CN106158692B - A kind of monitoring system and method for thermocolour smart membranes annealing - Google Patents
A kind of monitoring system and method for thermocolour smart membranes annealing Download PDFInfo
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- CN106158692B CN106158692B CN201510136864.0A CN201510136864A CN106158692B CN 106158692 B CN106158692 B CN 106158692B CN 201510136864 A CN201510136864 A CN 201510136864A CN 106158692 B CN106158692 B CN 106158692B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67242—Apparatus for monitoring, sorting or marking
- H01L21/67253—Process monitoring, e.g. flow or thickness monitoring
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67098—Apparatus for thermal treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
Abstract
The invention discloses a kind of monitoring systems of thermocolour smart membranes annealing, before and after being annealed using vanadium oxide thermocolour smart membrane, precursor film before annealing is compared with it can be realized the film layer of phase transition function after being properly completed annealing, especially near-infrared and in infrared transmitance there are significantly Variation Features, and the situation of change of more specific transmitance carries out the real time monitoring of film layer crystallization state.Detecting and analysing system provided by the present invention is suitable for vanadium oxide thermocolour smart membranes and is deposited on the substrate with certain translucency, then using the short annealing of radiant type heating, the annealing being particularly suitable in vacuum system.
Description
Technical field
The present invention relates to the production technologies of thermocolour smart membranes, more particularly, to a kind of monitoring of thermocolour smart membranes annealing
System and method.
Background technique
The preparation of vanadium oxide thermocolour smart membrane needs more harsh temperature environment, that is, shows as vanadium oxide film layer from amorphous
State is changed into the temperature of the crystalline state with phase transition function usually at 400 DEG C~600 DEG C, even higher temperature.Simultaneously for reality
The application range of existing vanadium oxide thermocolour smart membrane usually uses substrate of the different substrates as deposition film.Due to preparation temperature
The requirement of environment is spent, the plastic film substrate that may be used, glass substrate etc. are difficult to put for a long time within the scope of such temperature
It sets, general plastic supporting base such as PET is difficult to bear 400 DEG C or so of relatively-high temperature, and glass substrate is within the scope of above-mentioned temperature
There is damaged or tempering stress degenerate problem.It is CN that related glass tempering stress was degenerated, which applies in application publication number,
There is relevant description in the application for a patent for invention file of 104004888 A.
Based on above-mentioned problem, preparing vanadium oxide thermocolour smart membrane can usually be annealed using room temperature high temperature post-deposition, should
Preparation method application No. is 201410856240.1 and application No. is the Chinese invention patent application of 201410856004.X text
Also there is related description in part.It is fast to have the characteristics that power density height heats based on the heating of infra-red radiation fluorescent tube, during heating
Hot environment in, common spectral instrument is difficult to realize real-time quick monitoring, especially brilliant to vanadium oxide thermocolour smart membrane
The monitoring of change process.If vanadium oxide thermocolour film layer crystallization process cannot be monitored timely, real-time crystallization information is obtained, that
, in order to ensure the thorough crystallization of film layer, generally can extend heating time, still, this may cause tempered glass and stress occurs
The problem of degeneration, is affected so as to cause tempered glass security performance.
Currently, domestic also have the annealing monitoring problem for film to be studied.If Authorization Notice No. is CN
A kind of preparation of the polysilicon membrane that crystallite dimension is controllable disclosed in the patent of invention file of 101311344 B and detection device, should
Detection device receives system, Raman number by laser source, optical splitter, beam shaping system, optical focusing system, stimlated Raman spectrum
According to analysis and feedback system and mobile work platform composition, on-line checking is carried out while being the preparation of polysilicon membrane.Although should
Device is suitable for the preparation and real-time detection of industrialization polysilicon membrane, and still, the light source of the device is confined to laser source, device
Input cost is higher, cannot promote well.
The application for a patent for invention file that application publication number is 104393116 A of CN then discloses a kind of Nano thin film too
The ellipse garden polarization spectrum of positive energy battery monitors preparation method in real time, during depositing Nano thin film, using spectroscopic ellipsometry
Monitor thin film growth process in real time, still, which is to absorb to mix from xenon lamp or tungsten halogen lamp using fiber spectrometer
Light source generates and is incident in sample surfaces and the spectrum beam that reflects to form, and the position precision of each optical device is high, if substrate base
Shape change, the adjustment of each optical device is not easy, inconvenient for use.
The application for a patent for invention file that application publication number is 104078376 A of CN is disclosed to be used for furnace tube high temperature lehr attendant
The monitoring method of skill, however the monitoring method only after control wafer high-temperature annealing process measure control wafer surface amounts of particles and
The thicknesses of layers of silica membrane layer, there is no monitor the high-temperature annealing process of control wafer in real time, it is difficult to ensure control wafer
Quality.
For this reason, it is necessary to a kind of monitoring system of thermocolour smart membranes annealing be proposed, in particular for using infrared lamp
Radiant heating implements the monitoring system of the film layer state in the short annealing system of annealing.
Summary of the invention
The purpose of the present invention is to provide a kind of monitoring systems of thermocolour smart membranes annealing, are particularly suitable for vanadium oxide heat
The monitoring of the Annealing Crystallization process of color smart membrane, the precursor before and after being annealed using vanadium oxide thermocolour smart membrane, that is, before annealing
Film compared with it can be realized the film layer of phase transition function after being properly completed annealing, near-infrared and in infrared transmitance have it is big
The Variation Features of amplitude, and the situation of change of more specific transmitance rate carry out film layer crystallization state, i.e. film layer from amorphous
State structure is changed into the real time monitoring of the change procedure of crystalline structure.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of monitoring system of thermocolour smart membranes annealing, particularly, including annealing implementing device, at least one detection light
Source and at least one probe source reception device corresponding with the probe source；It is equipped in implementing device of annealing and is coated with thermocolour
The substrate of smart membranes and the annealing heat source that substrate is heated；Probe source reception device includes receiving transducer and computer
System；Receiving transducer is connect with computer system data；The light beam that probe source issues is radiated on substrate, which penetrates base
Piece is simultaneously received probe reception, and then the transmitance that the light beam penetrates substrate is transmitted to computer system by receiving transducer, is calculated
Machine system carries out data processing to the transmitance, generates the control signal of a working condition for controlling annealing implementing device,
The working condition of control annealing implementing device.
It includes the ultraviolet light source within the scope of infrared band, preferably optical wavelength that optical wavelength, which may be selected, in probe source
In 300nm~550nm or more than or equal to the light source in the near-infrared of 800nm, middle infrared band.
The principle of the present invention is as follows:
Transmitance is during the another side of light beam from the plane of incidence to the substrate of substrate leaves, and probe source is sent out
Light beam out the ratio between projects and penetrates the radiation energy of substrate and the integrated radiant emittance of light beam that probe source is issued.Wave band exists
300nm~550nm or wave band are greater than or equal to the near-infrared of 800nm, the light of middle infrared band is radiated at presoma film layer and moves back
On thermocolour smart membranes after thermocolour smart membranes or annealing process film layer complete crystallization before fire with phase transition function, penetrate
Rate has apparent difference, and the judgement of thermocolour smart membranes crystallization degree can be carried out using the difference of transmitance.Therefore, in use
It states the light source in wavelength band and penetrates the substrate coated with thermocolour smart membranes, and receive the light of transmission from the other side of substrate
By force, thermocolour smart membranes, the especially crystallization of vanadium oxide thermocolour smart membranes can accurately be known according to the variation tendency of light intensity
Degree determines the duration of annealing to control the working condition of annealing implementing device.
Probe source and probe source reception device of the invention can have one or more to be installed on annealing implementation dress
In setting, probe source and probe source reception device are generally matched, and are in one-to-one relationship.Substrate in implementing device of annealing
Can keep with cavity it is opposing stationary, move back and forth or toward same direction move mode annealing.Substrate is mobile toward a direction
When, two sets and its two sets or more of probe source and its probe source reception device, two sets or two sets or more of spy can be used
The moving direction that light source and its probe source reception device are surveyed along substrate is arranged.By a set of probe source therein and its spy
It surveys light source receiving device acquisition transmitance to be compared with the transmitance that other set system obtains, can obtain more accurate
Transmitance.
Probe source can choose wave band 300nm~550nm or wave band more than or equal to the near-infrared of 800nm, in it is red
The light source of wave section, but and it is non-limiting can only use above range in light source, it is only saturating before and after selective annealing herein
Cross the apparent wave-length coverage of rate comparison in difference.Light source of the wave band within the scope of 550nm-800nm is radiated at vanadium oxide thermocolour intelligence
On film, ordinary circumstance can also have the variation of lesser transmitance, and still, the transmitance of precursor film layer itself is relatively low
When, the variation of the transmitance in the wavelength band almost can be ignored.Transmitance according to thermocolour smart membranes changes
Trend, nearly middle infrared waves of the wave band of probe source preferably after 1500nm, the transmission become apparent can be obtained in this way
Rate difference characteristic and the accurate monitoring for realizing annealing process.
Probe source can penetrate substrate from the top incidence of film layer (for thermocolour smart membranes layer), by the spy below substrate
Survey the light intensity variation tendency for the light that light source receiving device receives after passing through substrate；Probe source can also be incident from the lower section of film layer
Substrate is penetrated, the light intensity variation tendency of the light of the transmission after passing through substrate is received by the probe source reception device above substrate.
This annealing monitoring system generally works under anneal environment, i.e., in a short time by amorphous vanadium oxide heat
Color smart membrane works in the environment of being changed into the film layer of the crystal state with phase transition function, it is therefore desirable to annealing implementing device
It is used cooperatively.Implementing device of annealing can existing conventional design, the annealing heat source such as heated to substrate is used to support substrate
Platform etc..Light source of annealing is amorphous vanadium oxide thermocolour smart membranes to be changed into phase transformation function in a short time
The light source of energy, can be any heat source including laser, infra-red radiation fluorescent tube, halogen lamp tube, iodine-tungsten lamp fluorescent tube.Its
In, the light source that infra-red radiation fluorescent tube is constituted has heating efficiency high and can be relatively easy to realize that the uniform of large area adds
Heat, therefore, annealing light source is preferably infra-red radiation fluorescent tube.
Probe source can be any one of xenon lamp, halogen lamp and laser, still, the temperature in Quick annealing device
Degree is universal higher, the light intensity and directionality of common detection light source by by certain limitation, as xenon lamp shorter apart from model
It can be used as probe source in enclosing, but in order to avoid the hot environment of annealing adversely affects Monitor Equipment, visit
The general distance measurement light source receiving device larger distance of light source is surveyed, usually in 0.5m or more, the even up to distance of 1.5m.Xenon
Lamp is generally difficult to reach such distance measurement requirement, and laser acquisition light source is due to good unidirectional sexual clorminance, then more suitable
Close the probe source being selected as in annealing monitoring system.
The radiation of light source wave-length coverage of infrared radiation lamp is concentrated mainly on nearly mid infrared region (1000nm~4000nm), and
The radiation of light source wave-length coverage of halogen lamp tube is then concentrated mainly on visible and near infrared region (500nm~2000nm), for not
With the fluorescent tube of material its radiation wave-length coverage difference, but main radiation intensity is included in above-mentioned wavelength model
In enclosing.For the radiation fluorescent tube quickly heated, the high-efficient and unit power of infra-red radiation fluorescent tube is also higher, and extensively
Be applied to the various environment quickly heated in, pretend as light source of preferably annealing.And according to wave band in 300nm~550nm or
Before near-infrared of the wave band more than or equal to 800nm, the light source within the scope of middle infrared band are radiated at vanadium oxide thermocolour smart membrane
The variation of transmitance when film layer after body film layer and annealing, the selected wave-length coverage of probe source should then be included in
The near-infrared of 300nm~550nm or wave band more than or equal to 800nm, within the scope of middle infrared band, such as can choose 460nm,
The laser of 532nm, 1064nm, 2000nm are as probe source.
In order to avoid probe source by the interference of annealing light source or reduces its interference, visited at the wave band of probe source
Survey light source when being radiated at vanadium oxide thermocolour smart membranes transmitance variation more apparent range when, can take following measure into
Row avoids or improves: first, probe source avoids the wavelength band of annealing light source；Second, the reception of probe source reception device
The settable probe source of probe distal end can by narrow-band optical filter.Such as select probe source wavelength for 2000nm, then
It can choose the passable filter plate of the wave bands such as 2000nm ± 100nm, 2000nm ± 50nm, 2000nm ± 5nm.It is so-called
Narrow-band refers to centered on probe source that the wavelength band of wavelength is small, and the degree being interfered in this way is smaller.In order to avoid
Remaining light of non-probe source enters receiving transducer and interferes in annealing process, can also be in probe source reception device
The leading portion of filter plate one reception device be set limit light aperture, the aperture that reception device limits light aperture is greater than probe source reception
The received detection light beam of device institute；It can also be installed along the direction of advance of light beam in the end of probe source and collimate anti-tampering pipe,
The end for collimating anti-tampering pipe is formed with probe source limit light aperture, meanwhile, it can also expand collimating installation light beam in anti-tampering pipe
Tread assembly, beam expander component are made of muti-piece with beam expander effect and/or the optical element pretended with uniform light,
And beam expander component is between probe source and probe source limit light aperture.The aperture that probe source limits light aperture, which is less than, to be expanded
Light beam after beam is irradiated on substrate so that the uniform detection light beam in part only be allowed to limit light aperture by probe source.Detect light
The shape of source limit light aperture and receiving apparatus limit light aperture can be round, rectangular and other irregular shapes, as long as not shadow
Probe source needed for ringing passes through.
Actual detection monitoring in, if selection probe source and heating radiation fluorescent tube optical source wavelength range coincide or
The wavelength of probe source is included in radial burner pipe wave-length coverage, then needs to subtract plus optical filter in probe source light path system
Influence of the radiation fluorescent tube light wave to the transmitance accuracy of detection less, on the contrary optical filter can be removed.For example, by using infra-red radiation
Fluorescent tube is as annealing heat source, and selecting the laser of 460nm as probe source, then probe source light path system can remove filter plate；
Select the laser of 2000nm then should add optical filter in light path system as probe source.
The light intensity of probe source may cause by force very much exploring laser light light source to the heating anneal effect of film or cause film
The etching of layer leads to actual crystallization process to the state that the film layer in annealing process reaches crystallization completion in advance occur
Detection inaccuracy.It therefore, can in order to avoid there is annealing effect and film layer etching problem caused by the probe source light intensity
It carries out expanding processing using beam expander component for probe source, the uniformity of light intensity is ensured while reducing light intensity.Foundation
The annealing substrate product or sample of different situations, the light intensity of probe source is different, and probe source can be visited by adjusting
It surveys the output power of light source, the position of beam expander component, the focal length of beam expander lens and position and reaches the effect for adjusting light intensity
Fruit makes the light beam of probe source be radiated on the thermocolour smart membranes of substrate the crystallization that can't cause thermocolour smart membranes.Extremely
Film layer annealing effect and superficial film whether is caused to etch in set probe source, it is intelligently thin for the thermocolour newly measured
The probe source that film can choose several groups of difference light intensity is scanned, and then carries out XRD (X-ray to the region through light source scanning
Diffraction) etc. the test of crystal structures, the test judgement of film surface SEM (scanning electron microscope) whether cause vanadium oxide film layer crystallize or
Person's film surface is by laser ablation.Under normal circumstances, the light beam that probe source issues is after beam expander component expands, the light beam
Light intensity power density between 0.2mw~20mw, preferably 1mw~5mw.
Annealing in the present invention monitors test macro, may operate in the annealing under atmospheric environment, also may operate in true
Annealing in air atmosphere environment.If working in the annealing in vacuum environment atmosphere, at the top and/or bottom of vacuum cavity
Need to be arranged optical path window, that is, the glass window for installing corresponding material can allow the probe source of corresponding wavelength to penetrate.
Annealing in the present invention monitors test macro, is directed to suitable for annealing device and exists comprising vanadium oxide thermocolour smart membrane
The annealing of interior single-layer or multi-layer composite film.Vanadium oxide thermocolour smart membrane, it is often the case that refer to the final tool obtained after annealing
There is the vanadium oxide thermocolour smart membrane of phase transition function.Therefore the precursor film before its annealing not complies fully with stoichiometry V:O=1:2
Atomic ratio.Compared to the vanadium oxide film layer of stoichiometric ratio, which is likely to occur oxygen debt or peroxide, implements annealing
Environment can be to be carried out in the non-reactive atmosphere under reducing atmosphere, oxidizing atmosphere and protective atmosphere.
Annealing process thermocolour smart membranes crystallization degree is monitored in real time using above-mentioned monitoring system the present invention also provides a kind of
Method, the specific steps are that:
1, the substrate for coating thermocolour smart membranes is placed between probe source and probe source reception device；Detect light
The light that source issues penetrates substrate and detected light source receiving device receives, and receiving transducer will transmit through rate and be transmitted to computer system,
The light that record probe source is issued penetrates the initial transmission T of substrate1；
2, the substrate for coating thermocolour smart membranes is sent into annealing implementing device；Annealing heat source heats substrate, to substrate
It is made annealing treatment；The substrate of annealing is monitored in real time, the light that probe source issues penetrates substrate and detected light
Source receiving device receives, and real-time transmitance is transmitted to computer system by receiving transducer, and the light that record probe source is issued is worn
The real-time transmitance T of saturating substraten；
3, compare TnWith T1Difference, calculate Δ Tn=T1-Tn；
4, to TnKeep stable or Δ Tn>=0.8 Δ T closes annealing heat source or substrate is moved to outside annealing heat source；ΔT
For the substrate transmitance changing value of annealing front and back.
So-called real time monitoring is that the data record of substrate transmitance is carried out using the second as time quantum, between adjacent data
Time interval t may be set in the range of 0.5s to 100s.So-called real-time transmitance TnIt keeps stablizing and refer to: will visit
That surveys is previous through rate score TnWith adjacent latter transmission rate score Tn+1Compare, change rateBudget
Numerical value x, default value x generally can be set as be less than or equal to 5%.Default value x can also in a certain range into
Row changes, wherein in detection process, precursor film compared with △ T-phase, judges with the film layer transmitance difference after high-temperature phase-change
Condition Δ Tn>=0.95 Δ T, but the condition is not intended as limiting, and being set at for this coefficient N=0.95 can determine that film layer is true
It is real to complete the crystalline state vanadium oxide film layer obtained close to stoichiometric ratio of annealing.The setting range of the coefficient can be set as N >=
0.8. ordinary circumstance is that probe source about changes wave band greatly close to middle infrared transmittivity difference, then coefficient N setting can be more
It is small, such as 0.8.
The performance measurement of nano coating under high temperature ultra-fast anneal environment is a difficult point in itself in terms of realizing angle, main
It wants the reason is that the safety for being that dependence test instrument works long hours in the high temperature environment under normal circumstances is difficult to stability
Guarantee.For optic test, the one-way and intensity of ordinary light source are difficult to reach a high temperature light source under ultra-fast anneal environment
Performance requirement, and how to solve the problems, such as that the heatproof of optical fiber usually used in optical system is also a problem, especially exist
Use in vacuum environment is also required to solve more technical problem.Therefore, the present invention is in order to solve in high annealing environment
The optical performance test problem of nano coating, for vanadium oxide thermocolour smart membrane before annealing and annealing after film layer in certain waves
Under the light beam irradiation of section, transmitance changes significantly this feature, and the oxidation in annealing process is penetrated using probe source
Vanadium thermocolour smart membrane, is monitored in real time.Avoid the close contact of optical system and test sample or product, while when first
Between control vanadium oxide thermocolour smart membrane Annealing Crystallization process, thus allow the present invention the real-time of non-contact hot environment can be realized
Monitoring, can also obtain vanadium oxide thermocolour smart membrane performance characteristic in time, and annealing system can also be controlled in time according to monitored results
The working of system improves the loss of tempered glass stress and reduces the energy consumption that annealing heat source generates.
Thermocolour smart membranes annealing monitoring system provided by the invention can also be applied to simple thermocolour smart membranes list
Wavelength before phase change after transmission measurement, obtain the transmission regulation rate of Single wavelength.At this time, which can simplify as with phase transformation
The thermocolour smart membranes of function can heat thermocolour smart membranes to heat source (the i.e. heretofore described annealing undergone phase transition
Heat source does not limit the lamp source that can only use high power density), probe source and its reception device.Initial measurement transmitance
And the difference of transmitance is the regulation rate of the thermocolour smart membrane at the wavelength after phase transformation.
Detailed description of the invention
Fig. 1 is the schematic diagram of annealing monitoring system in the embodiment of the present invention 1；
Fig. 2 is the schematic diagram of probe source in the embodiment of the present invention 1；
Fig. 3 is the schematic diagram of probe source reception device in the embodiment of the present invention 1；
Fig. 4 is that high transmission change rate of the invention and the low substrate annealing front and back transmittance curve through change rate are illustrated
Figure；
Fig. 5 is transmitance trend chart schematic diagram in substrate annealing process in the embodiment of the present invention 1；
Description of symbols: 1- probe source；2- annealing implementing device；3- probe source reception device；1-1- laser；
1-2- laser beam；1-3- beam expander lens group；1-4- probe source limits light aperture；1-5- collimates anti-tampering pipe；1-6- is quasi-
Straight anti-tampering pipe support；2-1- annealing heat source；2-2- substrate；2-3- substrate support platform；Light transmission under 2-4- annealing implementing device
Window；Optical transmission window in 2-5- annealing implementing device；3-1- optical filter；3-2- probe source receiving transducer；3-3- computer control
Device processed；3-4- reception device limits light aperture；A-1- high transmittance changes transmittance curve before substrate is annealed；A-2- high transmittance
Change substrate full annealing high-temperature-phase transmittance curve；B-1- low transmission changes transmittance curve before substrate is annealed；B-2- is low
Transmitance changes substrate full annealing high-temperature-phase transmittance curve；T1Transmission measurement value before precursor substrate is annealed；TnSubstrate
Any metrology moment transmitance in annealing process；Tn+1Any metrology moment transmitance in substrate annealing process.
Specific embodiment
Invention is further explained with reference to the accompanying drawings and examples.
Embodiment 1:
Monitoring system as shown in Figure 1 is made of probe source 1, annealing implementing device 2 and probe source reception device 3.
Implementing device 2 of annealing is using conventional annealing device.It is flat that annealing heat source 2-1, substrate support are equipped in implementing device 2 of annealing
Platform 2-3.Substrate 2-2 is then placed on substrate and is made on platform 2-3, and is in the lower section of annealing heat source 2-1.Probe source 1 is then pacified
Mounted in the top of annealing implementing device 2.Pass through optical transmission window 2-5 in the annealing implementing device of 2 top of annealing implementing device, detection
The light beam that light source 1 issues can be radiated on substrate 2-2.And probe source reception device 3 is then mounted on annealing implementing device 2
Lower section.By optical transmission window 2-4 under the annealing implementing device of 2 lower section of annealing implementing device, the light beam for penetrating substrate 2-2 can enter
It is incident upon probe source reception device 3.In the present embodiment 1, annealing heat source 2-1 is infra-red radiation fluorescent tube.
Annealing heat source 2-1 is not limited to the top setting of substrate 2-2 in the present invention, needs according to annealing process, can also
Annealing heat source 2-1 is arranged in the lower section of substrate.When the annealing that implementing device 2 of annealing is used under vacuum environment atmospheric condition, then
Need to be arranged optical transmission window 2-4 and optical transmission window 2-5 in annealing implementing device under annealing implementing device therein.Light inlet window essence
For the top and bottom housing openings of the vacuum cavity for implementing device of annealing, installation can penetrate glass, that is, shape of probe source in hole
At so-called light inlet window.
As shown in Fig. 2, probe source 1 includes laser 1-1 in the present embodiment 1, it is also equipped with below laser 1-1
Collimate anti-tampering pipe 1-5.It collimates anti-tampering pipe 1-5 and supports 1-6 to be mounted in annealing implementing device 2 by collimating anti-tampering pipe.
Collimating anti-tampering pipe support 1-6 can be the supporting element of independent support plate, supporting block or arbitrary shape, and it is real to be also possible to annealing
Apply the glass that window 2-5 is penetrated on device.It collimates and two pieces of beam expander lens is installed in the tube body of anti-tampering pipe 1-5, constitute
Beam expander lens group 1-3, i.e. beam expander component.In addition, the end for collimating anti-tampering pipe 1-5 is also formed with probe source limit
Light aperture 1-4.The laser beam 1-2 that laser 1-1 is issued is limited after beam expander lens group 1-3 is expanded through probe source
Light aperture 1-4 is appeared, and exposes to the surface of substrate 2-2.Beam expander lens group 1-3 shown in Fig. 2 is not limited in the present invention
In two simple optical lens groups at expand unit, herein signified optical beam-expanding lens group can also be arranged it is other be conducive to it is equal
Even laser energy density and the optical element expanded.
As shown in figure 3, probe source reception device 3 includes probe source receiving transducer 3-2 in the present embodiment 1, light is detected
Source receiving transducer 3-2 data connection has Computer Control Unit 3-3.Probe source receiving transducer 3-2 is connect using existing optics
Receive device.In addition, it is also equipped with optical filter 3-1 above probe source receiving transducer 3-2, and the top of optical filter 3-1 is then
It is formed with reception device limit light aperture 3-4.The light beam for penetrating substrate 2-2 is incident from reception device limit light aperture 3-4, and through filtering
After piece 3-1 filtering, expose on probe source receiving transducer 3-2.Probe source receiving transducer 3-2 is raw according to the received light beam of institute
At data information, it is transmitted to external computer system through computer control device 3-3, can be obtained probe source 1 and be radiated at
Transmitance on substrate 2-2, and computer system then uses existing routine data processing module.
As shown in figure 4, A-1 is that high transmittance changes transmittance curve before substrate is annealed；A-2 is that high transmittance changes substrate
Full annealing high-temperature-phase transmittance curve；B-1 is that low transmission changes transmittance curve before substrate is annealed；B-2 is low transmission
Change substrate full annealing high-temperature-phase transmittance curve；So-called high transmittance variation or low transmission variation generally refer to substrate
The opposite height that ultraviolet-visible light wavelength band transmitance changes before and after annealing.A-1 and A-2 is adopted by the embodiment of the present invention 1
With transmittance curve before and after the corresponding annealing of the substrate of high transmission change rate.
As shown in figure 5, T1Transmitance for the precursor before substrate annealing in probe source wavelength, Tn、Tn+1Exist for substrate
The transmitance of substrate in annealing process in probe source wavelength.
In the present embodiment 1, probe source 1 is the laser of 460nm, and the substrate 2-2 for implementing annealing is the transparent glass of 4mm thickness
Substrate is coated with mono-layer oxidized vanadium thermocolour smart membrane (G/VOx), atomic ratio V:O ≈ 1:2, i.e. x ≈ 2 on substrate 2-2.Annealing is real
Device 2 is applied to anneal in vacuum atmosphere.
N2 atmosphere is filled in vacuum infrared annealing furnace, and test substrate 2-2 precursor film and annealing after between film layer
Transmitance calculates difference DELTA T=18.24%.Annealing process prison is carried out as probe source 1 using the laser of wavelength 460nm
Control, after beam expander lens group 1-3 is expanded, the light intensity power density for reaching the film surface of substrate 2-2 reaches laser
4mw.Before annealing, it is radiated in precursor film layer by implementing this light intensity first and then carries out spectrum test, show
Probe source does not cause crystallization to film layer.
It is put into substrate 2-2 in annealing implementing device 2, opens infra-red radiation fluorescent tube, and open annealing monitoring system, data
Intra-record slack byte time 1s, initial transmission T1=31.5%.It anneals 60s or so transmitance significant change, transmitance tends to after 65s
Stably reach Tn=12.3%, with TnAdjacent latter transmitance Tn+1=12.09%, with Tn+1Adjacent latter transmitance Tn+2=
12.44%, adjacent transmitance change rate is less than 5% or Δ Tn>=0.8 Δ T, therefore, the after the unlatching of infra-red radiation fluorescent tube
68s can close infra-red radiation fluorescent tube and substrate 2-2 is moved away from annealing heat source 2-1, obtain the vanadium oxide membrane with phase transition function
The substrate 2-2 of layer.
Embodiment 2:
The present embodiment 2 difference from example 1 is that, in the present embodiment 2, the wavelength of probe source 1 is 1064nm,
The light intensity power density for reaching the film surface of substrate 2-2 is 0.2mw.Initial transmission T1=49.69%, Δ T=35.7%,
Transmitance after annealing 63s, which tends towards stability, reaches Tn=15.21%, Tn+1=15.09%, Tn+2=15.38%, adjacent transmission
Rate change rate is less than 5% or Δ Tn≥0.8ΔT.Therefore, infrared spoke can be closed after 65s after the unlatching of infra-red radiation fluorescent tube
Substrate 2-2 is simultaneously moved away from annealing heat source 2-1 by shot-light pipe, obtains the substrate 2-2 with the vanadium oxide film layer of phase transition function.
Embodiment 3:
The present embodiment 3 difference from example 1 is that, in the present embodiment 3, the wavelength of probe source 1 is 2000nm,
It is the bandpass filter near 2000nm that probe source reception device 3, which is equipped with specification, reaches the light intensity of the film surface of substrate 2-2
Power density is 2mw.Initial transmission T1=64.58%, Δ T=58.49%, the transmitance after the 68s that anneals tend towards stability and reach
To Tn=13.01%, Tn+1=8.25%, Tn+2=7.19%, adjacent transmitance change rate is less than 5% or Δ Tn≥0.8ΔT。
Therefore, infra-red radiation fluorescent tube can be closed after 68s after the unlatching of infra-red radiation fluorescent tube and substrate 2-2 is moved away from annealing heat source 2-
1, obtain the substrate 2-2 with the vanadium oxide film layer of phase transition function.
Embodiment 4:
The present embodiment 4 and embodiment 3 the difference is that, the vanadium oxide of the surface deposition of the substrate 2-2 of the present embodiment 4
Atomic ratio the V:O ≈ 1:2.5, i.e. x ≈ 2.5 of film layer.Annealing implementing device 2 is being filled with H of the content for 4%2Atmosphere in carry out
Reproducibility annealing.The light intensity power density for reaching the light beam of the film surface of substrate 2-2 is 5mw.Initial transmission T1=
77.38%, Δ T=65.44%, the transmitance after the 92s that anneals tend towards stability and reach Tn=13.31%, Tn+1=13.2%, Tn+2
=13.21%, adjacent transmitance change rate is less than 5% or Δ Tn≥0.8ΔT.Therefore, the after the unlatching of infra-red radiation fluorescent tube
Infra-red radiation fluorescent tube can be closed after 94s and substrate 2-2 is moved away from annealing heat source 2-1, obtain the vanadium oxide with phase transition function
The substrate 2-2 of film layer.
Embodiment 5
The present embodiment 5 and embodiment 3 the difference is that, the vanadium oxide of the surface deposition of the substrate 2-2 of the present embodiment 5
Atomic ratio the V:O ≈ 1:1.6, i.e. x ≈ 1.6 of film layer.Annealing implementing device 2 is annealed in atmospheric environment.Initial transmission
T1=31.22%, Δ T=27.13%, the transmitance after the 55s that anneals tend towards stability and reach Tn=5.10%, Tn+1=4.88%,
Tn+2=4.75%, adjacent transmitance change rate is less than 5% or Δ Tn≥0.8ΔT.Therefore, after the unlatching of infra-red radiation fluorescent tube
Infra-red radiation fluorescent tube can be closed after 55s and substrate 2-2 is moved away from annealing heat source 2-1, obtain the oxidation with phase transition function
The substrate 2-2 of vanadium film layer.
Embodiment 6:
The present embodiment 6 and embodiment 3 the difference is that, the surface of the substrate 2-2 of the present embodiment 6 is sequentially depositing nitridation
Silicon, vanadium oxide film layer and silicon nitride film layer, i.e. G/SiNx/VOx/SiNx.Annealing implementing device 2 is moved back in atmospheric environment
Fire.Initial transmission T1=43.11%, Δ T=37.22%, the transmitance after the 45s that anneals tend towards stability and reach Tn=5.21%,
Tn+1=4.98%, Tn+2=4.81%, adjacent transmitance change rate is less than 5% or Δ Tn≥0.8ΔT.Therefore, in infrared spoke
Infra-red radiation fluorescent tube can be closed after 48s after shot-light pipe is opened and substrate 2-2 is moved away from annealing heat source 2-1, and obtaining has phase
Become the substrate 2-2 of the vanadium oxide film layer of function.
Embodiment 7:
The present embodiment 7 and embodiment 3 the difference is that, the surface of the substrate 2-2 of the present embodiment 7 is sequentially depositing to be formed
Following film layer structure: G/SiNx/NiCr/NiCrOx/VOx/NiCrOx/NiCr/SiNx.Reach the film surface of substrate 2-2
Light beam light intensity power density be 20mw.Initial transmission T1=39.67%, Δ T=30.42%, anneal 40s after transmission
Rate, which tends towards stability, reaches Tn=9.98%, Tn+1=9.79%, Tn+2=10.01%, adjacent transmitance change rate less than 5% or
ΔTn≥0.8ΔT.Therefore, infra-red radiation fluorescent tube can be closed after 43s after the unlatching of infra-red radiation fluorescent tube and by substrate 2-2
It is moved away from annealing heat source 2-1, obtains the substrate 2-2 with the vanadium oxide film layer of phase transition function.
Embodiment 8:
Utilize the specific steps of thermocolour smart membranes crystallization degree in the monitoring system real time monitoring annealing process of embodiment 1
Are as follows:
1, the substrate of the coating thermocolour smart membranes not yet made annealing treatment is placed on laser and probe source connects
It receives between probe；Start laser, the light for allowing laser to issue penetrates substrate and detected light source receiving transducer receives, and detects light
Source receiving transducer will transmit through rate and be transmitted to computer system；The light that writing laser is issued penetrates the initial transmission of substrate
T1；
2, by finished product, that is, the substrate of the coating thermocolour smart membranes made annealing treatment is placed on laser and detection light
Between the receiving transducer of source；Start laser, the light for allowing laser to issue penetrates substrate and detected light source receiving transducer receives, and visits
Survey light source receiving transducer will transmit through rate and be transmitted to computer system；Record the transmitance changing value Δ T after annealing is finally completed；
3, the substrate for coating thermocolour smart membranes is sent into annealing implementing device and is made annealing treatment；
4, starting is in the laser within the scope of annealing implementing device, and the light that laser issues penetrates substrate and detected light
Source receiving transducer receives, and the real-time transmitance of substrate is transmitted to computer system, writing laser by probe source receiving transducer
The light issued penetrates the real-time transmitance T of substraten；
5, compare TnWith T1Difference, calculate Δ Tn=T1-Tn；
6, to TnKeep stable or Δ Tn>=0.8 Δ T, monitoring system issue instruction and close annealing heat source or substrate is mobile
To outside annealing heat source.
Glass substrate used by above-described embodiment is the tempered glass substrate of 4mm, the damage of the tempering stress after annealing
Consumption is smaller, and final result can satisfy the requirement of the tempering stress intensity of building energy conservation industry.Its heating for radiating fluorescent tube
Time can control within the time in seconds, and the energy that can preferably reduce the radiation fluorescent tube in annealing process disappears
Consumption is realized energy-saving.
Thickness, probe source wavelength, the probe source light intensity power of relevant embodiment glass substrate are close in examples detailed above
Degree is not intended as specifically limiting, as long as can implement annealing in annealing device, probe source can detect substrate
The variation of transmitance in annealing process and be unlikely to induce film layer crystallization then light intensity can all use, actual light
By force may light intensity more preferable than effect in embodiment it is big or small.Its same film layer structure, relevant transmitance coefficient of comparisons is also simultaneously
The non-restriction as in the present invention.As long as meeting the annealing process comprising single layer or multilayer complex films including vanadium oxide film layer
Monitoring is all contained in the monitoring test macro of annealing described in the invention.
Claims (8)
1. a kind of monitoring system of thermocolour smart membranes annealing, it is characterized in that: including annealing implementing device, at least one detection light
Source and at least one probe source reception device corresponding with the probe source；Direction of advance along light beam is in the detection light
The end in source, which is equipped with, collimates anti-tampering pipe, and the end of the anti-tampering pipe of collimation is formed with probe source limit light aperture, the standard
Beam expander component is installed in straight anti-tampering pipe；Be equipped in the annealing implementing device substrate coated with thermocolour smart membranes and
Substrate heat and is located at the annealing heat source above thermocolour smart membranes；The probe source reception device includes receiving to visit
Head and computer system, the receiving transducer are connect with computer system data；The probe source is in thermocolour smart membranes
Above or below, when the probe source is in the top of thermocolour smart membranes, the wave band of the probe source is moved back with described
The wave band in burning hot source is staggered or the receiving transducer front end be provided with for probe source can by narrow-band optical filter；
The light beam that the probe source issues is radiated on substrate, which penetrates substrate and received by the receiving transducer, then institute
State receiving transducer and the transmitance that the light beam penetrates substrate be transmitted to computer system, the computer system to the transmitance into
Row data processing generates the control signal of a working condition for controlling annealing implementing device, control annealing implementing device
Working condition.
2. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 1, it is characterized in that: the annealing heat source
It is any heat source of laser, infra-red radiation fluorescent tube, halogen lamp tube, iodine-tungsten lamp fluorescent tube.
3. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 1, it is characterized in that: the probe source
Optical wavelength in ultraviolet to close within the scope of infrared band.
4. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 3, it is characterized in that: the probe source
It is light source of the optical wavelength near infrared band.
5. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 1, it is characterized in that: the probe source
It is any one of xenon lamp, halogen lamp and laser.
6. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 1, it is characterized in that: the beam expander
Component is made of muti-piece with beam expander effect and/or the optical element pretended with uniform light, and the beam expander
Component is between probe source and probe source limit light aperture.
7. the monitoring system of a kind of thermocolour smart membranes annealing according to claim 1, it is characterized in that: the probe source
For the light beam of sending after beam expander component expands, the power density of the light beam is 0.2mw~20mw.
8. a kind of method for the monitoring system monitoring annealing process annealed using thermocolour smart membranes described in claim 1,
It is characterized in: the specific steps are that:
1) substrate for coating thermocolour smart membranes is placed between probe source and probe source reception device；Probe source hair
Light out penetrates substrate and detected light source receiving device receives, and receiving transducer will transmit through rate and be transmitted to computer system, record
The light that probe source is issued penetrates the initial transmission T of substrate1；
2) substrate for coating thermocolour smart membranes is sent into annealing implementing device；Annealing heat source heats substrate, carries out to substrate
Annealing；The substrate of annealing is monitored in real time, the light that probe source issues penetrates substrate and detected light source connects
It is received by device, real-time transmitance is transmitted to computer system by receiving transducer, and the light that record probe source is issued penetrates base
The real-time transmitance T of piecen；
3) compare TnWith T1Difference, calculate Δ Tn=T1-Tn；
4) to TnKeep stable or Δ Tn>=0.8 Δ T closes annealing heat source or substrate is moved to outside annealing heat source；Δ T is to move back
The substrate transmitance changing value of fiery front and back.
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| 《退火温度对二氧化钒薄膜红外透过率的影响》;殷智勇等;《INFRARED》;20090610;第30卷(第6期);第1-3页 * |
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