CN106017338A - Method for determining film continuity critical thickness - Google Patents
Method for determining film continuity critical thickness Download PDFInfo
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- CN106017338A CN106017338A CN201610363752.3A CN201610363752A CN106017338A CN 106017338 A CN106017338 A CN 106017338A CN 201610363752 A CN201610363752 A CN 201610363752A CN 106017338 A CN106017338 A CN 106017338A
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- G—PHYSICS
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- 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
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
- G01B11/0641—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating with measurement of polarization
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Abstract
The invention discloses a method for determining film continuity critical thickness. The method includes that a dispersion formula model and a fitting mode are arranged on a spectrum ellipsometer, under the condition that the thickness of the film growing on a substrate is less than the preset film thickness, an indirect fitting method is adopted to obtain a change curve showing the phase difference of the film reflected light polarization state changing with the incident light wavelength and a change curve showing the corresponding tangent angle of the film reflection coefficient amplitude ratio changing with the incident light wavelength; under the condition that the thickness of the film growing on the substrate is greater than or equal to the preset film thickness, a direct fitting method is adopted to obtain a change curve showing the phase difference of the film reflected light polarization state changing with the incident light wavelength and a change curve showing the corresponding tangent angle of the film reflection coefficient amplitude ratio changing with the incident light wavelength; and the film continuity critical thickness is determined based on the change curves. The method solves the problem of difficulty in determining the film continuity critical thickness, and has important guiding significance for the precise preparation and application of nano-optoelectronic devices and the related theoretical researches.
Description
Technical field
The present invention relates to optics and nanoscale science and technology, in particular it relates to a kind of critical thickness determining film continuity
Method.
Background technology
Thin-film material is an important branch in modern material field.When film thickness is in sub-micrometer scale, its thing
Rationality matter such as mechanics, electricity, magnetics and optics etc. can occur significant change relative to three-dimensional block materials, and when film thickness enters
One step reduces, when surface becomes discrete and discontinuous nano-particle, owing to quantum size effect, skin effect and dielectric limit
The factor impacts such as territory effect can make the change of its physical property the most notable.Therefore, accurately judgement is continuous and discontinuous thin film
Critical thickness, for experimentally preparing the high-precision filrn photovoltaic devices of high-quality and analysing in depth two kinds of thin film in theory
Microcosmic mechanism tool is of great significance.
According to the physical process of thin film deposition, at the film forming initial stage, for reducing the free energy on surface and interface, atom is agglomerated into
Core, becomes discontinuous nanometer island structure.Along with the continuation of thin film deposits, elementide is constantly formed, decomposes, captures, combines
With grow up, first grow up to discrete nanometer island structure, then island structure gap is gradually reduced formation discontinuous chain knot
Structure, is finally grown to serve as continuous film.Generally, major part thin film thickness less than 5nm time, surface topography show as from
The nanometer island structure dissipated, forms discontinuous chain thin film in 5～10nm, complete in 10～20nm the combination between nano island and
Growth, reaches continuous.Therefore, become the growth course of continuous film from discontinuous island thin film and can regard nano-particle as
Between air be gradually reduced to disappear process, therefore between granule air from have to without this progressive formation exist a critical bar
Part, can distinguish continuous film and discontinuous thin film intuitively with this.
But, current research report detects the most not differentiation to both thin film by instrument and provides strict boundary
Limit, mainly due to the film preparation instrument in existing investigative technique, characterization technique, the requirement of experiment height of method of testing, and
The theory analysis difficulty of intermediate physical process is big, cause the critical thickness accurately determining both thin film at present be one great
Challenge.
Based on existing preparation condition and means of testing, accurately determine the continuous critical thickness needs gram with discontinuous thin film
The Major Difficulties of clothes has:
1, the experimental apparatus selecting to prepare high accuracy high-quality thin film is needed；
2, need to select the characterization technique of energy accurately testing film character；
3, in the characterization technique used, need to update method of testing, make test result the most accurate；
4, according to experimental results, the discontinuous thin film transition process to continuous film is analyzed theoretically.
Summary of the invention
A kind of method that it is an object of the invention to provide critical thickness determining film continuity.Described method can solve the problem that
The problem determining the critical thickness difficulty of film continuity present in prior art, and can improve and turn from noncontinuity thin film
Change to the theoretical research of continuous film.
To achieve these goals, a kind of method that the present invention provides critical thickness determining film continuity.Use light
The thickness of the thin film that spectrum ellipsometer measurement is grown on substrate and optical property, described method includes:
Described spectroscopic ellipsometers arranges dispersion equation model and fit approach；
In the case of the thickness of the thin film grown over the substrate is less than the film thickness preset, use indirect approach to fitting
Obtain the tangent angle corresponding to the reflection phase contrast of polarization state of described thin film and reflection coefficient amplitude ratio respectively with incidence
The change curve of optical wavelength；
In the case of the thickness of the thin film grown over the substrate is more than or equal to the film thickness preset, use directly
Tangent angle corresponding to the phase contrast of the reflection polarization state of the fitting process described thin film of acquisition and reflection coefficient amplitude ratio is respectively
Change curve with lambda1-wavelength；
The successional critical thickness of described thin film is determined according to described change curve.
Alternatively, described employing indirect approach to fitting obtains the phase contrast reflecting polarization state and the reflection coefficient of described thin film
Tangent angle corresponding to amplitude ratio respectively with the change curve of lambda1-wavelength, including:
Thickness is fitted less than the thin film of the film thickness preset, obtains simple metal level；
Described metal level adds the mixed layer of metal and air, and removes described metal level；
Thickness and the scale parameter of changing described mixed layer carry out matching again, and obtain the reflection light polarization of described thin film
Tangent angle corresponding to the phase contrast of state and reflection coefficient amplitude ratio is with the change curve of lambda1-wavelength.
Alternatively, described employing direct approach to fitting obtains the phase contrast reflecting polarization state and the reflection coefficient of described thin film
Tangent angle corresponding to amplitude ratio respectively with the change curve of lambda1-wavelength, including:
Measure the reeflectance ratio of the reflection polarization state of described thin film；
It is calculated the phase contrast of the reflection polarization state of described thin film by below equation according to described reeflectance ratio
With the tangent angle corresponding to reflection coefficient amplitude ratio with the change curve of lambda1-wavelength:
Wherein, tan (Ψ)=| Rp/Rs|,Tan (Ψ) represents p light and the s of described reflection polarization state
The reflection coefficient amplitude ratio of light, Δ represents p light and the phase contrast of s luminous reflectivity, the R of described reflection polarization statepAnd RsRespectively
Represent described p light and the Fresnel reflection coefficient of s light,Represent described p light and the phase place of s luminous reflectivity respectively,
eiΔRepresenting the twiddle factor of plural number, ρ represents the reeflectance ratio of the reflection polarization state of described thin film, and ψ represents described reflection system
Number tangent angle corresponding to amplitude ratio.
Alternatively, the described successional critical thickness determining described thin film according to described change curve, including:
Obtain described thin film during thickening according to described change curve, along with described thin film by noncontinuity by
Gradually being changed into seriality, the peak shape of described change curve and peak position are also with change, and face the successional of described thin film
Undergo mutation at boundary's thickness, so that it is determined that the successional critical thickness of described thin film.
Alternatively, described method also includes:
According to scanning electron microscope, transmission electron microscope and atomic force microscope, the morphology characterization of described thin film is tested
Demonstrate,prove the accuracy of described change curve.
Alternatively, described method also includes:
Fresnel reflection coefficient according to described p light and s light be calculated the refractive index of described thin film, extinction coefficient and
Dielectric constant；
By described refractive index, extinction coefficient and dielectric constant and refractive index, extinction coefficient and the dielectric constant preset
Contrast, thus verify the accuracy of described change curve.
Alternatively, the material of described thin film be following at least one:
Au、Ag、Pt、Cu、Al、Ni、Fe、Co、V、Zn、Cr、W、C、Si、Ge、GaAs、SiC、TiO2、ZnO、ZnS、NiO、
Ta2O5、Nb2O5、V2O5、V2O3、CoO、Fe2O3、FeO、CuO、SiO2、Si3N4、、Al2O3, AlN, PMMA, Muscovitum, polyethylene, poly-
Tetrafluoroethene, polyvinylidene fluoride and polyimides.
Alternatively, the material of described substrate be following at least one:
Silicon, silicon dioxide, silicon nitride, carborundum, GaAs, gallium nitride, zinc oxide, microscope slide, mica sheet, FTO conduct electricity
Glass and ITO electro-conductive glass.
Alternatively, the manufacture method of described thin film include following at least one:
Electron beam evaporation, thermal evaporation, magnetron sputtering, ion beam sputtering, ion plating, atom sediment, pulsed laser deposition,
Chemical gaseous phase deposition, molecular beam epitaxy, sol-gel process, metal-organic decomposition method, liquid-solid method, oxidizing process, ion
Injection method and diffusion method.
Alternatively, the measuring method of the thickness of described thin film include following at least one:
Spiral micrometry, step instrument, atomic force microscope, scanning electron microscope, weighing method, capacitance method, electric-resistivity method, electricity
Sub-diffraction approach, equal thickness interference method, angle interferometric method, optical absorption method and Ellipsometric.
By technique scheme, spectroscopic ellipsometers arranges dispersion equation model and fit approach；Life on substrate
In the case of the thickness of long thin film is less than the film thickness preset, indirect approach to fitting is used to obtain the reflection polarization state of thin film
Phase contrast and reflection coefficient amplitude ratio corresponding to tangent angle respectively with the change curve of lambda1-wavelength；On substrate
In the case of the thickness of the thin film of growth is more than or equal to the film thickness preset, direct approach to fitting is used to obtain the reflection of thin film
Tangent angle corresponding to the phase contrast of polarization state and reflection coefficient amplitude ratio is respectively with the change curve of lambda1-wavelength；
And the successional critical thickness of thin film is determined according to change curve, solve the critical thickness determining film continuity at present
The problem of difficulty, accurately preparing and answering for nano photoelectric device, solaode, Infrared Detectors and biosensor
With, and relevant theoretical research has important directive significance.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described.It should be evident that the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to
Other accompanying drawing is obtained according to these figures.
Fig. 1 is the flow chart of the method for the critical thickness of the determination film continuity that one embodiment of the invention provides；
Fig. 2 is the AFM shape appearance figure of the 10nm thickness gold thin film that one embodiment of the invention provides；
Fig. 3 is the AFM shape appearance figure of the 15nm thickness gold thin film that one embodiment of the invention provides；
Fig. 4 is the AFM shape appearance figure of the 20nm thickness gold thin film that one embodiment of the invention provides；
Fig. 5 is the first change curve of the 10nm thickness gold thin film that the embodiment of the present invention provides；
Fig. 6 is the second change curve of the 10nm thickness gold thin film that the embodiment of the present invention provides；
Fig. 7 is the first change curve of the 15nm thickness gold thin film that the embodiment of the present invention provides；
Fig. 8 is the second change curve of the 15nm thickness gold thin film that the embodiment of the present invention provides；
Fig. 9 is the first change curve of the 20nm thickness gold thin film that the embodiment of the present invention provides；
Figure 10 is the second change curve of the 20nm thickness gold thin film that the embodiment of the present invention provides.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into the scope of protection of the invention.
Fig. 1 is the flow chart of the method for the critical thickness of the determination film continuity that one embodiment of the invention provides.Such as Fig. 1
Shown in, the method for the critical thickness of the determination film continuity that one embodiment of the invention provides includes:
In step S101, described spectroscopic ellipsometers arranges dispersion equation model and fit approach.
Then, in step s 102, the thickness of the thin film grown over the substrate is less than the feelings of the film thickness preset
Under condition, indirect approach to fitting is used to obtain corresponding to the phase contrast reflecting polarization state and the reflection coefficient amplitude ratio of described thin film
Tangent angle is respectively with the change curve of lambda1-wavelength.
And then, in step s 103, the thickness of the thin film grown over the substrate is more than or equal to the thin film preset
In the case of thickness, direct approach to fitting is used to obtain the phase contrast reflecting polarization state and the reflection coefficient amplitude ratio of described thin film
Corresponding tangent angle is respectively with the change curve of lambda1-wavelength.
Finally, in step S104, determine the successional critical thickness of described thin film according to described change curve.
Wherein, phase contrast and the reflection coefficient of the reflection polarization state of the described thin film of described employing direct approach to fitting acquisition shakes
Tangent angle corresponding to amplitude ratio respectively with the change curve of lambda1-wavelength, including: the reflection light measuring described thin film is inclined
The reeflectance ratio of polarization state；It is calculated the reflection polarization state of described thin film by below equation according to described reeflectance ratio
Phase contrast and reflection coefficient amplitude ratio corresponding to tangent angle with the change curve of lambda1-wavelength:
Wherein, tan (Ψ)=| Rp/Rs|,Tan (Ψ) represents p light and the s of described reflection polarization state
The reflection coefficient amplitude ratio of light, Δ represents p light and the phase contrast of s luminous reflectivity, the R of described reflection polarization statepAnd RsRespectively
Represent described p light and the Fresnel reflection coefficient of s light,Represent described p light and the phase of s luminous reflectivity respectively
Position, eiΔRepresent plural number twiddle factor, ρ represent described thin film reflection polarization state reeflectance ratio, ψ represent described instead
Penetrate the tangent angle corresponding to coefficient amplitude ratio.
Preferably, described method also includes: be calculated described thin according to the Fresnel reflection coefficient of described p light and s light
The refractive index of film, extinction coefficient and dielectric constant；By described refractive index, extinction coefficient and dielectric constant and the refraction preset
Rate, extinction coefficient and dielectric constant contrast, thus verify the accuracy of described change curve.Thereby, change can be improved
Change the accuracy of curve chart, thus can accurately determine the critical thickness of film continuity.
Specifically, from Fresnel reflection law:
Then, according to the law of refraction:Finally can try to achieve the thickness of thin film, refraction
The optical physics amounts such as rate, extinction coefficient and dielectric constant.Wherein, θ1Represent the angle of incidence of incident beam, θ2Represent incident beam
Refraction angle, ε1Represent dielectric constant of air, ε2Represent thin-film material refractive index.
Wherein, phase contrast and the reflection coefficient of the reflection polarization state of the described thin film of described employing indirect approach to fitting acquisition shakes
Tangent angle corresponding to amplitude ratio respectively with the change curve of lambda1-wavelength, including: thick less than the thin film preset to thickness
The thin film of degree is fitted, and obtains simple metal level；Described metal level adds the mixed layer of metal and air, and removes
Described metal level；Thickness and the scale parameter of changing described mixed layer carry out matching again, and obtain the reflection light of described thin film
Tangent angle corresponding to the phase contrast of polarization state and reflection coefficient amplitude ratio is with the change curve of lambda1-wavelength.
Specifically, the thin-skin model obtained after changing the thickness of described mixed layer and scale parameter arranges and can not only increase
Degree of fitting, and more meet actual pattern.Then, the reflection light of described thin film can be obtained according to the computing formula of direct approach to fitting
Tangent angle corresponding to the phase contrast of polarization state and reflection coefficient amplitude ratio is with the change curve of lambda1-wavelength.
Preferably, described method also includes: according to scanning electron microscope, transmission electron microscope and atomic force microscope
Morphology characterization to described thin film verifies the accuracy of described change curve.Thereby, can the most accurately determine that thin film is continuous
The critical thickness of property.
The application has carried out corresponding matching to the thin film of different-thickness.Less for thickness and be not by discrete nanometer
The thin film of grain composition, the most discontinuous chain thin film, then use the indirect approximating method of three step matchings.From fitting result,
Chain thin film discontinuous to same type, during the first step to the 3rd step matching, Minimum Mean Square Error is all gradually lowered,
Degree of fitting is gradually increased, and mathematical credibility is higher, illustrates to use the accuracy of air mixed layer；Simultaneously from scanning electron
The morphology characterizations such as microscope (SEM), transmission electron microscope (TEM) and atomic force microscope (AFM) also observe that and does not connects
There is narrow and small gap between granule in continuous thin film, i.e. demonstrate the existence of air layer.For the thin film that thickness is bigger, due to air
Layer disappears, and can use direct approach to fitting, i.e. directly adds simple material layer and is fitted, knowable to the result of matching, and matching
Thickness with experiment nominal thickness basically identical, illustrate in continuous film without air layer, i.e. use the accurate of direct approach to fitting
Degree height, also observes that continuous film surfacing from the morphology characterizations such as SEM, TEM and AFM simultaneously, can't see and deposit between granule
In gap, demonstrate the accuracy of fitting result.
Wherein, the described successional critical thickness determining described thin film according to described change curve, including: according to institute
State change curve and obtain described thin film during thickening, along with described thin film is gradually converted into by noncontinuity continuously
Property, the peak shape of described change curve and peak position are also with change, and occur at the successional critical thickness of described thin film
Sudden change, so that it is determined that the successional critical thickness of described thin film.
The information that thin film is relevant to seriality can be obtained further according to the change curve that matching obtains.Obtain from matching
The first change curve understand, along with the increase of film thickness, the optical information of independent substrate is destroyed, and amplitude ratio gradually increases
Adding, the signal of thin-film material gradually strengthens, and the signal of substrate gradually weakens.Knowable to the second change curve that matching obtains,
The peak shape when existence of thin film can change only independent substrate and peak position, and Substrate signal is first weakened at long-wave band,
And retained at short-wave band, the light mainly due to short-wave band can be directly over substrate reflection arrive without thin-film material
In air, the light of long-wave band arrives substrate after then must first passing through thin-film material again, is finally re-reflected in air, therefore,
The optical signalling of substrate is weakened.When thin film increases to certain thickness to the continuous critical localisation with discontinuous thin film, shortwave
Peak shape at Duan can change and becomes apparent from, and at long-wave band, thin-film material signal increases higher, now can at certain wave band middle phase
Undergoing mutation in position, the now coupling of air, thin-film material and substrate three is the strongest, can be used as distinguishing continuously with discontinuous
The mark of thin film.When critical localisation is crossed in film thickness continuation increase, in detection wavelength band, the signal of substrate is all cut
Weak, what the first change curve and the second change curve directly reflected is the optical information of thin-film material, i.e. substrate quilt completely
Thin-film material is covered, and thus can determine the successional critical thickness of thin-film material according to the technical method of ellipse inclined matching
Degree.
The comprehensive existing ellipse inclined matching means of the application, have been carried out accurately the thin-film material of dissimilar different-thickness
Matching, wherein uses three step fitting processs to discontinuous chain thin film, in conjunction with fitting result and scanning shape appearance figure, the method is described
Not only meet mathematical degree of fitting, and the most more meet the actual pattern of thin film, test the optics thing obtained simultaneously
The results such as reason amount such as refractive index n and extinction coefficient k are the most accurate.Thicker continuous film is then used direct approach to fitting, root
Can judge continuous and discontinuous thin film exactly according to the first change curve in fitting result and the second change curve
Boundary, the method is prepared for the accurate of nano photoelectric device, solaode, Infrared Detectors and biosensor etc. and answer
With and relevant theoretical research there is important directive significance.
Wherein, thin-film material can be metal, quasiconductor and insulator.Wherein, metal material include but not limited to
Au, Ag, Pt, Cu, Al, Ni, Fe, Co, V, Zn, Cr, W etc., prioritizing selection Au, Ag, Pt, Cu, Al；Semi-conducting material includes, but
It is not limited only to C, Si, Ge, GaAs, SiC, TiO2、ZnO、ZnS、NiO、Ta2O5、Nb2O5、V2O5、V2O3、CoO、Fe2O3、FeO、CuO
Deng, prioritizing selection C, Si, Ge, GaAs, SiC, TiO2、ZnO；Semi-conducting material include but not limited to SiO2、Si3N4、、
Al2O3, AlN, PMMA, Muscovitum, polyethylene, politef, polyvinylidene fluoride and polyimides etc., prioritizing selection SiO2、
Si3N4、、Al2O3、AlN、PMMA.The number of plies of thin film is 1～100 layer, prioritizing selection 1～10 layers；The thickness of thin film be 1nm～
10mm, prioritizing selection 1nm～1 μm, backing material include but not limited to silicon, silicon dioxide, silicon nitride, carborundum, arsenic
Gallium, gallium nitride, zinc oxide, microscope slide, mica sheet, FTO electro-conductive glass and ITO electro-conductive glass etc., prioritizing selection silicon, titanium dioxide
Silicon, microscope slide, mica sheet, FTO electro-conductive glass and ITO electro-conductive glass.The preparation method of thin film include but not limited to electron beam
Evaporation, thermal evaporation, magnetron sputtering, ion beam sputtering, ion plating, atom sediment, pulsed laser deposition, chemical gaseous phase deposition,
Molecular beam epitaxy, sol-gel process, metal-organic decomposition method, liquid-solid method, oxidizing process, ion implantation and diffusion method
Deng, prioritizing selection electron beam evaporation, thermal evaporation, magnetron sputtering, atom sediment, pulsed laser deposition and chemical gaseous phase deposition.
For above-mentioned prepared thin-film device, for accurately analyzing its thin film physics character, especially optical property, first
Needing to test film thickness, the method that can accurately test thickness generally has direct method and indirect method, wherein direct method bag
Include but be not limited only to spiral micrometry, step instrument, atomic force microscope and scanning electron microscope etc., indirect method include but not
It is only limitted to weighing method, capacitance method, electric-resistivity method, method of electron diffraction, equal thickness interference method, angle interferometric method, optical absorption method and ellipse inclined
Shake method etc..
The method that the present invention provides is described below in detail as a example by gold nanometer film.
For the matching of gold nanometer film, the test instrunment used is spectroscopic ellipsometers, the model that dispersion equation selects
It it is Drude-Lorentz model.The fit approach selected is direct matching and indirect matching.Wherein, film thickness more than or etc.
Direct approach to fitting is used when 15nm.Use indirect approach to fitting, i.e. three-step approach matching when film thickness is 10nm, the most directly intend
Close simple metal level, add the mixed layer of metal and air the most on the metal layer, finally remove metal level, change mixed layer
Thickness and scale parameter after matching again, model now arranges and can not only increase degree of fitting and more meet actual pattern.
The test instrunment that the surface topography map of the three kinds of different gold nanometer films related in the present embodiment uses is AFM, three
Plant the surface topography map of different gold nanometer films as in Figure 2-4, AFM scheme, along with the increase of gold nanometer film thickness,
I.e. growth time gradually increases, and the size of clustered particles is gradually increased, thickness from 10nm, 15nm to 20nm time, gold grain exists
The when of cross growth, between granule, the distance of slit is gradually reduced, i.e. composition of air reduces, and thin film surface planeness increases, by
Gradually form continuous print thin film.
Gold nanometer film thick for 10nm uses the optical results after ellipsometer matching as follows.Between the fit approach used is
Connecing matching, i.e. three step fitting processs, its fitting result is as shown in Table 1.
The ellipse inclined three-step approach fitting data of table one 10nm gold thin film
As shown in Table 1, the gold nanometer film that 10nm is thick, the thickness of directly matching first and MSE are respectively
11.40nm and 0.902；After second time adds air mixed layer, MSE is 0.901, and degree of fitting is almost unchanged, individually the thickness of gold
For the thickness 1.35nm of 10.00nm and mixed layer, wherein air proportion is 0.030, therefore the effective thickness of gold is
11.31nm；After third time removes layer gold, MSE is 0.900, the most small raising of degree of fitting, and the thickness of mixed layer is 11.36nm, empty
Gas proportion is 0.038, therefore the effective thickness of gold is 10.93nm.The gold nanometer film of 10nm thickness is understood from fitting result
The composition of middle air is considerably less, this thin film is described neither discrete nano-particle, also the most continuously, is discontinuous
Chain thin film, this conclusion also can be proved from scanning electron microscope (SEM) photograph.First change curve figure of matching and the second change song
Line chart figure is distinguished the most as shown in Figure 5 and Figure 6, as seen from the figure, on the premise of high precision matching, when in substrate Si O2Upper plating
During thick for 10nm gold thin film, the peak width of the second change curve is relative to single SiO2Become narrower, and peak shape becomes more acute
Sharp, the load mainly due to gold thin film destroys SiO2Interference periods；Can be also found that simultaneously the first change curve and
First there is significantly change in long-wave band in the second change curve, the signal of substrate silicon dioxide is fallen into oblivion by the signal of gold thin film
Not yet, this is that directly in substrate reflection to air, Gu Duanboduanchu remains with owing to the light that wavelength is shorter can be without gold
SiO2The signal of silicon oxide, longer wavelengths of light then must first pass through gold thin film, be reflected to sky again after then arriving substrate
In gas, therefore SiO2Signal weakened.
Gold nanometer film thick for 15nm uses the optical results after ellipsometer matching as follows.The fit approach used is straight
Connect matching.Due in the gold thin film that 10nm is thick air component content seldom, the difference of direct matching and indirect matching not quite,
Therefore thick more than 10nm gold thin film can use direct fit approach, by the first change curve and the second change curve peak
The change of shape, it is judged that the seriality of thin film.First change curve of matching and the second change curve are respectively such as Fig. 7 and Fig. 8
Shown in, as seen from the figure, the amplitude ratio of the long-wave band in the first change curve that 15nm is thick is higher relative to 10nm gold thin film, mainly
The signal being gold is higher, makes the reflexive of light weaken；Second change curve moves to right than 10nm gold thin film entirety, at short-wave band
Peak shape is more sharp-pointed, and the peak shape of long-wave band is more smooth, and there occurs sudden change at the middle wave band of about 500nm, i.e. the shortest
In wave-length coverage, phase place there occurs the change of 2 π.It can thus be appreciated that the composition of air has already decreased to pole in thin film thick for 15nm
Limit, during now light wave enters into minimum slit, air, gold and SiO2The coupling of three kinds of materials is the strongest, and therefore phase place is sent out
Having given birth to sudden change, thickness now can be as the demarcation line of discontinuous thin film to continuous film.
Gold nanometer film thick for 20nm uses the optical results after ellipsometer matching as follows.Gold thin film thick for 20nm is directly intended
The first change curve closed and the second change curve are respectively such as Fig. 9 and Figure 10.Knowable to the first change curve of matching,
Along with gold thin film thickness increases, amplitude ratio is gradually increased, and the signal of gold gradually strengthens；Understand from the second change curve, thick
Degree increases peak position and continues to move to right, and from 15nm to 20nm, the peak position pop-off of sudden change, independent SiO2Signal by completely
Falling into oblivion, i.e. gold is when being grown into, and is covered by minimum air layer, and thin film now has reached the most continuously, the first change
Moving in the peak shape of curve chart, the peak position of the second change curve is pressed narrower, and the signal of gold is higher.
The pattern test data of summary and ellipse inclined fitting result, it is known that gold thin film thick for 15nm is to discriminate between continuous and non-
The critical point of continuous film, is i.e. discontinuous chain thin film when 10～15nm, is complete continuous film when more than 15nm.With
The increase of gold thickness, from amplitude image, the signal of substrate silicon dioxide gradually weakens, and the signal of gold gradually strengthens, by phase
Bitmap understands, and gold thickness increase can cause peak position to move to right, and at critical point, phase place can be undergone mutation, air, gold and substrate three
The coupling planting material is the strongest, in this, as the mark distinguishing two kinds of thin film.This next really from film preparation to ellipse inclined matching
The method of the critical thickness determining film continuity has important finger for experiment and the theoretical research of current nano photoelectric device
Lead meaning.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, technical scheme can be carried out multiple letter
Monotropic type, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention, at not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy illustrates the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the method for the critical thickness determining film continuity, it is characterised in that use spectroscopic ellipsometers measurement to be grown in
The thickness of the thin film on substrate and optical property, described method includes:
Described spectroscopic ellipsometers arranges dispersion equation model and fit approach；
In the case of the thickness of the thin film grown over the substrate is less than the film thickness preset, indirect approach to fitting is used to obtain
Tangent angle corresponding to the phase contrast of the reflection polarization state of described thin film and reflection coefficient amplitude ratio is respectively with incident light wave
Long change curve；
In the case of the thickness of the thin film grown over the substrate is more than or equal to the film thickness preset, use direct matching
Tangent angle corresponding to the phase contrast of the reflection polarization state of the method described thin film of acquisition and reflection coefficient amplitude ratio is respectively with entering
Penetrate the change curve of optical wavelength；
The successional critical thickness of described thin film is determined according to described change curve.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that between described employing
Connect the tangent angle that fitting process obtains corresponding to the reflection phase contrast of polarization state of described thin film and reflection coefficient amplitude ratio to divide
Not with the change curve of lambda1-wavelength, including:
Thickness is fitted less than the thin film of the film thickness preset, obtains simple metal level；
Described metal level adds the mixed layer of metal and air, and removes described metal level；
Change the thickness of described mixed layer and scale parameter carries out matching again, and obtain the reflection polarization state of described thin film
Tangent angle corresponding to phase contrast and reflection coefficient amplitude ratio is with the change curve of lambda1-wavelength.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described employing is straight
Connect the tangent angle that fitting process obtains corresponding to the reflection phase contrast of polarization state of described thin film and reflection coefficient amplitude ratio to divide
Not with the change curve of lambda1-wavelength, including:
Measure the reeflectance ratio of the reflection polarization state of described thin film；
The phase contrast of reflection polarization state of described thin film it is calculated by below equation with anti-according to described reeflectance ratio
Penetrate the change curve with lambda1-wavelength of the tangent angle corresponding to coefficient amplitude ratio:
Wherein, tan (Ψ)=| Rp/Rs|,Tan (Ψ) represents the p light of described reflection polarization state and s light
Reflection coefficient amplitude ratio, Δ represents p light and the phase contrast of s luminous reflectivity, the R of described reflection polarization statepAnd RsRepresent respectively
Described p light and the Fresnel reflection coefficient of s light,Represent described p light and the phase place of s luminous reflectivity, e respectivelyiΔ
Representing the twiddle factor of plural number, ρ represents the reeflectance ratio of the reflection polarization state of described thin film, and ψ represents described reflection coefficient
Tangent angle corresponding to amplitude ratio.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described according to institute
State change curve and determine the successional critical thickness of described thin film, including:
Described thin film is obtained during thickening, along with described thin film is gradually turned by noncontinuity according to described change curve
Becoming seriality, the peak shape of described change curve and peak position are also with change, and in the successional critical thickness of described thin film
Undergo mutation at degree, so that it is determined that the successional critical thickness of described thin film.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described method is also
Including:
According to scanning electron microscope, transmission electron microscope and atomic force microscope, the morphology characterization of described thin film is verified institute
State the accuracy of change curve.
The method of the critical thickness determining film continuity the most according to claim 3, it is characterised in that described method is also
Including:
Fresnel reflection coefficient according to described p light and s light is calculated the refractive index of described thin film, extinction coefficient and dielectric
Constant；
Described refractive index, extinction coefficient and dielectric constant are carried out with refractive index, extinction coefficient and the dielectric constant preset
Contrast, thus verify the accuracy of described change curve.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described thin film
Material be following at least one:
Au、Ag、Pt、Cu、Al、Ni、Fe、Co、V、Zn、Cr、W、C、Si、Ge、GaAs、SiC、TiO2、ZnO、ZnS、NiO、Ta2O5、
Nb2O5、V2O5、V2O3、CoO、Fe2O3、FeO、CuO、SiO2、Si3N4、、Al2O3, AlN, PMMA, Muscovitum, polyethylene, polytetrafluoroethyl-ne
Alkene, polyvinylidene fluoride and polyimides.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described substrate
Material be following at least one:
Silicon, silicon dioxide, silicon nitride, carborundum, GaAs, gallium nitride, zinc oxide, microscope slide, mica sheet, FTO electro-conductive glass
And ITO electro-conductive glass.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described thin film
Manufacture method include following at least one:
Electron beam evaporation, thermal evaporation, magnetron sputtering, ion beam sputtering, ion plating, atom sediment, pulsed laser deposition, chemistry
Vapour deposition, molecular beam epitaxy, sol-gel process, metal-organic decomposition method, liquid-solid method, oxidizing process, ion implanting
Method and diffusion method.
The method of the critical thickness determining film continuity the most according to claim 1, it is characterised in that described thin film
The measuring method of thickness include following at least one:
Spiral micrometry, step instrument, atomic force microscope, scanning electron microscope, weighing method, capacitance method, electric-resistivity method, electronics spread out
Penetrate method, equal thickness interference method, angle interferometric method, optical absorption method and Ellipsometric.
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| CN107192857A (en) * | 2016-03-14 | 2017-09-22 | 中国科学院沈阳自动化研究所 | A kind of nano film thickness detection means and its method based on ultrasonic AFM |
| CN107514977A (en) * | 2017-08-31 | 2017-12-26 | 长江存储科技有限责任公司 | A kind of method and device for monitoring storage medium thickness abnormity |
| CN107560557A (en) * | 2017-08-31 | 2018-01-09 | 长江存储科技有限责任公司 | A kind of method and device for measuring deep hole wall films thickness |
| CN108180879A (en) * | 2017-11-30 | 2018-06-19 | 中国电子科技集团公司第十三研究所 | The valued methods and preparation method of ultra-thin silica membrane print |
| CN108728812A (en) * | 2017-04-24 | 2018-11-02 | 神华集团有限责任公司 | A method of preparing film |
| CN109470154A (en) * | 2018-12-26 | 2019-03-15 | 武汉颐光科技有限公司 | Value measurement method at the beginning of a kind of film thickness suitable for spectroscopic ellipsometers |
| CN111076668A (en) * | 2019-12-24 | 2020-04-28 | 天津大学 | Differential reflection spectrum measurement method for nano-thickness SiO2 thickness |
| CN111121653A (en) * | 2019-12-31 | 2020-05-08 | 武汉颐光科技有限公司 | Single-layer film critical thickness estimation value calculation method |
| CN111207677A (en) * | 2020-01-13 | 2020-05-29 | 中国人民解放军国防科技大学 | Method for measuring thickness and refractive index of dielectric film |
| CN111207678A (en) * | 2020-01-13 | 2020-05-29 | 中国人民解放军国防科技大学 | Non-rotating film thickness and refractive index measuring method |
| CN113267454A (en) * | 2021-05-26 | 2021-08-17 | 中国工程物理研究院激光聚变研究中心 | Thin film quality detection method, thin film quality detection device, electronic device, and storage medium |
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| CN107192857A (en) * | 2016-03-14 | 2017-09-22 | 中国科学院沈阳自动化研究所 | A kind of nano film thickness detection means and its method based on ultrasonic AFM |
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| CN107514977A (en) * | 2017-08-31 | 2017-12-26 | 长江存储科技有限责任公司 | A kind of method and device for monitoring storage medium thickness abnormity |
| CN107560557A (en) * | 2017-08-31 | 2018-01-09 | 长江存储科技有限责任公司 | A kind of method and device for measuring deep hole wall films thickness |
| CN108180879A (en) * | 2017-11-30 | 2018-06-19 | 中国电子科技集团公司第十三研究所 | The valued methods and preparation method of ultra-thin silica membrane print |
| CN109470154A (en) * | 2018-12-26 | 2019-03-15 | 武汉颐光科技有限公司 | Value measurement method at the beginning of a kind of film thickness suitable for spectroscopic ellipsometers |
| CN111076668A (en) * | 2019-12-24 | 2020-04-28 | 天津大学 | Differential reflection spectrum measurement method for nano-thickness SiO2 thickness |
| CN111121653A (en) * | 2019-12-31 | 2020-05-08 | 武汉颐光科技有限公司 | Single-layer film critical thickness estimation value calculation method |
| CN111207677A (en) * | 2020-01-13 | 2020-05-29 | 中国人民解放军国防科技大学 | Method for measuring thickness and refractive index of dielectric film |
| CN111207678A (en) * | 2020-01-13 | 2020-05-29 | 中国人民解放军国防科技大学 | Non-rotating film thickness and refractive index measuring method |
| CN111207678B (en) * | 2020-01-13 | 2021-06-15 | 中国人民解放军国防科技大学 | Non-rotating film thickness and refractive index measuring method |
| CN113267454A (en) * | 2021-05-26 | 2021-08-17 | 中国工程物理研究院激光聚变研究中心 | Thin film quality detection method, thin film quality detection device, electronic device, and storage medium |
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