CN106932993A - Magnesium yittrium alloy and tungsten oxide film are the total solids electrochromism light modulation device of base - Google Patents
Magnesium yittrium alloy and tungsten oxide film are the total solids electrochromism light modulation device of base Download PDFInfo
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- CN106932993A CN106932993A CN201511025316.7A CN201511025316A CN106932993A CN 106932993 A CN106932993 A CN 106932993A CN 201511025316 A CN201511025316 A CN 201511025316A CN 106932993 A CN106932993 A CN 106932993A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
Abstract
It is the total solids electrochromism light modulation device of base the present invention relates to a kind of magnesium yittrium alloy and tungsten oxide film, including tungstic acid hydrogen storage layer, magnesium yittrium alloy light modulation layer and the proton conduction layer between trioxide hydrogen storage layer, magnesium yittrium alloy light modulation layer and precious metal catalyst layer.The present invention is intended to provide a kind of new total solids electrochromism light modulation device, with the advantage of the gentle mutagens color device of electrochromic device.
Description
Technical field
The present invention relates to a kind of total solids electrochromic device of multi-layer compound structure, more particularly to use WO 3 film
With magnesium yittrium alloy thin-film multilayer composite construction, device can be made to regulate and control the transmission of light by applied voltage, absorb and reflect, with
The light regulation of the glass and other outer walls of building and mobile object is realized, belongs to the intellectual material of energy-conserving and environment-protective.
Background technology
Human social development is faced with that the energy and shortage of resources, environmental pollution, population expansion, global warming etc. are many to ask
Topic.Wherein, energy and environment are particularly problematic, and there is the contact of countless ties between the two, such as energy resource consumption certainty
Bring CO2Discharge increases, and is further exacerbated by global warming and greenhouse effects.Issued according to BP《Statistical Review of
World Energy 2014 Full Report》Statistics shows that China's primary energy consumption in 2013 is up to 2852.4 million tons of oil
Equivalent, CO29524.3 million tons of discharge capacity, occupies the first in the world in pairs.And Building Trade in China energy consumption accounts for the 33% of total power consumption
Left and right (cut-off is counted for 2012), and also increase with annual 1 percentage point of speed at present.Work as in whole building energy consumption
In, exterior window loss (presently mainly windowpane) has accounted for more than 50%.Therefore building energy consumption how is reduced, is especially reduced
The loss of glass exterior window, the focus as current various countries scientific research personnel research.
At present, in the market sale energy-saving glass or energy-conservation pad pasting (abbreviation Energy Saving Windows), belong to low-launch-rate (Low-E)
Category, feature be have visible light transmissivity and relatively low far infrared transmissivity (winter is heat-insulated) higher, can realize it is heat-insulated
While insulation, carry out the infrared part in sunshine blocking (being suitable for hot area) high or high transmission (is suitable for cold ground
Area).But, it is uncomfortable because low-launch-rate Energy Saving Windows optical property is fixed, it is impossible to realize summer in winter bidirectional modulation with environmental change
Winter warm summer heat is closed to make a clear distinction between the four seasons the application in area.
And the intelligent type energy saving glass for occurring recently, due to its optical property can with external environment or occupant the need for realize
Bidirectional modulation, can be suitably used for thermally area of warm summer in most of winter, make the more comfortable energy-conservation in living space, be called follow-on glass
Glass product.Cause metachromatic principle according to material can be divided into electrochromism, gas-discoloration, thermochromism and several masters such as photochromic
Want type.Gas-discoloration window is the change for realizing window different conditions with abjection by the implantation of gas (mainly hydrogen), is entered
And control the flux that light gets in.Although active control can be crossed, it is related to use the security of hydrogen, durability is asked
The research incompleteness of topic and its air supply system and cause the popularization of magnesium alloy gas-discoloration glass to have many key issue needs at present
Solve.Photochromic window and Thermochromic window belong to passive control, the change of restraining oneself with the change of the power or temperature of light
Change, it is impossible to which the wish according to people changes the flux that light and heat get in.And electrochromic can be by external voltage
Regulation realize control to luminous flux, so as to realize the purposes such as energy-saving and emission-reduction, reducing energy consumption, beautifying and decorating, and electrochromism
Window be not limited solely to it is architectural use, while can apply at traffic (such as vehicle glass, Antiglaring rear mirror), communicate
(light path control switch), military (hidden), satellite etc., it may be said that the research of electrochromic, especially electrochromism phase
Close device research to improve human lives, energy-saving and emission-reduction, promoting social development has extremely important meaning.
Smart window can be divided into absorption-type and reflection-type again by its control mode to light.Most off-color materials are all
Absorption-type, although such off-color material can play the effect of energy-conservation, but because there is a problem of own radiation, actual energy-saving effect
It is bad, and gas-discoloration material belongs to reflective material, but security and stability is not high, therefore manufacture reflection-type Energy Saving Windows are current
Study the new focus of smart window.
The content of the invention
The present invention is intended to provide a kind of new total solids electrochromism light modulation device, with the gentle cause of electrochromic device
The advantage of Electrochromic device.
The present invention provides a kind of magnesium total solids electrochromism light modulation device, including tungstic acid hydrogen storage layer, the light modulation of magnesium yittrium alloy
Layer and the proton conduction layer between trioxide hydrogen storage layer, magnesium yittrium alloy light modulation layer and precious metal catalyst layer.
Present invention incorporates electrochromic material tungstic acid and reflection-type gas-discoloration material magnesium yittrium alloy, in applied voltage
When, device can be with the transmission of light regulating, absorption and reflection：Magnesium yittrium alloy it is laminated can minute surface state (silvery white) and thoroughly
Change between bright state (colourless), its another tungstic acid face can turn between absorbing state (blueness) and clear state (colourless)
Become, be expected to be applied to energy-conservation intelligent window, moving body window, ultraviolet, visible, infrared full spectrum intercepts device, or complete
Solid electrochromic device is embedded on any light modulation part.
In the present invention, tungstic acid hydrogen storage layer is noncrystalline membrane, and thickness can be 50~500nm, preferably 100~
200nm。
In the present invention, the proton conduction layer can be that transparent inorganic-oxide conductive film or organic polymer proton conductive are thin
Film.Such as described proton conduction layer can be tantalum pentoxide or five two neodymium amorphous state colorless and transparent films of oxidation, and thickness can be
50~500nm, preferably 100~120nm.Again for example, the proton conduction layer can be polytetrafluoroethylene (PTFE) proton exchange membrane,
Thickness can be 10~500 μm, preferably 100 μm.
In the present invention, the chemical composition of the precious metal catalyst layer is Metal Palladium or its alloy PdMy, PdMxM in alloy
It is Sc, Y, Ti, Zr, V, Nb, Ta, Fe, Ni, Co, Mo, at least one in W, wherein y are 0<y≤0.5.
The thickness of the precious metal catalyst layer can be 5~10nm.
The chemical composition of heretofore described magnesium yittrium alloy light modulation layer is MgxY, wherein 0≤x≤1.Thickness can for 20~
200nm, preferably 100~200nm.
Brief description of the drawings
Fig. 1 is total solids electrochromic device structural representation；
Fig. 2 is WO 3 film X-ray diffractogram；
Fig. 3 is five oxidation two tantalum film X-ray diffractogram；
Fig. 4 is that tungstic acid contacts section SEM signs with tantalum pentoxide；
Fig. 5 is that tungstic acid surface SEM is characterized；
Fig. 6 is that tantalum pentoxide surface SEM is characterized；
Transmission when Fig. 7 is corresponding time and the 670nm of total solids device, reflectance spectrum；
Fig. 8 is the relation of the electrical conductivity with nafion concentration of polyelectrolyte；
Fig. 9 is Roll-To-Roll laminating schematic diagrames；
Figure 10 is the alloy minute surface of total solids device and the reflection optical photograph in tungsten oxide face.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following implementation methods, it should be appreciated that accompanying drawing and following implementation methods are only
For illustrating the present invention, it is not intended to limit the present invention.
Referring to Fig. 1, its exemplary construction for showing total solids electrochromic device, including positioned at the tungstic acid of device side
(WO3) layer as electrochromic layer and positioned at device with respect to opposite side magnesium yittrium alloy layer as gas-discoloration layer (be also conduct
The light modulation layer of whole device).Tungstic acid layer should be previously implanted (injection) Hydrogen Proton using simultaneously as hydrogen storage layer.Tungstic acid
The thickness of layer can be 50~500nm, preferably 100~200nm.Magnesium yittrium alloy layer chemical composition is MgxY, wherein
0≤x≤1, thickness can be 20~200nm, preferably 100~200nm.
Precious metal catalyst layer and proton conduction layer (proton conductive are also set up between tungstic acid layer and magnesium yittrium alloy layer
Layer), wherein proton conduction layer is near tungstic acid layer side, and precious metal catalyst layer is then positioned close to magnesium yittrium alloy layer one
Side.Proton conduction layer can use the thin-film materials such as inorganic transparent conductive oxide material, such as tantalum pentoxide, five two neodymiums of oxidation
(thickness can be 50~500nm, preferably 100~120nm), can also use organic proton conductive material, including but not limited to gather
Tetrafluoroethene proton exchange membrane, such as commercialization nafion films (thickness can be 10~500 μm, preferably 100 μm) etc..It is expensive
Metal catalytic layer can use metal Pd or its alloy PdMx, in alloy M be Sc, Y, Ti, Zr, V, Nb, Ta, Fe,
In Ni, Co, Mo, W at least, wherein y is 0<y≤0.5.The thickness of precious metal catalyst layer can be 5~10nm.
In the outside of tungstic acid layer or tungstic acid layer and magnesium yittrium alloy layer respective outside, transparent conductive material is set
Layer.It should be understood that although Fig. 1 shows to be respectively provided with transparent conductive material layer in tungstic acid layer and the respective outside of magnesium yittrium alloy layer,
But can be that transparent conductive material layer only is set in the outside of tungstic acid layer, without setting electrically conducting transparent on the outside of magnesium yittrium alloy layer
Material layer, because, magnesium yittrium alloy layer itself also can be used as conductive layer.Transparent conductive material in itself can be used as device support
Body, or be further attached on supporter.Transparent conductive material includes but is not limited to electro-conductive glass (such as ito glass), has
Machine transparent conductive film.Supporter includes but is not limited to the materials such as glass, transparent organic film, crystalline ceramics, silicon chip.
Circuit connects saturating on the outside of transparent conductive material layer (such as the ITO layer shown in Fig. 1), or connection tungstic acid layer
(applied voltage can make device to the electrochromism function of bright conductive material layer and magnesium yittrium alloy layer and realization with gas-discoloration advantage
Regulate and control the transmission of light, absorb and reflect), magnesium yittrium alloy is laminated can be in minute surface state (silvery white) and clear state (nothing
Color) between change, its another tungstic acid face can change between absorbing state (blueness) and clear state (colourless).Its table
Existing form is to change control of the device to light by applied voltage.Main performance is as follows：When tungstic acid layer applies negative voltage,
When magnesium yittrium alloy layer applies positive voltage, tungstic acid layer shows as blue (absorbing state), can be to light absorption；Magnesium yittrium alloy
Layer shows as silvery white (minute surface state), and light can be totally reflected；When tungstic acid layer applies positive voltage, magnesium yittrium alloy layer is applied
Plus during negative voltage, tungstic acid layer shows as colourless (clear state), can be with transmitted light；Magnesium yittrium alloy layer shows as colourless
(clear state), can be with transmitted light.When device is in mirror-reflection state, magnesium yittrium alloy layer is not small to the reflectivity of visible ray
In 60%, overall visible light transmissivity is not more than 5%；When forms are for clear state, overall visible ray (380~780nm)
Transmitance is not less than 50%.External circuit uses dc source, and power output end polarity is adjustable, and voltage output amplitude is not more than
10V, preferably 1.0~5.0V, particularly preferred 3V.After voltage applies to finish, device can keep existing form, not send out
Raw obvious change, both with open circuit memory effect.When in use, mirror metal state direction is outdoor, when need for device of the invention
When wanting light to get in, magnesium yittrium alloy layer applies negative voltage, and tungstic acid layer applies positive voltage, makes forms transparent；When being not required to
When wanting light to get in, magnesium yittrium alloy layer applies positive voltage, and tungstic acid layer applies negative voltage, makes forms outside be anti-minute surface
State is penetrated, and forms inner side is blue absorbing state (accompanying drawing 10).
The preparation method of reflective electrochromic total solids device of the invention further explained below.
The selection of substrate
Substrate uses transparent conductive material, the clean smooth free from admixture in surface, or the supporter for being attached with transparent conductive material.Electrically conducting transparent
Material such as ito glass or organic transparent conductive material.
The preparation of tungstic acid electrochromic layer
Using magnetron sputtering technique, sputtering system its background pressure is not more than 10-4Pa, sputter gas select argon gas and oxygen.Target is adopted
With metal tungsten target or tungstic acid ceramic target, preferably metal tungsten target.Sputtering power is not less than 150W, preferably 200W, sputtering
Room air pressure controls 0.6~1.1Pa.Sputtering duration 8 to 11 minutes, preferably 10 minutes, target to substrate distance was arrived for 15
20cm.Between 100nm to 150nm, color is transparent, and X-ray diffraction analysis for the WO 3 film thickness for being obtained
Without obvious diffraction maximum.
It should be understood that also WO 3 film can be prepared using electron beam hair or sol-gal process.
Proton is implanted into
The WO 3 film connection power cathode that will have been sputtered, positive pole uses Pt electrodes, the acid of 0.5M/L~1.0M/L is put into together
Property solution, the preferably sulfuric acid solution of 0.5M/L.Applied voltage, between voltage control 1.5V to 3V, application time is arrived for 5 seconds
20 seconds, obtain blue film.The cleaning of tungstic acid surface acid ion, navy blue WO 3 film is molten from acid
Taken out in liquid, successively with deionized water, ethanol solution cleaning, wash number is no less than 3 times.
Or Hydrogen Proton, such as argon gas are injected by the reactive sputtering of metal tungsten target:Oxygen:The ratio of hydrogen is 40:10:5
Environment in prepare the blue oxide W film of Proton Implantation.
The preparation of proton conduction layer
Proton conduction layer can be used, such as tantalum pentoxide, and the thin-film material time such as five two neodymiums of oxidation can be using the method system of magnetron sputtering
Standby, sputtering system its background pressure is not more than 10-4Pa.Sputter gas select argon gas and oxygen, target to use metal included a tantalum target or five
Aoxidize two tantalum ceramic targets, preferably metal included a tantalum target.Sputtering power is not less than 150W, preferably 200W, the control of sputtering chamber air pressure
0.6~1.1Pa.Sputtering duration 50 to 70 minutes, preferably 60 minutes, target to substrate distance was 15 to 20cm.Obtained
Five oxidation two tantalum film thickness between 380nm to 780nm, without color transparent thin-film material, and X-ray diffraction analysis
Without obvious diffraction maximum (accompanying drawing 3, accompanying drawing 6).Five oxidation two tantalum film and the good (accompanying drawing of WO 3 film film interface contact
4)。
During using organic proton conductive film, can directly fit WO 3 film layer；Such as commercially available Nafion membrane can be straight
Connect as proton film (50~300 μm) is led, soaked more than one hour with dilute sulfuric acid using preceding, immersion is finished and washed with water, is done
It is dry standby；Or the commercially available Nafion aqueous solution carries out solution and mixes with the ethanol of polyvinyl butyral resin (PBV), as volume
Volume laminating device is used.During response when the Nafion aqueous solution and polyvinyl butyral resin (PBV) mixed conducting layer are used
Between (Fig. 7), and the change in resistance (Fig. 8) corresponding to various concentrations Nafion.
The preparation of Catalytic Layer Pd
Sputtering system its background pressure is not more than 10-5Pa.Sputter gas select argon gas, power 16W to 20W, pressure control 0.5Pa
To between 0.8Pa, preferably 0.6Pa, sputtering time 60 seconds.Obtain the Catalytic Layer of thickness 6nm or so.
The preparation of magnesium yittrium alloy light modulation layer
Sputtering system its background pressure is not more than 10-5Pa.Sputter gas select argon gas.The preparation of magnesium yittrium alloy uses producing high purity metal magnesium target
With high pure metal yttrium target co-sputtering.It is 1 to 2 to reach magnesium yttrium atom ratio, magnesium metal target sputtering power uses 20w, metallic yttrium
Target sputtering power 60w, air pressure control 0.5Pa to 1.0Pa, preferably 0.8Pa, sputtering time 120 seconds, acquisition thickness be
The alloy-layer of 50nm or so.
Circuit is connected
Using common conductive glue, when using successively compound tense, connection ito glass and magnesium yittrium alloy light modulation mirror layer, made of tantalum pentoxide
Proton conductive layer；When being fitted using volume to volume, with proton macromolecule membrane is led as conducting shell (accompanying drawing 7), outermost layer is connected
Conductive electrode.External circuit uses dc source, and power output end polarity is adjustable, and voltage output amplitude is not more than 10V, excellent
Select 3V (accompanying drawing 7).
The present invention is combined closely without air between layers by being successively combined, difficult for drop-off, and each thickness degree is homogeneous,
It is stable in properties.
The present invention is further illustrated below in conjunction with accompanying drawing and following specific embodiments, it should be appreciated that accompanying drawing and following specific implementations
Example is merely to illustrate the present invention, is not intended to limit the present invention.
Example one, successively composite mode：
1) selection of substrate and cleaning
Substrate uses commercially available common ito glass；
Ito glass is put into deionized water, is cleaned by ultrasonic 10 minutes；
Ito glass is taken out and is put into ethanol solution, be cleaned by ultrasonic 10 minutes；
Repeat above-mentioned cleaning step three times；
2) preparation of tungstic acid electrochromic layer
Preparation uses magnetron sputtering apparatus, and sputtering system its background pressure is not more than 10-4Pa, sputter gas select argon gas and oxygen, pure
Degree more than 99.999%；
Metal tungsten target uses 4 inch circular targets, purity 99.9%, pure argon environment pre-sputtering 30 minutes；
The ito glass substrate feeding sample presentation room that will be cleaned up, sputtering chamber is sent into by sample presentation room；
The formal sputtering of WO 3 film, sputtering power 200W, sputtering chamber air pressure control 0.7Pa, argon gas oxygen flux control 42
Than 4.Sputtering duration 10 minutes, target to substrate distance is 17cm；
WO 3 film thickness 130nm, SEM (SEM) Surface Characterization Fig. 4；
3) proton implantation
The WO 3 film link power supply negative pole that will have been sputtered, positive pole uses Pt electrodes, and the sulfuric acid solution of 0.5M/L is put into together
Applied voltage, between voltage control 2.5V, application time 20 seconds；
The cleaning of tungstic acid surface acid ion, navy blue WO 3 film is taken out from acid solution, is put into deionized water
Cleaning 10 minutes, is then placed in being cleaned 10 minutes in ethanol；
Repeat above-mentioned cleaning step three times, after dried up with nitrogen；
4) preparation of tantalum pentoxide proton conduction layer
Sputtering system its background is not more than 10-4Pa, sputter gas select argon gas and oxygen, purity more than 99.999%；
Metal tantalum uses 4 inch circular targets, purity 99.9%, pure argon environment pre-sputtering 30 minutes；
The formal sputtering of five oxidation two tantalum film, sputtering power 200W, sputtering chamber air pressure control 0.7Pa, argon gas oxygen flux control
42 to 5.Sputtering duration 60 minutes, target is apart from ITO apart from 17.5cm；
Five oxidation two tantalum film thickness 400nm, SEM (SEM) Surface Characterization Fig. 5；
5) preparation of Catalytic Layer Pd
Sputtering system its background pressure 10-5Pa, sputter gas select argon gas, purity more than 99.999%；
Pd targets use the Metal Palladium of purity 99.9%, 2 inch circular targets；
Pd targets pre-sputtering under ar gas environment, sputtering power 16w, sputtering time 80 seconds, between air pressure control 0.5Pa；
In tantalum pentoxide surface formal sputtering Pd, power 16w, pressure control 0.5Pa, sputtering time 60 seconds；
Obtained Pd Catalytic Layers thickness is 6nm；
6) magnesium yittrium alloy dims the preparation of mirror layer
Sputtering system its background pressure 10-5Pa, sputter gas select argon gas, purity more than 99.999%；
The preparation of magnesium yittrium alloy uses producing high purity metal magnesium target and high pure metal yttrium target co-sputtering；
Magnesium metal target sputtering power uses 20w, metallic yttrium target sputtering power 60w, air pressure control 0.8Pa, pre-sputtering 3 minutes；
In Pd layer surface formal sputtering magnesium yittrium alloys, sputtering power magnesium target uses 20w, yttrium target to use 60w, sputtering atmosphere straight argon
Gas, air pressure control 0.8Pa, sputtering time 120 seconds；
Obtained magnesium yittrium alloy film thickness 50nm；
7) circuit connection
Using common conductive glue, laminating ito glass and magnesium yittrium alloy dim mirror layer；
The link of external circuit control, external circuit uses dc source, and power output end polarity is adjustable, voltage output amplitude 2-
10V。
Example two, volume to volume laminating pattern：
1) selection of substrate and cleaning
Substrate uses organic transparent conductive film；
By organic transparent conductive film laminating tiling on the glass substrate；
2) preparation of tungstic acid electrochromic layer
Preparation uses magnetron sputtering apparatus；
Sputtering system its background pressure is not more than 10-4Pa, sputter gas select argon gas and oxygen, purity 99.999%；
Metal tungsten target uses 4 inch circular targets, purity 99.999%, pure argon environment pre-sputtering 30 minutes；
By organic transparent conductive film feeding sample presentation room, sputtering chamber is sent into by sample presentation room；
The formal sputtering of WO 3 film, sputtering power 200W, sputtering chamber air pressure control 0.7Pa, argon gas oxygen flux control 42
Than 4.Sputtering duration 10 minutes, target to substrate distance is 17cm；
WO 3 film thickness 130nm；
3) proton implantation
The WO 3 film link power supply negative pole that will have been sputtered, positive pole uses Pt electrodes, and the sulfuric acid solution of 0.5M/L is put into together
Applied voltage, between voltage control 2.5V, application time 20 seconds；
The cleaning of tungstic acid surface acid ion, navy blue WO 3 film is taken out from acid solution, is put into deionized water
Cleaning 10 minutes, is then placed in being cleaned 10 minutes in ethanol；
Repeat above-mentioned cleaning step three times, after dried up with nitrogen；
4) magnesium yittrium alloy dims the preparation of mirror layer
Preparation uses magnetron sputtering apparatus；
Sputtering system its background pressure 10-5Pa, sputter gas select argon gas, purity 99.999%；
The preparation of magnesium yittrium alloy uses producing high purity metal magnesium target and high pure metal yttrium target co-sputtering；
Organic transparent conductive material is sent into sputtering chamber；
Magnesium yittrium alloy is sputtered, and sputtering power magnesium target uses 20W, yttrium target to use 60W, sputtering atmosphere pure argon, air pressure control
0.8Pa, sputtering time 120 seconds；
Obtained magnesium yittrium alloy film thickness 100nm；
5) preparation of Catalytic Layer Pd
Sputtering system its background pressure 10-5Pa, sputter gas select argon gas, purity 99.999%；
Pd targets use the Metal Palladium of purity 99.9%, 2 inch circular targets；
Pd targets pre-sputtering under ar gas environment, sputtering power 16w, sputtering time 80 seconds, between air pressure control 0.5Pa；
Magnesium yittrium alloy layer is put into magnetron sputtering chamber, to its splash-proofing sputtering metal Pd；
Formal sputtering Pd, power 16w, pressure control 0.5Pa, sputtering time 60 seconds；
Obtained Pd Catalytic Layers thickness is 6nm；
6) volume to volume laminating
WO 3 film layer, organic transparent proton conducting material nafion, magnesium yittrium alloy layer are fitted successively, bubble-free, aptychus
Wrinkle.Laminating type accompanying drawing 9；
7) circuit connection
Using common conductive glue, external circuit is linked, using dc source, power output end polarity is adjustable, voltage output amplitude
6V。
In the present invention based on above-mentioned, can be used for energy-conservation smart window, privacy curtain, vehicle glass, satellite, military affairs are sheltered
Equipment of this device etc. is embedded in Deng field, and any one.
In the present invention, if without illustrating, all targets and gas are all from commercially available, and purity reaches more than 99.999%.
The selection of magnetron sputtering apparatus can meet above-mentioned power, background air pressure, sputtering pressure, flow-rate ratio etc..
Claims (10)
1. a kind of total solids electrochromism light modulation device, it is characterised in that proton conduction layer and precious metal catalyst layer including tungstic acid hydrogen storage layer, magnesium yittrium alloy light modulation layer and between trioxide hydrogen storage layer, magnesium yittrium alloy light modulation layer.
2. total solids electrochromism light modulation device according to claim 1, it is characterised in that the tungstic acid hydrogen storage layer is noncrystalline membrane, thickness is 50~500 nm, preferably 100~200nm.
3. total solids electrochromism light modulation device according to claim 1 and 2, it is characterised in that the proton conduction layer is transparent inorganic-oxide conductive film or organic polymer proton conductive film.
4. total solids electrochromism light modulation device according to claim 3, it is characterised in that the proton conduction layer is tantalum pentoxide or five two neodymium amorphous state colorless and transparent films of oxidation.
5. total solids electrochromism light modulation device according to claim 4, the thickness of the proton conduction layer is 50~500nm, preferably 100~120nm.
6. total solids electrochromism light modulation device according to claim 3, it is characterised in that the proton conduction layer is polytetrafluoroethylene (PTFE) proton exchange membrane, thickness is 10~500 μm, preferably 100 μm.
7. the total solids electrochromism light modulation device according to any one of claim 1-6, it is characterised in that the chemical composition of the precious metal catalyst layer is Metal Palladium or its alloy PdM y , PdM x M is Sc, Y, Ti, Zr, V, Nb, Ta, Fe, Ni, Co, Mo in alloy, and at least one in W, wherein y are 0<y≤0.5.
8. total solids electrochromism light modulation device according to claim 7, it is characterised in that the thickness of the precious metal catalyst layer is 5~10nm.
9. the total solids electrochromism light modulation device according to any one of claim 1-8, it is characterised in that the chemical composition of the magnesium yittrium alloy light modulation layer is MgxY, wherein 0≤x≤1.
10. total solids electrochromism light modulation device according to claim 9, it is characterised in that the thickness of the magnesium yittrium alloy light modulation layer is 20~200nm, preferably 100~200nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511025316.7A CN106932993A (en) | 2015-12-30 | 2015-12-30 | Magnesium yittrium alloy and tungsten oxide film are the total solids electrochromism light modulation device of base |
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| CN201511025316.7A CN106932993A (en) | 2015-12-30 | 2015-12-30 | Magnesium yittrium alloy and tungsten oxide film are the total solids electrochromism light modulation device of base |
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| CN201511025316.7A Pending CN106932993A (en) | 2015-12-30 | 2015-12-30 | Magnesium yittrium alloy and tungsten oxide film are the total solids electrochromism light modulation device of base |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112864263A (en) * | 2019-11-26 | 2021-05-28 | 中国建材国际工程集团有限公司 | Solar cell panel and application thereof |
| CN112951944A (en) * | 2019-11-26 | 2021-06-11 | 中国建材国际工程集团有限公司 | Preparation method of solar cell panel |
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| CN1316544A (en) * | 2001-01-19 | 2001-10-10 | 中国科学院广州能源研究所 | Process for preparing gas-sensitive allochroic WO3 film by vacuum evaporation |
| CN1821812A (en) * | 2006-01-13 | 2006-08-23 | 中国科学院广州能源研究所 | Alloy gas chromism film material |
| CN103797411A (en) * | 2011-09-16 | 2014-05-14 | 独立行政法人产业技术综合研究所 | Reflective dimming electrochromic element inserted with non-water based hydrogen ion conductive electrolyte layer, and dimming element using said reflective dimming electrochromic element |
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| CN1316544A (en) * | 2001-01-19 | 2001-10-10 | 中国科学院广州能源研究所 | Process for preparing gas-sensitive allochroic WO3 film by vacuum evaporation |
| CN1821812A (en) * | 2006-01-13 | 2006-08-23 | 中国科学院广州能源研究所 | Alloy gas chromism film material |
| CN103797411A (en) * | 2011-09-16 | 2014-05-14 | 独立行政法人产业技术综合研究所 | Reflective dimming electrochromic element inserted with non-water based hydrogen ion conductive electrolyte layer, and dimming element using said reflective dimming electrochromic element |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112864263A (en) * | 2019-11-26 | 2021-05-28 | 中国建材国际工程集团有限公司 | Solar cell panel and application thereof |
| CN112951944A (en) * | 2019-11-26 | 2021-06-11 | 中国建材国际工程集团有限公司 | Preparation method of solar cell panel |
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