa.Then DC power supply is opened, to the required metal tantalum Ta for carrying out the second tunic growth
Target carries out pre-sputtering processing, and the time of processing is then 10~15min is beaten for removing the impurity on original target material surface
The sputtering growth process that substrate baffle plate carries out the second tunic is opened, for power control in 130w, the time of sputtering is 30min, giving birth to
Long TaO2Film thickness monitoring 100nm this numerically.
Embodiment 3:
Numberical range selected by sputtering principle and technological parameter of the present embodiment with embodiment 1 is essentially identical, and institute is different
Mainly metal targets.
Step 1: clean ito glass or FTO glass being placed in magnetron sputtering chamber, pipeline vacuum is evacuated to 1.0x10- 4Pa~1.0x10-5Pa controls the indoor parameter of sputtering chamber, and controlling gas gross in chamber is 80sccm, wherein oxygen with
The ratio of argon gas is controlled in 24sccm:56sccm.
Step 2: opening the indoor temperature device of chamber, the temperature of chamber is adjusted at 50 DEG C, molecular pump and vacuum are controlled
Angle is got through between chamber, controls in 18 ° this angle, the indoor pressure of chamber is made to reach 2pa.
Step 3: open DC power supply, to it is required carry out the first tunic growth metal tungsten target material and Titanium target into
The pre-sputtering of row cosputtering is handled, and the processing time is then 10~15min is beaten for removing the impurity on original target material surface
The sputtering growth process that substrate baffle plate carries out the first tunic is opened, wherein the sputtering power of metal tungsten target material is controlled in 150w, and golden
The sputtering power for belonging to titanium target material is controlled in 50w, and sputtering time is 17min, the WO to be grown3Adulterate TiO2Film film
Thickness control is in this numerical value of 360nm.
Step 4: the substrate for the second tunic that will be grown is placed in the same position of substrate with the growth of the first tunic, the
One layer of WO grown3Adulterate TiO2On the basis of electrochomeric films by way of d.c. sputtering Ta target, the second layer is carried out
Film TaO2Sputtering growth, make the second tunic TaO2It is covered on first layer WO3Adulterate TiO2The surface of film.
Step 5: the proportional amount of the gas gross and oxygen and argon gas in second of sputtering chamber is controlled, wherein comparing
Then example content control opens temperature device again, the temperature of chamber is adjusted in suitable temperature range in 24sccm:56sccm
It is interior, such as temperature is controlled at 50 degrees Celsius.
Step 6: controlling the angle of getting through between molecular pump and vacuum chamber, control in 18 ° this angle, make chamber
Indoor pressure reaches 2pa.Then DC power supply is opened, the required metal tantalum Ta target for carrying out the second tunic growth is carried out
The time of pre-sputtering processing, processing is 10~15min, for removing the impurity on original target material surface, then opens substrate gear
Plate carries out the sputtering growth process of the second tunic, and power control is in 130w, and the time of sputtering is 30min, the TaO to be grown2
Film thickness monitoring in this numerical quantities of 100nm.
As seen from the above embodiment, what the present invention took is that the method for magnetron sputtering carries out plated film, thus film and substrate
Adhesiveness is fabulous.Furthermore film growth rate is high, technological parameter is easy to control, can prepare refractory material film, be able to achieve large area
Film, has the advantages that stability is good, it is convenient to prepare.It is pure due to monofilm for the pure electrochomeric films of monofilm
The electrochromic performances such as electrochomeric films cyclic voltammetric stability still have improved space, pass through compound electrochromic membrane
Preparation, the stability of the electrochromic material of monofilm can actually be improved, improve electrochromic discoloration.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of production method of novel electrochromic film, which comprises the following steps:
Step 1: clean transparent conductive material is placed in magnetron sputtering chamber, and pipeline vacuumizes, and is controlled in sputtering chamber
The proportional amount of total gas flow rate and oxygen and argon gas；
Step 2: sputtering chamber temperature being adjusted within the required range, getting through between molecular pump and vacuum sputtering chamber is controlled
Angle, within the required range by gas pressure intensity control in sputtering chamber；
Step 3: pre-sputtering processing being carried out to the required metal targets for carrying out the first tunic growth, for removing original target table
Then impurity on face opens the sputtering growth process that substrate baffle plate carries out the first tunic, controls sputtering power and sputtering time,
The first tunic is allowed to increase to suitable thickness；
Step 4: the substrate for the second tunic that will be grown is placed in the same position of substrate with the growth of the first tunic, in first layer
The growth of the second tunic is carried out on the basis of the inorganic electrochromic film grown；
Step 5: controlling the proportional amount of the total gas flow rate and oxygen and argon gas in second of sputtering chamber, adjust chamber
Temperature, and control the indoor gas pressure intensity of chamber；
Step 6: pre-sputtering processing being carried out to the required metal targets for carrying out the second tunic sputtering, for removing original target table
Impurity on face, then opens the sputtering growth process that substrate baffle plate carries out the second tunic, and sputtering time control is to allowing the second layer
Film increases to suitable thickness；
Second tunic is the protective film of the protective film with electrochromic property or good ionic conductivity.
2. the production method of novel electrochromic film according to claim 1, which is characterized in that step 3 is to first layer
The metal tungsten target material of film growth carries out pre-sputtering processing, or carries out to the metal tungsten target material and Titanium target of the growth of the first tunic
The pre-sputtering of cosputtering is handled.
3. the production method of novel electrochromic film according to claim 2, which is characterized in that pre-sputtering handles the time
For 10~15min.
4. the production method of novel electrochromic film according to claim 2, which is characterized in that when step 3 is to first
When the metal tungsten target material of tunic growth carries out pre-sputtering processing, sputtering power is controlled between 50w~200w, and sputtering time exists
Between 10min~1h, the WO to be grown3Film thickness monitoring is between 100nm~400nm.
5. the production method of novel electrochromic film according to claim 2, which is characterized in that when step 3 is to first
When the pre-sputtering that the metal tungsten target material and Titanium target of tunic growth carry out cosputtering is handled, the sputtering power of metal tungsten target material
Control is controlled in 150w, the sputtering power of Titanium target in 50w, and sputtering time is 17min, the WO to be grown3Doping
TiO2Film film thickness monitoring in 360nm.
6. the production method of novel electrochromic film according to claim 1, which is characterized in that the second layer in step 6
The metal targets of film sputtering are Titanium target or metal tantalum target.
7. the production method of novel electrochromic film according to claim 6, which is characterized in that the second layer in step 6
The sputtering growth process of film, for Titanium target power control in 150w, sputtering time 11min, the TiO to be grown2
Film thickness monitoring in 100nm；And metal tantalum target power is controlled in 130w, sputtering time 30min, what is grown
TaO2Film thickness monitoring in 100nm.
8. the production method of novel electrochromic film according to claim 1, which is characterized in that pipeline is true in step 1
Empty pump is to 1.0x10-4Pa~1.0x10-5Pa, total gas flow rate are controlled in 40sccm~100sccm, the ratio of oxygen and argon gas
Content is controlled 20%~40%；Chamber temp scope control in step 2 is at 30 DEG C~150 DEG C, sputtering chamber indoor gas pressure
Strong scope control is in 0.5pa~3pa；Total gas flow rate control is in 40sccm~100sccm, the ratio of oxygen and argon gas in step 5
The control of example content is 20%~40%, and chamber temp control is at 30 DEG C~150 DEG C, and the indoor gas pressure intensity control of chamber is in 0.5pa
~3pa.
9. the production method of novel electrochromic film according to claim 8, which is characterized in that in step 1 oxygen with
The ratio of argon gas is controlled in 24sccm:56sccm.
10. the production method of novel electrochromic film according to claim 1, which is characterized in that in step 2, molecule
Angle of getting through between pump and vacuum chamber is controlled at 18 °.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107892571A (en) * | 2017-11-14 | 2018-04-10 | 北京富兴凯永兴光电技术有限公司 | A kind of lower valency tantalum oxide optical filming material and preparation method |
| CN110171931A (en) * | 2019-07-15 | 2019-08-27 | 吉林农业科技学院 | A kind of preparation method for mixing vanadium bilayer electro-allochromatic nickel oxide film |
| CN110282880A (en) * | 2019-07-15 | 2019-09-27 | 吉林农业科技学院 | A kind of preparation method for the double-deck nickel oxide film introducing ion diffusion layer |
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