CN105136047A - Equipment and method for measuring change in thickness of film in situ - Google Patents
Equipment and method for measuring change in thickness of film in situ Download PDFInfo
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Abstract
The invention discloses a piece of equipment and a method for measuring the change in thickness of a film in situ. The equipment comprises a sample stage, a laser source, and a laser detector. The sample stage bears a sample to be measured. A first laser beam and a second laser beam emitted by the laser source are respectively irradiated on the surface of a film and the surface of a substrate of the sample to be measured. The laser detector receives the first laser beam and the second laser beam reflected by the sample to be measured, and calculates the change in the difference between the positions of the surface of the film and the surface of the substrate in the vertical direction, thus obtaining the change in thickness of the film.
Description
Technical field
The present invention relates to membraneous material technical field, particularly relate to equipment and method that a kind of heat treatment process situ at chemical solution deposition measures change in film thickness.
Background technology
Chemical solution deposition technique (ChemicalSolutionDeposition) is a kind of method preparing membraneous material in chemically solution, mainly comprises the common methods such as sol-gel process, deposition of metal organic method, homogeneous co-precipitation process.Chemical solution deposition technique can control film stoichiometry ratio accurately, require lower to the size and dimension of substrate, the uniformity of film obtained is better, particularly this technology has significant low-cost advantage owing to not needing to use vacuum equipment, and 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, precursor aqueous solution is coated in thermal treatment substrate being formed precursor film, precursor film.Wherein, first the complicated change such as substance decomposition, air accumulation and the diffusions such as solvent volatilization, organism can be there is in precursor film in heat treatment process, therefore be easy to produce film internal stress, when the compressive stress in film or tension excessive time, harmful patterns such as the appearance fold that meeting is corresponding or cracking, cause film performance to be badly damaged.Therefore, in the middle of the thermal treatment of chemical solution deposition technique, the analysis and research in counter stress source are necessary very much.
In this research, the situation of change that original position investigates film thickness in heat treatment process is significant.In the evaporating deposition technique of film preparation, there is the in-situ technique of multiple change in film thickness, these technology all based thin film have the prerequisite of uniform and stable physical property in deposition process, by carrying out in site measurement to a certain physical quantity (as reflectivity, resonance frequency etc.), the situation of change of film thickness effectively can be calculated.But, in chemical solution deposition heat treatment process, the composition transfer, the air accumulation that there will be complexity because film is inner cause hole, substance decomposition and loss etc., cause the physical property of film to change in heat treatment process always, thus existing original position thickness measurement technique cannot be used.
Some researcher uses at different temperatures by the method that film quenches, and by the situation of change of technique study thickness in heat treatment process measured of offing normal, but also can cause the change of thickness due to quenching process itself, and conclusion therefore can be caused to there is dispute.Such as, in the Yt-Ba-Cu-O high-temperature superconductive film preparation research that Japanese ISTEC carries out, find that the thermal treatment initial stage there will be the phenomenon (PhysicaC, 2008,468 (14): 1017.) of film thickness expansion; In the similar research of Spain ICMB, then do not measure the result of film expansion, only measure the monotonic decreasing (ChemistryofMaterials, 2006,18 (25): 5897.) of film thickness in this process.Owing to cannot determine whether thickness swelling exists, cause the compressive stress of buckling phenomena to be originated and whether relevantly to air accumulation also cannot to determine, obstacle is clearly constituted to the further investigation of this area.
Disclosing only for auxiliary understanding inventive concept of the present invention and technical scheme of upper background technology content, it must not belong to the prior art of present patent application, show that not having tangible proof the applying date of foregoing in present patent application is in disclosed situation, above-mentioned background technology should not be used for novelty and the creativeness of evaluating the application.
Summary of the invention
The present invention (mainly) object is the equipment and the method that propose a kind of in site measurement change in film thickness, with the technical matters that the accuracy of measurement solving the existence of above-mentioned prior art is low.
For this reason, the present invention proposes the equipment that a kind of heat treatment process situ at chemical solution deposition measures change in film thickness, comprise sample stage, lasing light emitter and laser detector, described sample stage carrying testing sample, described lasing light emitter sends beam of laser, the second bundle laser is radiated at testing sample respectively film surface and substrate surface, the beam of laser and second that described laser detector receives by testing sample reflects is restrainted laser, is calculated the change of the position difference of described film surface and substrate surface vertical direction, thus obtains the variation in thickness of film.
The equipment measuring change in film thickness at the heat treatment process situ of chemical solution deposition also comprises cavity, and in described cavity, atmosphere is controlled.
Described beam of laser, second restraints the hot spot of laser at sample surfaces without overlapping region, and spot size is less than 3 millimeters × 3 millimeters scopes.
Described laser detector is suitable for trigonometry, described laser detector detects the beam of laser of reflection and the displacement of the facula position of the second bundle laser on laser detector respectively, thus calculate the change in location situation that reflection occurs two bundle laser, and then obtain film surface and the position difference change in the vertical direction of exposed substrate surface.
Described laser detector is suitable for interferometric method, interference information between the described beam of laser of described laser detector detection, the second bundle laser, calculate the optical path difference situation of change of described beam of laser, the second bundle laser, and then utilize the incident angle of laser to calculate the position difference change of described film surface and substrate surface vertical direction.
Measure a method for change in film thickness at the heat treatment process situ of chemical solution deposition, comprise the steps: testing sample to be placed on sample stage; Lasing light emitter sends beam of laser, the second bundle laser is radiated at testing sample respectively film surface and substrate surface; Laser detector receive reflected by testing sample beam of laser, the second bundle laser, calculate the position difference change in described film surface and substrate surface vertical direction thus obtain the variation in thickness of film.
Also comprising in the method for the heat treatment process situ measurement change in film thickness of chemical solution deposition selects suitable temperature variation curve and corresponding atmosphere to heat-treat described testing sample.
Testing sample can obtain exposed substrate surface in the following ways: control precursor aqueous solution coating scope and make the local of testing sample substrate not coated; Or before coating the local mask of testing sample substrate is covered and remove mask after application and expose substrate surface; Or corrode a part of film after application to expose substrate surface.
Also comprise the thickness variation with temperature situation of adding up described film, obtain the net result of change in film thickness in site measurement.
Described laser detector uses trigonometry or interferometric method to obtain the position difference change of described film surface and substrate surface vertical direction.
The beneficial effect that the present invention is compared with the prior art comprises: the equipment of in site measurement change in film thickness of the present invention and method can change in film thickness in site measurement chemical solution deposition heat treatment process efficiently and accurately, have very clear and definite significance of scientific research and using value.
Accompanying drawing explanation
Fig. 1 is the structural representation of the equipment of 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, and this sample has film surface and exposed substrate surface simultaneously.
Fig. 3 is the heat treatment cycle curve of the embodiment of the present invention 1.
Fig. 4 is the triangulation schematic diagram related in the embodiment of the present invention 1.
Fig. 5 is the interferometric method measuring principle figure related in the embodiment of the present invention 1.
Embodiment
Contrast accompanying drawing below in conjunction with embodiment the present invention is described in further detail.It is emphasized that following explanation is only exemplary, instead of in order to limit the scope of the invention and apply.
With reference to the following drawings, will describe the embodiment of non-limiting and nonexcludability, wherein identical Reference numeral represents identical parts, unless stated otherwise.
Those skilled in the art will recognize that, it is possible for making numerous accommodation to above description, so embodiment is only used to describe one or more particular implementation.
Embodiment 1
As shown in Figure 1, a kind of heat treatment process situ at chemical solution deposition measures the equipment of change in film thickness, comprise sample stage 1, lasing light emitter and laser detector 3, sample stage 1 carries testing sample 2, lasing light emitter sends beam of laser 4, second and restraints laser 5 and be radiated at film surface and the substrate surface of testing sample 2 respectively, and laser detector 3 receives and restrainted laser 5 by the beam of laser 4, second that testing sample 2 reflects, calculate the position difference change of film surface and substrate surface vertical direction thus obtain the variation in thickness of film.
Also should comprise cavity at the equipment of the heat treatment process situ measurement change in film thickness of chemical solution deposition, in cavity, atmosphere is controlled.Fig. 1 essentially describes the inner structure of the controlled cavity of atmosphere, and the shell mechanism of closed cavity does not draw.
Beam of laser 4, second restraints the hot spot of laser 5 at sample surfaces without overlapping region, and spot size is less than 3 millimeters × 3 millimeters scopes.
Testing sample 2 is fixed on the sample stage 1 in cavity, and the temperature of sample stage 1 is controlled within the scope of room temperature to 1000 DEG C.The beam of laser 4, second introduced in cavity restraints two positions that laser 5 is radiated at testing sample 2 surface respectively, and beam of laser 4, second restraints the hot spot of laser 5 at sample surfaces without overlapping region, and spot size is less than 3 millimeters × 3 millimeters scopes.The folded light beam that beam of laser 4, second restraints laser 5 can be detected by laser detector 3, laser detector 3 can detect the facula position of reflects laser on laser detector 3, or can detect the interference information between beam of laser 4, second bundle laser 5.
In one case, if use laser detector 3 to detect the facula position of reflects laser on laser detector 3, then can according to trigonometry principle, calculate beam of laser 4, second respectively and restraint the misalignment that the position of reflection occurs laser 5, and then obtain film surface and the position difference change in the vertical direction of exposed substrate surface.
In another case, if use laser detector 3 detects the interference information between beam of laser 4, second bundle laser 5, then can according to interferometric method principle, calculate the optical path difference change that beam of laser 4, second restraints laser 5, and then utilize the incident angle of laser to calculate the position difference change of film surface and substrate surface vertical direction.
Measure a method for change in film thickness at the heat treatment process situ of chemical solution deposition, comprise the steps: testing sample 2 to be placed on sample stage 1; Lasing light emitter sends beam of laser 4, second and restraints film surface and the substrate surface that laser 5 is radiated at testing sample 2 respectively; Laser detector 3 receives the beam of laser 4, second reflected by testing sample 2 and restraints laser 5, calculates the position difference change in film surface and substrate surface vertical direction thus obtain the variation in thickness of film.
Particularly, measure the method for change in film thickness at the heat treatment process situ of chemical solution deposition, comprise the steps:
(S1) precursor aqueous solution is coated in substrate, controls coating procedure or process after application, making testing sample 2 possess film surface and exposed substrate surface.
In the present patent application, film needs to use chemical solution deposition method to prepare.In the present embodiment, what use the method to prepare is Yt-Ba-Cu-O high-temperature superconductive film, and its precursor aqueous solution composition comprises yttrium acetate, barium acetate, copper acetate, trifluoroacetic acid, methyl alcohol, polyglycol.
In step sl, the substrate used can possess minute surface even curface character, so that reflection lasering beam.In the present embodiment, the lanthanuma luminate single crystal that the substrate of use is polishing, its surface undulation is only atomic scale, therefore has good flatness.
In step sl, the film surface that coating obtains is due to the surface tension effects of precursor aqueous solution, and its surface also has the smooth feature of minute surface.Coating procedure can use spin coating (spin-coating), dip-coating (dip-coating), slot coated (slot-diecoating) and spraying to print modes such as (ink-jetprinting).In the present embodiment, dip coating manner is used.
In order to make testing sample 2 possess film surface and exposed substrate surface simultaneously, following several mode can be adopted: control precursor aqueous solution coating scope and do not make the local of substrate coated or covered by the local mask of substrate before coating and remove mask after application and expose substrate surface or coating post-etching part film to expose substrate surface.In the present embodiment, use first kind of way, immerse the degree of depth of precursor aqueous solution by controlling substrate in dip coating process, make the part surface of substrate not coated, testing sample 2 structural representation finally obtained as shown in Figure 2.
(S2) testing sample 2 is fixed on temperature and the controlled sample stage of atmosphere, selects suitable temperature variation curve and corresponding atmosphere, heat-treat process.
In step s 2, prepare heat-treat condition selective temperature curve corresponding to film and atmosphere according to required, need to ensure in heat treatment process, make film keep minute surface even curface feature always.In the present embodiment, use temperature curve and wherein each stage name as shown in Figure 3.The thermal decomposition stage uses by the high purity oxygen of washing as atmosphere, and the sintering stage uses the oxygen-nitrogen mixture by washing, and wherein oxygen content is 100ppm, and oxygenation and stove cold stage use dry high purity oxygen.In the present embodiment, film surface remains the feature that minute surface is smooth, and as the pattern of the film surface of qtenched sample when 400 DEG C, the sweep limit that atomic force microscope is measured is 50 microns × 50 microns, measures the surfaceness R obtained
qvalue is only 0.7nm, illustrates that its surface is very smooth.The film thickness of testing sample 2 does not exceed the scope of 100 nanometers to 100 micron in heat treatment process.
(S3) in heat treatment process, make laser beam respectively in film surface and substrate surface reflection, obtain the position difference change in the vertical direction of two surfaces, i.e. the variation in thickness of film.
In step s3, use laser beam oblique incidence, respectively in film surface and the reflection of exposed substrate surface, obtain two surfaces method that position difference changes in the vertical direction and can use trigonometry or interferometric method.
When using trigonometry, can oblique fire formula principle of triangulation figure in reference diagram 4, and principles illustrated below carries out Measurement and analysis.What reflect in Fig. 4 is the principle using beam of laser to measure reflection position displacement on a measured surface, wherein 41 is laser instrument, 42 is convergent lens, 43 is measured surface, 44 is receiver lens, 45 is CCD photoelectric detector, a and b is respectively object distance and the image distance of receiver lens, and the angle of incident laser and measured surface normal, receiver lens axis and measured surface normal is all set to θ.When measured surface 43 there occurs displacement x as shown in the figure, the corresponding meeting of the facula position of reflects laser on CCD is subjected to displacement y, according to image-forming principle triangle geometric relationship as shown in the figure, has following approximate function between x and y:
Use said method, according to the displacement of two bundle reflects laser facula positions on CCD, the misalignment of two measured surfaces can be calculated respectively, by two surperficial displacement calculated difference, the situation of change of film thickness can be obtained.
When using interferometric method, can interferometric method measuring principle figure in reference diagram 5, and principles illustrated below carries out Measurement and analysis.First the beam of laser (wavelength X) using light splitting optical path to be sent by laser instrument in the method is divided into the two bundle laser with coherence, reflect at film surface and exposed substrate surface respectively, incident angle is all θ, uses laser detector can obtain the interference information of two bundle reflects laser.When the two optical path difference is the even-multiple of half-wavelength, form bright fringes, being reflected on oscillograph is exactly crest; When the two optical path difference is the odd-multiple of half-wavelength, form dark fringe, the oscillograph being reflected in detector is exactly trough; When optical path difference there occurs the change of a wavelength X, now oscillograph just there will be complete Wave crest and wave trough cycle.If record N number of Wave crest and wave trough cycle on oscillograph, then can obtain two reflecting surfaces alternate position spike change x is in the vertical direction:
Trigonometry is used to measure in the present embodiment.
(S4) add up film thickness variation with temperature situation, obtain the net result of change in film thickness in site measurement.
In step s 4 which, film thickness variation with temperature situation in chemical solution heat treatment process can be obtained, thus may be used for analyzing information such as the reaction of film internal chemical, air accumulation and diffusions.In present patent application, the film thickness of testing sample 2 does not exceed the scope of 100 nanometers to 100 micron in heat treatment process.
Embodiment 2:
The present embodiment uses the equipment identical with embodiment 1, in site measurement chemical solution deposition method prepares the variation in thickness situation in ceria film process, the composition of precursor aqueous solution comprises cerous nitrate, diacetone, ethylene glycol monoemethyl ether etc., heat-treat condition is: be warming up to 400 DEG C from room temperature with 2 DEG C/min, 1000 DEG C are warming up to again with 5 DEG C/min, atmosphere controls to mix with argon gas for hydrogen, and wherein the volume fraction of hydrogen is 4%.Other preparation is identical with embodiment 1 with measuring condition.
Embodiment 3:
The present embodiment uses the equipment identical with embodiment 1, in site measurement chemical solution deposition method prepares the variation in thickness situation in strontium titanate film process, the composition of precursor aqueous solution comprises strontium acetate, butyl titanate, diacetone, ethylene glycol monoemethyl ether, acetic acid, ethylene glycol etc., heat-treat condition is: be warming up to 450 DEG C from room temperature with 2 DEG C/min, be warming up to 950 DEG C with 10 DEG C/min again, atmosphere is air.Other preparation is identical with embodiment 1 with measuring condition.
Compared to the prior art of in site measurement change in film thickness, present patent application does not need by measuring the physical property of film to calculate its variation in thickness, thus overcomes the obstacle that internal component and physical property in the chemical solution deposition heat treatment process of film do not stop to change; In addition, changed by the position difference measured between film surface and exposed substrate surface and obtain variation in thickness, the impact that deformation that sample stage occurs in heat treatment process brings can be eliminated.Therefore, present patent application effectively can carry out in site measurement to the situation of change of film thickness in heat treatment process.
Present patent application proposes a kind of equipment and method can carrying out variation in thickness in site measurement in the chemical solution deposition heat treatment process of film, it makes testing sample 2 possess film surface and exposed substrate surface, use laser beam respectively at two surface reflections, by obtaining the position difference change in the vertical direction of two surfaces, obtain the variation in thickness of film.In present patent application, the substrate surface used has the smooth feature of minute surface, film surface also keeps minute surface smooth in heat treatment process, being fixed on by testing sample 2 can on the sample stage of control temperature and atmosphere, design temperature change curve and corresponding atmosphere heat-treat process, can carry out in site measurement in the process to change in film thickness.Compared to the prior art of in site measurement change in film thickness, present patent application does not need by measuring the physical property of film to calculate its variation in thickness, thus overcomes the obstacle that internal component and physical property in the chemical solution deposition heat treatment process of film do not stop to change.In addition, changed by the position difference measured between film surface and exposed substrate surface and obtain variation in thickness, the impact that deformation that sample stage occurs in heat treatment process brings can be eliminated.Therefore, present patent application effectively can carry out in site measurement to the situation of change of film thickness in heat treatment process.
Chemical solution deposition heat treatment process initial film is generally gel mould, has certain mobility, and the present invention adopts non-contacting method to measure, and has ensured the feasibility measured.Simultaneously, due to the surface tension effects of precursor aqueous solution in the film application process of chemical solution deposition, apply the film surface obtained and there is the smooth feature of minute surface, and by controlling the suitable parameter such as heating rate, atmosphere in heat treatment process, film can be made always to keep minute surface even curface feature, therefore use the present invention to carry out non-cpntact measurement to film surface position and there is high accuracy.
In addition, sample stage due to fixing testing sample 2 needs to heat, change must be there is in the position of sample stage itself in heat treatment process, so simple change of measuring film surface position can not reflect the situation of change of film thickness, the present invention also measures the position to substrate surface simultaneously, thus utilizes two surperficial differences to obtain change in film thickness.The substrate surface used in present patent application also has the smooth feature of minute surface, and has carried out measuring accurately to the sample simultaneously with film surface and exposed substrate surface.
Technical scheme provided by the invention can be worth by film thickness in the heat treatment process of Measurement accuracy chemical solution deposition over time.If after the measurement of the technical program terminates, use the method for measuring thickness (measuring as used step instrument) of offing normal to obtain film thickness value, then can obtain the one-tenth-value thickness 1/10 of random time in heat treatment process further.
Although described and described and be counted as example embodiment of the present invention, it will be apparent to those skilled in the art that and can make various change and replacement to it, and spirit of the present invention can not have been departed from.In addition, many amendments can be made so that particular case is fitted to religious doctrine of the present invention, and central concept of the present invention described here can not be departed from.So the present invention is not limited to specific embodiment disclosed here, but the present invention also may comprise all embodiments and equivalent thereof that belong to the scope of the invention.
Claims (10)
1. the equipment of the measurement of the heat treatment process situ at a chemical solution deposition change in film thickness, it is characterized in that: comprise sample stage, lasing light emitter and laser detector, described sample stage carrying testing sample, described lasing light emitter sends beam of laser, the second bundle laser is radiated at testing sample respectively film surface and substrate surface, the beam of laser and second that described laser detector receives by testing sample reflects is restrainted laser, is calculated the change of the position difference of described film surface and substrate surface vertical direction, thus obtains the variation in thickness of film.
2. measure the equipment of change in film thickness as claimed in claim 1 at the heat treatment process situ of chemical solution deposition, it is characterized in that: also comprise cavity, in described cavity, atmosphere is controlled.
3. the equipment of change in film thickness is measured as claimed in claim 1 at the heat treatment process situ of chemical solution deposition, it is characterized in that: described beam of laser, second restraints the hot spot of laser at sample surfaces without overlapping region, and spot size is less than 3 millimeters × 3 millimeters scopes.
4. the equipment of change in film thickness is measured as claimed in claim 1 at the heat treatment process situ of chemical solution deposition, it is characterized in that: described laser detector is suitable for trigonometry, described laser detector detects the beam of laser of reflection and the displacement of the facula position of the second bundle laser on laser detector respectively, thus calculate the change in location situation that reflection occurs two bundle laser, and then obtain film surface and the position difference change in the vertical direction of exposed substrate surface.
5. the equipment of change in film thickness is measured as claimed in claim 1 at the heat treatment process situ of chemical solution deposition, it is characterized in that: described laser detector is suitable for interferometric method, interference information between the described beam of laser of described laser detector detection, the second bundle laser, calculate the optical path difference situation of change of described beam of laser, the second bundle laser, and then utilize the incident angle of laser to calculate the position difference change of described film surface and substrate surface vertical direction.
6. measure a method for change in film thickness at the heat treatment process situ of chemical solution deposition, it is characterized in that comprising the steps:
Testing sample is placed on sample stage;
Lasing light emitter sends beam of laser, the second bundle laser is radiated at testing sample respectively film surface and substrate surface;
Laser detector receive reflected by testing sample beam of laser, the second bundle laser, calculate the position difference change in described film surface and substrate surface vertical direction thus obtain the variation in thickness of film.
7. measure the method for change in film thickness as claimed in claim 6 at the heat treatment process situ of chemical solution deposition, it is characterized in that: also comprise and select suitable temperature variation curve and corresponding atmosphere to heat-treat described testing sample.
8. measure the method for change in film thickness as claimed in claim 6 at the heat treatment process situ of chemical solution deposition, it is characterized in that: testing sample can obtain exposed substrate surface in the following ways: control precursor aqueous solution coating scope and make the local of testing sample substrate not coated; Or before coating the local mask of testing sample substrate is covered and remove mask after application and expose substrate surface; Or corrode a part of film after application to expose substrate surface.
9. the method for change in film thickness is measured as claimed in claim 6 at the heat treatment process situ of chemical solution deposition, it is characterized in that: also comprise the thickness variation with temperature situation of adding up described film, obtain the net result of change in film thickness in site measurement.
10. measure the method for change in film thickness as claimed in claim 6 at the heat treatment process situ of chemical solution deposition, it is characterized in that: described laser detector uses trigonometry or interferometric method to obtain the position difference change of described film surface and substrate surface vertical direction.
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CN107218895A (en) * | 2017-06-07 | 2017-09-29 | 深圳市华星光电技术有限公司 | A kind of optical thickness monitor device and monitoring method |
CN108844500A (en) * | 2018-04-10 | 2018-11-20 | 苏州久越金属科技有限公司 | A kind of radium-shine automatic high-efficiency measurement method |
CN109084694A (en) * | 2018-09-20 | 2018-12-25 | 王顺 | A kind of film thickness detection method |
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