CN109001122B - Optical constant measuring device and method for gradient or graded index film - Google Patents
Optical constant measuring device and method for gradient or graded index film Download PDFInfo
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- CN109001122B CN109001122B CN201811149497.8A CN201811149497A CN109001122B CN 109001122 B CN109001122 B CN 109001122B CN 201811149497 A CN201811149497 A CN 201811149497A CN 109001122 B CN109001122 B CN 109001122B
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract
The invention relates to a device and a method for measuring optical constants of a gradient or graded index film. The device comprises a vacuum system, an ellipsometric parameter detection system, a film thickness monitoring system and an ion source, wherein the vacuum system comprises a vacuum chamber and a sample stage; the film thickness monitoring system comprises a quartz crystal oscillator film thickness meter; the sample stage is arranged at the top of the vacuum chamber, the ion source is arranged at the bottom of the vacuum chamber, and the ion beam output port of the ion source is arranged opposite to the sample stage. The measuring method comprises the following steps: firstly measuring initial ellipsometry parameters of a gradient refractive index film sample, thinning the film by using an ion beam, then measuring the ellipsometry parameters of the thinned film, repeating the thinning and testing steps until the film is thinned below a set step length, and obtaining the refractive index and extinction coefficient of the last film, on the basis, sequentially obtaining the optical constants of all the films on the last film, finally obtaining the optical constant distribution of the film sample along the thickness direction, and realizing the measurement of the optical constants of the gradient refractive index film.
Description
Technical Field
The invention relates to the technical field of measurement of film optical constants, in particular to an optical constant measurement device and method for a gradient or graded index film.
Technical Field
Commonly used optical films such as antireflection films, high reflection films, optical filters, polarizing films, etc. are generally multilayer film structures made by alternate plating of two (or more) film-plating materials having different refractive indices. Among these films, although the refractive index of two adjacent films is different, the refractive index of the same film is approximately uniform, and the refractive index of the same film is stable and uniform without variation with thickness. Since interfaces exist between layers of the multilayer film, defects and impurities are most easily enriched at the interfaces, the absorption coefficient at the interfaces is often several orders of magnitude larger than that of bulk absorption, and great stress exists, which often causes the film to be easily damaged under strong laser, the existence of the interfaces is an important reason that the damage threshold of the multilayer film system in a laser system is not high.
On the other hand, many studies have shown that the electric field intensity distribution inside the film is also an important factor affecting its laser damaging ability: if the electric field intensity at the interface between the film layers is large, it is difficult to increase the laser damage threshold of the whole film system. Therefore, the design needs to be continuously optimized, a reasonable film system structure is sought, the peak value of the standing wave electric field intensity is far away from the interface area, and the laser damage resistance of the film can be improved to a certain extent, but due to the limitation of the layered dielectric film system, all peak values of the electric field intensity are difficult to be far away from the film layer interface, so that the obtained effect is very limited.
Since the function of the single-layer film is very limited, the optical film generally used is a multi-layer film, but the existence of the interface between the layers of the multi-layer film limits the increase of the laser damage threshold of the film. The above problems can be avoided if a film with a continuously varying refractive index can be produced such that the interface between the film layers is not present. The graded index film, or graded index film, has a refractive index and an extinction coefficient continuously varying along the thickness direction of the film, and no interface is present, and it is possible to solve this problem. Therefore, the preparation and application research of the gradient refractive index film has long attracted extensive attention from researchers at home and abroad. However, research has been very slow for many years, and the main obstacle is that the optical constants (refractive index, extinction coefficient) of the gradient refractive index film cannot be detected. For a uniform monolayer, the detection of the optical constants is not problematic, and accurate measurements can be obtained with ellipsometers. However, for gradient films, there is no effective refractive index detection means and method, which makes thin film process research difficult to break through. At present, two main ways are adopted for detecting the gradient refractive index film: firstly, estimating gradient distribution of refractive index, adopting optical film system design software to calculate optical transmissivity or reflectivity of the film, comparing with actual test result, if deviation is large, repeatedly regulating the distribution of estimated refractive index until the calculated value and actual measured value are close, namely, considering the estimated refractive index distribution as actual distribution of sample refractive index. Secondly, starting from the process, the refractive index and extinction coefficient of the uniform monolayer film prepared under different process conditions are firstly determined. Because the preparation of the gradient film is realized by the change of the technological parameters, when the gradient film is actually prepared, the technological parameters are adjusted according to the preset design, and the optical constants of the film corresponding to different technological parameters are regarded as the optical constants of the part of the gradient film. It is obvious that both methods are not truly reflective of the optical constants of the film sample and thus deviate greatly from the actual situation.
Disclosure of Invention
The invention provides an optical constant measuring device and method for a gradient or graded index film, which are used for solving the problem that the gradient or graded index cannot be measured in the prior art.
In order to achieve the purpose of the invention, the technical solution provided by the invention is as follows:
the optical constant measuring device of the gradient or graded index film comprises a vacuum system, an ellipsometry parameter detecting system, a film thickness monitoring system and an ion source, wherein the vacuum system comprises a vacuum chamber and a sample table; the film thickness monitoring system comprises a quartz crystal oscillator film thickness meter;
the sample stage is arranged at the top of the vacuum chamber, the ion source is arranged at the bottom of the vacuum chamber, the ion source and the ion source are opposite to each other, and an ion beam output port of the ion source is arranged opposite to the sample stage.
Further, the wavelength of the light source is 300-900 nm; the incidence angle of the test light is 65 degrees.
Further, the ion energy of the ion source is between 0 and 3000 eV.
The method for measuring the optical constant of the gradient or graded index film comprises the following steps:
step 1, calibrating initial geometric thickness of a film sample: measuring the geometric thickness of the film by adopting a profiler to obtain initial thickness information of the film, and determining the thickness step length of each thinning according to the test requirement of a sample;
step 2, clamping a sample to be tested on the lower surface of the sample table, wherein the coating surface of the sample to be tested is opposite to the ion source, and vacuumizing the vacuum chamber to enable the vacuum chamber to reach the working vacuum degree of the ion source;
Step 4, turning on an ion source, etching and thinning the film by using an argon ion beam to obtain a thickness of one step, detecting the thinned film thickness by using a quartz crystal diaphragm thickness meter, and marking the etched film thickness as d n Corresponds to the L n A layer;
measuring ellipsometry parameters psi of thinned film sample by using ellipsometry parameter detection system n-1 And delta n-1 ;
re-measuring ellipsometry information ψ of thinned film sample by adopting ellipsometry parameter detection system n-2 And delta n-2 ;
Step 6, repeating the step 5 until the thickness of the film is reduced to be lower than the thickness step length, corresponding to the L 1 The film thickness of the layer is denoted as d 1 Ellipsometric information ψ of a sample is measured by an ellipsometric parameter detection system 1 And delta 1 ;
Compared with the prior art, the invention has the advantages that:
1. the invention is not only suitable for measuring gradient or graded index films, but also suitable for measuring refractive index distribution of common multilayer dielectric films, can be used for analyzing refractive indexes and extinction coefficients of the multilayer dielectric films, and can truly reflect optical constants of film samples.
2. The invention can obtain the distribution of the optical constants (refractive index and extinction coefficient) of the film sample along the film thickness direction, and provides basis for determining the process control condition of each layer of film.
3. The invention is not only suitable for measuring the gradient or graded index of the dielectric film, but also suitable for detecting the extinction coefficient and the thickness, and is also suitable for measuring the refractive index distribution of the common multilayer dielectric film.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 is a schematic illustration of gradient index film thinning.
In the figure, a 1-light source, a 2-polarizer, a 3-wave plate, a 4-vacuum chamber, a 5-sample stage, a 6-sample to be tested, a 7-ion source, an 8-quartz crystal oscillator film thickness meter, a 9-analyzer, a 10-detector and an 11-computer are shown.
Detailed Description
The present invention will be further described with reference to examples and drawings, but the scope of the present invention should not be limited thereto.
Referring to fig. 1, an optical constant measuring device of a gradient or graded index film comprises a vacuum system, an ellipsometry parameter detection system, a film thickness monitoring system and an ion source 7, wherein the vacuum system comprises a vacuum chamber 4 and a sample stage 5; the film thickness monitoring system comprises a quartz crystal oscillator film thickness meter 8;
the sample stage 5 is arranged at the top of the vacuum chamber 4, the ion source 7 is arranged at the bottom of the vacuum chamber 4, the ion source and the vacuum chamber are opposite to each other, and an ion beam output port of the ion source 7 is arranged opposite to the sample stage.
The wavelength of the light source is 300-900 nm; the incidence angle of the test light is 65 degrees.
The ion energy of the ion source 7 is between 0 and 3000 and eV.
The vacuum system is mainly used for providing the environment for the normal operation of the ion source, and the vacuum chamber can reach 1X 10 -4 Vacuum degree of Pa.
The ellipsometry parameter detection system consists of a light source 1, a polarizer 2, a wave plate 3, an analyzer 9 and a detector 10, wherein the polarizer 2 and the wave plate 3 are sequentially arranged on an incident light path of the light source 1, the analyzer 9 and the detector 10 are sequentially arranged on an emergent light path, the system is used for ellipsometry parameter measurement of a film sample, natural light (with the wavelength range of 300-900 nm) emitted by the light source 1 is changed into linear polarized light after passing through the polarizer 2, passes through a window arranged on a vacuum chamber after passing through a quarter wave plate, is incident on the surface of the film sample at 65 degrees, is reflected by the surface of the film, passes through a window on the other side of the vacuum chamber, and is received by the photoelectric detector 10 after passing through the analyzer 9. According to the relative theory of polarization and extinction, the ellipsometry parameter detection system can measure ellipsometry parameters psi and delta of the film, wherein,
in the middle ofAnd->Reflection coefficient of p-light and s-light on the film surface, respectively, +.>And->The phase difference between p-light and s-light.
The quartz crystal oscillator film thickness meter 8 is used for measuring the geometric thickness information of the thin film. After the sample 6 to be measured is clamped on the sample table 5, the electrode on the surface of the sample 6 to be measured is connected with the quartz crystal diaphragm thickness gauge, and the surface of the film to be measured faces the ion source. After the quartz crystal oscillator film thickness meter starts to work, the quartz crystal oscillator film thickness meter is calibrated by using the actually measured film thickness according to the oscillation frequency of the quartz crystal wafer.
The ion source 7 is a cold cathode ion source 7, which forms an ion beam etching system, the ion source 7 can emit argon ion beam, and the ion energy is 0-3000 eV and is adjustable. In the embodiment, the ion source is regulated to have the output ion energy of 800eV and the beam current density of 2mA/cm 2 And obtaining an output ion beam, and etching and thinning the film on the surface of the sample.
The computer control system 11 is connected to each functional component to perform data analysis processing. And obtaining the geometric thickness of the film through a quartz crystal diaphragm thickness monitoring system. By the cooperation of the detector 10, the polarizer 2, the wave plate 3 and the analyzer 9, ellipsometric parameter information of the film surface can be obtained. Meanwhile, the ion energy and output parameters of the ion source 7, the horizontal state of the sample stage and the like are controlled.
Referring to fig. 2, the method for measuring using the optical constant measuring device of the gradient or graded index film provided by the invention comprises the following steps:
(1) Calibrating the initial geometric thickness of the film sample: before the optical constants of the gradient film are tested, the geometric thickness of the film is measured by adopting a profilometer, the initial thickness of the film is 358nm, and the thickness step length of each thinning can be determined to be 10 nm. The thickness step can be set according to the specific requirements of the sample, the smaller the step, the higher the resolution, but the lower the test efficiency.
Requirements of sample 6 to be tested: the gradient refractive index film to be measured is deposited on a quartz wafer along with a workpiece in a furnace during preparation, au electrodes are prepared on two surfaces of the quartz wafer in advance, one surface is completely covered by the Au film, the periphery of the other surface is provided with the Au electrode, the central part of the other surface is provided with the bare quartz wafer, and the gradient refractive index film to be measured is deposited on the surface. The film to be tested of the device must be plated on a quartz wafer, which is currently standard in the market, which has been previously plated with electrodes. For measuring the refractive index profile of the coating under a certain process, a standard quartz wafer with electrodes already coated is used, and then a thin film is deposited on the quartz wafer to be used as the sample 6 to be measured.
(2) Clamping a sample 6 to be measured on a sample table 5 in a vacuum chamber, enabling a film plating surface on the sample 6 to be measured to be opposite to an ion source 7, and connecting two electrodes on the upper surface and the lower surface of the sample 6 to be measured with a quartz crystal oscillator film thickness meter 8; the sample stage 5 is driven by two stepping motors to slightly adjust the levelness of the clamping surface of the sample stage 5, so that the light beam reflected by the surface of the film completely enters the detector 10, and the sample stage is provided with water cooling, so that the temperature of the sample in the test process can be ensured to be constant.
Vacuumizing the vacuum chamber to make it reach 1×10 working vacuum degree of ion source -3 Pa。
(3) Measuring initial ellipsometry information of film sample by using ellipsometry parameter detection system, namely ellipsometry parameter ψ n And delta n This is the integrated ellipsometric parameter of the initial gradient film.
(4) The ion source 7 was turned on and the film was etched with an argon ion beam to reduce its thickness by 10 a nm a. In the etching process, a quartz crystal oscillator film thickness meter 8 is adopted to monitor the thinned film thickness, and the removed layer is marked as L n A layer corresponding to a film thickness d n (10 nm in this example). Measuring ellipsometry parameters psi of thinned film sample by using ellipsometry parameter detection system n-1 And delta n-1 。
(5) The ion source is turned on again and the argon ion beam is used for etching and thinning the film, so that the thickness of the film is reduced by 10 percent nm. In the etching process, a quartz crystal diaphragm thickness gauge is adopted to detect the thinned film thickness, and the thinned layer is marked as L n-1 A layer corresponding to a film thickness d n-1 (10 nm in this example). Re-measuring ellipsometry information ψ of thinned film sample by adopting ellipsometry parameter detection system n-2 And delta n-2 。
(6) Repeating step 5 until the thickness of the film is reduced to less than 10nm, and the layer is denoted as L 1 A layer with a film thickness d 1 (remaining 8 nm). Using ellipsometric parametersDetection system for measuring ellipsometric information ψ of sample 1 And delta 1 。
(7) And (5) data processing and analysis. According to ψ 1 ,Δ 1 And d 1 Calculating L 1 Refractive index n of layer film 1 And extinction coefficient k 1 。
(8) At L 1 Calculating L sequentially based on known layer optical constant and thickness 2 、L 3 Up to L n The refractive index and the extinction coefficient of the layer are obtained, so that the optical constant distribution of the film sample along the thickness direction is obtained, the change curve of the refractive index and the extinction coefficient along with the thickness of the film is drawn, and the measurement of the optical constant of the gradient refractive index film is realized.
Claims (1)
1. An optical constant measurement method of a gradient or graded index film, which is characterized in that: the method comprises the following steps:
step 1, calibrating initial geometric thickness of a film sample: measuring the geometric thickness of the film by adopting a profiler to obtain initial thickness information of the film, and determining the thickness step length of each thinning according to the test requirement of a sample;
step 2, clamping a sample (6) to be tested on the lower surface of a sample table (5), wherein a coating surface of the sample is opposite to an ion source (7), and vacuumizing a vacuum chamber (4) to enable the vacuum chamber to reach the working vacuum degree of the ion source (7);
step 3, measuring initial ellipsometry information of the film sample by using an ellipsometry parameter detection system, namely an ellipsometry parameter ψ n And delta n ;
Step 4, turning on an ion source (7), etching and thinning the film by one step by using an argon ion beam, detecting the thinned film thickness by using a quartz crystal diaphragm thickness gauge (8), and marking the etched film thickness as d n Corresponds to the L n A layer;
measuring ellipsometry parameters psi of thinned film sample by using ellipsometry parameter detection system n-1 And delta n-1 ;
Step 5, turning on the ion source (7) again, and etching and thinning the film by using an argon ion beam while adopting stoneThe thickness of the film etched by the quartz crystal diaphragm thickness gauge (8) is recorded as d n-1 Corresponds to the L n-1 A layer;
re-measuring ellipsometry information ψ of thinned film sample by adopting ellipsometry parameter detection system n-2 And delta n-2 ;
Step 6, repeating the step 5 until the thickness of the film is reduced to be lower than the thickness step length, corresponding to the L 1 The film thickness of the layer is denoted as d 1 Ellipsometric information ψ of a sample is measured by an ellipsometric parameter detection system 1 And delta 1 ;
Step 7, data processing and analysis: according to ψ 1 ,Δ 1 And d 1 Calculating L 1 Refractive index n of layer film 1 And extinction coefficient k 1 ;
Step 8, calculating L in turn 2 、L 3 Up to L n The refractive index and extinction coefficient of the layer, so as to obtain the optical constant distribution of the film sample along the thickness direction, and realize the measurement of the optical constant of the gradient refractive index film;
the optical constant measuring device of the gradient or graded index film used by the measuring method comprises a vacuum system, an ellipsometry parameter detecting system, a film thickness monitoring system and an ion source (7), wherein the vacuum system comprises a vacuum chamber (4) and a sample table (5); the film thickness monitoring system comprises a quartz crystal oscillator film thickness meter (8);
the sample table (5) is arranged at the top of the vacuum chamber (4), the ion source (7) is arranged at the bottom of the vacuum chamber (4) and is opposite to the vacuum chamber, and an ion beam output port of the ion source (7) is arranged opposite to the sample table;
the light source wavelength of the ellipsometry parameter detection system is 300-900 nm; the incidence angle of the test light is 65 degrees;
the ion energy of the ion source (7) is between 0 and 3000 and eV.
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CN1144906A (en) * | 1995-09-06 | 1997-03-12 | 东南大学 | Imaging detecting method and its equipment for film thickness and refractive index |
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CN103743349A (en) * | 2013-12-30 | 2014-04-23 | 中国科学技术大学 | Method and device for measuring nano film |
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DE4108329A1 (en) * | 1991-03-14 | 1992-09-24 | Plasmos Gmbh Prozesstechnik | Ellipsometric determn. of material parameters of successive layers of multilayer sample - by successive removal of layers, continuous ellipsometric measurement and computation of thickness, refractive index and absorption coefft. from test values |
JPH05232298A (en) * | 1992-02-25 | 1993-09-07 | Nikon Corp | X-ray multilayer film reflector |
US5354575A (en) * | 1993-04-16 | 1994-10-11 | University Of Maryland | Ellipsometric approach to anti-reflection coatings of semiconductor laser amplifiers |
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