CN106441124A - Novel method for measuring film thickness by time response based on laser-induced thermoelectricity voltage - Google Patents
Novel method for measuring film thickness by time response based on laser-induced thermoelectricity voltage Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000004044 response Effects 0.000 title claims description 15
- 230000005619 thermoelectricity Effects 0.000 title 1
- 238000005259 measurement Methods 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 239000010409 thin film Substances 0.000 claims description 96
- 239000010408 film Substances 0.000 claims description 69
- 238000009792 diffusion process Methods 0.000 claims description 17
- 238000013016 damping Methods 0.000 claims description 13
- 238000001182 laser chemical vapour deposition Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 3
- 230000001360 synchronised effect Effects 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 2
- 238000005562 fading Methods 0.000 claims 2
- 238000000407 epitaxy Methods 0.000 abstract description 4
- 239000000523 sample Substances 0.000 description 16
- 230000003287 optical effect Effects 0.000 description 10
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001066 destructive effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
Abstract
The invention provides a novel method for nondestructive measurement of the thickness of a film growing on a beveled substrate from an epitaxy or approximate epitaxy. The method includes adopting an ultraviolet short-pulsed laser with the pulse width less than 20ns to radiate the film, utilizing the short-pulsed laser to heat the surface of the epitaxial film as an instant thermal source, generating temperature gradient in the direction perpendicular to the surface of the film, then detecting attenuation of a transverse thermoelectric voltage signal (called as an LITV signal) with time due to temperature difference to obtain time Td needed for the LITV signal attenuating from the peak value to 1/e of the peak value, and acquiring a thickness measured value of the film on the beveled film based on the linear relation of the square root of Td and the thickness d of the film.
Description
Technical field：
The present invention relates to a kind of new method of the time response measurement film thickness based on laser induced chemical vapor deposition thermoelectric voltage, especially
It is a kind of non-destructive measuring method of extension (or approximate extension) film thickness on measurement miscut substrate, belongs to the light of film thickness
Learn field of measuring technique.
Background technology：
For in the optoelectronic film device of nanoscale and microelectronic films device, the thickness of thin film is either to device
The performance of part is still to the stable all very crucial of technological parameter, it is necessary to measure the thickness of epitaxial film as accurately as possible.
At present, the measuring method of film thickness can mainly be divided into non optical method and optical meanss.
Non optical method mainly measures the thickness of thin film by scanning the observation such as probe, ultramicroscope.For example：Probe
Scanning method (also referred to as consistency profiles) be using small mechanical probes contact measured thin film surface measuring the thickness of thin film, this
The method of kind needs to prepare the film thickness step for testing, and therefore, the size of probe and the steep of step determine survey
The precision of amount.Therefore, roughness to altofrequency thin film and thin films step prepare undesirable sample, it is impossible to obtain good
Test effect, and the method can also bring certain damage to the surface of thin film.
Scanning electron microscope (SEM) is also commonly used for the thickness for detecting thin film, and this method is using focusing electron beam
As probe, the scanning of raster pattern being done in tested film surface, detects two for being excited by incident electron in tested film surface
Secondary electronics, after amplifying data and processing, obtains the scanning electron image of a secondary high-amplification-factor, by SEM viewing film
The transverse section of sample can obtain the information of film thickness.Sample and its surface conductance are required using SEM viewing film sample, because
When this measures to non-conductor thin film, the one layer of conductive metal film of plated surface in tested thin film is needed, this can affect measurement
Precision.
With respect to non optical method, had using the thickness of optical method for measuring thin film and sample nondestructive is hindered.Mesh
Before, mainly there are spectrographic method, Ellipsometric and optical thin film position phase method for the optical meanss of measured film thickness.
Spectrographic method can cause dual-beam or multiple beam according in thin film with the transmission (or reflection) of substrate interface light beam
Interfere, the thin film of different-thickness will have different spectral reflectivities (or absorbance), by detect the spectral characteristic of thin film come
The thickness of thin film is derived in inverting.The absorbance of current thin film and reflectance are mainly surveyed using grating test analysis system
Examination, and required according to different measuring, spectrographic method is needed by selecting suitable optimization method or using multiple method simultaneous,
More high-precision measured film thickness can be realized.In addition, the method also requires that film layer is thicker to produce certain dry
Vibration is related to, and is only used for measuring weak absorbing film.The measuring principle of Ellipsometric is to pass through thin film by detecting polarized beam
Reflection (or transmission) afterwards its polarization state change come inverting derive thin film thickness.High-selenium corn substrate is measured using Ellipsometric
On dielectric film thickness when, its certainty of measurement is than the high an order of magnitude of optical interference method, or even the spirit with atomic level
Sensitivity.However, Ellipsometric has a thickness cycle, if measurement range exceedes this cycle, the thickness of thin film will
There are multiple uncertain values, therefore, film sample of the thickness in 10nm or so is measured using Ellipsometric, measurement effect is optimal.
Not only need in this way reflective light intensity is accurately measured, and need accurately to measure analysis polarization intensity, it means that need
High-precision mobile optics is wanted, measurement cost is higher.Optical thin film position phase method refers to be interfered using interferometer detection
Signal mutually carrys out inverting by measuring reflection (or transmission) position asking for reflection (or transmission) the position phase relevant with film thickness
Derive the exact value of film thickness.For Ellipsometric, measurement apparatus simple structure, low cost, it is suitable for application
High-acruracy survey in thickness of multilayer film.As optical thin film position phase method is limited to the sensitivity of the non-linear position phase of thin film, reason
Only has 0.18 μm by the minimum Film thickness measurements for being above capable of accurately repeats realization, for the thinner nano thin-film sample of thickness
Thickness measure, its measurement error is larger.
Therefore, the material impact based on film thickness to material devices performance, and conventional films method for measuring thickness each
Drawback is planted, a kind of certainty of measurement height in the range of nanoscale is needed, and the non-destructive measuring method of low cost carrys out accurate measurement
The thickness of thin film.
Content of the invention：
It is an object of the invention to overcoming deficiency of the prior art, proposition one kind can be obtained and is grown on miscut substrate
Thin film thickness nondestructive measurement new method.The scope of the film thickness that can measure in this way is in 50nm
1000nm, measurement cost is cheap, and certainty of measurement is higher, and convenient and swift.Using technical scheme be:
The working mechanism of the present invention is：Thin to heat in the thermal source of film surface one transient state of generation after laser irradiation thin film
The upper surface of film, forms thermograde in the upper and lower surface of thin film.As thin film is relatively thin, and thermal phonon diffusion in the film
Migration is more much bigger than the speed of diffusive migration in air dielectric, and therefore, the change in the temperature field of thin film upper and lower surface is main
Come from thermal phonon to be moved towards the lower surface of thin film by thin film upper table, the motion of thermal phonon causes the upper and lower surface of thin film finally to reach
To thermal balance.Then the inventive method is multiplied by thermal phonon by measuring thermal phonon diffusive migration to the time required for thermal balance
Thermal diffusion speed in the film, so as to obtain the thickness of thin film.
The transient state thermal source of film surface is produced using the pulse width short-pulse laser irradiation thin film ultraviolet less than 20ns.Purple
Outer laser penetration depth in the film is little, and short pulse may insure during photothermal deformation that thermal phonon also has little time diffusion and moves
Move, the upper surface of thin film surface temperature moment after photon energy is absorbed reaches maximum.
Thermal diffusion makes thin film upper and lower surface progressively reach thermal balance, and the time required for this process is by measurement in thin film
The die-away time of the horizontal photovoltage produced by surface obtains.The thin film for being grown in miscut substrate surface is off-diagonal due to existing
Seebeck coefficient Szx, in temperature difference T that thin film upper and lower surface is produced0(t)-TdT () can produce laterally electricity in film surface induction
Pressure response (referred to as LITV signal), its size U (t), such as following formula：
Sab, ScCorresponding thin-film material is in ab crystal face and the Seebeck coefficient along c-axis crystal orientation, and the exposure that l and d is respectively thin film is long
Degree and the thickness of thin film, θ is the mis-cut angle of miscut substrate；A is the constant unrelated with the time, T0(t) and TdWhen () is respectively t t
The temperature of unkind film upper and lower surface, therefore, because thermal diffusion, U (t) is gradually reduced and synchronous declines with the thin film upper and lower surface temperature difference
Subtract.
Detection obtains LITV signal by peak atenuation to peak value as the LITV signal produced by the temperature difference is with the decay of time
1/e (wherein：E ≈ 2.71828) when required time τd(τdThe damping time constant of LITV signal can be referred to as again).
The die-away time τ of LITV signaldRelation such as following formula with the thickness d of thin film：
D is the thermal diffusion coefficient of thin-film material, and K is constant.
Using the following two kinds mode, the measured value of film thickness is obtained by the die-away time of LITV signal.First, by thin film
The value of thermal diffusion coefficient and the measured value of the die-away time of LITV signal, be directly substituted into the thickness that (2) formula is calculated thin film.
Second, choosing the film sample 15 of the same material of known thickness as standard sample, detection criterion sample is in laser spoke
According under LITV signal damping time constant, by thickness d and the τ of thin filmdSubduplicate linear relationship, such as formula (3),
Obtain the constant K of thin film to be measured.The damping time constant of the LITV signal of other thin film to be measured is measured, can be obtained by (3) formula
Obtain the exact value of film thickness.In this way while the value of the thermal diffusion coefficient of thin film can also be obtained.As following formula：
Description of the drawings：
The schematic diagram of Fig. 1 film thickness measurement system；
Fig. 2 YBa2Cu3O7The time-evolution curve of the LITV signal of thin film；
Fig. 3 YBa2Cu3O7The thickness d of thin film and LITV signal attenuation time τdSubduplicate linear relationship；
Fig. 4 (La1.45Nd0.4)Ba0.15CuO4LITV signal time-evolution curve；
Specific embodiment：
Ultraviolet short-pulse laser irradiation thin film of the present invention using pulse width less than 20ns, produces an instant therm source
So that epitaxial film surface is heated, thermograde is being produced perpendicular to the direction of film surface, then in film surface along thin film
Cut sth. askew on direction, detect as horizontal LITV signal produced by the temperature difference is with the decay of time, obtain LITV signal decay when
Between constant, τd, then, based on τdSquare root and the linear relationship of the thickness d of thin film obtain thin film on miscut substrate degree accurate
Value.
The schematic diagram of film thickness measurement system as shown in figure 1, measuring system includes short-pulse laser, for detecting
The probe of LITV signal, LITV signal acquiring system data is processed and computing system.The thin film edge being grown on miscut substrate
Substrate miscut direction is fixed between two electrodes by conductive fixture, ultraviolet short-pulse laser of the pulse width less than 20ns
Irradiation thin film, heats the upper surface of epitaxial film when producing an instant therm source, producing temperature perpendicular to the direction of film surface
Degree gradient, resulting LITV signal is transferred to oscillograph (or high number number capture card) by coaxial cable to carry out data and adopts
Collection and record, obtain the time-evolution curve of LITV signal, and the time precision of oscillograph (or high number number capture card) has high demands
In 1ns.If LITV signal of the surveyed thin film produced by under laser irradiation is less, can be big by increasing incident laser energy
The spacing of little and two electrode holders come increase LITV response, improve signal to noise ratio.
By the time-evolution curve of LITV signal, LITV signal is obtained to the time t of peaking1, and declined by crest voltage
Reduce to the time t of the 1/e of crest voltage2, damping time constant τ of LITV signald=t2-t1.Equally, it would however also be possible to employ (5) formula
Decaying exponential function the attenuation process of LITV signal is fitted, the damping time constant of LITV signal is obtained.
Finally, by τdThe linear relationship of square root and d obtain the thickness exact value of thin film on miscut substrate.
Embodiment 1, YBa2Cu3O7The measurement of film thickness, YBa2Cu3O7The LaAlO that cut sth. askew is grown in thin film epitaxy3Single
Brilliant substrate surface, the incline direction of substrate is (001) crystal face 15 degree to (100) crystallographic tilt.By YBa2Cu3O7Thin film passes through
Conductive fixture is fixed between two electrodes, and the spacing of electrode is pulse laser irradiation thin film 2mm, using wavelength for 248nm,
The pulse width of laser is 20ns, and laser energy density is 0.26mJ/mm2, produced LITV signal passed by coaxial cable
Defeated data acquisition and record is carried out to oscillograph.It is illustrated in figure 2 in YBa2Cu3O7The LITV signal that film surface is detected
Time-evolution curve.
LITV signal is obtained to the time t of peaking by the data in Fig. 21, and crest voltage is decayed to by crest voltage
1/e time t2, damping time constant τ of LITV signald=t2-t1.Or adopt decay of (5) formula to LITV signal
Journey is fitted, and damping time constant τ of LITV signal is obtainedd, substitute into YBa2Cu3O7The thermal diffusion coefficient D value of thin film, by
Formula (2) is calculated film thickness for 204nm.
According to method as described above, the YBa of different-thickness is measured respectively2Cu3O7The response time of the LITV signal of thin film,
Obtain damping time constant τ of LITV signaldSquare root as shown in Figure 3 with the linear relationship of the thickness d of thin film.Other thin film
The determination of thickness can be by the die-away time of the LITV signal of measurement thin film to be measured, and the linear relationship according to figure (3) is also
The thickness of thin film is obtained.Meanwhile, YBa can be calculated by the result of (3) formula and figure (3)2Cu3O7Thin film thermal diffusion system
Number is 6.98 × 10-7m2/s.
Embodiment 2, (La1.45Nd0.4)Ba0.15CuO4The measurement of film thickness, (La1.45Nd0.4)Ba0.15CuO4Thin film epitaxy
Be grown in the LaAlO that cuts sth. askew3When crystalline substrates surface, the incline direction of substrate is (001) crystal face to (100) crystallographic tilt
15 degree.By (La1.45Nd0.4)Ba0.15CuO4Thin film is fixed between two electrodes by conductive fixture, and the spacing of electrode is 2mm,
Using wavelength for 248nm pulse laser irradiation thin film, it is 0.26mJ/ that the pulse width of laser is 20ns, laser energy density
mm2, produced LITV signal is transferred to oscillograph by coaxial cable carries out data acquisition and record.It is illustrated in figure 4
(La1.45Nd0.4)Ba0.15CuO4The time-evolution curve of the LITV signal that film surface is detected.
LITV signal is obtained to the time t of peaking by the data in Fig. 41, and crest voltage is decayed to by crest voltage
1/e time t2, damping time constant τ of LITV signald=t2-t1.Or adopt decay of (5) formula to LITV signal
Journey is fitted, and damping time constant τ of LITV signal is obtaineddFor 134ns, by the τ for measuringdValue and (La1.45Nd0.4)
Ba0.15CuO4The thermal diffusion coefficient D value of thin film substitutes into formula (2), is calculated film thickness for 196nm.
Claims (7)
1. the time response based on laser induced chemical vapor deposition thermoelectric voltage measures the new method of film thickness, it is characterised in that first using ultraviolet
Laser irradiation thin film, allows Ultra-Violet Laser heat the upper surface of epitaxial film as an instant therm source, perpendicular to film surface
Direction produce thermograde, so as to induce the horizontal photoelectric signal of generation along the direction of cutting sth. askew of thin film in film surface
(abbreviation LITV signal)；Thermal diffusion makes thin film upper and lower surface progressively reach thermal balance, correspondingly the synchronous fading therewith of LITV signal,
The time-evolution of detection LITV signal, obtain LITV signal by peak atenuation to peak value 1/e when required time τd, it is based on
τdThe linear relationship of square root and the thickness d of thin film obtain the measured value of film thickness on miscut substrate.
2. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 1 measures the new method of film thickness,
It is characterized in that the scope of the film thickness of the measurement is in 50nm 1000nm.
3. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 1 measures the new method of film thickness,
It is characterized in that the Ultra-Violet Laser is less than the ultraviolet short-pulse laser of 20ns for pulse width.
4. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 1 measures the new method of film thickness,
It is characterized in that the thermal diffusion makes thin film upper and lower surface reach the die-away time of the time required for thermal balance and LITV signal
Corresponding, by measuring the die-away time τ in the horizontal photovoltage (LITV) produced by film surfacedObtain；It is grown in cutting sth. askew
There is off-diagonal Seebeck coefficient S in the thin film of substrate surfacezx, temperature difference T of t thin film upper and lower surface0(t)-TdT () is permissible
Horizontal LITV response U (t), such as following formula are produced in film surface induction：
U (t)=∫ SzxΔ T=A [T0(t)-Td(t)] (1)
In formula：A is the constant unrelated with the time,
T0(t) and TdT () is respectively the temperature of t thin film upper and lower surface.
Due to thermal diffusion, U (t) with the temperature difference of thin film upper and lower surface be gradually reduced and synchronous fading；Measurement LITV signal when
Between develop curve, obtain LITV signal to the time t of peaking1, and the time for being decayed to the 1/e of crest voltage by crest voltage
t2, you can to obtain damping time constant τ of LITV signald=t2-t1；
Or, the die-away time for being fitted obtaining LITV signal to the attenuation process of LITV signal using decaying exponential function is normal
Number τd.
5. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 1 measures the new method of film thickness,
It is characterized in that the LITV signal by peak atenuation to peak value 1/e when required time τd, horizontal pyroelectric signal LITV
The die-away time τ of signaldRelation such as following formula with the thickness d of thin film：
In formula：D is the thickness of thin film,
τdFor die-away time,
D is the thermal diffusion coefficient of thin-film material,
K is constant.
6. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 1 measures the new method of film thickness,
It is characterized in that the measured value that the die-away time by LITV signal obtains film thickness is obtained using following two ways：
First, by the value of the thermal diffusion coefficient of thin film and the measured value of the die-away time of LITV signal, being directly substituted into the calculating of (2) formula
Obtain the thickness of thin film；Or
Second, choosing the film sample 15 of the same material of known thickness as standard sample, detection criterion sample is swashing
The damping time constant of the LITV signal under photoirradiation, by thickness d and the τ of thin filmdSubduplicate linear relationship, as formula
(3) the constant K of thin film to be measured, is obtained, the damping time constant of the LITV signal of other thin film to be measured is measured, by (3) formula be
Film thickness can be obtained, in this way while the value of the thermal diffusion coefficient of thin film can be obtained.As following formula：
7. the time response based on laser induced chemical vapor deposition thermoelectric voltage according to claim 6 measures the new method of film thickness,
It is characterized in that the measured value for obtaining the thickness of thin film on miscut substrate, if surveyed thin film is produced by under laser irradiation
LITV signal less, by increasing incident laser energy size and can increase for gathering between two electrodes of LITV signal
Away from come increase LITV response, improve signal to noise ratio.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330446A (en) * | 2018-03-29 | 2018-07-27 | 昆明理工大学 | A kind of adjustable lanthanum calcium manganese oxygen film Preparation equipment of LIV effects |
| CN109557129A (en) * | 2018-10-29 | 2019-04-02 | 同济大学 | A kind of measurement method of film thermal diffusion coefficient |
| CN110852021A (en) * | 2018-07-26 | 2020-02-28 | 上海新昇半导体科技有限公司 | Method for obtaining epitaxial flatness based on simulation mode |
| CN114046736A (en) * | 2021-11-09 | 2022-02-15 | 北京理工大学 | Method for determining metal electron trajectory depth based on pumping detection analysis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330446A (en) * | 2018-03-29 | 2018-07-27 | 昆明理工大学 | A kind of adjustable lanthanum calcium manganese oxygen film Preparation equipment of LIV effects |
| CN110852021A (en) * | 2018-07-26 | 2020-02-28 | 上海新昇半导体科技有限公司 | Method for obtaining epitaxial flatness based on simulation mode |
| CN110852021B (en) * | 2018-07-26 | 2024-02-06 | 上海新昇半导体科技有限公司 | Method for obtaining epitaxial flatness based on simulation mode |
| CN109557129A (en) * | 2018-10-29 | 2019-04-02 | 同济大学 | A kind of measurement method of film thermal diffusion coefficient |
| CN114046736A (en) * | 2021-11-09 | 2022-02-15 | 北京理工大学 | Method for determining metal electron trajectory depth based on pumping detection analysis |
| CN114046736B (en) * | 2021-11-09 | 2023-02-28 | 北京理工大学 | Method for determining metal electron trajectory depth based on pumping detection analysis |
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