CN109883956A - The measuring device and measurement method that thin-film optical constant varies with temperature - Google Patents
The measuring device and measurement method that thin-film optical constant varies with temperature Download PDFInfo
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- CN109883956A CN109883956A CN201910078617.8A CN201910078617A CN109883956A CN 109883956 A CN109883956 A CN 109883956A CN 201910078617 A CN201910078617 A CN 201910078617A CN 109883956 A CN109883956 A CN 109883956A
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Abstract
A kind of measuring device and measurement method that thin-film optical constant varies with temperature, by the way that film sample, temperature control is heated in closed environment, the ellipsometric parameter that the substrate of measurement same sample and film surface vary with temperature respectively, the floor parameter that measured substrate optical constant is fitted as film layer optical constant using at identical temperature, substrate face shape and changes in optical properties and influence to film layer measurement result in thermal histories are excluded, realizes the precise measurement that thin-film optical constant varies with temperature.The influence that the measurement of thin-film optical constant effectively excludes that substrate characteristics vary with temperature in the present invention improves measurement accuracy.Strict control Variable Conditions in measurement process reduce measurement error, easy to operate effective, are conducive to the accuracy and stability that improve measurement.
Description
Technical field
The present invention relates to ellipsometer measurement, especially a kind of device for accurately measuring that thin-film optical constant varies with temperature with
Measurement method
Background technique
The optical constant of optical thin film will directly affect the properties such as the mechanics, optics, electromagnetism of film, in hot conditions
Under, optical thin film can not only absorb the distortion of heat generating surface shape, while the variation of optical constant can also occur.For a long time,
Laser limits always laser to the thermal damage of optical thin film element to be developed to high power, high-energy, and influences thin-film component
The principal element of service life.Therefore, precise measurement thin-film optical constant variation with temperature, for study its hot object characteristic and
Improve its in high energy laser system using particularly important.
Ellipsometry is a kind of currently used method for measuring film thickness and optical constant., number high with measurement accuracy
It is high according to measurement repetitive rate, contact the features such as destructiveness caused by sample is minimum with sample, be widely used in optics industry,
In many fields such as electronics industry, physics and medical research.Ellipsometry is the measurement side based on the polarization state for measuring light
Method, the variation of measurement film surface reflection polarization state.(Ψ, Δ meet ellipsometric parameterrp,rsIt is p light
With the reflection coefficient of s light) with film thickness, light refractive index, extinction coefficient have corresponding relationship, thus inverting obtains film
Thickness and optical constant.Ellipsometry has On-line sampling system, and measuring speed is fast, measuring accuracy is high, to measurement environment and sample
It is required that low advantage, is widely applied in film thickness and optical constant measurement at present.
Since optical constant in varying degrees and face shape can occur in thermal histories for the film surface and substrate of film sample
Change, therefore directly have very big error using the optical constant of film surface under ellipsometer measurement different temperatures.The present invention adopts
With respectively measure same sample film surface and substrate ellipsometric parameter, using the measurement result of substrate at a certain temperature as this temperature
Primary condition when lower film layer optical constant is fitted excludes shadow of the change to film layer measurement result of basal surface shape and optical constant
It rings.It realizes the precise measurement that thin-film optical constant varies with temperature, and is expected to the research for changing thin-film optical constant under high temperature
Apply in the element damage research of high energy laser system.
Summary of the invention
To overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of survey that measurement thin-film optical constant varies with temperature
Device and method are measured, by the way that temperature control heats under closed environment to film sample, measure the substrate and film surface of same sample respectively
The ellipsometric parameter varied with temperature, the primary condition being fitted using the ellipsometric parameter of substrate at identical temperature as film layer exclude base
Bottom face shape and changes in optical properties and influence to film layer measurement result in thermal histories realize thin-film optical constant with temperature
The precise measurement of variation.And it is expected to the research application for changing thin-film optical constant under high temperature and is studied in the damage of superlaser
In.
Technical solution of the invention is as follows:
A kind of measuring device that thin-film optical constant varies with temperature, it is characterized in that: including ellipsometer incidence arm, for sample
Alternating temperature platform and ellipsometer the outgoing arm that product are placed are externally provided with alternating temperature platform sealing cover in the alternating temperature platform；
Light outbound course along ellipsometer incidence arm is successively alternating temperature platform sealing cover and sample, after sample reflection,
Along film surface, alternating temperature platform sealing cover and ellipsometer the outgoing arm outgoing of plating membrane sample；
The sample is coating single side, is on one side film surface, another side is substrate.
The temperature of sample is controlled by alternating temperature platform, measures the optical constant of sample under different temperatures, it is real by overturning sample
The now ellipsometric parameter that the substrate of measurement same sample and film surface vary with temperature, it is normal with substrate optics measured at identical temperature
The primary condition that are fitted as film layer optical constant of number, exclusion substrate in thermal histories face shape and changes in optical properties and to film
The measurement that thin-film optical constant varies with temperature is realized in the influence of layer measurement result.
The window side of the alternating temperature platform sealing cover is vertical with incident ray direction.
On the other hand, the present invention provides a kind of measurement methods that thin-film optical constant varies with temperature, including following step
It is rapid:
Step 1) rotates ellipsometer incidence arm and outgoing arm, and sample is placed on alternating temperature platform, alternating temperature platform sealing cover structure is covered
At confined chamber, adjusting incident light angle keeps the window side of alternating temperature platform sealing cover vertical with incident light；
The film surface that step 2) chooses the sample is surface to be measured, adjusts spot center and the inclination angle of ellipsometer, is utilized
Alternating temperature platform heats up to sample, and after reaching preset temperature T1, constant temperature for a period of time, keeps sample surface temperature conduction uniformly laggard
Row measurement, recording film plane ellipsometric parameter (Ψ1, Δ1) and save, it then proceedes to heat up to sample, reaches preset temperature T2
Afterwards, constant temperature for a period of time, measures, recording film plane ellipsometric parameter (Ψ after making sample surface temperature conduction uniformly2, Δ2) and protect
It deposits, until having measured all preset temperature points；
The substrate that step 3) chooses the sample is surface to be measured, adjusts spot center and the inclination angle of ellipsometer, is utilized
Alternating temperature platform heats up to sample, reaches preset temperature T1Afterwards, constant temperature for a period of time, keeps sample surface temperature conduction uniformly laggard
Row measurement, records substrate ellipsometric parameter (Ψ '1, Δ '1), and inverting obtains the normal (n ' of substrate optics at this temperature1,k’1), record
And save, it then proceedes to heat up to sample, reaches preset temperature T2Afterwards, constant temperature for a period of time, passes sample surface temperature
It is measured after leading uniformly, records substrate ellipsometric parameter (Ψ '2, Δ '2), and inverting obtains the normal (n ' of substrate optics at this temperature2,
k’2), it records and saves, until having measured all preset temperature points；
Step 4) passes through the substrate optical constant that step 3) obtains, the substrate when film surface optical constant as sample is fitted
Parameter, in conjunction with the film surface ellipsometric parameter that step 2) is obtained, fitting obtains the thickness and optical constant of film surface.
Consider sample deformation before heating measurement every time, realign spot center, adjust gradient, avoid because sample by
Measurement error caused by thermal deformation.
Compared with existing measurement method, the invention has the following beneficial effects:
(1) it is based on oval thickness spectral technology and temperature control heating device, excludes substrate face shape and optical characteristics in thermal histories
Change and the influence to film layer measurement result, the accurate Characterization of thin-film optical constant when suitable for temperature change.
(2) the plating membrane sample described in is unilateral plated film, and surface side is film, and side is substrate, and overturning can be realized and survey
Measure the oval thickness parameter of substrate and film under identical conditions.
Measure the ellipsometric parameter of film sample film side and substrate side respectively using overturning film sample, and ellipse partially with substrate
Parameter is fitted the optical constant of film layer as primary condition, realizes the strict control of Variable Conditions in experimentation, excludes
Substrate face shape and changes in optical properties and influence to film layer measurement result in thermal histories, reduce measurement error.
(3) film sample temperature control is heated using closed temperature control platform, it can be achieved that conventional elliptic polarization spectrometer measurement is thin
The regular relationship that film optical constant varies with temperature.
Detailed description of the invention
Fig. 1 is in the block diagram for the measuring device that thin-film optical constant of the present invention varies with temperature: 1- ellipsometer incidence arm,
2- alternating temperature platform seals room, 3- sample film surface, 4- sample substrate, 5- alternating temperature platform, 6- ellipsometer outgoing arm
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described, but protection model of the invention should not be limited with this
It encloses.
First referring to Fig. 1, Fig. 1 is the block diagram for the measuring device that thin-film optical constant of the present invention varies with temperature, You Tuke
See, the device for accurately measuring that thin-film optical constant of the present invention varies with temperature, is placed including ellipsometer incidence arm 1, for sample
Alternating temperature platform 5 and ellipsometer are emitted arm 6 and are externally provided with alternating temperature platform sealing cover 2 in the alternating temperature platform 5；Along the light of ellipsometer incidence arm 1
Line outbound course is successively alternating temperature platform sealing cover 2 and sample, and after sample reflection, film surface 3, the alternating temperature platform along plating membrane sample are close
Capping 2 and ellipsometer outgoing arm 6 are emitted；The sample is coating single side, is on one side film surface 3, and another side is substrate 4.Pass through
Alternating temperature platform 5 controls the temperature of sample, measures the optical constant of sample under different temperatures, realizes measurement with by overturning sample
The ellipsometric parameter that the substrate and film surface of product vary with temperature, measured substrate optical constant is as film layer light using at identical temperature
Learn fitting of constant primary condition, exclude substrate in thermal histories face shape and changes in optical properties and to film layer measurement result
It influences, realizes the measurement that thin-film optical constant varies with temperature.
Embodiment: steps are as follows for the measurement method that thin-film optical constant varies with temperature:
1) ellipsometer incidence arm and outgoing arm are rotated, adjustment incident light angle is 70 °, and sealed window and incident light is made to hang down
Directly, sample to be tested diaphragm is placed at heating platform center, is isolated by confined chamber with external environment, and temperature is room temperature 20 at this time
DEG C, adjusting incident light and reflected light in sample surfaces is in 140 ° of angles, and measurement wavelength is 300nm-1100nm, is waited to be measured；
2) choosing sample film surface (3) side is surface to be measured, adjusts spot center and inclination angle, right using alternating temperature platform (5)
Sample heating, preset temperature o'clock, for interval, are set as 20 DEG C, 70 DEG C, 120 DEG C, 170 DEG C, 220 DEG C, 270 DEG C, 320 with 50 DEG C
DEG C, since 20 DEG C of room temperature, temperature it is every rise 50 DEG C when steady temperature, wait 20min after start to measure, continue after measurement
It is warming up to next temperature, the ellipsometric parameter of the film under repeated measurement different temperatures records and saves；
3) for cooling sample to 20 DEG C of room temperature, it is surface to be measured that overturning sample, which chooses the uncoated one side of substrate (4), adjusts light
Spot center and inclination angle heat up to sample using alternating temperature platform (5), and preset temperature o'clock, for interval, is set as 20 DEG C, 70 with 50 DEG C
DEG C, 120 DEG C, 170 DEG C, 220 DEG C, 270 DEG C, 320 DEG C, since 20 DEG C of room temperature, temperature it is every rise 50 DEG C when steady temperature, wait
Start to measure after 20min, continue to be warming up to next temperature after measurement, the substrate under repeated measurement different temperatures it is ellipse partially
Parameter records and saves；
4) fit procedure 2), 3) in the ellipsometric parameter (Ψ, Δ) and thicknesses of layers, incident wavelength, incident angle that extract
Corresponding relationship curve establishes ellipse inclined dispersive model, using the data of substrate (4) at a certain temperature as film surface at a temperature of this (3) light
Primary condition when fitting of constant is learned, the fit range of 500nm-800nm wavelength is chosen, until finding optimal solution.
Experiment shows that the present invention has device easy to operate, effectively reduces error, online non-cpntact measurement will not destroy
Sample to be tested surface and the high feature of measurement accuracy.
Claims (6)
1. a kind of measuring device that thin-film optical constant varies with temperature, it is characterised in that: including ellipsometer incidence arm (1), supply
Alternating temperature platform (5) and the ellipsometer outgoing arm (6) that sample is placed are externally provided with alternating temperature platform sealing cover (2) in the alternating temperature platform (5)；
Light outbound course along ellipsometer incidence arm (1) is successively alternating temperature platform sealing cover (2) and sample, is reflected through the sample
Afterwards, along film surface (3), alternating temperature platform sealing cover (2) and ellipsometer outgoing arm (6) outgoing of plating membrane sample；
The sample is coating single side, is on one side film surface (3), and another side is substrate (4).
2. the measuring device that thin-film optical constant according to claim 1 varies with temperature, it is characterised in that: pass through alternating temperature
Platform (5) controls the temperature of sample, measures the optical constant of sample under different temperatures, realizes measurement same sample by overturning sample
Substrate and the ellipsometric parameter that varies with temperature of film surface, measured substrate optical constant is as film layer optics using at identical temperature
The primary condition of fitting of constant, exclude substrate in thermal histories face shape and changes in optical properties and to the shadow of film layer measurement result
It rings, realizes the measurement that thin-film optical constant varies with temperature.
3. the measuring device that thin-film optical constant according to claim 1 or 2 varies with temperature, it is characterised in that: described
The window side of alternating temperature platform sealing cover (2) is vertical with incident ray direction.
4. the measuring device varied with temperature using thin-film optical constant described in claim 1 measures method, feature
It is that this method includes the following steps:
Step 1) rotates ellipsometer incidence arm and outgoing arm, and sample is placed on alternating temperature platform (5), alternating temperature platform sealing cover (2) is covered
Confined chamber is constituted, adjustment incident light angle keeps the window side of alternating temperature platform sealing cover (2) vertical with incident light；
The film surface (3) that step 2) chooses the sample is surface to be measured, adjusts spot center and the inclination angle of ellipsometer, utilizes change
Warm platform (5) heats up to sample, after reaching preset temperature T1, constant temperature for a period of time, make sample surface temperature conduction uniformly after
It measures, recording film plane ellipsometric parameter (Ψ1, Δ1) and save, it then proceedes to heat up to sample, reaches preset temperature T2
Afterwards, constant temperature for a period of time, measures, recording film plane ellipsometric parameter (Ψ after making sample surface temperature conduction uniformly2, Δ2) and protect
It deposits, until having measured all preset temperature points；
The substrate (4) that step 3) chooses the sample is surface to be measured, adjusts spot center and the inclination angle of ellipsometer, utilizes change
Warm platform (5) heats up to sample, reaches preset temperature T1Afterwards, constant temperature for a period of time, make sample surface temperature conduction uniformly after
It measures, records substrate ellipsometric parameter (Ψ '1, Δ '1), and inverting obtains substrate optical constant (n ' at this temperature1,k’1),
It records and saves, then proceedes to heat up to sample, reach preset temperature T2Afterwards, constant temperature for a period of time, makes sample surfaces temperature
It is measured after degree conduction uniformly, records substrate ellipsometric parameter (Ψ '2, Δ '2), and substrate optics is normal at this temperature for inverting acquisition
(n’2,k’2), it records and saves, until having measured all preset temperature points；
Step 4) passes through the substrate optical constant that step 3) obtains, the base when optical constant of the film surface (3) as sample is fitted
Bottom parameter, in conjunction with the film surface ellipsometric parameter that step 2) is obtained, fitting obtains the thickness and optical constant of film surface (3).
5. measurement method according to claim 3, it is characterised in that consider sample deformation before heating measurement every time, again
It is directed at spot center, adjusts gradient.
6. measurement method according to claim 3, it is characterised in that preset temperature T1, T2……TnAccording to experiment demander
To set, and temperature interval is identical.
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| CN110823945A (en) * | 2019-11-14 | 2020-02-21 | 中国科学院光电技术研究所 | Optical thin film thermal expansion coefficient measuring device based on ellipsometer and measuring method thereof |
| CN112378859A (en) * | 2020-10-05 | 2021-02-19 | 华中科技大学 | Optical constant measuring method and device for quartz glass window polarization effect in-situ calibration |
| CN113655592A (en) * | 2021-08-20 | 2021-11-16 | 中国科学院国家天文台南京天文光学技术研究所 | Large-caliber high-precision optical element film stress deformation regulation and control method |
| CN114486191A (en) * | 2022-01-18 | 2022-05-13 | 湖北航天技术研究院总体设计所 | Laser load capacity testing system and method |
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| CN113655592A (en) * | 2021-08-20 | 2021-11-16 | 中国科学院国家天文台南京天文光学技术研究所 | Large-caliber high-precision optical element film stress deformation regulation and control method |
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