CN100498493C - An inorganic full-solid electric driven color-changing part making method - Google Patents
An inorganic full-solid electric driven color-changing part making method Download PDFInfo
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Abstract
The invention provides an inorganic all-solid state electrochromism component and the preparation method thereof. The component has the structure that a tungsten oxide film, a compound film of lithium metaborate and lithium sulfate, a nickel oxide film and an indium tin oxide film are deposited in turn on a tin doped indium oxide glass substrate. The preparation method has the following steps: tin doped indium oxide conductive glass is incised into substrates, the size of which is suitable to that of an instrument and equipment, and the substrates are ultrasonic washed in turn in acetone, anhydrous alcohol and demineralized water; the sputter foil cavity of a multi-target magnetic control sputtering apparatus which is loaded with the substrates is vacuumized to 1*10<-4> Pa; then the tungsten oxide film, the compound film of lithium metaborate and lithium sulfate, the nickel oxide film and the indium tin oxide film are deposited in turn. The invention has great value in the research and the application of dichroic glass, an antidazzle viewfinder, an information display screen and an energy conservation promoting window according as the electrochromism component prepared by the method of the invention has the performance of changing the transmittivity of visible light, and has the characteristics of wide modulation range and short action time.
Description
(1) technical field:
A kind of inorganic full-solid electric driven color-changing part of the present invention and preparation method thereof, refer in particular to preparation electrochromism multilayer film on transparent conducting glass, this multilayer film is formed an electric driven color-changing part, can by apply voltage realize element blue and transparent between change; Belong to preparation electrochromism multilayer film technical field on transparent conducting glass.
(2) background technology:
Electrochromism (Electrochromic, being EC) material can have under electric field action light absorption and the adjustability that sees through, optionally absorb or reflect External Heat Flux and spread, reduce buildingss such as office block and residential houses and feel nice and cool warm and a large amount of energy that must expend with the maintenance in winter in the maintenance in summer with the prevention internal heat.Simultaneously, also play and improve the natural lighting degree, peep-proof, anti-dazzle is regulated effects such as surperficial heat radiation.In view of these advantages, the researcher is widely used in this kind glass on buildings, automobile, aircraft and the spaceship etc.Normally two transparent conductive films are as electrode for the EC element, and the centre is respectively off-color material, ion conductive material and ion storage material in order.The ion storage material also can be the complementary off-color material with ion storage performance.Existing the EC element have three kinds: when ion conductive material was liquid electrolyte, at this moment the EC element was to be made of two glass-encapsulated that plate transparent conductive film and optically variable films and transparent conductive film and ion storage film respectively; When ion conductive material was the organic polymer electrolyte, at this moment the EC element was to be made of two glass laminates that plate respectively by transparent conductive film and optically variable films and transparent conductive film and ion storage film, forms the structure of similar sandwich; When ion conductive material is the inorganic electrolyte film, at this moment the EC element is transparent conductive film, off-color material film, ion-conductive film, ion storage film and a transparent conductive film of plating in a certain order on glass at individual layer, be a monolithic glass structure, be also referred to as full film EC element.The preceding two kinds of EC elements of mostly being of application are arranged at present, but because liquid electrolyte and organic polymer electrolyte all have certain corrosive attack to adjacent electrochromism off-color material and ion storage material, and ion is easy to spread, so its serviceable life and retention of color are not very desirable.The EC element of full membrane structure is all having superior performance aspect serviceable life and the retention of color, it is very harsh that but the preparation condition of this electric driven color-changing part requires, have at present two or more methods in the methods such as many employings electron beam evaporation, sputter, thermal evaporation, pulsed laser deposition of report to carry out the multilayer film preparation abroad, and ion conductive material has adopted expensive lithium niobate (LiNbO more
3), lithium tantalate (LiTaO
3) wait material, and domestic EC element research to full membrane structure is also fewer.
(3) summary of the invention:
The object of the present invention is to provide a kind of inorganic full-solid electric driven color-changing part and preparation method thereof, utilize magnetically controlled sputter method to prepare inorganic full-solid electric driven color-changing part, use a kind of ion conductive material, promptly lithium metaborate and lithium sulfate mix (LiBO according to mol ratio 3:7
2+ LiSO
4, to call LiBSO in the following text) as electrolytic thin-membrane, reaching electrochromic property preferably, and can reduce cost.
The present invention relates to a kind of inorganic full-solid electric driven color-changing part, its structure is:
Transparent conduction base sheet;
The negative electrode photochromic layer that on transparent conduction base sheet, deposits;
The ion conductive layer that on the negative electrode photochromic layer, deposits;
The anode photochromic layer that on ion conductive layer, deposits;
The transparency electrode that on the anode photochromic layer, deposits;
Wherein, described transparent conduction base sheet is tin-doped indium oxide (Sn-In
2O
3, to call ITO in the following text) and glass substrate, described negative electrode photochromic layer is tungsten oxide (WO
3) film; Described ion conductive layer is the LiBSO film; Described anode photochromic layer is nickel oxide (NiO
x) film; Described transparency electrode is an ito thin film.
Wherein, the thickness of described negative electrode photochromic layer is 300～800nm.
Wherein, the thickness of described ion conductive layer is 300～500nm.
Wherein, the thickness of described anode photochromic layer is 300～500nm.
Wherein, the thickness of described transparency electrode is 300～500nm.
The preparation method of a kind of inorganic full-solid electric driven color-changing part of the present invention, its concrete step is as follows:
(1) preparation of substrate
The ITO electro-conductive glass of buying is cut out the substrate that is fit to the instrument and equipment size, with the ultrasonic cleaning 1～3 hour in acetone earlier of the substrate of well cutting, use the absolute ethyl alcohol ultrasonic cleaning then 1～3 hour, in deionized water, cleaned at last 1～3 hour, obtain standby ito glass substrate.This substrate is contained in the sample holder that depositing device is the multi-target magnetic control sputtering device.
(2) vacuumize
Open the sputtering film-forming cavity of multi-target magnetic control sputtering device, the sample support that substrate is housed on rotatable specimen holder, is closed sputtering film-forming cavity, be evacuated down to 1 * 10
-4Pa.
(3) deposition cathode photochromic layer
In the vacuum film coating chamber of multi-target magnetic control sputtering device, feed argon gas (Ar) and oxygen (O by mass flowmeter
2), after the adjusting parameters, the cooled with liquid nitrogen substrate is used in pre-sputter 20～50 minutes, makes substrate temperature between-100 ℃～-150 ℃, begins then to deposit WO on the ito glass substrate
3Film, described concrete parameter is as follows:
Target: tungsten
Sputter type: d.c. sputtering
Target-cardinal distance: 8～10cm
Gas flow ratio is: Ar:O
2Be 1:1～3:1
Deposition pressure: 2～5Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300～800nm
(4) deposition ion conductive layer
At WO
3Thin film deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, makes substrate temperature between-100 ℃～-150 ℃, then at WO
3Deposition LiBSO film on the thin layer, described concrete parameter is as follows:
Target: LiBSO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 4～8cm
Gas flow ratio is: Ar:O
2Be 5:1～9:1
Deposition pressure: 1～3Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 50～100W
Film thickness: 300nm
(5) deposition anode photochromic layer
After the LiBSO thin film deposition finishes, every deposition parameter to be adjusted, the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, makes substrate temperature between-100 ℃～-150 ℃, deposits NiO then on the LiBSO thin layer
xFilm, described concrete parameter is as follows:
Target: metallic nickel target
Sputter type: excitation sputter
Exciting current: 1～3A
Target-cardinal distance: 4～8cm
Gas flow ratio is: Ar:O
2Be 1:1～3:1
Deposition pressure: 2～5Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300nm
(6) deposit transparent electrode
At NiO
xThin film deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, makes substrate temperature between-100 ℃～-150 ℃, then at NiO
xDeposit ito thin film on the thin layer, described concrete parameter is as follows:
Target: ITO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 4～8cm
Gas flow: Ar 50～100sccm
Deposition pressure: 1～3Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300nm
(7) shut down, treat to take out when substrate temperature is raised to room temperature sample.
Wherein, the purpose of pre-sputter is to remove the impurity on target surface; Purpose with the cooled with liquid nitrogen substrate is to obtain the non crystalline structure film, and reduces in each layer film deposition process heat affecting each other.
A kind of inorganic full-solid electric driven color-changing part of the present invention and preparation method thereof, its advantage and effect are: this electric driven color-changing part has the performance that changes transmission of visible light, and it is big to have modulation range, characteristics such as the reaction time is short, at photo chromic glass, anti-dazzle reflective mirror, there is using value very aspects such as information display screen; The present invention has positive impetus to aspects such as the research that promotes Energy Saving Windows and application.
Potential application below the present invention also has:
(a) Light modulating device
Constitute described substrate with transparence parts such as transparency glass plates, constitute described internal layer and outer electrode with transparent conductive films such as ITO.Constitute thus and present the blue Light modulating device (transmittance variable element) of color when painted.This Light modulating device can constitute camera exposure regulating element (ND optical filter, aperture etc.), sunglasses, dimming glass, sunlight roof etc.In all cases can be by applying the voltage-regulation transmitted intensity.
(b) the adjustable reflective mirror of reflectivity
Constitute described substrate with plate-shaped member, constitute described internal layer electrode, constitute described outer electrode with transparent conductive films such as ITO with metallic reflective coating.Constitute and to present the blue variable mirror of reflectivity of color when painted.This element can be used on the rear-view mirror of automobile, realizes anti-dazzle reflective effect.
(c) display element
Constitute described substrate with transparent plate-shaped members such as transparency glass plates, constitute described internal layer and outer electrode, constitute the display element that presents blue Show Color with transparent conductive films such as ITO.Perhaps, constitute described substrate, constitute electrode layer, constitute the display element that presents blue Show Color with ELD such as ITO with opaque background parts such as white glass plates.
(4) description of drawings:
Fig. 1 is the cross section structure synoptic diagram of expression EC element of the present invention
Fig. 2 is the adjustment curve of expression EC element of the present invention to transmission of visible light
Unit is described as follows among the present invention:
Pa: handkerchief nm: nanometer
Cm: centimetre mm: millimeter
W: watt ℃: degree centigrade
Sccm: standard cubic centimeters per minute A: peace
(5) embodiment:
A kind of inorganic full-solid electric driven color-changing part of the present invention, as shown in Figure 1, its structure is:
Substrate;
The negative electrode photochromic layer that on substrate, deposits;
The ion conductive layer that on the negative electrode photochromic layer, deposits;
The anode photochromic layer that on ion conductive layer, deposits;
The transparency electrode that on the anode photochromic layer, deposits;
Wherein, described substrate is a tin-doped indium oxide ito glass substrate, and described negative electrode photochromic layer is WO
3Film; Described ion conductive layer is the LiBSO film; Described anode photochromic layer is NiO
xFilm; Described transparency electrode is an ito thin film.
Wherein, the thickness of described negative electrode photochromic layer is 300～800nm.
Wherein, the thickness of described ion conductive layer is 300～500nm.
Wherein, the thickness of described anode photochromic layer is 300～500nm.
Wherein, the thickness of described transparency electrode is 300～500nm.
Its preparation method of a kind of inorganic full-solid electric driven color-changing part of the present invention, its specific embodiment is as follows:
Embodiment 1
(1) preparation of substrate
The ITO electro-conductive glass of buying is cut into the substrate of 2 * 3cm, the substrate that cuts ultrasonic cleaning 2 hours in acetone earlier, used the absolute ethyl alcohol ultrasonic cleaning then 2 hours, cleaning 2 hours in deionized water at last obtains standby ito glass substrate; This substrate is contained in the sample holder of multi-target magnetic control sputtering.
(2) vacuumize
Open sputtering film-forming cavity, the sample support that substrate is housed on rotatable specimen holder, is closed sputtering chamber, be evacuated down to 1 * 10
-4Pa.
(3) deposition WO
3Film
In vacuum film coating chamber, feed Ar and O by mass flowmeter
2, regulate parameters, the cooled with liquid nitrogen substrate is used in pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, begins then to deposit WO on the ITO substrate
3Film, described concrete parameter is as follows:
Target: tungsten
Sputter type: d.c. sputtering
Target-cardinal distance: 8cm
Gas flow: Ar 70sccm, O
230sccm
Deposition pressure: 3Pa
Substrate temperature :-120 ℃
Sputtering power: 100W
Film thickness: 600nm
(4) deposition LiBSO film
At WO
3Deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-150 ℃, then at WO
3Deposition LiBSO film on the thin layer, described concrete parameter is as follows:
Target: LiBSO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 4cm
Gas flow: Ar 90sccm, O
210sccm
Deposition pressure: 1Pa
Substrate temperature :-150 ℃
Sputtering power: 70W
Film thickness: 300nm
(5) deposition NiO
xFilm
After the LiBSO thin film deposition finishes, every deposition parameter to be adjusted, the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, deposits NiO then on the LiBSO thin layer
xFilm, described concrete parameter is as follows:
Target: metallic nickel target
Sputter type: excitation sputter
Exciting current: 1.5A
Target-cardinal distance: 5cm
Gas flow: Ar 70sccm, O
230sccm
Deposition pressure: 3Pa
Substrate temperature :-120 ℃
Sputtering power: 90W
Film thickness: 300nm
(6) deposition ito thin film
At NiO
xThin film deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, then at NiO
xDeposit ito thin film on the rete, described concrete parameter is as follows:
Target: ITO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 6cm
Gas flow: Ar 100sccm
Deposition pressure: 1Pa
Substrate temperature :-120 ℃
Sputtering power: 90W
Film thickness: 300nm
(7) shut down, treat to take out when substrate temperature is raised to room temperature sample.
Embodiment 2
(1) preparation of substrate
The ITO electro-conductive glass of buying is cut into the substrate of 2 * 3cm, the substrate that cuts ultrasonic cleaning 2.5 hours in acetone earlier, used the absolute ethyl alcohol ultrasonic cleaning then 2.5 hours, cleaning 2.5 hours in deionized water at last obtains standby ito glass substrate.This substrate is contained in the sample holder of multi-target magnetic control sputtering.
(2) vacuumize
Open sputtering film-forming cavity, the sample support that substrate is housed on rotatable specimen holder, is closed sputtering chamber, be evacuated down to 1 * 10
-4Pa.
(3) deposition WO
3Film
In vacuum film coating chamber, feed Ar and O by mass flowmeter
2, regulate parameters, the cooled with liquid nitrogen substrate is used in pre-sputter 30 minutes, makes substrate temperature probably at-130 ℃, begins then to deposit WO on the ITO substrate
3Film, described concrete parameter is as follows:
Target: tungsten
Sputter type: d.c. sputtering
Target-cardinal distance: 9cm
Gas flow: Ar 80sccm, O
240sccm
Deposition pressure: 5Pa
Substrate temperature :-130 ℃
Sputtering power: 110W
Film thickness: 500nm
(4) deposition LiBSO film
At WO
3Deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, then at WO
3Deposition LiBSO film on the thin layer, described concrete parameter is as follows:
Target: LiBSO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 6cm
Gas flow: Ar 70sccm, O
210sccm
Deposition pressure: 2Pa
Substrate temperature :-120 ℃
Sputtering power: 90W
Film thickness: 300nm
(5) deposition NiO
xFilm
After the LiBSO thin film deposition finishes, every deposition parameter to be adjusted, the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, deposits NiO then on the LiBSO thin layer
xFilm, described concrete parameter is as follows:
Target: metallic nickel target
Sputter type: excitation sputter
Exciting current: 2.5A
Target-cardinal distance: 7cm
Gas flow: Ar 90sccm, O
240sccm
Deposition pressure: 5Pa
Substrate temperature :-120 ℃
Sputtering power: 1W
Film thickness: 300nm
(6) deposition ito thin film
At NiO
xThin film deposition after finishing is adjusted every deposition parameter, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 30 minutes, makes substrate temperature probably at-120 ℃, then at NiO
xDeposit ito thin film on the thin layer, described concrete parameter is as follows:
Target: ITO ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 5cm
Gas flow: Ar 90sccm
Deposition pressure: 2Pa
Substrate temperature :-120 ℃
Sputtering power: 100W
Film thickness: 300nm
(7) shut down, treat to take out when substrate temperature is raised to room temperature sample.
Used target is the circular that diameter is 60mm in the embodiment of the invention, and thickness is 3-5mm.
Adopt the one chip inorganic full-solid electric driven color-changing part of this method preparation that visible light transmittance is had regulating action, when on two transparency electrodes, adding the voltage of 3V, can realize transformation between blueness and the Transparent color by changing polarity.Fig. 2 is that EC element of the present invention is at 400-800nm wavelength coverage internal transmission factor adjustment curve.The color of this element when impressed voltage not is light brown, and at this moment the average transmittance in the 400-800nm wavelength coverage is 29.4% as shown in Figure 2, when and WO
3Add on the ITO electrode of contact-during 3V voltage, because Li
+Be injected into WO
3In the rete, WO
3Become blueness, at this moment average transmittance is 4.6%, and when the reversing of additional power source, element changes into transparent, and average transmittance is 56.8%.This shows that this element is 52.2% in the transmissivity toning scope of visible-range.Wherein painted, the reaction that takes place in the process of bleaching mainly is:
(colour killing) (painted)
With
(painted) (colour killing).
Claims (2)
1, a kind of preparation method of inorganic full-solid electric driven color-changing part, wherein, the structure of this inorganic full-solid electric driven color-changing part is: substrate; The negative electrode photochromic layer that on this substrate, deposits; The ion conductive layer that on this negative electrode photochromic layer, deposits; The anode photochromic layer that on this ion conductive layer, deposits; The transparency electrode that on this anode photochromic layer, deposits; Described substrate is the tin-doped indium oxide glass substrate, and described negative electrode photochromic layer is a tungsten oxide film; Described ion conductive layer is lithium metaborate and lithium sulfate mixture film; Described anode photochromic layer is the nickel oxide film; Described transparency electrode is a tin-doped indium oxide film; It is characterized in that: this preparation method's concrete step is as follows:
(1) preparation of substrate
The tin-doped indium oxide electro-conductive glass of buying is cut out the substrate that is fit to the instrument and equipment size, with the ultrasonic cleaning 1～3 hour in acetone earlier of the substrate of well cutting, used the absolute ethyl alcohol ultrasonic cleaning then 1～3 hour, in deionized water, cleaned at last 1～3 hour, and obtained standby tin-doped indium oxide glass substrate; This substrate is contained in the sample holder that depositing device is the multi-target magnetic control sputtering device;
(2) vacuumize
Open the sputtering film-forming cavity of multi-target magnetic control sputtering device, the sample support that substrate is housed on rotatable specimen holder, is closed sputtering film-forming cavity, be evacuated down to 1 * 10
-4Pa;
(3) deposition cathode photochromic layer
In the vacuum film coating chamber of multi-target magnetic control sputtering device, feed argon gas and oxygen by mass flowmeter, after regulating parameters, pre-sputter 20～50 minutes, use the cooled with liquid nitrogen substrate, make substrate temperature between-100 ℃～-150 ℃, begin then on the tin-doped indium oxide glass substrate, to deposit tungsten oxide film;
(4) deposition ion conductive layer
After the tungsten oxide film deposition finishes, every deposition parameter is adjusted, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, make substrate temperature between-100 ℃～-150 ℃, then deposition lithium metaborate and lithium sulfate mixture film on the tungsten oxide film layer;
(5) deposition anode photochromic layer
After lithium metaborate and the end of lithium sulfate mixture film deposition, every deposition parameter is adjusted, and the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, make substrate temperature between-100 ℃～-150 ℃, then nickel deposited sull on lithium metaborate and lithium sulfate mixed film layer;
(6) deposit transparent electrode
After the nickel oxide thin film deposition finishes, every deposition parameter to be adjusted, the cooled with liquid nitrogen substrate is used in earlier pre-sputter 20～50 minutes, makes substrate temperature between-100 ℃～-150 ℃, deposits tin-doped indium oxide film then on the nickel oxide thin layer;
(7) shut down, treat to take out when substrate temperature is raised to room temperature sample;
Wherein, the adjusting parameters described in the step (3), this parameter is specific as follows:
Target: tungsten
Sputter type: d.c. sputtering
Target-cardinal distance: 8～10cm
Gas flow ratio is: argon gas: oxygen is 1:1～3:1
Deposition pressure: 2～5Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300～800nm;
Every deposition parameter is adjusted described in the step (4), this parameter is specific as follows:
Target: lithium metaborate and lithium sulfate hybrid ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 4～8cm
Gas flow ratio is: argon gas: oxygen is 5:1～9:1
Deposition pressure: 1～3Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 50～100W
Film thickness: 300nm;
Every deposition parameter is adjusted described in the step (5), this parameter is specific as follows:
Target: metallic nickel target
Sputter type: excitation sputter
Exciting current: 1～3A
Target-cardinal distance: 4～8cm
Gas flow ratio is: argon gas: oxygen is 1:1～3:1
Deposition pressure: 2～5Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300nm;
Every deposition parameter is adjusted described in the step (6), this parameter is specific as follows:
Target: tin-doped indium oxide ceramic target
Sputter type: radio-frequency sputtering
Target-cardinal distance: 4～8cm
Gas flow: argon gas 50～100sccm
Deposition pressure: 1～3Pa
Substrate temperature :-100 ℃～-150 ℃
Sputtering power: 60～120W
Film thickness: 300nm.
2, the preparation method of a kind of inorganic full-solid electric driven color-changing part according to claim 1 is characterized in that: described lithium metaborate and lithium sulfate mixed film mix according to mol ratio 3:7.
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