CN111435123A - Metal TiN measurementxMethod for film absorption coefficient - Google Patents
Metal TiN measurementxMethod for film absorption coefficient Download PDFInfo
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- CN111435123A CN111435123A CN201910042818.2A CN201910042818A CN111435123A CN 111435123 A CN111435123 A CN 111435123A CN 201910042818 A CN201910042818 A CN 201910042818A CN 111435123 A CN111435123 A CN 111435123A
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract
The invention relates to a method for measuring metallic TiNxMethod of absorption coefficient of thin film. Firstly, a P-GaN substrate and a metallic TiN coating layer with the thickness of about 50nm are coatedxPerforming cathode fluorescence test (C L) at different voltages on the same position of the thin film P-GaN to obtain corresponding cathode fluorescence intensity, and obtaining TiN at different voltages according to Lambert's lawxThe absorption coefficient of the film, and further obtaining the average absorption coefficient value; finally, the square resistance of the film is tested by utilizing the four-probe technology to further determine the TiNxMetallic thin film the present invention utilizes SEM in combination with C L to obtain metallic TiNxAbsorption coefficient of the film, thereby providing a semi-conductivityA novel method for measuring the absorption coefficient of a metallic thin film having a thickness of several tens of nanometers on a bulk substrate.
Description
Technical Field
The invention relates to a method for measuring the absorption coefficient of a film, in particular to a metallic TiN filmxA method for measuring the absorption coefficient of the film.
Background
Titanium nitride (TiN)x) Is a refractory non-stoichiometric transition metal nitride, has a melting point as high as 2930 ℃, metallic TiNx is golden yellow, and exhibits plasma excitation behavior in the visible and near infrared spectral ranges. Compared with conventional plasma materials, e.g. gold and silver, TiNxHas the advantages of high melting point, good chemical stability, high mechanical strength, corrosion resistance, biocompatibility, easy integration with standard silicon-based technology, and TiNxHas tunability with variations of growth parameters, and thus, TiNxBecomes a plasma ceramic material for replacing the traditional noble metal material gold, marks a new technical start of a plasma device and is TiN with nanometer sizexThe film comprises a nano-sized film, a nano antenna, nano particles, a super surface and a nano pattern structure, and has wide application prospects in the aspects of solar thermal photovoltaic systems (S/TPV), biological medical treatment, heat-assisted magnetic recording (HAMR), High-temperature sensors (High-T sensors), planar photonic devices (flat optics) and the like. In addition to this, metallic TiNx thin films are also being widely studied and used as diffusion barrier layers, ohmic contact layers, rectifying layers in device metallization mechanisms, and gate electrodes in CMOS devices due to their low resistivity and high temperature resistance.
At present, TiNx thin films can be grown by a variety of deposition techniques, including Chemical Vapor Deposition (CVD), atomic layer deposition (A L D), and Physical Vapor Deposition (PVD) such as reactive magnetron sputtering (reactive sputtering), pulsed laser deposition (P L D), etcThe ellipsometry parameters of the TiNx film include the total amplitude and phase of the reflected light at the surface and interfaces of the film, so as to fit the optical parameters of the film, such as refractive index, extinction coefficient, etc., however, in our test, we found that when the metallic TiN film is usedxWhen the thickness of the thin film reaches several tens of nanometers, metal TiN is usedxThe specular reflection and absorption of light by the film make it difficult to accurately fit the optical parameters of the film.
Disclosure of Invention
The invention provides a metallic TiNxThe method for measuring the absorption coefficient of the film can accurately estimate the absorption coefficient of the TiNx film and further determine the growing TiNxThe film is metallic.
The invention provides a metallic TiNxA method for measuring an absorption coefficient of a thin film, the method comprising:
providing a P-GaN substrate with sapphire as a base, and performing a C L test at different voltages on the same position of the P-GaN substrate by utilizing a cathode fluorescence (C L) component attached to a scanning electron microscope;
cleaning the P-GaN substrate;
TiN on P-GaN surface by Pulsed laser Deposition system (Pulsed L ase Deposition, P L D)xGrowing a thin film;
using X-ray diffraction (XRD) and Atomic Force Microscope (AFM) to grow TiNxThe crystal structure, orientation and surface morphology of the film are characterized;
using Scanning Electron Microscope (SEM) to treat TiNxThe section morphology of the film is characterized to obtain the thickness of the TiNx film;
are oppositely coated with TiNxCathodic fluorescence tests (C L) were carried out on samples of the film at the same position and at different voltages to obtain grown TiNxThe cathode fluorescence intensity of the sample after film formation was determined according to Lambert's law, I ═ I0e-αdThereby obtaining TiN under different voltagesxThe absorption coefficient of the film is obtained, and then the average absorption coefficient value is obtained, and the average absorption coefficient value is compared with the range of the absorption coefficient of the metal, so as to determine the TiNxThe metallic nature of the film;
finally, the square resistance of the film is tested by utilizing the four-probe technology to further determine the TiNxThe metallic nature of the film.
The method has the beneficial effects that the metallic TiN is obtained by combining SEM and C LxThe absorption coefficient of the film, thereby providing a new method for measuring the absorption coefficient of a metallic film having a thickness of several tens of nanometers on a semiconductor substrate.
Drawings
In order to make the objects, technical solutions and advantages of the present invention clearer and more clear, the present invention is further described in detail with reference to the accompanying drawings, in which:
TiN grown on P-GaN substrate of FIG. 1xXRD pattern of the film;
figure 2 TiN grown on P-GaN substratexAFM topography of the film;
figure 3 TiN grown on P-GaN substratexA cross-sectional SEM topography of the film;
FIG. 4C L results for P-GaN at different voltages;
FIG. 5 is a TiN coated layerxC L results for P-GaN of the film at different voltages;
FIG. 6P-GaN and TiN cappingxComparison of the results of the C L test at different voltages for P-GaN of thin films.
Detailed Description
The TiNx film grown on the Mg-doped C-plane P-GaN substrate by utilizing the pulse laser deposition (P L D) system of the laboratory presents golden yellow and has metallic luster, wherein the pulse laser deposition system is an excimer laser with the wavelength of 248nm, the pulse width is 25ns, the maximum pulse frequency is 10HZ, the P-GaN substrate is sapphire, the sample is tested and characterized, and the TiN is obtained according to the Lambert law by combining SEM and C LxThe absorption coefficient of the film is further determined to be metallic by testing the square resistance, and the method comprises the following specific steps:
providing Mg-doped P-GaN with sapphire as a substrate, performing C L tests under different voltages at the same position of the P-GaN substrate by utilizing a cathode fluorescence (C L) component attached to a scanning electron microscope, as shown in figure 4, and then cleaning the substrate;
putting the cleaned P-GaN wafer dried by nitrogen into a deposition chamber, and vacuumizing until the background vacuum reaches 10 DEG-6Pa above, heating to 600 deg.C, heat treating for 1h, then heating to 650 deg.C, introducing high purity N2When the preset pressure is reached, N is generated by using a plasma device carried by a P L D system2Plasma, the P-GaN surface is pretreated for 10 minutes, and a surface oxide layer is removed;
laser is incident at an angle of 45 degrees, enters a deposition chamber through lens focusing, a baffle plate before a substrate is put down before deposition, TiN target materials with the purity of 99.9 percent are pre-sputtered for 2-3 minutes, then the baffle plate is removed, deposition is started, the deposition temperature is 650 ℃, the air pressure is 3Pa, the deposition time is 1h, the target spacing is 8cm, the laser energy is 250mJ, the pulse repetition frequency is 2HZ, the deposition is finished, in-situ annealing is carried out for 1h, and a sample is taken out after the temperature is reduced to the room temperature, wherein the sample is golden yellow and has metallic luster as shown in figure 1;
the crystal structure and crystal orientation of the sample were characterized by X-ray diffraction (XRD), as shown in FIG. 1, for a P-GaN substrate and TiN grownxTheta-2 theta scan curve of the film, with scan angles ranging from 20 deg. -90 deg., as can be seen from fig. 1, TiN grown on P-GaN substratexThe film presents (111) preferred orientation, the corresponding diffraction peak position is face-centered cubic structure TiNxThe (111) and (222) crystal planes of (a);
using Atomic Force Microscope (AFM) to TiNxThe surface morphology of the film was characterized as shown in FIG. 2, TiNxThe film presents a flat and smooth surface with a surface roughness of 0.259 nm;
the cross-sectional morphology of the sample was characterized by Scanning Electron Microscopy (SEM), and as can be seen from FIG. 3, the TiN grown by usxThe film is flat and compact, has a clear interface and the thickness of 49.6nm, thereby obtaining TiN on the P-GaN substratexThe average growth rate of the film is about 0.8 nm/min;
to deposition of TiNxThe same position of the thin film sample was subjected to C L test at different voltages, as shown in FIG. 5, to deposit TiNxAfter the film, the C L intensity was greatly reduced, indicating that the cathode fluorescence emitted by P-GaN was reflected by TiNxThe film is greatly attenuated after absorption, and only the luminescence peak position of GaN is present and the peak position is not moved, which also indicates that the TiNx film grown by us is metallicity, and the C L intensity of the P-GaN substrate is rapidly increased along with the increase of the voltage, and TiN is grown completelyxAfter the film, the strength of C L slightly increased with increasing voltage, as shown in FIG. 6;
the peak values of the C L intensities at different voltages are shown in table 1, according to lambert's law I ═ I0e-αdIn which I0C L strength of P-GaN substrate, I TiN growthxC L Strength of the sample after film formation, d film thickness, α TiNxAbsorption coefficient of the thin film, thereby obtaining TiNxAbsorption coefficient of filmThe specific calculation results are shown in table 1;
TABLE 1
Voltage(KV) | (P-GaN)CL I0 | CL I | Ln(I/I0) | α(cm-1) |
10 | 11337.05 | 2635.57 | -1.45898 | 2.94×105 |
12 | 18867.76 | 2781.09 | -1.91461 | 3.86×105 |
14 | 24499.71 | 3140.55 | -2.05426 | 4.14×105 |
16 | 35538.33 | 3410.45 | -2.34377 | 4.73×105 |
Thus, we found that the average absorption coefficient of the film sample was 3.92 × 10^ (5) cm ^ -1 at 105Magnitude, and the absorption coefficient of the metal is in the range of 10^ (4) to 10^ (5), which indicates that TiN is grownxThe film is metallic;
finally, the square resistance of the TiNx film is tested by utilizing a four-probe technology, the test result is 14.36 omega/□, and the TiN is tested according to the SEM testxThe film had a thickness of 49.6nm and thus had a resistivity of p ═ Rd, where R represents the sheet resistance and d represents the thickness of the film, to obtain a film having a resistivity of 7.12 × 10 < SP > -5 </SP >. omega.cm, while the resistivity of typical metals is in the range of 10 < SP > -5 </SP > -10 < SP > -6 </SP >. omega.cm, which further determined that the TiN we grown wasxThe thin film exhibits metallicity and has excellent conductivity.
The invention utilizes SEM and C L to combine to obtain metallic TiNxThe absorption coefficient of the film, thereby providing a new method for measuring the absorption coefficient of a metallic film having a thickness of several tens of nanometers on a semiconductor substrate.
Claims (3)
1. A method for measuring the absorption coefficient of a metallic TiNx film is characterized by comprising the following steps:
(1) providing a P-GaN substrate with sapphire as a substrate, and performing cathode fluorescence tests (C L) on the same position of the P-GaN substrate under different voltages;
(2) cleaning the P-GaN substrate;
(3) TiN on P-GaN surface by using pulsed laser deposition systemxGrowing a thin film;
(4) characterizing the crystal structure, orientation and surface morphology of the growing TiNx film by X-ray diffraction (XRD) and an Atomic Force Microscope (AFM);
(5) using Scanning Electron Microscope (SEM) to treat TiNxThe section morphology of the film is characterized to obtain the thickness of the TiNx film;
(6) performing cathode fluorescence tests (C L) at different voltages on the same position of the sample coated with the TiNx film to obtain the growing TiNxThe cathode fluorescence intensity of the sample after film formation was determined according to Lambert's law, I ═ I0e-αdThereby obtaining TiN under different voltagesxThe absorption coefficient of the film is obtained, and then the average absorption coefficient value is obtained, and the average absorption coefficient value is compared with the range of the absorption coefficient of the metal to determine the metallicity of the TiNx film;
(7) finally, the square resistance of the film is tested by utilizing the four-probe technology to further determine the TiNxThe metallic nature of the film.
2. The TiN film as defined in claim 1 for measuring metallic propertiesxThe method for measuring the absorption coefficient of the thin film is characterized in that the laser in the step (3) is a KrF excimer laser with the wavelength of 248nm, the laser pulse width is 25ns, and the maximum pulse repetition frequency is 10 HZ.
3. A measured metallic TiN as set forth in claim 1xA method for decreasing the absorption coefficient of a thin film, characterized in that the TiN is used in the step (5)xThe thickness of the film is about 50 nm.
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CN105917035A (en) * | 2014-01-17 | 2016-08-31 | 三菱化学株式会社 | GaN substrate, method for producing GaN substrate, method for producing GaN crystal, and method for manufacturing semiconductor device |
CN106206951A (en) * | 2016-07-19 | 2016-12-07 | 郑州大学 | The new application of polyvinylamine, perovskite thin film, perovskite solaode and preparation method thereof |
CN108107066A (en) * | 2017-12-19 | 2018-06-01 | 北京工业大学 | For the SEM/ESEM cathode-luminescence imaging methods of biological nano probe |
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CN1746617A (en) * | 2005-09-30 | 2006-03-15 | 电子科技大学 | Thin-membrane thickness and density measurement without sampler |
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CN105917035A (en) * | 2014-01-17 | 2016-08-31 | 三菱化学株式会社 | GaN substrate, method for producing GaN substrate, method for producing GaN crystal, and method for manufacturing semiconductor device |
CN105552171A (en) * | 2016-02-01 | 2016-05-04 | 上海理工大学 | Method for preparing Cu2ZnSnS4 extra-thin sunlight absorption layer by one-step spraying method |
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