CN112857270A - Method for in-situ real-time quantitative detection of film roughness by using RHEED - Google Patents
Method for in-situ real-time quantitative detection of film roughness by using RHEED Download PDFInfo
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- CN112857270A CN112857270A CN202110022387.0A CN202110022387A CN112857270A CN 112857270 A CN112857270 A CN 112857270A CN 202110022387 A CN202110022387 A CN 202110022387A CN 112857270 A CN112857270 A CN 112857270A
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002128 reflection high energy electron diffraction Methods 0.000 title claims description 45
- 238000001514 detection method Methods 0.000 title claims description 13
- 230000003746 surface roughness Effects 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 12
- 238000010894 electron beam technology Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 45
- 239000010409 thin film Substances 0.000 abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910002372 SrTiO3(001) Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910002370 SrTiO3 Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000005533 two-dimensional electron gas Effects 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910002244 LaAlO3 Inorganic materials 0.000 description 1
- 241000405414 Rehmannia Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000004772 tellurides Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/30—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces
- G01B11/306—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces for measuring evenness
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a method for detecting the roughness of a film in situ in real time by a reflection type high-energy electron diffractometer (RHEED). RHEED is an instrument widely used in the epitaxial growth of thin films, and can observe the diffraction pattern of an epitaxial thin film in situ in real time by combining a fluorescent screen and a charge coupled device (hereinafter, referred to as CCD). The invention establishes a definite functional relation between the diffraction pattern characteristic parameter and the film surface flatness by collecting the characteristic parameter of the epitaxial film diffraction pattern, thereby obtaining the accurate surface roughness of the epitaxial film according to the diffraction pattern of the epitaxial film in the growth process, and greatly expanding the application of RHEED in the film growth.
Description
Technical Field
The invention relates to the field of condensed state substance structure detection, in particular to a method for detecting the surface roughness of a film in situ and in real time.
Background
The surface roughness of the film is always a very basic and important information in studying surface and interface physics in condensed state physics. Surface area, e.g. in single crystal SrTiO3(001) Growing a buffer layer on the surface of the substrate, wherein whether the buffer layer is flat or not is directly related to the quality of a subsequent film; interfaces such as LaAlO3/SrTiO3The two-dimensional electron gas at the interface has high requirement on the interface flatness of the two materials during growth, so that the two-dimensional electron gas is thinThe roughness of the film surface is directly related to the quality of the epitaxial thin film. Furthermore, for most electronic devices that rely on interfaces, the flatness of the interface has a critical effect on the performance of the device, such as magnetic tunnel junctions, ferroelectric tunnel junctions, and quantum cascade lasers.
In surface and interfacial physics studies, sample preparation is typically accomplished in vacuum. In the sample preparation process, a reflection-type high-energy electron diffractometer (hereinafter referred to as RHEED) is a widely used in-situ characterization means. But most of the current methods are only used for qualitatively observing growth conditions, such as growth modes, growth layer numbers and the like. The current detection means for the roughness of the surface of the thin film, such as an atomic force microscope, an ellipsometer, etc., needs to take the sample out of the vacuum equipment for testing, while the main means for measuring the interface, such as a transmission electron microscope, needs to take the sample out of the vacuum equipment, or even further process the sample. However, many thin films are unstable in air, and the properties of the thin films are often changed or even samples are directly damaged after the thin films are taken out of vacuum equipment into the air, such as active metals including aluminum, lead and the like, silylene, most selenides and tellurides and the like, so that the intrinsic information of the thin films cannot be detected. It is very important to develop a technical means for detecting the roughness of the surface and the interface in situ in real time.
Disclosure of Invention
The purpose of the invention is: a RHEED-based method for in-situ and real-time detection of surface and interface roughness is provided.
In order to achieve the above object, the technical solution of the present invention is to provide a method for in-situ real-time quantitative detection of film roughness by using RHEED, which is characterized in that the method for in-situ real-time and quantitatively obtaining surface roughness of an epitaxial film comprises the following steps:
a) epitaxially growing a film on a single crystal substrate in a vacuum coating device system;
b) irradiating the epitaxial film by using a RHEED electron beam, projecting the epitaxial film on a fluorescent screen, and shooting the epitaxial film by using a CCD image sensor to obtain a diffraction pattern;
c) obtaining a brightness distribution of the diffraction pattern;
d) obtaining a shape parameter A of the diffraction pattern through the brightness distribution of the diffraction pattern;
e) and obtaining the surface roughness of the film through the functional relation between the shape parameter A of the diffraction pattern and the surface roughness.
Preferably, in the step b), the epitaxial film is irradiated with the RHEED electron beam during or after the epitaxial growth of the film on the single crystal substrate.
Preferably, in the step b), when the epitaxial film is irradiated by using the RHEED electron beam, the RHEED beam is incident at a small angle, which is preferably between 0.1 and 10 degrees, so that the RHEED beam can better detect the surface of the film and obtain a more obvious diffraction pattern.
Preferably, in the step b), when the epitaxial film is irradiated with the RHEED electron beam, the voltage of the RHEED is set to be between 5 and 50kV, so that the RHEED can obtain a better diffraction pattern.
Preferably, in the step b), the magnitude of the RHEED filament current is controlled to control the diffraction pattern to be larger than the resolution (minimum pixel point) of the CCD image sensor, so as to facilitate the subsequent extraction of the characteristic parameters.
Preferably, in the step b), the diffraction pattern should include all diffraction features such as diffraction spots, lines or Kikuchi lines, which makes the subsequent extraction of feature parameters more accurate.
Preferably, in the step c), the magnitude of the RHEED filament current is controlled to control the brightness of the diffraction pattern within the brightness range capable of being collected by the CCD image sensor, so as to obtain accurate brightness later. The brightness distribution of the diffraction pattern is obtained by converting the pattern obtained by the CCD image sensor into a gray level image to obtain the distribution of gray levels in the space pixel points
Preferably, in the step e), the functional relationship between the shape parameter a and the surface roughness of the diffraction pattern is calculated based on a diffraction condition equation.
Preferably, in the step e), the functional relationship between the shape parameter a and the surface roughness of the diffraction pattern is:
where σ is the roughness of the surface of the film, k is the incident wave vector of the reflective high-energy electron diffractometer, and d0、σ0Respectively is the width and the surface roughness of the column of the inverted space on the surface of the single crystal substrate, and theta is the incident angle of the reflection type high-energy electron diffractometer.
Preferably, the roughness σ is defined as a root mean square value of coordinates of all particles on the surface of the epitaxial thin film in a direction perpendicular to the substrate, and the expression is as follows:
wherein z (k) is the spatial coordinate value of the kth particle on the surface of the film perpendicular to the surface, and n is the total number of all particles on the surface of the epitaxial film.
In the invention, the vacuum device system can adopt pulse laser deposition, molecular beam epitaxy, magnetron sputtering or chemical vapor deposition systems and the like, and the systems can grow epitaxial films on prepared rehmannia roots and are suitable for mounting RHEED. The single crystal substrate adopts various semiconductors such as silicon, gallium arsenide and the like, metals and compounds thereof, perovskites and various doped single crystals, and is easy to obtain and suitable for growing epitaxial films.
In order to be able to detect the information of surface and interface roughness in situ and in real time, the present invention utilizes RHEED which is able to monitor the film growth in situ and in real time. Through the brightness distribution of the film RHEED diffraction pattern, the method provided by the invention extracts the characteristic parameters from the film RHEED diffraction pattern, and the functional relation between the characteristic parameters of the diffraction pattern and the surface roughness is deduced based on the diffraction equation, so that the important function of in-situ real-time surface and interface roughness detection is realized.
Drawings
FIG. 1 shows LaCoO grown at 560 ℃, 580 ℃, 600 ℃, 620 ℃ and 640 DEG C3Film and SrTiO3RHEED image of the substrate.
FIG. 2 shows LaCoO grown at different temperatures3Characteristic value of thin film RHEED diffraction pattern;
FIG. 3 shows the atomic force microscope test and LaCoO obtained based on the method at different growth temperatures3The roughness of the film;
FIG. 4 shows the real-time surface roughness of the film and the oscillation of RHEED diffraction spot intensity.
Detailed Description
The invention is further illustrated by the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example (1)
By pulsed laser deposition on SrTiO3(001) Growth of LaCoO on single crystal substrate3The film grows under the conditions of introducing pure oxygen, oxygen pressure of 10Pa and laser energy density of 2J/cm2The laser frequency was 1Hz, RHEED voltage was set to 30kV, and the incident angle was set to 2 °.
Heating the substrate to grow LaCoO with different surfaces at different temperatures3The growth temperatures of the film are 560 ℃, 580 ℃, 600 ℃, 620 ℃ and 640 ℃ respectively.
After the growth, the RHEED diffraction image obtained by the CCD is intercepted, as shown in fig. 1.
Then, a brightness distribution map of the RHEED diffraction image is obtained, a characteristic parameter a of the surface roughness is extracted from the diffraction pattern, and the value thereof is calculated, as shown in fig. 2.
And (3) bringing the value of A into a functional relation of the surface roughness:
the functional relationship table is looked up to obtain the roughness sigma value of the film, as shown in FIG. 3.
Example (2)
By pulsed laser deposition on SrTiO3(001) Growth of LaCoO on single crystal substrate3The growth conditions of the film are that the substrate temperature is 650 ℃, the oxygen pressure is 20Pa, and the laser energy density is 1.5J/cm2RHEED voltage is 30kV, and incident angle is 1.8 deg.
And acquiring a RHEED diffraction pattern every 5 seconds in the growth process, acquiring the brightness distribution of the diffraction pattern in real time, and simultaneously extracting the characteristic parameter A of the diffraction pattern.
And (3) bringing the value of A into a functional relation of the surface roughness:
the roughness σ of the film was obtained in real time from this function table, as shown in FIG. 4.
Example (3)
Growing an InGaN/GaN multi-quantum well film on a silicon single crystal substrate by a Metal Organic Chemical Vapor Deposition (MOCVD) system, growing an AlN buffer layer at 400-500 ℃, growing an undoped GaN layer at 500-700 ℃, and growing an InGaN/GaN multi-quantum well at 700-800 ℃. RHEED voltage was 15kV, and incident angle was 0.5 °.
And acquiring a RHEED diffraction pattern every 3 seconds in the growth process, acquiring the brightness distribution of the diffraction pattern in real time, and simultaneously extracting the characteristic parameter A of the diffraction pattern.
And (3) bringing the value of A into a functional relation of the surface roughness:
and obtaining the roughness sigma value of the film in real time according to the functional relation table.
Example (4)
Growing Bi on sapphire substrate by molecular beam epitaxy2Se3The film has substrate temperature of 390 deg.c, Bi and Se evaporating temperature of 600 deg.c, 400 deg.c, RHEED voltage of 15kV and incident angle of 0.5 deg.c.
And after the growth, intercepting the RHEED diffraction image acquired by the CCD.
Then, a brightness distribution diagram of the RHEED diffraction image is obtained, a characteristic parameter A of the surface roughness is extracted from the diffraction image, and the value of the characteristic parameter A is calculated.
And (3) bringing the value of A into a functional relation of the surface roughness:
and searching the functional relation table to obtain the roughness sigma value of the film.
Example (5)
A titanium film is grown on a gold substrate by magnetron sputtering under the conditions of air pressure of 0.5Pa, RHEED voltage of 20kV and an incidence angle of 3 degrees.
And obtaining a RHEED diffraction pattern after growth, obtaining the brightness distribution of the diffraction pattern, and simultaneously extracting the characteristic parameter A of the diffraction pattern.
And (3) bringing the value of A into a functional relation of the surface roughness:
and obtaining the roughness sigma value of the film in real time according to the functional relation table.
Claims (10)
1. A method for detecting the roughness of a film in real time in situ by using RHEED (RHEED detection device) is characterized by being used for obtaining the surface roughness of an epitaxial film in real time in situ and quantitatively, and comprising the following steps of:
a) epitaxially growing a film on a single crystal substrate in a vacuum coating device system;
b) irradiating the epitaxial film by using an electron beam of a reflection type high-energy electron diffractometer, projecting the epitaxial film on a fluorescent screen, and shooting the epitaxial film by using a CCD image sensor to obtain a diffraction pattern;
c) obtaining a brightness distribution of the diffraction pattern;
d) obtaining a shape parameter A of the diffraction pattern through the brightness distribution of the diffraction pattern;
e) and obtaining the surface roughness of the film through the functional relation between the shape parameter A of the diffraction pattern and the surface roughness.
2. The method for in-situ real-time quantitative determination of film roughness using RHEED as claimed in claim 1, wherein in the step b), the epitaxial film is irradiated with electron beam using a reflective high energy electron diffractometer during or after the epitaxial growth of the film on the single crystal substrate.
3. The method for in-situ real-time quantitative determination of film roughness using RHEED as claimed in claim 1, wherein in step b), the incident angle of the reflective high energy electron diffractometer is selected to be in the range of 0.1 degree to 10 degrees when the epitaxial film is irradiated with the electron beam of the reflective high energy electron diffractometer.
4. The method for in-situ real-time quantitative determination of film roughness using RHEED as claimed in claim 1, wherein in step b), the voltage setting range of the reflective high energy electron diffractometer is between 5kV and 50kV while the epitaxial film is irradiated with the electron beam of the reflective high energy electron diffractometer.
5. The method for in-situ real-time quantitative detection of film roughness using RHEED of claim 1, wherein in the step b), the diffraction pattern obtained by the CCD image sensor is larger than the resolution of the CCD image sensor.
6. The method for in-situ real-time quantitative detection of film roughness using RHEED as claimed in claim 1, wherein in step b), the diffraction pattern comprises all diffraction features.
7. The method for in-situ real-time quantitative detection of film roughness using RHEED as claimed in claim 1, wherein in step c), the brightness of the diffraction pattern is within the range of brightness that can be collected by the CCD image sensor.
8. The method for in-situ real-time quantitative detection of film roughness using RHEED as claimed in claim 1, wherein in step e), the functional relationship between the shape parameter a of the diffraction pattern and the surface roughness is calculated based on the diffraction condition equation.
9. The method for in-situ real-time quantitative detection of film roughness by RHEED according to claim 1, wherein in the step e), the functional relationship between the shape parameter A and the surface roughness of the diffraction pattern is as follows:
where σ is the roughness of the surface of the film, k is the incident wave vector of the reflective high-energy electron diffractometer, and d0、σ0Respectively is the width and the surface roughness of the column of the inverted space on the surface of the single crystal substrate, and theta is the incident angle of the reflection type high-energy electron diffractometer.
10. The method for in-situ real-time quantitative detection of film roughness by using RHEED as claimed in claim 8, wherein the roughness σ is defined as the root mean square value of all the particles on the surface of the epitaxial film in the direction perpendicular to the substrate, and the expression is:
wherein z (k) is the spatial coordinate value of the kth particle on the surface of the film perpendicular to the surface, and n is the total number of all particles on the surface of the epitaxial film.
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| CN202110022387.0A CN112857270B (en) | 2021-01-08 | 2021-01-08 | Method for in-situ real-time quantitative detection of film roughness by using RHEED |
| PCT/CN2021/138645 WO2022148223A1 (en) | 2021-01-08 | 2021-12-16 | Method for in-situ real-time quantitative measurement of roughness of film by using rheed |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114717539A (en) * | 2022-05-12 | 2022-07-08 | 季华实验室 | MOCVD (metal organic chemical vapor deposition) cavity with reflective high-energy electron diffractometer |
| WO2022148223A1 (en) * | 2021-01-08 | 2022-07-14 | 上海科技大学 | Method for in-situ real-time quantitative measurement of roughness of film by using rheed |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022148223A1 (en) * | 2021-01-08 | 2022-07-14 | 上海科技大学 | Method for in-situ real-time quantitative measurement of roughness of film by using rheed |
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| CN112857270B (en) | 2022-12-09 |
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