CN108728812A - A method of preparing film - Google Patents
A method of preparing film Download PDFInfo
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- CN108728812A CN108728812A CN201710269837.XA CN201710269837A CN108728812A CN 108728812 A CN108728812 A CN 108728812A CN 201710269837 A CN201710269837 A CN 201710269837A CN 108728812 A CN108728812 A CN 108728812A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
- C23C14/547—Controlling the film thickness or evaporation rate using measurement on deposited material using optical methods
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Abstract
This application discloses a kind of determination method of optical parameter of film and preparation technology parameter correspondence, the properties such as consistency for solving the problems, such as cannot to quantitatively determine each layer film in the prior art, including：Film is prepared respectively under multiple predetermined preparation technology parameters；The optical parameter for determining each film prepared under the multiple predetermined preparation technology parameter obtains the optical parameter and preparation technology parameter correspondence of the film, to prepare the film for meeting preparation demand according to the correspondence.Disclosed herein as well is a kind of methods preparing film.
Description
Technical field
This application involves field of photoelectric technology more particularly to a kind of method preparing film and a kind of optics of film
The determination method of parameter and preparation technology parameter correspondence.
Background technology
With the development of micro fabrication, film is widely used in every field, and wherein metallic film exists
The fields such as mechanical subject, electronics, magnetics and optics suffer from important application.Thin film preparation process can be widely applied to light
Electro-technical field, for example it is applied to copper indium gallium selenide (CuInGaSe2, CIGS) thin-film solar cells preparation in.
During preparing film, the different film of consistency is often prepared according to different needs, for example,
The molybdenum back electrode layer of CIGS thin film solar cell usually contains the different molybdenum film of multiple dense degree, wherein first layer molybdenum film is used
It combines closely in the substrate with CIGS thin film solar cell, the performance meeting of solar cell when the gas porosity of the layer film is higher
Preferably, second layer molybdenum film is for reducing resistivity, then the performance of solar cell can be preferable when the layer film density is higher.
In the prior art, when expectation prepares the different film of consistency, the cause of each layer film cannot be quantitatively determined
The properties such as density.
Invention content
The embodiment of the present application provides a kind of determination method of the optical parameter of film and preparation technology parameter correspondence, uses
In properties such as the consistency for solving the problems, such as cannot to quantitatively determine each layer film in the prior art.
The embodiment of the present application provides a kind of method preparing film, each for solving to quantitatively determine in the prior art
The problem of properties such as the consistency of layer film.
The embodiment of the present application uses following technical proposals：
A kind of determination method of the optical parameter of film and preparation technology parameter correspondence, including：
Film is prepared respectively under multiple predetermined preparation technology parameters；
The optical parameter for determining each film prepared under the multiple predetermined preparation technology parameter, obtains the light of the film
Parameter and preparation technology parameter correspondence are learned, to prepare the film for meeting preparation demand according to the correspondence.
A method of film is prepared, including：
According to the preparation demand of film to be prepared, the first correspondence and the second correspondence, determination prepares the film
Preparation technology parameter and preparation time, wherein the preparation demand includes the thickness and optical parameter of film to be prepared, described
First correspondence is the optical parameter and preparation technology parameter correspondence of the film, and second correspondence is described
The preparation time of film and the correspondence of thickness；
According to determining preparation technology parameter and preparation time, the film is prepared.
Above-mentioned at least one technical solution that the embodiment of the present application uses can reach following advantageous effect：
In the application, it can be determined according to the preparation demand of film to be prepared, the first correspondence and the second correspondence
Prepare the preparation technology parameter and preparation time of the film, wherein preparation demand includes the thickness and Optical Parametric of film to be prepared
Number, the first correspondence are the optical parameter and preparation technology parameter correspondence of the film, and the second correspondence is the film
The correspondence of preparation time and thickness prepare the film then according to determining preparation technology parameter and preparation time.This
In application, the properties such as consistency for quantitatively characterizing film by the optical parameter of film just can pass through film in this way
Optical parameter quantitatively characterizes the preparation demand of film, when it is expected to prepare the film of certain consistency, can pass through Optical Parametric
Correspondence between number and preparation technology parameter prepares the film for meeting preparation demand by controlling preparation technology parameter.
Description of the drawings
Attached drawing described herein is used for providing further understanding of the present application, constitutes part of this application, this Shen
Illustrative embodiments and their description please do not constitute the improper restriction to the application for explaining the application.In the accompanying drawings：
Fig. 1 is a kind of structural schematic diagram of molybdenum back electrode layer provided by the embodiments of the present application；
The measured value and match value for the molybdenum film that Fig. 2, which is sputtering pressure provided by the embodiments of the present application, to be prepared when being 0.1Pa show
It is intended to；
The measured value and match value for the molybdenum film that Fig. 3, which is sputtering pressure provided by the embodiments of the present application, to be prepared when being 0.2Pa show
It is intended to；
The measured value and match value for the molybdenum film that Fig. 4, which is sputtering pressure provided by the embodiments of the present application, to be prepared when being 0.3Pa show
It is intended to；
The measured value and match value for the molybdenum film that Fig. 5, which is sputtering pressure provided by the embodiments of the present application, to be prepared when being 0.7Pa show
It is intended to；
Measured value and the match value signal for the molybdenum film that Fig. 6, which is sputtering pressure provided by the embodiments of the present application, to be prepared when being 1Pa
Figure；
Fig. 7 is the refractive index and extinction coefficient of the molybdenum film prepared under multiple predetermined sputtering pressures provided by the embodiments of the present application
With the variation relation schematic diagram of wavelength；
Fig. 8 is the molybdenum film prepared under multiple predetermined sputtering pressures provided by the embodiments of the present application, when wavelength is 550nm
Refractive index and extinction coefficient with sputtering pressure variation relation schematic diagram；
Fig. 9 is the structural schematic diagram of the molybdenum back electrode layer under the first specific implementation mode provided by the embodiments of the present application；
Figure 10 is the structural schematic diagram of the molybdenum back electrode layer under second of specific implementation mode provided by the embodiments of the present application.
Specific implementation mode
To keep the purpose, technical scheme and advantage of the application clearer, below in conjunction with the application specific embodiment and
Technical scheme is clearly and completely described in corresponding attached drawing.Obviously, described embodiment is only the application one
Section Example, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, shall fall in the protection scope of this application.
Below in conjunction with attached drawing, the technical solution that each embodiment of the application provides is described in detail.
Implement for properties, the application such as the consistency that solves the problems, such as cannot to quantitatively determine each layer film in the prior art
Example provides a kind of determination method of the optical parameter of film and preparation technology parameter correspondence, and the implementation process of this method includes
The following steps：
Step 11, film is prepared respectively under multiple predetermined preparation technology parameters；
Wherein, the preparation technology parameter in the embodiment of the present application at least can be that sputtering pressure and sputtering power etc. prepare work
Skill parameter.It should be noted that the film in the embodiment of the present application can be metallic film, such as molybdenum, titanium, can also be inorganic
Material film, such as glass, silica etc. have the film of light transmitting property.
It, first can be to being used to prepare the glass of film before preparing film respectively under multiple predetermined preparation technology parameters
Substrate is cleaned, and carries out drying and processing to the surface of the glass substrate after cleaning, then using the glass substrate as substrate,
Film is prepared under multiple predetermined preparation technology parameters.It will be apparent to those skilled in the art that described here is multiple pre-customized standby
Technological parameter is determined by the characteristic for specific a certain film, under multiple preparation technology parameters of these determinations,
The optical parameter of the film of preparation should have certain correspondence with corresponding preparation technology parameter.
Step 12, the optical parameter for determining each film prepared under multiple predetermined preparation technology parameters, obtains the light of film
Parameter and preparation technology parameter correspondence are learned, to prepare the film for meeting preparation demand according to the correspondence.
Before the optical parameter for determining each film prepared under multiple predetermined preparation technology parameters, first have to determine prepare it is thin
Then first optical parameter of the glass substrate after cleaning, drying before film determines the glass base for preparing and having each film respectively again
Second optical parameter of piece finally has the second optical parameter of each film further according to the first optical parameter and preparation, determines respectively
The optical parameter of each film, and establish the preparation technology parameters such as multiple scheduled sputtering pressures and multiple scheduled sputtering powers with
The correspondence of the optical parameter of the first film, to obtain the optical parameter and preparation technology parameter correspondence of film.This
Apply for that the optical parameter in embodiment at least may include refractive index and extinction coefficient etc..
It should be noted that the first optical parameter and the second optical parameter in the embodiment of the present application are to pass through following methods
Determining：First can use ellipsometer measurement measured medium ellipsometric parameter, that is, determine measured medium relative amplitude decaying and
The difference of phase shift；Then according to the difference of determining relative amplitude decaying and phase shift, the optical parameter of measured medium is determined,
Wherein, which can be the glass substrate that glass substrate and/or preparation described above have film.In addition, tested be situated between
The optical parameter of matter can also be the reflectance spectrum of measured medium determining first, then determine measured medium according to the reflectance spectrum
Relative amplitude decaying and relative displacement difference, finally according to the relative amplitude of determining measured medium decaying and relative displacement it
Difference determines.
In the application, since film can be prepared respectively under multiple predetermined preparation technology parameters, then determine multiple pre-
Determine the optical parameter of each film prepared under preparation technology parameter, obtains the film prepared under multiple predetermined preparation technology parameters
Optical parameter and preparation technology parameter correspondence, due to optical parameter and the properties such as its consistency of film have it is direct corresponding
Relationship can prepare the film for meeting preparation demand, so as to solve the prior art according to determining determination relationship in this way
In the problem of cannot quantitatively determining the properties such as the consistency of each layer film.
Based on the determination method of the optical parameter and preparation technology parameter correspondence of film provided by the present application, the application
Embodiment also provides a kind of method preparing film, the densification for solving cannot to quantitatively determine each layer film in the prior art
The problem of properties such as degree, including the following steps：
Step 21, it according to the preparation demand of film to be prepared, the first correspondence and the second correspondence, determines to prepare and be somebody's turn to do
The preparation technology parameter and preparation time of film；
Wherein, preparation demand includes the thickness and optical parameter of film to be prepared, and the first correspondence is the light of the film
Parameter and preparation technology parameter correspondence are learned, the second correspondence is the correspondence of the preparation time and thickness of the film.
Preparation technology parameter includes at least one of sputtering pressure and sputtering power.Optical parameter includes refractive index and extinction coefficient.
For ease of when preparing film, the properties such as the consistency of film can be quantitatively determined according to the preparation demand of film,
The embodiment of the present application predefines the correspondence between the optical parameter and preparation technology parameter of film, i.e., first corresponds to pass
The determination process of system, the first correspondence is the optical parameter pass corresponding with preparation technology parameter of film described above
System, will not be described in great detail here.
Second correspondence can measure the thickness and preparation time of film to be prepared by ellipsometer, obtain the film
Deposition rate, to obtain the thickness of film to be prepared and the correspondence of preparation time, wherein the specific calculating of deposition rate
Formula is：Deposition rate=thickness/time.
After determining the first correspondence and the second correspondence, then can according to the preparation demand of film to be prepared,
That is the optical parameter and thickness of the film to be prepared, the first correspondence and the second correspondence determine the preparation for preparing the film
Technological parameter and preparation time.
Step 22, according to determining preparation technology parameter and preparation time, the film is prepared.
It, then can be according to the preparation technology parameter after the preparation technology parameter and preparation time of film to be prepared is determined
And preparation time, prepare the film for meeting preparation demand.
In conjunction with inventive concept same as described above, for ease of quantitatively determine molybdenum back electrode layer each layer film consistency
Etc. properties below for preparing molybdenum back electrode layer, be described in detail to the better CIGS thin film solar cell of processability
Method provided by the embodiments of the present application.
With the increasingly depleted of the energy and increasingly sharpening for environmental pollution, solar energy is as the unlimited reproducible no dirt of the earth
The energy is contaminated, extensive concern is gradually caused, wherein since CIGS thin film solar cell only needs several microns of thickness can be real
Existing opto-electronic conversion, is the ideal material for reducing cost and improving photon cycle, becomes a kind of following most potential battery.CIGS
Thin-film solar cells is generally by substrate, back electrode, CIGS absorbed layers, CdS buffer layers, ZnO Window layers, transparent electrode and aluminium electricity
Pole forms.Since molybdenum back electrode layer is directly contacted with CIGS absorbed layers, the performance of CIGS absorbed layers will be directly affected, to influence
The performance of entire thin-film solar cells.
The embodiment of the present application provides a kind of preferred embodiment, as shown in Figure 1, being carried on the back for molybdenum provided by the embodiments of the present application
The structural schematic diagram of electrode layer, the molybdenum back electrode layer include weaker zone, compacted zone and passivation layer.Wherein, weaker zone is used for and lining
Bottom is tightly combined, and compacted zone is used to control the growth of CIGS absorbed layers for reducing resistivity, passivation layer.The molybdenum back electrode layer
It prepares, may include the following steps：
Step 31, it according to the preparation demand of molybdenum back electrode layer to be prepared, the first correspondence and the second correspondence, determines
When prepared by the first preparation technology parameter and the first preparation time of weaker zone, the second preparation technology parameter of compacted zone and second
Between and passivation layer third preparation technology parameter and third preparation time；
Wherein, preparation demand includes the thickness and optical parameter of molybdenum back electrode layer to be prepared, and the first correspondence is molybdenum film
Optical parameter and preparation technology parameter correspondence, the second correspondence be molybdenum film preparation time it is corresponding with thickness pass
System.Optical parameter includes refractive index and extinction coefficient.Preparation technology parameter includes sputtering pressure, and/or sputtering power.
For ease of when preparing molybdenum back electrode layer, the property such as the consistency of each layer molybdenum film of molybdenum back electrode layer can be quantitatively determined
Matter, the embodiment of the present application predefine the correspondence between the optical parameter and preparation technology parameter of molybdenum film, i.e., first corresponds to
Relationship includes the following steps：
Step i determines the optical parameter of glass substrate.Specifically, glass substrate is cleaned first, then determines the glass base
The the first parameter Is and the second parameter Ic of piece determine the optics of glass substrate finally according to the first parameter Is and the second parameter Ic
Parameter, the i.e. refractive index and extinction coefficient of glass substrate.Wherein, the first parameter Is=sin (2 ψ) × sin (Δ), the second parameter
Ic=sin (2 ψ) × cos (Δ), ψ is relative amplitude decaying, and Δ is the difference of phase shift, and ψ and Δ can be surveyed by ellipsometer
?.
Step ii prepares molybdenum film using the glass substrate as substrate under multiple predetermined preparation technology parameters.Determining glass
After the optical parameter of substrate, using the glass substrate as substrate, molybdenum film is prepared under multiple predetermined preparation technology parameters.The application is real
Apply example and a kind of optional embodiment be provided, under multiple scheduled sputtering pressures, i.e., respectively sputtering pressure be 0.1Pa,
When 0.2Pa, 0.3Pa, 0.7Pa and 1Pa, using glass substrate as substrate, molybdenum film of the thickness within the scope of 10~30nm is prepared.
Step iii determines the optical parameter of the molybdenum film prepared under multiple predetermined preparation technology parameters, obtains the first correspondence pass
System.Distinguished in measuring process ii by ellipsometer, prepared by when sputtering pressure 0.1Pa, 0.2Pa, 0.3Pa, 0.7Pa and 1Pa
The ellipsometric parameter of molybdenum film determines the refractive index and extinction coefficient of these molybdenum films further according to the ellipsometric parameter of measurement, such as Fig. 2~6 point
It Wei not sputtering pressure the first parameter Is and the second parameter of the molybdenum film that prepare when being 0.1Pa, 0.2Pa, 0.3Pa, 0.7Pa and 1Pa
The measured value and match value of Ic.
The match value of according to fig. 2~Fig. 6, establishes optical model, obtains preparing molybdenum film under this five kinds of scheduled sputtering pressures
Refractive index and extinction coefficient with wavelength variation relation, as shown in Figure 7.Such as draw a conclusion as can be drawn from Figure 7：Work as sputtering pressure
When relatively low, the refractive index and extinction coefficient of molybdenum film work as sputtering pressure closer to the refractive index and extinction coefficient of intrinsic metal molybdenum
When gradually rising from 0.1Pa to 1Pa, the refractive index and extinction coefficient of molybdenum film then continuously decrease.
According to effective media theory (Effective Medium Theory, EMT), in multiple predetermined preparation technology parameters
The molybdenum film of lower preparation can be equivalent to molybdenum mixed with air composition structure, when molybdenum film interior solid degree is smaller, refractive index and
Extinction coefficient got over then closer to the refractive index of air and extinction coefficient, inside molybdenum film consistency it is larger when, then its refractive index and disappear
Refractive index and extinction coefficient of the photosystem closer to intrinsic molybdenum.As shown in figure 8, the molybdenum prepared under five kinds of predetermined sputtering pressures
Film, wavelength be 550nm when refractive index and extinction coefficient with sputtering pressure variation relation schematic diagram.It can be according to Fig. 8
Wavelength sputtering pressure required when being prepared to it according to the consistency of molybdenum film when being 550nm carries out quantitative calculating.
It should be noted that in practical applications, since weaker zone is used to be tightly combined with substrate, then needing to prepare fine and close
Lower molybdenum film is spent as the weaker zone, such as wavelength refractive index n ∈ [2,3] at 550nm and extinction coefficient k ∈ [1,
2.4] the molybdenum film prepared under corresponding preparation technology parameter, compacted zone then need the higher molybdenum of consistency for reducing resistivity
Film is as the compacted zone, such as refractive index n ∈ [2,3] and extinction coefficient k ∈ [1,2] corresponding preparation of the wavelength at 550nm
The molybdenum film prepared under technological parameter, passivation layer are used to control the growth of CIGS absorbed layers, then need to prepare consistency between loose
Molybdenum film between layer and compacted zone is as the passivation layer.
Then the specific implementation of step 31 is the preparation demand first according to each layer molybdenum film to be prepared, determines dredge respectively
Then the optical parameter and thickness of loose layer, compacted zone and passivation layer determine system according to the first correspondence and the second correspondence
The preparation technology parameter and preparation time of the standby film.
Step 32, it is prepared according to the first preparation technology parameter and the first preparation time, the second preparation technology parameter and second
Time and third preparation technology parameter and third preparation time, prepare weaker zone, compacted zone and passivation layer respectively.
First according to the first preparation technology parameter and the first preparation time, the first film is prepared on a glass substrate as thin
Loose layer；Then according to the second preparation technology parameter and the second preparation time, the second film is prepared on weaker zone as compacted zone；
Finally according to third preparation technology parameter and the third preparation time, third film is prepared on compacted zone as passivation layer.
In the application, it can be determined according to the preparation demand of film to be prepared, the first correspondence and the second correspondence
Prepare the preparation technology parameter and preparation time of the film, wherein preparation demand includes the thickness and Optical Parametric of film to be prepared
Number, the first correspondence are the optical parameter and preparation technology parameter correspondence of the film, and the second correspondence is the film
The correspondence of preparation time and thickness prepare the film then according to determining preparation technology parameter and preparation time.This
In application, the properties such as consistency for quantitatively characterizing film by the optical parameter of film just can pass through film in this way
Optical parameter quantitatively characterizes the preparation demand of film, when it is expected to prepare the film of certain consistency, can pass through Optical Parametric
Correspondence between number and preparation technology parameter prepares the film for meeting preparation demand by controlling preparation technology parameter.
Refined, Yu Tao, Zhang Chuansheng according to document Song Bin wait influence of the sputtering pressures to magnetron sputtering Mo back electrode layers pattern and structure
[J] material Leaders, 2016,30 (16):The record of 35-38., it is possible to understand that sputtering pressure has consistency/roughness of film
Great influence, the present invention is i.e. according to the correspondence between sputtering pressure and optical parameter by selecting suitable sputtering pressure
Consistency/roughness to control prepared film further can also pass through the optics of film made by detection if necessary
Sputtering pressure value is adjusted with the presence or absence of difference, and then improve and to be finally prepared between parameter and desired optical parameter
The quality of film.
The embodiment of the present application also provides two specific embodiments, the realization for preparing molybdenum back electrode layer is described in detail
Journey：
As shown in figure 9, for the structure of the molybdenum back electrode layer under the first specific implementation mode provided by the embodiments of the present application
Schematic diagram, preparation process include：
First according to the preparation demand of weaker zone, i.e., refractive index n=2.85, extinction coefficient k=when wavelength is 550nm
1.92 and preparation demand that thickness is 150nm determine weaker zone the first preparation technology parameter (i.e. sputtering pressure is 1.0Pa) and
First preparation time, refractive index n=3.63, extinction coefficient k=3.95 when the preparation demand of compacted zone, i.e. wavelength are 550nm
The second preparation technology parameter (i.e. sputtering pressure is 0.2Pa) and second of compacted zone is determined with preparation demand that thickness is 800nm
Refractive index n=2.88, extinction coefficient k=2.82 when the preparation demand of preparation time and passivation layer, i.e. wavelength are 550nm
The third preparation technology parameter (i.e. sputtering pressure is 0.7Pa) and third system of passivation layer are determined with preparation demand that thickness is 35nm
The standby time；
When then being prepared according to the first preparation technology parameter and the first preparation time, the second preparation technology parameter and second
Between and third preparation technology parameter and third preparation time, prepare weaker zone, compacted zone and passivation layer respectively.
The preparation that other each layers of CIGS thin film solar cell are completed in this molybdenum back electrode layer, passes through x-ray fluorescence light
The percentage composition that spectrum analysis obtains Cu, In, Ga and Se of CIGS absorbed layers is respectively 23.69%, 17.21%, 8.73% and
50.37%.Voc, Jsc and the FF for not preparing the CIGS thin film solar cell of antireflection layer be respectively 0.5895V,
32.53A/cm2With 60.84, the efficiency to obtain the CIGS thin film solar cell is 11.67%.
As shown in Figure 10, it is the structure of the molybdenum back electrode layer under second of specific implementation mode provided by the embodiments of the present application
Schematic diagram, preparation process include：
First according to the preparation demand of weaker zone, i.e., refractive index n=2.85, extinction coefficient k=when wavelength is 550nm
1.92 and preparation demand that thickness is 150nm determine weaker zone the first preparation technology parameter (i.e. sputtering pressure is 1.0Pa) and
First preparation time, refractive index n=3.63, extinction coefficient k=4.00 when the preparation demand of compacted zone, i.e. wavelength are 550nm
The second preparation technology parameter (i.e. sputtering pressure is 0.1Pa) and second of compacted zone is determined with preparation demand that thickness is 800nm
Refractive index n=2.88, extinction coefficient k=2.82 when the preparation demand of preparation time and passivation layer, i.e. wavelength are 550nm
The third preparation technology parameter (i.e. sputtering pressure is 0.7Pa) and third system of passivation layer are determined with preparation demand that thickness is 35nm
The standby time.
When then being prepared according to the first preparation technology parameter and the first preparation time, the second preparation technology parameter and second
Between and third preparation technology parameter and third preparation time, prepare weaker zone, compacted zone and passivation layer respectively.
The preparation that other each layers of CIGS thin film solar cell are completed in this molybdenum back electrode layer, passes through x-ray fluorescence light
The percentage composition that spectrum analysis obtains Cu, In, Ga and Se of CIGS absorbed layers is respectively 24.50%, 16.61%, 9.29% and
49.60%.Voc, Jsc and the FF for not preparing the CIGS thin film solar cell of antireflection layer be respectively 634.3m V,
32.21A/cm2With 72.64, the efficiency to obtain the CIGS thin film solar cell is 14.84%.
When the extinction coefficient of the compacted zone of molybdenum back electrode layer is larger, the consistency of film can be larger, CIGS thin film solar energy
The efficiency of battery is often higher, then can be selected according to the correspondence of predetermined preparation technology parameter and optical parameter
Suitable preparation technology parameter is selected, so as to accurately obtain the molybdenum back electrode layer for meeting preparation demand, you can obtain photoelectricity
The higher thin-film solar cells of transfer efficiency.
The method provided by the present application for preparing film, can quantitatively determine the properties such as the consistency of each layer film, this field
Technical staff should be understood that due to by measurement method, survey tool, method for manufacturing thin film and to prepare tool etc. various uncertain
The influence of factor, when quantitatively determining the properties such as film consistency by optical parameter, it is so-called quantitatively be not entirely accurate without
That misses quantifies, but quantifying in the error range of permission.
It should be noted that the terms "include", "comprise" or its any other variant are intended to the packet of nonexcludability
Contain, so that process, method, commodity or equipment including a series of elements include not only those elements, but also includes
Other elements that are not explicitly listed, or further include for this process, method, commodity or the intrinsic element of equipment.
In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that in the mistake including element
There is also other identical elements in journey, method, commodity or equipment.
It these are only embodiments herein, be not intended to limit this application.To those skilled in the art,
The application can have various modifications and variations.It is all within spirit herein and principle made by any modification, equivalent replacement,
Improve etc., it should be included within the scope of claims hereof.
Claims (10)
1. a kind of determination method of optical parameter of film and preparation technology parameter correspondence, which is characterized in that including：
Film is prepared respectively under multiple predetermined preparation technology parameters；
The optical parameter for determining each film prepared under the multiple predetermined preparation technology parameter, obtains the Optical Parametric of the film
Number and preparation technology parameter correspondence, to prepare the film for meeting preparation demand according to the correspondence.
2. the method as described in claim 1, which is characterized in that determine prepared under the multiple predetermined preparation technology parameter it is each
The optical parameter of film, specifically includes：
Determine the first optical parameter of glass substrate；
Determine the second optical parameter for preparing the glass substrate for having the film；
According to first optical parameter and second optical parameter, the optical parameter of the film is determined.
3. method as claimed in claim 2, which is characterized in that first optical parameter and second optical parameter are logical
Cross following methods determination：
Determine measured medium relative amplitude decaying and phase shift difference, the measured medium include the glass substrate and/
Or the preparation has the glass substrate of the film；
According to the difference of relative amplitude decaying and phase shift, the optical parameter of measured medium is determined.
4. the method as described in claim 1, which is characterized in that the preparation technology parameter includes at least sputtering pressure, described
Optical parameter includes at least refractive index and extinction coefficient.
5. a kind of method preparing film, which is characterized in that including：
According to the preparation demand of film to be prepared, the first correspondence and the second correspondence, the system for preparing the film is determined
Standby technological parameter and preparation time, wherein the preparation demand includes the thickness and optical parameter of film to be prepared, and described first
Correspondence is the optical parameter and preparation technology parameter correspondence of the film, and second correspondence is the film
Preparation time and thickness correspondence；
According to determining preparation technology parameter and preparation time, the film is prepared.
6. method as claimed in claim 4, which is characterized in that the preparation technology parameter includes at least sputtering pressure, described
Optical parameter includes at least refractive index and extinction coefficient.
7. method as claimed in claim 4, which is characterized in that when the film is molybdenum back electrode layer, the molybdenum back electrode
Layer includes weaker zone, compacted zone and passivation layer, is corresponded to and is closed according to the preparation demand of film to be prepared, the first correspondence and second
System determines the preparation technology parameter and preparation time for preparing the film, specifically includes：
According to the preparation demand of molybdenum back electrode layer to be prepared, the first correspondence and the second correspondence, the weaker zone is determined
The first preparation technology parameter and the first preparation time, the second preparation technology parameter of the compacted zone and the second preparation time,
And the third preparation technology parameter and third preparation time of the passivation layer, wherein the preparation demand includes molybdenum to be prepared
The thickness and optical parameter of back electrode layer, first correspondence are the optical parameter and preparation technology parameter of the molybdenum film
Correspondence, second correspondence are the correspondence of the preparation time and thickness of the molybdenum film.
8. method as claimed in claim 4, when the film is molybdenum back electrode layer, according to determining preparation technology parameter and
Preparation time prepares the film, specifically includes：
According to first preparation technology parameter and first preparation time, second preparation technology parameter and described second
Preparation time and the third preparation technology parameter and the third preparation time, prepare the weaker zone, the cause respectively
Close layer and the passivation layer.
9. method as claimed in claim 8, which is characterized in that prepared according to first preparation technology parameter and described first
Time, second preparation technology parameter and second preparation time and the third preparation technology parameter and described
Three preparation times prepare the weaker zone, the compacted zone and the passivation layer, specifically include respectively：
According to first preparation technology parameter and first preparation time, the first film is prepared on a glass substrate as institute
State weaker zone；
According to second preparation technology parameter and second preparation time, the second film conduct is prepared on the weaker zone
The compacted zone；
According to the third preparation technology parameter and the third preparation time, third film conduct is prepared on the compacted zone
The passivation layer.
10. the method as described in any claim in claim 5~9, which is characterized in that first correspondence, is to pass through
The optical parameter of any film is determined with the determination method of preparation technology parameter correspondence in Claims 1 to 4.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109768094A (en) * | 2018-12-28 | 2019-05-17 | 北京铂阳顶荣光伏科技有限公司 | A kind of multilayer back electrode, thin-film solar cells and preparation method thereof |
| CN112553581A (en) * | 2019-09-10 | 2021-03-26 | 株式会社斯库林集团 | Film forming apparatus and film forming method |
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|---|---|---|---|---|
| CN1947062A (en) * | 2004-02-23 | 2007-04-11 | Asml荷兰有限公司 | Method to determine the value of process parameters based on scatterometry data |
| CN101871093A (en) * | 2010-06-19 | 2010-10-27 | 大连交通大学 | Method for preparing selective absorbing coating for steel core of solar collection tube |
| CN106017338A (en) * | 2016-05-26 | 2016-10-12 | 国家纳米科学中心 | Method for determining film continuity critical thickness |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1947062A (en) * | 2004-02-23 | 2007-04-11 | Asml荷兰有限公司 | Method to determine the value of process parameters based on scatterometry data |
| CN101871093A (en) * | 2010-06-19 | 2010-10-27 | 大连交通大学 | Method for preparing selective absorbing coating for steel core of solar collection tube |
| CN106017338A (en) * | 2016-05-26 | 2016-10-12 | 国家纳米科学中心 | Method for determining film continuity critical thickness |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109768094A (en) * | 2018-12-28 | 2019-05-17 | 北京铂阳顶荣光伏科技有限公司 | A kind of multilayer back electrode, thin-film solar cells and preparation method thereof |
| CN112553581A (en) * | 2019-09-10 | 2021-03-26 | 株式会社斯库林集团 | Film forming apparatus and film forming method |
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