CN105136047B - The apparatus and method of in site measurement change in film thickness - Google Patents
The apparatus and method of in site measurement change in film thickness Download PDFInfo
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- CN105136047B CN105136047B CN201510284769.5A CN201510284769A CN105136047B CN 105136047 B CN105136047 B CN 105136047B CN 201510284769 A CN201510284769 A CN 201510284769A CN 105136047 B CN105136047 B CN 105136047B
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Abstract
The invention discloses a kind of apparatus and method of in site measurement change in film thickness, wherein equipment includes sample stage, lasing light emitter and laser detector, the sample stage carries testing sample, the lasing light emitter sends beam of laser, the second beam laser is radiated at the film surface and substrate surface of testing sample respectively, the laser detector receives the change of the position difference by the beam of laser of testing sample reflection and the second beam laser, the calculating film surface and substrate surface vertical direction, so as to obtain the thickness change of film.
Description
Technical field
The present invention relates to thin-film material technical field, more particularly to a kind of in the heat treatment process of chemical solution deposition
The apparatus and method of in site measurement change in film thickness.
Background technology
Chemical solution deposition technique (Chemical Solution Deposition) is prepared in a kind of chemically solution
The method of thin-film material, mainly including common methods such as sol-gel process, deposition of metal organic method, homogeneous co-precipitation process.Change
Film stoichiometry ratio can be accurately controlled by learning solution deposition techniques, required relatively low to the size and dimension of substrate, obtained
Uniformity of film is preferable, and the particularly technology has significant low-cost advantage due to that need not use vacuum equipment, therefore
It is widely used in field of film preparation.
The process that chemical solution deposition technique prepares film generally comprises following three steps:The preparation of precursor aqueous solution, incite somebody to action
Precursor aqueous solution is coated in the heat treatment that precursor film, precursor film are formed in substrate.Wherein, can first in precursor film in heat treatment process
The complicated change such as substance decomposition, air accumulation and the diffusions such as the volatilization of generation solvent, organic matter, therefore be easy to produce film planted agent
Power, when the compression or excessive tension in film, there is harmful pattern such as fold or cracking corresponding to meeting, cause film
Performance is badly damaged.Therefore among the heat treatment of chemical solution deposition technique, the analysis and research to stress source have very much must
Will.
In this research, the situation of change that film thickness in heat treatment process is investigated in original position is significant.Thin
In the evaporating deposition technique of film preparation, there is the in-situ technique of a variety of change in film thickness, these technologies are all based on film and existed
There is the premise of uniform and stable physical property, by entering to a certain physical quantity (such as reflectivity, resonant frequency) in deposition process
Row in site measurement, the situation of change of film thickness can effectively be calculated.However, in chemical solution deposition heat treatment process
In, due to occurring that the composition transfer of complexity, air accumulation cause hole, substance decomposition and loss etc. inside film, cause thin
The physical property of film changes always in heat treatment process, so that existing thickness measurement technique in situ can not use.
Some researchers pass through the technique study thickness for measurement of offing normal using the method at different temperatures quenching film
Situation of change in heat treatment process, but because quenching process can also cause the change of thickness in itself, therefore can cause to tie
Disputed on by existing.For example, in the Yt-Ba-Cu-O high-temperature superconductive film preparation research that Japanese ISTEC is carried out, heat treatment initial stage is found
Phenomenon (Physica C, 2008,468 (14) of film thickness expansion occur:1017.);And ground in the similar of Spain ICMB
The result of film expansion is then not measured by studying carefully, has only measured the monotonic decreasing (Chemistry of film thickness during this
of Materials,2006,18(25):5897.).Due to that can not determine that thickness swelling whether there is, cause the pressure of buckling phenomena
Whether stress source is related to air accumulation can not also to determine, the further investigation to this area constitutes apparent obstacle.
The disclosure of upper background technology content is only used for inventive concept and the technical scheme that auxiliary understands the present invention, and it is not necessarily
So belong to the prior art of present patent application, no tangible proof show the above present patent application the applying date
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
(main) purpose of the invention is to propose a kind of apparatus and method of in site measurement change in film thickness, with solution
State the low technical problem of accuracy of measurement existing for prior art.
Therefore, the present invention proposes that a kind of heat treatment process situ in chemical solution deposition measures change in film thickness
Equipment, including sample stage, lasing light emitter and laser detector, the sample stage carry testing sample, and the lasing light emitter sends first
Shu Jiguang, the second beam laser are radiated at the film surface and substrate surface of testing sample respectively, and the laser detector receives quilt
The beam of laser of testing sample reflection and the second beam laser, the position for calculating the film surface and substrate surface vertical direction
The change of difference, so as to obtain the thickness change of film.
The equipment of change in film thickness is measured in the heat treatment process situ of chemical solution deposition also includes cavity, described
Atmosphere is controllable in cavity.
The beam of laser, the second beam laser are less than 3 millimeters in the hot spot of sample surfaces without overlapping region, spot size
× 3 millimeters of scopes.
The laser detector is applicable trigonometry, and the laser detector separately detects the beam of laser and second of reflection
The displacement of facula positions of the Shu Jiguang on laser detector, so as to calculate the change in location situation that two beam laser reflect,
And then obtain the alternate position spike value changes of film surface and exposed substrate surface in vertical direction.
The laser detector is applicable interferometric method, and the laser detector detects the beam of laser, the second beam laser
Between interference information, calculate the beam of laser, the optical path difference situation of change of the second beam laser, and then entering using laser
Penetrate the alternate position spike value changes of film surface described in angle calculation and substrate surface vertical direction.
A kind of method that heat treatment process situ in chemical solution deposition measures change in film thickness, including following step
Suddenly:Testing sample is placed on sample stage;Lasing light emitter sends beam of laser, the second beam laser is radiated at testing sample respectively
Film surface and substrate surface;Laser detector is received by the beam of laser of testing sample reflection, the second beam laser, calculated
In the alternate position spike value changes of the film surface and substrate surface vertical direction so as to obtaining the thickness change of film.
The method of change in film thickness is measured in the heat treatment process situ of chemical solution deposition also includes selection properly
Temperature variation curve the testing sample is heat-treated with corresponding atmosphere.
Testing sample can obtain exposed substrate surface in the following ways:Control precursor aqueous solution coating scope makes to be measured
The part of sample substrate is not coated with;Or the part of testing sample substrate is covered with mask before coating and removed after application
Mask exposes substrate surface;Or corrode a part of film after application to expose substrate surface.
Also include the thickness variation with temperature situation for counting the film, obtain change in film thickness in site measurement most
Terminate fruit.
The laser detector obtains film surface and the substrate surface vertical direction using trigonometry or interferometric method
Alternate position spike value changes.
The beneficial effect that the present invention is compared with the prior art includes:The equipment of the in site measurement change in film thickness of the present invention
With method can efficiently and accurately change in film thickness in site measurement chemical solution deposition heat treatment process, have very bright
True significance of scientific research and application value.
Brief description of the drawings
Fig. 1 is the structural representation of the equipment of the in site measurement change in film thickness of the present invention.
Fig. 2 is the sample structural representation in the embodiment of the present invention 1, the sample have simultaneously film surface and
Exposed substrate surface.
Fig. 3 is the heat treatment cycle curve of the embodiment of the present invention 1.
Fig. 4 is the triangulation schematic diagram being related in the embodiment of the present invention 1.
Fig. 5 is the interferometric method measuring principle figure being related in the embodiment of the present invention 1.
Embodiment
With reference to embodiment and compare accompanying drawing the present invention is described in further detail.It is emphasized that
What the description below was merely exemplary, the scope being not intended to be limiting of the invention and its application.
With reference to the following drawings, non-limiting and nonexcludability embodiment will be described, wherein identical reference represents
Identical part, unless stated otherwise.
It would be recognized by those skilled in the art that it is possible that numerous accommodations are made to above description, so embodiment is only
For describing one or more particular implementations.
Embodiment 1
As shown in figure 1, the equipment that a kind of heat treatment process situ in chemical solution deposition measures change in film thickness,
Including sample stage 1, lasing light emitter and laser detector 3, sample stage 1 carries testing sample 2, and lasing light emitter sends beam of laser 4, the
Two beam laser 5 are radiated at the film surface and substrate surface of testing sample 2 respectively, and laser detector 3 receives anti-by testing sample 2
The beam of laser 4 penetrated, the second beam laser 5, calculate the alternate position spike value changes of film surface and substrate surface vertical direction so as to
Obtain the thickness change of film.
The equipment that change in film thickness is measured in the heat treatment process situ of chemical solution deposition also includes cavity, chamber
Internal atmosphere is controllable.Fig. 1 essentially describes the internal structure of the controllable cavity of atmosphere, the shell mechanism of closed cavity
And it is not drawn into.
Beam of laser 4, the second beam laser 5 sample surfaces hot spot without overlapping region, spot size be less than 3 millimeters ×
3 millimeters of scopes.
Testing sample 2 is fixed on the sample stage 1 in cavity, and the temperature of sample stage 1 is in room temperature to can in the range of 1000 DEG C
Control.The beam of laser 4 that introduces in cavity, the second beam laser 5 are radiated at two positions on the surface of testing sample 2 respectively, and first
Shu Jiguang 4, the second beam laser 5 are less than 3 millimeters × 3 millimeters scopes in the hot spot of sample surfaces without overlapping region, spot size.The
Beam of laser 4, the reflected beams of the second beam laser 5 can be detected by laser detector 3, and laser detector 3 can detect
Facula position of the reflection laser on laser detector 3, or can detect dry between beam of laser 4, the second beam laser 5
Relate to information.
In one case, if detecting hot spot position of the reflection laser on laser detector 3 using laser detector 3
Put, then beam of laser 4, the displacement feelings for the position that the second beam laser 5 reflects can be calculated respectively according to trigonometry principle
Condition, and then obtain the alternate position spike value changes of film surface and exposed substrate surface in vertical direction.
In another case, if detected using laser detector 3 dry between beam of laser 4, the second beam laser 5
Information is related to, then beam of laser 4, the change of the optical path difference of the second beam laser 5 can be calculated, and then utilize according to interferometric method principle
The incident angle of laser calculates the alternate position spike value changes of film surface and substrate surface vertical direction.
A kind of method that heat treatment process situ in chemical solution deposition measures change in film thickness, including following step
Suddenly:Testing sample 2 is placed on sample stage 1;Lasing light emitter sends beam of laser 4, the second beam laser 5 be radiated at respectively it is to be measured
The film surface and substrate surface of sample 2;Laser detector 3 receives the beam of laser 4 reflected by testing sample 2, the second beam
Laser 5, calculate in the alternate position spike value changes of film surface and substrate surface vertical direction so as to obtain the thickness change of film.
Specifically, the method for measuring change in film thickness in the heat treatment process situ of chemical solution deposition, including such as
Lower step:
(S1) precursor aqueous solution is coated in substrate, controls coating procedure or handled after application, have testing sample 2
Standby film surface and exposed substrate surface.
In the present patent application, film needs to prepare using chemical solution deposition method.In the present embodiment, use
Prepared by this method is Yt-Ba-Cu-O high-temperature superconductive film, and its precursor aqueous solution composition includes yttrium acetate, barium acetate, copper acetate, three
Fluoroacetic acid, methanol, polyethylene glycol.
In step sl, used substrate can possess minute surface even curface property, so as to reflection laser beam.At this
In embodiment, the substrate used is the lanthanuma luminate single crystal of polishing, and its surface undulation is only atomic scale, therefore with flat well
Whole degree.
In step sl, the film surface for coating to obtain also has due to the surface tension effects of precursor aqueous solution, its surface
The characteristics of minute surface is smooth.Coating procedure can use spin coating (spin-coating), dip-coating (dip-coating), slot coated
The mode such as (slot-die coating) and spraying printing (ink-jet printing).In the present embodiment, dip-coating side is used
Formula.
In order that testing sample 2 is provided simultaneously with film surface and exposed substrate surface, following several ways can be used:
Control precursor aqueous solution coating scope makes the part of substrate be not coated with or before coating cover the local of substrate simultaneously with mask
Mask is removed after application exposes substrate surface or coating a part of film of post-etching to expose substrate surface.The present embodiment
In, using first way, by controlling the depth of substrate immersion precursor aqueous solution in dip coating process, make a part of surface of substrate
It is not coated with, the structural representation of testing sample 2 finally obtained is as shown in Figure 2.
(S2) testing sample 2 is fixed on temperature with the controllable sample stage of atmosphere, selecting suitable temperature change
Curve and corresponding atmosphere, carry out heat treatment process.
In step s 2, according to it is required prepare film corresponding to heat treatment condition selection temperature curve and atmosphere, need
Ensure to make film be always maintained at minute surface even curface feature in heat treatment process.In the present embodiment, the temperature used
The name in curve and wherein each stage is as shown in Figure 3.The thermal decomposition stage uses is used as atmosphere by the high pure oxygen washed, and burns
The knot stage uses the oxygen-nitrogen mixture for passing through and washing, and wherein oxygen content is 100ppm, and oxygenation and stove cold stage use drying
High pure oxygen.Film surface remains the characteristics of minute surface is smooth in the present embodiment, such as the film surface of qtenched sample at 400 DEG C
Pattern, the scanning range of AFM measurement is 50 microns × 50 microns, measures obtained surface roughness RqValue is only
0.7nm, illustrate that its surface is very smooth.The film thickness of testing sample 2 is in heat treatment process without departing from 100 nanometers to 100
The scope of micron.
(S3) in heat treatment process, laser beam is reflected respectively in film surface and substrate surface, obtain two surfaces
In the thickness change of the alternate position spike value changes, i.e. film of vertical direction.
In step s3, using laser beam oblique incidence, reflect, obtain in film surface and exposed substrate surface respectively
Two surfaces can use trigonometry or interferometric method in the method for vertical direction alternate position spike value changes.
During using trigonometry, the oblique fire formula principle of triangulation figure in Fig. 4 is may be referred to, and following principles illustrated is entered
Row measurement analysis.What is reflected in Fig. 4 is the principle that reflection position displacement on a measured surface is measured using beam of laser, wherein
41 be laser, and 42 be convergent lens, and 43 be measured surface, and 44 be receiving lens, and 45 be CCD photoelectric detector, a and b difference
For the object distance and image distance of receiving lens, the folder of incident laser and measured surface normal, receiving lens axis and measured surface normal
Angle is both configured to θ.When measured surface 43 is there occurs during displacement x as depicted, facula position of the reflection laser on CCD is corresponding
Y can be subjected to displacement, according to image-forming principle triangle geometrical relationship as depicted, there is following approximate function between x and y:
Using the above method, two can be calculated respectively according to the displacement of two beam reflection laser facula positions on CCD
The misalignment of measured surface, by the displacement calculating difference on two surfaces, you can obtain the situation of change of film thickness.
During using interferometric method, the interferometric method measuring principle figure in Fig. 5 is may be referred to, and following principles illustrated is surveyed
Amount analysis.The beam of laser (wavelength X) for sending laser first by light splitting optical path in this method is divided into coherence's
Two beam laser, reflect in film surface and exposed substrate surface respectively, and incident angle is all θ, uses laser detector
The interference information of two beam reflection lasers can be obtained.When the two optical path difference is the even-multiple of half-wavelength, bright fringes, reflection are formed
It is exactly crest on oscillograph;When the two optical path difference is the odd-multiple of half-wavelength, dark fringe is formed, is reflected in showing for detector
It is exactly trough on ripple device;When optical path difference is there occurs the change of a wavelength X, a complete ripple now just occurs on oscillograph
The spike paddy cycle.If measuring N number of Wave crest and wave trough cycle on oscillograph, two reflecting surfaces can be obtained in vertical direction
Alternate position spike change x be:
Measured in the present embodiment using trigonometry.
(S4) film thickness variation with temperature situation is counted, obtains the final result of change in film thickness in site measurement.
In step s 4, film thickness variation with temperature situation in chemical solution heat treatment process can be obtained, so as to
It can be used for analyzing the reaction of film internal chemical, air accumulation and the information such as diffusion.Testing sample 2 in present patent application
Scope of the film thickness in heat treatment process without departing from 100 nanometers to 100 microns.
Embodiment 2:
The present embodiment uses equipment same as Example 1, and it is thin that in site measurement chemical solution deposition method prepares cerium oxide
Thickness change situation in membrane process, the composition of precursor aqueous solution include cerous nitrate, acetylacetone,2,4-pentanedione, ethylene glycol monoemethyl ether etc., heat
Treatment conditions are:400 DEG C are warming up to from room temperature with 2 DEG C/min, then 1000 DEG C are warming up to 5 DEG C/min, atmosphere control
Mixed for hydrogen with argon gas, wherein the volume fraction of hydrogen is 4%.Others prepare same as Example 1 with measuring condition.
Embodiment 3:
The present embodiment uses equipment same as Example 1, and it is thin that in site measurement chemical solution deposition method prepares strontium titanates
Thickness change situation in membrane process, the composition of precursor aqueous solution are only including strontium acetate, butyl titanate, acetylacetone,2,4-pentanedione, ethylene glycol
Methyl ether, acetic acid, ethylene glycol etc., heat treatment condition are:450 DEG C are warming up to from room temperature with 2 DEG C/min, then with 10 DEG C/min of heatings
To 950 DEG C, atmosphere is air.Others prepare same as Example 1 with measuring condition.
Compared to the prior art of in site measurement change in film thickness, present patent application need not be by measuring the thing of film
Rationality matter is to calculate its thickness change, so as to overcome internal component and physics in the chemical solution deposition heat treatment process of film
Property does not stop the obstacle of change;In addition, obtained by the alternate position spike value changes measured between film surface and exposed substrate surface
Thickness change is obtained, the influence that the deformation band that sample stage occurs in heat treatment process comes can be eliminated.Therefore, present patent application can
Effectively to carry out in site measurement to the situation of change of film thickness in heat treatment process.
Present patent application proposition is a kind of can to carry out thickness change original in the chemical solution deposition heat treatment process of film
The apparatus and method of position measurement, it makes testing sample 2 possess film surface and exposed substrate surface, is existed respectively using laser beam
The reflection of two surfaces, by obtaining two surfaces in the alternate position spike value changes of vertical direction, obtain the thickness change of film.This is specially
In profit application, the substrate surface used has the characteristics of minute surface is smooth, and film surface also keeps minute surface to put down in heat treatment process
It is whole, testing sample 2 is fixed on the sample stage that can control temperature and atmosphere, design temperature change curve with it is corresponding
Atmosphere carries out heat treatment process, can carry out in site measurement to change in film thickness in the process.Surveyed compared to original position
The prior art of change in film thickness is measured, present patent application need not calculate that its thickness becomes by measuring the physical property of film
Change, so as to overcome the obstacle that internal component and physical property in the chemical solution deposition heat treatment process of film do not stop change.
In addition, obtaining thickness change by measuring the alternate position spike value changes between film surface and exposed substrate surface, can eliminate
The influence that the deformation band that sample stage occurs in heat treatment process comes.Therefore, present patent application can have in heat treatment process
Effect ground carries out in site measurement to the situation of change of film thickness.
Chemical solution deposition heat treatment process initial film is generally gel mould, has certain mobility, and the present invention adopts
Measured with non-contacting method, ensured the feasibility of measurement.Meanwhile in the film application process of chemical solution deposition by
In the surface tension effects of precursor aqueous solution, the film surface for coating to obtain has the characteristics of minute surface is smooth, and heat treated
By controlling the parameters such as suitable heating rate, atmosphere in journey, film can be made to be always maintained at minute surface even curface spy
Point, therefore there is high accuracy to film surface position progress non-cpntact measurement using the present invention.
Further, since the sample stage of fixed testing sample 2 needs to be heated, the position of sample stage in itself is heat treated
Necessarily change in journey, so the change of measurement film surface position can not reflect the change feelings of film thickness merely
Condition, the present invention also measure simultaneously to the position of substrate surface, become so as to obtain film thickness using the difference on two surfaces
Change.The substrate surface used in present patent application also has the characteristics of minute surface is smooth, and pair has film surface and naked simultaneously
The sample of the substrate surface of dew has carried out accurate measurement.
Technical scheme provided by the invention can in the heat treatment process of accurate measurement chemical solution deposition film thickness with
The changing value of time.If after the measurement of the technical program terminates, using the method for measuring thickness offed normal (as used step
Instrument measures) obtain film thickness value, then it can further obtain the thickness value of random time in heat treatment process.
Although having been described above and describing the example embodiment for being counted as the present invention, it will be apparent to those skilled in the art that
It can be variously modified and replaced, without departing from the spirit of the present invention.Furthermore it is possible to many modifications are made with by spy
Condition of pledging love is fitted to the religious doctrine of the present invention, without departing from invention described herein central concept.So the present invention is unrestricted
In specific embodiment disclosed here, but the present invention all embodiments that may also include belonging to the scope of the invention and its equivalent
Thing.
Claims (7)
- A kind of 1. equipment that heat treatment process situ in chemical solution deposition measures change in film thickness, it is characterised in that: Including sample stage, lasing light emitter and laser detector, the sample stage carries testing sample, and the sample includes substrate and chemical solution Liquid deposits the film to be formed on the substrate, and the lasing light emitter sends beam of laser, the second beam laser is radiated at treats respectively The film surface of test sample product and exposed substrate surface, the laser detector receive the beam of laser reflected by testing sample With the second beam laser, the change for the position difference for calculating the film surface and substrate surface vertical direction, so as to obtain film Thickness change;The laser detector uses trigonometry, the laser detector separately detect reflection beam of laser and The displacement of facula position of the second beam laser on laser detector, so as to calculate the change in location feelings that two beam laser reflect Condition, and then obtain the alternate position spike value changes of film surface and exposed substrate surface in vertical direction;Or the laser acquisition Device uses interferometric method, and the laser detector detects the interference information between the beam of laser, the second beam laser, calculates institute Beam of laser, the optical path difference situation of change of the second beam laser are stated, and then the film table is calculated using the incident angle of laser Face and the alternate position spike value changes of substrate surface vertical direction.
- 2. measure setting for change in film thickness in the heat treatment process situ of chemical solution deposition as claimed in claim 1 It is standby, it is characterised in that:Also include cavity, atmosphere is controllable in the cavity.
- 3. measure setting for change in film thickness in the heat treatment process situ of chemical solution deposition as claimed in claim 1 It is standby, it is characterised in that:The beam of laser, the second beam laser are small without overlapping region, spot size in the hot spot of sample surfaces In 3 millimeters × 3 millimeters scopes.
- 4. a kind of method that heat treatment process situ in chemical solution deposition measures change in film thickness, it is characterised in that bag Include following steps:Testing sample is placed on sample stage, the sample includes substrate and chemical solution deposition is formed on the substrate Film;Lasing light emitter sends beam of laser, the second beam laser is radiated at the film surface of testing sample and exposed substrate table respectively Face;Laser detector receive by the beam of laser of testing sample reflection, the second beam laser, calculate in the film surface and For the alternate position spike value changes of substrate surface vertical direction so as to obtain the thickness change of film, the laser detector uses trigonometry Or interferometric method obtains the alternate position spike value changes of film surface and the substrate surface vertical direction.
- 5. as claimed in claim 4 chemical solution deposition heat treatment process situ measure change in film thickness side Method, it is characterised in that:Also include selecting suitable temperature variation curve to carry out the testing sample with corresponding atmosphere Heat treatment.
- 6. as claimed in claim 4 chemical solution deposition heat treatment process situ measure change in film thickness side Method, it is characterised in that:Testing sample can obtain exposed substrate surface in the following ways:Control precursor aqueous solution coating scope It is not coated with the part of testing sample substrate;Or the part mask of testing sample substrate is covered and coated before coating Mask is removed afterwards exposes substrate surface;Or corrode a part of film after application to expose substrate surface.
- 7. as claimed in claim 4 chemical solution deposition heat treatment process situ measure change in film thickness side Method, it is characterised in that:Also include the thickness variation with temperature situation for counting the film, obtain change in film thickness original position The final result of measurement.
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CN111964580B (en) * | 2020-07-30 | 2022-02-11 | 广东工业大学 | Device and method for detecting position and angle of film based on optical lever |
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