CN108085645A - A kind of magnesium yittrium alloy fully-reflected type dimming film and its preparation method and application - Google Patents
A kind of magnesium yittrium alloy fully-reflected type dimming film and its preparation method and application Download PDFInfo
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- CN108085645A CN108085645A CN201611022561.7A CN201611022561A CN108085645A CN 108085645 A CN108085645 A CN 108085645A CN 201611022561 A CN201611022561 A CN 201611022561A CN 108085645 A CN108085645 A CN 108085645A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
The present invention relates to a kind of magnesium yittrium alloy fully-reflected type dimming film and its preparation method and application, magnesium yittrium alloy light modulation layer, buffer layer and precious metal catalyst layer including being sequentially formed in matrix surface, the buffer layer are at least one of Zr, Y, Ti, Zn and Ta.The addition of buffer layer is to the oxidation of Mg in film and is diffused with inhibitory action, and effectively improves its Light-modulating mirror cycle life, obtains a kind of dimming film haveing excellent performance.
Description
Technical field
The invention belongs to glazing light-regulating technical fields more particularly to a kind of fully-reflected type light modulation film and preparation method thereof
And application.
Background technology
With the development of society, energy and environment problem is increasingly severe.According to incompletely statistics, China's building energy consumption accounts for society
The 34% of meeting total energy consumption, and glass door and window is building and the extraneous main thoroughfare for carrying out photo-thermal and exchanging.Research is marked between showing one
The heat that quasi- house has 58% in winter is lost in by windowpane；Equally in summer, 73% heat be by windowpane into
Enter.Therefore, it is intended that applying one layer of dimmability thin-film material on windowpane, freely adjust and controlled by glass so as to reach
The light and heat amount of window disengaging is finally reached the purpose of energy-saving and emission-reduction.
The Low-E glass of current industrialization, film plating layer have high to visible ray high transmission and centering far infrared
The characteristic of reflection makes it compared with simple glass and traditional coated glass for building, with excellent heat insulation and well
Translucency.But an obvious shortcoming of Low-E glass is made of once product, it is impossible to its optical states of dynamic regulation, it is only suitable
For single season, the area largely to make a clear distinction between the four seasons for China is not advantageous.
Therefore, develop it is a kind of can the smart windows of dynamic regulation optical states be particularly important.Gas-discoloration Light-modulating mirror is
Referring to the interaction of metal alloy and oxidation-reduction quality gas makes the optical property of film generate reversible variation.Gas-discoloration tune
Light microscopic is different from absorption-type smart window, and there is no to indoor secondary exothermic process.It can be simply fast according to the change of ambiance
Its optical states of the change of speed realize that Various Seasonal and period adjust the photo-thermal got in, keep indoor cool in summer and warm in winter, from
And reduce air conditioning energy consumption.When solar irradiation is very strong, by putting hydrogen, that film is made to become mirror state (total reflection state) is anti-sunlight
It is shot out；When solar irradiation is very weak, control film inhales hydrogen and becomes transparent state from mirror state (total reflection state).By inhale hydrogen and
The conversion between hydrogen realization mirror state and transparent state is put, there is intelligent control to visible and infrared light district spectrum.Research shows
Mg-Y alloy firms are a kind of more satisfactory light control materials.The film solves studies wide Mg-M (Ni, Ti) at present
Dimming film cycle life is low, dimming capability is low, there are the problems such as tinting strength, tinting power.
But when commercial application is related to, the performance of Mg-Y Light-modulating mirrors cannot still meet current demand, follow
The low ring service life is one of the main reasons.
International patent application《Reflection-Type Light Control Element》(application publication number
WO2013191085A1) and《Gaschromic Light Control Member》(application publication number WO2014109182A1)
Although being fully-reflected type Light-modulating mirror Deng magnesium base alloy film is referred to, there is gasochromic property, its cycle life is shorter, does not have
Have and propose suitable solution.
The content of the invention
For dimming film in the prior art rapid degradation the problems such as, it is an object of the invention to provide a kind of cycling longevity
The fully-reflected type dimming film that life is long, has excellent performance.
On the one hand, the present invention provides a kind of magnesium yittrium alloy fully-reflected type dimming film, including being sequentially formed in matrix table
Magnesium yittrium alloy light modulation layer, buffer layer and the precious metal catalyst layer in face, the buffer layer are at least one in Zr, Y, Ti, Zn and Ta
Kind.Preferably, the buffer layer is at least one of Zr, Ti and Ta.It is highly preferred that the buffer layer is one in Zr and Ta
Kind.
Work as inventors realized that the main reason for Mg-Y Light-modulating mirror cycle lives are low Mg elements put hydrogen process in constantly suction
It is middle to be migrated to film surface, the slow MgO of generation hydrogen diffusion velocity is combined with the oxygen in the external world.With the life of film surface MgO
Into the free entry and exit for preventing hydrogen molecule, make inside film cannot completely hydrogenated or dehydrogenation, ultimately result in the rapid degradation of film.
In the present invention, by between magnesium yittrium alloy light modulation layer and precious metal catalyst layer introduce buffer layer (such as Zr, Y, Ti, Zn and
Ta etc.), the Mg in magnesium yittrium alloy light modulation layer on the one hand can be prevented to be migrated to film surface, generation hydrogen diffusion speed is combined with oxygen
Spend slow MgO.It is thin not interfere with the light modulation of magnesium yittrium alloy for the inherently fast metal of hydrogen diffusion velocity of buffer layer selected by another aspect
Film is by inhaling hydrogen and putting the conversion between hydrogen realization mirror state and transparent state.Oxidation and diffusion of the addition of buffer layer to Mg in film
There is inhibitory action, and effectively improve its Light-modulating mirror cycle life, obtain a kind of dimming film haveing excellent performance.
It is preferred that the thickness of the buffer layer is 1~100nm.
It is preferred that the chemical formula of the magnesium yittrium alloy light modulation layer is MgxY1-x, wherein 0.1 ＜ x ＜ 0.5.
It is preferred that the thickness of the magnesium yittrium alloy light modulation layer is 5~100nm.
It is preferred that the precious metal catalyst layer is Pd.
It is preferred that the thickness of the precious metal catalyst layer is 1~30nm.
It is preferred that described matrix is transparent base or opaque matrix, it is preferably glass or macromolecule membrane.
On the other hand, the present invention also provides a kind of preparation method of magnesium yittrium alloy fully-reflected type dimming film, using magnetic
Control sputtering technology is sequentially depositing magnesium yittrium alloy light modulation layer, buffer layer and precious metal catalyst layer (such as Pd) on described matrix surface,
Obtain the magnesium yittrium alloy fully-reflected type dimming film.
It is preferred that after matrix is loaded, argon gas is passed through, keeps argon gas deposition 0.3~1.5Pa of total head, and it is whole afterwards
Maintain pressure constant in a sputtering process.
In another aspect, the present invention also provides a kind of magnesium yittrium alloy fully-reflected type dimming film prepare gas-discoloration window,
Application in hydrogen gas sensor, hydrogen-permeation membrane.
Application field of the present invention includes building energy conservation, automobile window and all band spectrum regulation and control optical device.It can be plated in
Glass surface, as dimming glass, the preparation of the dimming film and using being to carry out at room temperature, so with low energy consumption,
The advantages of cheap；Also macromolecule membrane, ordinary solid surface etc., which can be plated in, needs the place adjusted to optics；Also can apply
In gas-discoloration window (building energy conservation window, vehicle glass), hydrogen gas sensor, hydrogen-permeation membrane etc..
It is had the advantage that compared with the prior art：The dimming film material of the present invention can be used at room temperature, response speed
Degree is fast, and service life cycle is long, can prepare at room temperature, and molding step is simple, the time is short, use scope is wide.
Description of the drawings
Fig. 1 is the structure diagram of Mg-Y/Zr/Pd dimming films in the present invention；
Fig. 2 is the x-ray photoelectron spectroscopy figure of Mg-Y/Pd dimming films prepared by comparative example 1；
Fig. 3 is the self assembly schematic device that the dimming film of the present invention is tested for the property；
Fig. 4 is the light modulation hodograph of Mg-Y/Zr/Pd dimming films prepared by embodiment 1；
Fig. 5 is the light modulation hodograph of Mg-Y/Pd dimming films prepared by comparative example 1；
The cycle life comparison for the Mg-Y/Zr/Pd dimming films that Fig. 6 is Mg-Y/Pd prepared by comparative example 1 and prepared by embodiment 1
Collection of illustrative plates；
Fig. 7 is logical H2350~2600nm reflectivity collection of illustrative plates of Mg-Y/Zr/Pd dimming films prepared by front and rear embodiment 1；
Fig. 8 is logical H2350~2600nm light transmittance collection of illustrative plates of Mg-Y/Zr/Pd dimming films prepared by front and rear embodiment 1；
Fig. 9 is Mg-Y/Ti/Pd dimming film cycle life collection of illustrative plates prepared by embodiment 7；
Figure 10 is Mg-Y/Ta/Pd dimming film cycle life collection of illustrative plates prepared by embodiment 8.
Specific embodiment
It is further illustrated the present invention below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention introduces a buffer layer between magnesium yittrium alloy light modulation layer and precious metal catalyst layer can prevent Mg to table
The phenomenon that face migrates realizes the purpose for improving cycle life.Magnesium yittrium alloy fully-reflected type dimming film prepared by the present invention, knot
Structure is referring to Fig. 1, including matrix (substrate) 1, the magnesium yittrium alloy light modulation layer 2 for being sequentially formed in described matrix surface, buffer layer 3 and expensive
Metal catalytic layer 4.Wherein the chemical formula of magnesium yittrium alloy light modulation layer can be MgxY1-x, wherein 0.1 ＜ x ＜ 0.5, thickness can be 5~
100nm.The precious metal catalyst layer can be Pd, and thickness can be 1~30nm.
It is fast that buffer layer between the magnesium yittrium alloy light modulation layer and precious metal catalyst layer is chosen as hydrogen diffusion velocity
Metal can be at least one of Zr, Y, Ti, Zn and Ta, be preferably at least one of Zr, Ti and Ta.The buffering thickness
Degree can be 1~100nm.When buffer layer thickness be more than 100nm when film visible light transmittance rate and film sunlight regulation rate meeting
It is influenced to different extents, and film cycle life can decline therewith.
The preparation method of the magnesium yittrium alloy fully-reflected type dimming film of the present invention further explained below.
The selection and cleaning of matrix (substrate).Described matrix can be transparent base or opaque matrix, be preferably common glass
Glass, quartz, silicon chip or macromolecule membrane etc..As an example, sheet glass is placed in beaker, respectively in 0.5mol/LNaOH
10min is respectively ultrasonically treated in solution, deionized water, ethyl alcohol, deionized water, in determining that last cleaning solution is in pH test paper afterwards
Property.As another example, silicon chip is put into beaker, adds in ethanol in proper amount, is ultrasonically treated 10min.
The preparation of magnesium yittrium alloy light modulation layer.Specifically, cosputtering method is used on described matrix surface by target of Mg and Y
Deposit magnesium yittrium alloy light modulation layer.Magnetic control sputtering system uses DC current method, and vacuum system is by molecular pump and mechanical pump secondary groups
Into, vacuum chamber background vacuum up to 10-5The Pa orders of magnitude.After substrate is loaded, argon gas deposition 0.3~1.5Pa of total head, and afterwards
Entire sputtering process in maintain pressure it is constant.The power W (Mg) for controlling the Mg targets is 20-100W, sputtering time t (Mg)
=50-400 seconds.Construction power W (Y)=20-200W of Y targets, sputtering time are t (Y)=50-400 seconds.
The preparation of buffer layer.Specifically, it is target at least one of Zr, Y, Ti, Zn and Ta, it is controlled to sputter work(
Rate is 5-50W, and sputtering time is 10-100 seconds, in the deposition magnesium yittrium alloy light modulation layer surface buffer layer.
The preparation of precious metal catalyst layer.Specifically, using precious metals pd as target, its sputtering power is controlled to be splashed for 5-50W
The time is penetrated as 10-100 seconds, in the buffer-layer surface depositing noble metal Catalytic Layer.
The present invention between magnesium yittrium alloy layer (light modulation layer) and precious metal catalyst layer (such as palladium chtalyst layer) by increasing by one
Light transmittance difference significantly improves before and after a buffer layer, film cycle life and hydrogenation.The film is passed through 4% under normal temperature and pressure conditions
Changed after hydrogen from metallic state to transparent state, be passed through after oxygen or air by transparent state (film in transparent state, almost without
Color) change to mirror state (metallic state).With this reversible transition, the light transmittance of thin-film material can also change accordingly,
Light transmittance poor (in visual range) is maximum up to 60% before and after film hydrogenation.
Thin-film material in the present invention can be plated in simple glass, quartz and macromolecule membrane and other film surfaces.This
Invention can achieve the purpose that reversible control by changing gas component to adjust the transmitance of film and reflectivity, so as to fulfill
A kind of exploitation of gas-discoloration intelligent dimming film.Application field of the present invention includes building energy conservation, automobile window and all band light
Spectrum regulation and control optical device.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
The preparation of 1 magnesium yittrium alloy fully-reflected type film of embodiment
The present embodiment has clearly described a kind of preparation method of Mg-Y alloys gas-discoloration dimming film, is as follows：
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards.Silicon chip is put into beaker, adds in ethanol in proper amount, ultrasound
Handle 10min；
2) preparation of magnesium yittrium alloy layer, buffer layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals, 2 inches of pure Zr metals and 2 English
Very little pure Pd metals.After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, then to being filled in vacuum chamber
Inbound traffics are the high-purity argon gas of 50sccm, and it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited is in 0.3~0.5Pa
Afterwards, sputtering sedimentation is started.Mg and Y uses cosputtering method, continues buffer layer after sputtering in its surface, finally deposits
Pd Catalytic Layers.Sputtering parameter is respectively：W (Mg)=30W, t (Mg)=145s；W (Y)=80W, t (Y)=145s；W (Zr)=
10W, t (Zr)=20s；W (Pd)=15W, t (Pd)=60s.
Membrane structure schematic diagram prepared by the present embodiment 1 is as shown in Figure 1,1 is substrate, and 2 be Mg-Y alloy light modulation layers, and 3 are
Buffer layer, buffer layer are then Zr metals, and 4 be Pd Catalytic Layers.The present invention detects film thickness by film thickness gauge, it is known that embodiment 1
The thickness of Mg-Y alloy light modulation layers is 50nm in the magnesium yittrium alloy fully-reflected type film of preparation, and the thickness of buffer layer is 4nm, and Pd is urged
The thickness for changing layer is 6nm.
Comparative example 1 does not include the magnesium yittrium alloy fully-reflected type film of buffer layer
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards；
2) preparation of magnesium yittrium alloy layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals and 2 inches of pure Pd metals.It treats
After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, is then to flow is filled in vacuum chamber
The high-purity argon gas of 50sccm, it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited starts to splash after 0.3~0.5Pa
Penetrate deposition.Mg and Y uses cosputtering method, continues Pd Catalytic Layers after sputtering in its surface.Sputtering parameter is respectively：W
(Mg)=30W, t (Mg)=145s；W (Y)=80W, t (Y)=145s；W (Pd)=15W, t (Pd)=60s.It is prepared by comparative example 1
Mg-Y/Pd dimming films in Mg-Y alloy light modulation layers thickness for 50nm, the thickness of Pd Catalytic Layers is 6nm.
X-ray photoelectron diffraction is carried out to thin-film material prepared by comparative example 1, tests the depth profile of its component, as a result
As shown in Figure 2.
The light modulation speed ability test of 2 film of embodiment
Mg-Y/Pd dimming films prepared by the magnesium yittrium alloy fully-reflected type dimming film and comparative example 1 prepared to embodiment 1 are distinguished
Carry out light modulation speed ability test.Film light modulation speed is evaluated using device shown in Fig. 3, will be coated with magnesium yittrium alloy film
Glass plate 5 be oppositely arranged with a simple glass plate 6, the one side for making to be coated with magnesium yittrium alloy film is towards simple glass plate 6, two
Separated between glass plate with silica gel pad 7, being formed one can be passed through hydrogen or the cavity of deuterium, using gas flow detector 8 come
Gas is controlled, semiconductor laser 9 and silicon photoelectric diode 10 are separately positioned on to the glass for the thin-film material for being coated with magnesium yittrium alloy
Signal processing system 11 is connected on silicon photoelectric diode 9 and semiconductor laser 10 by the outside of glass plate 5 and simple glass plate 6
Between.During test, the volume fraction of hydrogen is passed through between layer glass plate as 4% hydrogen-argon-mixed body, then swashing with 670nm
Light irradiates two glass plates, measures its light modulation speed in 670nm.The results are shown in Figure 4, magnesium yittrium alloy prepared by embodiment 1
The metallic state film light transmittance about 10% of thin-film material, light transmittance about 40% after hydrogenation, light transmission difference about 30%, hydrogen before and after hydrogenation
The change time is 90s, dehydrogenation 900s.The results are shown in Figure 5, and Mg-Y/Pd dimming film metallic state films prepared by comparative example 1 are saturating
Light rate about 15%, light transmittance about 45% after hydrogenation, light transmission difference about 30% before and after hydrogenation, hydrogenation time 90s, dehydrogenation are
900s.Comparison diagram 4 and Fig. 5 understand that the addition of buffer layer can't influence its film light modulation speed.
3 film cycle life testing example of embodiment
Cycle life test is still evaluated with device shown in Fig. 3.During test, hydrogen is passed through between layer glass plate
Volume fraction is 4% hydrogen-argon-mixed body, irradiates two glass plates with the laser of 670nm, measures it with hydrogenation and dehydrogenation not
The disconnected light transmittance changed.When light transmittance difference is less than 10%, it is believed that the thin-film material basic cracking.As shown in fig. 6, top
It is the film without buffer layer prepared by comparative example 1, following is the film increased after buffer layer prepared by embodiment 1.It is right
Find that film cycle life is increased to 450 times or more by introducing buffer layer by 200 times than afterwards.Illustrate that buffer layer can be effective
Inhibit the migration of Mg, achieve the purpose that improve cycle life.It should be noted that two kinds of films lead to the hydrogen time for 90s, during disconnection
Between be 900s.
4 film light transmittance of embodiment and reflectivity performance test
1) reflectivity collection of illustrative plates is tested using HITACHI U-4100 spectrophotometers.Baseline is done to photometer first to sweep
It retouches, then test parameter is set：Start wavelength：2600nm terminates wavelength：350nm, sweep speed：600nm/min tests mould
Formula：R% finally puts the thin-film material of embodiment 1 in test box into, scans reflectivity collection of illustrative plates.The results show that such as Fig. 7 institutes
Show, thin-film material has light in metallic state very high reflectivity, only exists few absorption, it was demonstrated that the thin-film material is one
Kind reflection-type dimming film；
2) light transmittance properties are tested using HITACHI U-4100 spectrophotometers.Baseline is done to photometer first to sweep
It retouches, then test parameter, start wavelength is set：2600nm terminates wavelength：350nm, sweep speed：600nm/min tests mould
Formula：T% finally puts the thin-film material of embodiment 1 in test box into, scans light transmittance collection of illustrative plates, as shown in Figure 8.As a result show
Show, the light transmittance after thin-film material suction hydrogen is 40% or so, it was demonstrated that the film is transparent state in hydrogenation.
Embodiment 5
The present embodiment has clearly described a kind of preparation method of Mg-Y alloys gas-discoloration dimming film, is as follows：
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards.Silicon chip is put into beaker, adds in ethanol in proper amount, ultrasound
Handle 10min；
2) preparation of magnesium yittrium alloy layer, buffer layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals, 2 inches of pure Zr metals and 2 English
Very little pure Pd metals.After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, then to being filled in vacuum chamber
Inbound traffics are the high-purity argon gas of 50sccm, and it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited is in 0.3~0.5Pa
Afterwards, sputtering sedimentation is started.Mg and Y uses cosputtering method, continues buffer layer after sputtering in its surface, finally deposits
Pd Catalytic Layers.Sputtering parameter is respectively：W (Mg)=30W, t (Mg)=145s；W (Y)=80W, t (Y)=145s；W (Zr)=
20W, t (Zr)=30s；W (Pd)=15W, t (Pd)=60s.
Membrane structure schematic diagram prepared by the present embodiment 5, as shown in Figure 1,1 is substrate, 2 be Mg-Y alloy light modulation layers, and 3 are
Buffer layer, buffer layer are then Zr metals, and 4 be Pd Catalytic Layers.Mg-Y in magnesium yittrium alloy fully-reflected type film prepared by the present embodiment 5
The thickness of alloy light modulation layer is 50nm, and the thickness of buffer layer is 12nm, and the thickness of Pd Catalytic Layers is 6nm.
Embodiment 6
The present embodiment has clearly described a kind of preparation method of Mg-Y alloys gas-discoloration dimming film, is as follows：
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards.Silicon chip is put into beaker, adds in ethanol in proper amount, ultrasound
Handle 10min；
2) preparation of magnesium yittrium alloy layer, buffer layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals, 2 inches of pure Zr metals and 2 English
Very little pure Pd metals.After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, then to being filled in vacuum chamber
Inbound traffics are the high-purity argon gas of 50sccm, and it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited is in 0.3~0.5Pa
Afterwards, sputtering sedimentation is started.Mg and Y uses cosputtering method, continues buffer layer after sputtering in its surface, finally deposits
Pd Catalytic Layers.Sputtering parameter is respectively：W (Mg)=30W, t (Mg)=145s；W (Y)=80W, t (Y)=145s；W (Zr)=
30W；T (Zr)=40s；W (Pd)=15W, t (Pd)=60s.
Membrane structure schematic diagram prepared by the present embodiment 6 is as shown in Figure 1,1 is substrate, and 2 be Mg-Y alloy light modulation layers, and 3 are
Buffer layer, buffer layer are then Zr metals, and 4 be Pd Catalytic Layers.Mg-Y in magnesium yittrium alloy fully-reflected type film prepared by the present embodiment 6
The thickness of alloy light modulation layer is 50nm, and the thickness of buffer layer is 24nm, and the thickness of Pd Catalytic Layers is 6nm.
Embodiment 7
The present embodiment has clearly described a kind of preparation method of Mg-Y alloys gas-discoloration dimming film, is as follows：
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards.Silicon chip is put into beaker, adds in ethanol in proper amount, ultrasound
Handle 10min；
2) preparation of magnesium yittrium alloy layer, buffer layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals, 2 inches of pure Ti metals and 2 English
Very little pure Pd metals.After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, then to being filled in vacuum chamber
Inbound traffics are the high-purity argon gas of 50sccm, and it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited is in 0.3~0.5Pa
Afterwards, sputtering sedimentation is started.Mg and Y uses cosputtering method, continues buffer layer after sputtering in its surface, finally deposits
Pd Catalytic Layers.Sputtering parameter is respectively：W (Mg)=30W, t (Mg)=120s；W (Y)=80W, t (Y)=130s；W (Ti)=
5W；T (Ti)=120s；W (Pd)=15W, t (Pd)=60s.
Membrane structure schematic diagram prepared by the present embodiment 7 is as shown in Figure 1,1 is substrate, and 2 be Mg-Y alloy light modulation layers, and 3 are
Buffer layer, buffer layer are then Ti metals, and 4 be Pd Catalytic Layers.Mg-Y in magnesium yittrium alloy fully-reflected type film prepared by the present embodiment 7
The thickness of alloy light modulation layer is 50nm, and the thickness of buffer layer is 12nm, and the thickness of Pd Catalytic Layers is 6nm.
Film cycle life figure prepared by the present embodiment 7 is as shown in figure 9, cycle life is tested still with dress shown in Fig. 3
It puts and is evaluated.After introducing Ti buffer layers in the film, film Xun Huan, which is inhaled, puts hydrogen 350 times or so, the embodiment 7 compared with comparison 1
Cycle life still increase.It should be noted that film leads to the hydrogen time for 90s, turn-off time 900s.
Embodiment 8
The present embodiment has clearly described a kind of preparation method of Mg-Y alloys gas-discoloration dimming film, is as follows：
1) cleaning of substrate
Sheet glass is placed in beaker, respectively each ultrasound in 0.5mol/L NaOH solutions, deionized water, ethyl alcohol, deionized water
10min is handled, determines that last cleaning solution is in neutrality with pH test paper afterwards.Silicon chip is put into beaker, adds in ethanol in proper amount, ultrasound
Handle 10min；
2) preparation of magnesium yittrium alloy layer, buffer layer and Catalytic Layer
Magnetic control sputtering system uses DC current method, and vacuum system is made of molecular pump and mechanical pump two level, and vacuum chamber background is true
Reciprocal of duty cycle is up to 10-5The Pa orders of magnitude.Target component is respectively 2 inches of pure Mg metals, 2 inches of pure Y metals, 2 inches of pure Ta metals and 2 English
Very little pure Pd metals.After background vacuum reaches requirement, the substrate after cleaning is put into settling chamber, then to being filled in vacuum chamber
Inbound traffics are the high-purity argon gas of 50sccm, and it is 15r/min to control substrate rotating speed.Chamber pressure stabilization to be deposited is in 0.3~0.5Pa
Afterwards, sputtering sedimentation is started.Mg and Y uses cosputtering method, continues buffer layer after sputtering in its surface, finally deposits
Pd Catalytic Layers.Sputtering parameter is respectively：W (Mg)=30W, t (Mg)=145s；W (Y)=80W, t (Y)=145s；W (Ta)=
20W；T (Ta)=10s；W (Pd)=15W, t (Pd)=60s.
Membrane structure schematic diagram prepared by the present embodiment 8 is as shown in Figure 1,1 is substrate, and 2 be Mg-Y alloy light modulation layers, and 3 are
Buffer layer, buffer layer are then Ta metals, and 4 be Pd Catalytic Layers.Mg-Y in magnesium yittrium alloy fully-reflected type film prepared by the present embodiment 8
The thickness of alloy light modulation layer is 50nm, and the thickness of buffer layer is 5nm, and the thickness of Pd Catalytic Layers is 6nm.
Film cycle life figure is as shown in Figure 10 prepared by the present embodiment 8, and Mg-Y/Ta/Pd films Xun Huan, which is inhaled, puts hydrogen 450 times
Left and right.Cycle life test is still evaluated with device shown in Fig. 3.It should be noted that film leads to the hydrogen time for 90s, break
ETAD expected time of arrival and departure is 900s.Fast metal buffer layer is spread when in membrane structure, introducing hydrogen, film cycle life is significantly improved, shown
Buffer layer is the effective ways for improving film cycle life.
Claims (10)
1. a kind of magnesium yittrium alloy fully-reflected type dimming film, which is characterized in that the magnesium yttrium including being sequentially formed in matrix surface closes
Golden light modulation layer, buffer layer and precious metal catalyst layer, the buffer layer are at least one of Zr, Y, Ti, Zn and Ta.
2. magnesium yittrium alloy fully-reflected type dimming film according to claim 1, which is characterized in that the thickness of the buffer layer
For 1~100nm.
3. magnesium yittrium alloy fully-reflected type dimming film according to claim 1 or 2, which is characterized in that the magnesium yittrium alloy
The chemical formula of light modulation layer is MgxY1-x, wherein 0.1 ＜ x ＜ 0.5.
4. magnesium yittrium alloy fully-reflected type dimming film according to any one of claim 1-3, which is characterized in that the magnesium
The thickness of yittrium alloy light modulation layer is 5~100nm.
5. the magnesium yittrium alloy fully-reflected type dimming film according to any one of claim 1-4, which is characterized in that described expensive
Metal catalytic layer is Pd.
6. the magnesium yittrium alloy fully-reflected type dimming film according to any one of claim 1-5, which is characterized in that described expensive
The thickness of metal catalytic layer is 1~30nm.
7. the magnesium yittrium alloy fully-reflected type dimming film according to any one of claim 1-6, which is characterized in that the base
Body is transparent base or opaque matrix, is preferably simple glass, quartz, silicon chip or macromolecule membrane.
8. a kind of preparation method of the magnesium yittrium alloy fully-reflected type dimming film as any one of claim 1-7, feature
It is, magnesium yittrium alloy light modulation layer, buffer layer and precious metal catalyst is sequentially depositing on described matrix surface using magnetron sputtering technique
Layer, obtains the magnesium yittrium alloy fully-reflected type dimming film.
9. preparation method according to claim 8, which is characterized in that after matrix is loaded, be passed through argon gas, argon gas is kept to sink
0.3~1.5Pa of product total head.
10. one kind as any one of claim 1-7 magnesium yittrium alloy fully-reflected type dimming film prepare gas-discoloration window,
Application in hydrogen gas sensor, hydrogen-permeation membrane.
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| CN109136841A (en) * | 2018-08-17 | 2019-01-04 | 上海交通大学 | Fluorine carbon/palladium/magnesium-niobium pentaoxide gas causes dimming film and preparation method thereof |
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| JP2012220740A (en) * | 2011-04-08 | 2012-11-12 | National Institute Of Advanced Industrial & Technology | All solid-state reflective dimming electrochromic element given wavelength selectivity and dimming member using the same |
| CN104995555A (en) * | 2013-01-10 | 2015-10-21 | 独立行政法人产业技术综合研究所 | Gaschromic light control member |
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| JP2007301778A (en) * | 2006-05-10 | 2007-11-22 | National Institute Of Advanced Industrial & Technology | Light control mirror having controlled structure of interface |
| JP2012220740A (en) * | 2011-04-08 | 2012-11-12 | National Institute Of Advanced Industrial & Technology | All solid-state reflective dimming electrochromic element given wavelength selectivity and dimming member using the same |
| CN104995555A (en) * | 2013-01-10 | 2015-10-21 | 独立行政法人产业技术综合研究所 | Gaschromic light control member |
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