AU2020101087A4 - A Method of Preparing Nanometer Aluminum Film by Radio Frequency Magnetron Sputtering - Google Patents
A Method of Preparing Nanometer Aluminum Film by Radio Frequency Magnetron Sputtering Download PDFInfo
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
The invention, belonging to the technical field of aluminum film preparation,
discloses a method for preparing nanometer aluminum film by radio frequency
magnetron sputtering, which goes like this: adopt magnetron sputtering machine,
aluminum target (as sputtering target) and microslide (as substrate) to prepare
aluminum film by radio frequency sputtering; clean the substrate with anhydrous
ethanol for 20min before placing it into the vacuum chamber, dry it and place it on the
rotating sample stage; adjust the target-substrate distance to 100mm, and the base
pressure of the sputtering device is up to 5.0x10-4Pa by vacuum pumping; introduce
argon with purity of 99.999% and flow of 40sccm, at room temperature, sputtering
time: 600s; adjust negative bias voltage, RF power and working gas pressure, and
discuss the effects of the three parameters on film deposition rate by orthogonal
experiment. By selecting process parameters, the invention designs an aluminum film
with higher deposition rate, better film quality, thicker film and fine grain size.
Drawings
Use MSP-300B magneton sputtering machine (Beijmg Chuangshiweina Technology Co. LTD, Beijng) sti
aluminum target (as sputtering target) with <b8omm thickness of 5m and purity of 99.99%, and microshde (25.4x
76.2mm) as the substrate topreparealuinum film by radiofreqencysputtenng
Clean the substrate with anhydrous ethanol for 20m before placing it into the vacuum chamber dry it and place
it on the rotating sample stage
Adjust the target-substrate distance to 100% and the base pressure of the sputtering device is up to 5.0x 4Pa S1
by vacuum pumping; introduce argon with purity of 99.999. and flow of 40scm at room temperature
sputteg . t ZZ 60
1 . 5104
Adjust negative bias voltage, RF power and working gas pressure, and discuss the effects of the three parameters
on film deposition rate by orthogonal experiment
FIG.1
1/3
Description
Drawings
Use MSP-300B magneton sputtering machine(Beijmg Chuangshiweina Technology Co. LTD, Beijng) sti aluminum target (as sputtering target) with <b8omm thickness of 5m and purity of 99.99%, and microshde (25.4x 76.2mm) as the substrate topreparealuinum film by radiofreqencysputtenng
Clean the substrate with anhydrous ethanol for 20m before placing it into the vacuum chamber dry it and place it on the rotating sample stage
Adjust the target-substrate distance to 100% and the base pressure of the sputtering device is up to5.0x 4Pa S1 by vacuum pumping; introduce argon with purity of 99.999. and flow of 40scm at room temperature sputteg . t ZZ 60
1 . 5104 Adjust negative bias voltage, RF power and working gas pressure, and discuss the effects of the three parameters on film deposition rate by orthogonal experiment
FIG.1
1/3
Description
A Method of Preparing Nanometer Aluminum Film by Radio
Frequency Magnetron Sputtering
Technical Field The invention, belonging to the technical field of aluminum film preparation, relates to a method of preparing nanometer aluminum film by radio frequency magnetron sputtering
Background Technology Since the 1970s, thin film technology and materials have developed by leaps and bounds, and have achieved fruitful results in both academic and practical applications. They have become the hottest field of research in vacuum science and technology and material science, which play a pivotal role in the high-tech industry. Thin film technology and thin film materials have penetrated into every important field of modem science and technology and national economy. With the development of thin film science and technology and thin film physics, thin film has been widely used in the fields of aerospace, medicine, energy, transportation, communication and information, etc., which has stimulated the vigorous development of thin film technology and related materials. With excellent mechanical properties, good corrosion resistance and wettability, good corrosion resistance, adhesion, reflectivity and beautiful silver-white appearance, nanometer aluminum film has been widely used in semiconductor devices, large-scale integrated hybrid circuits, daily necessities and decorative building materials. In addition, with fine and uniform grains, nanometer aluminum film has good stress coordination ability, so that the whole coating maintains a good adhesion form. It is often used in the bottom or middle layer of multilayer film to improve the performance of the whole film substrate system. Moreover, aluminum is rich in content and cheap in price, and its manufacturing cost is low. Therefore, cheap and durable nanometer materials with excellent properties should be widely promoted and used in industrial production. From the current research status of nano-metal materials, most researchers in China and abroad have conducted a series of studies on nano-Al films, but they cannot fully explain the nucleation mechanism of nano-Al films and the factors influencing the microstructure properties, the effects of sputtering current and power change, working gas pressure and sputtering time on morphology, micromechanical properties and corrosion resistance of nanometer aluminum film. The results show that the quality of the coating can be improved by decreasing the argon pressure and increasing the sputtering current. With the prolonging of coating time, the migration time of sputtering atoms from the surface to the inside increases, and the film is densified to a certain extent. The surface roughness and particle size of aluminum films prepared by AFM are compared between DC sputtering and RF sputtering. Under the condition of DC sputtering, the deposition rate is increased with the increase of sputtering power,
Description
resulting in the increase of surface roughness and grain size. Under the condition of RF sputtering, the surface roughness and particle size of the film are increased with the extension of coating time. Single crystal aluminum film cannot be formed on Si(OO1) substrate, while on Si(111) substrate, when the substrate temperature is 473K and the Al film thickness reaches 500nm, single crystal aluminum film can be obtained after 748K annealing treatment. The middle layer of aluminum film is prepared by DC sputtering. The results show that the surface roughness of the substrate is directly related to the grain size distribution and surface roughness of Al film. Al film is prepared on the surface of AZ31 magnesium alloy by RF magnetron sputtering method. The results show that the mechanical properties of AZ31 surface are improved by the prepared film. The deposition rate increases with the increase of target power, but the surface roughness of the film also increases and the film structure becomes loose. At present, there is no systematic and complete theoretical experimental guidance for the manufacture and coating design of Al film by RF magnetron sputtering at home and abroad. It is intended to improve the performance of the nano-Al film, which depends on the structure of the tissue, which is controlled by the process parameters of the deposition process. Therefore, the main purpose of this experiment is to explain the law of surface morphology of Al film by using the change of process parameters, and to obtain the deposition rate of nanometer aluminum film under different process parameters. Therefore, the effects of various process parameters on the preparation of nanometer Al film by radio frequency magnetron sputtering are obtained through experiments, and the individual effects and the correlation between them are pointed out in this patent. Excellent film is obtained by optimizing the process parameters. According to domestic and foreign reports, the deposition rate of the film prepared by magnetron sputtering method is relatively low, and the film thickness usually does not exceed 1 m. However, when using RF magnetron sputtering to prepare Al film, it is found that the thickness of the film is 3.7-12.1 m when sputtering for 10 minutes with different process parameters. It shows that the process parameters have a great influence on the deposition rate of thin films. In this experiment, the deposition rate is relatively high, and the film prepared by X-ray diffractometer includes amorphous aluminum film and polycrystalline aluminum film. At present, there are many methods to prepare aluminum coating, such as thermal spraying, electroplating, rolling and magnetron sputtering. Thermal spraying may change the original characteristics of aluminum material, so it is not suitable for preparation in non-high-temperature resistant substrates. Moreover, the coating prepared by this method has low adhesion, high porosity and poor uniformity. The film thickness of aluminum coating prepared by electroplating method is not uniform. In addition, it is unable to accurately select the electroplating position, and electroplating may cause environmental pollution. The pure aluminum foil produced by rolling will produce texture, which will seriously affect the mechanical properties and cannot be compared with the pure aluminum material of nanostructure. Based on the shortcomings of the prior art, the magnetron sputtering technology is used to prepare aluminum film. Magnetron sputtering technology is environmentally friendly without polluting waste gas, and the lower deposition temperature will not change the
Description
substrate size. The prepared film is relatively dense and has a good adhesion to the film substrate, so the coating can be deposited on a large area of substrate.
To sum up, the problems existing in the prior art are as follows: at present, the preparation methods of nanometer aluminum film are characterized by poor bonding ability between the film and substrate, high porosity and poor uniformity. The traditional preparation process consumes a lot of energy and causes great pollution to the environment.
Invention Summary Based on the shortcomings of the prior art, the invention provides a method of preparing nanometer aluminum film by radio frequency magnetron sputtering.
The invention is realized in this way. A method of preparing nanometer aluminum film by radio frequency magnetron sputtering uses microslide as substrate to prepare aluminum film by radio frequency sputtering, with negative bias voltage of 20-60v, RF power of 100-150w, and working gas pressure of 0.7-0.9 Pa.
Another purpose of the invention is to provide a measurement method for the method of preparing nanometer aluminum film by radio frequency magnetron sputtering. The film thickness is measured by field emission scanning electron microscope, the surfaces of the samples are coated with erosion agent to measure the total film thickness of the two samples, and the deposition rate is obtained by the ratio of the thickness of a single sample to the deposition time; optical metallographic microscope is used to observe the film surface morphology; low-angle X-ray diffractometer is used to determine the phase structure of the coating (Cu target, 40kV, 150mA); the full width at half maximum and diffraction angle of diffraction peak of aluminum film sample are obtained by X-ray diffraction, thus obtaining the grain size of the film.
Further, the calculation formula of the grain size of the film:
D is the grain size of the aluminum film; k is the experimental instrument coefficient; k is X-ray wavelength; 0 is the diffraction angle; P is full width half maximum of diffraction peak.
Another purpose of the invention is to provide a nanometer aluminum film prepared by the method of preparing nanometer aluminum film by radio frequency magnetron sputtering.
The invention uses the existing magnetron sputtering technology to design an
Description
aluminum film with higher deposition rate, better film quality, thicker film and fine grain size by selecting appropriate process parameters. The film thickness and surface morphology have important effects on the microstructure and intrinsic properties, such as optical properties and dielectric properties. The invention adopts radio frequency magnetron sputtering technology to prepare nanometer aluminum film on the surface of microslide with high purity aluminum as the target material. In the process of preparing aluminum film, it is important to select process parameters. At the same time, the effects of RF power, working gas pressure and negative bias voltage on aluminum film surface morphology and deposition rate are analyzed.
Brief Description of the Drawings FIG. 1 is flow chart of the method for preparing nanometer aluminum film by radio frequency magnetron sputtering provided in the embodiment of the invention.
FIG. 2 is the surface morphology of 6 groups of thin film samples under different process parameters in the method of preparing nanometer aluminum film by radio frequency magnetron sputtering provided in the embodiment of the invention.
In the figures: (a) negative bias voltage OV, RF power 150W, working gas pressure 0.7 Pa; (b) negative bias voltage 20V, RF power 150W, working gas pressure 0.9 Pa; (c) negative bias voltage 20V, RF power 200W, working gas pressure 1.1Pa; (d) negative bias voltage 40V, RF power 200W, working gas pressure 1.3Pa; (e) negative bias voltage 60V, RF power 150W, working gas pressure 1.3Pa; (f) negative bias voltage V, RF power 200W, working gas pressure 0.5Pa.
FIG. 3 is the relation curve between the process parameters and the film thickness in the method for preparing nanometer aluminum film by radio frequency magnetron sputtering provided in the embodiment of the invention.
Detailed Description of the Presently Preferred Embodiments In order to make the purposes, technical solutions and advantages of the present invention clear, the present invention will be further described in detail below in combination with the embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the invention, the magnetron sputtering technology is used to prepare the aluminum film. Magnetron sputtering technology is environmentally friendly without polluting waste gas, and the lower deposition temperature will not change the substrate size. The prepared film is relatively dense and has a good adhesion to the film substrate, so the coating can be deposited on a large area of substrate.
The following description is made for the purpose of illustrating the general principles of the invention in the attached drawings.
Description
As shown in FIG. 1, the method of preparing nanometer aluminum film by RF magnetron sputtering provided in the embodiment of the invention includes the following steps:
S1O, use MSP-300B magnetron sputtering machine (Beijing Chuangshiweina Technology Co., LTD., Beijing), aluminum target (as sputtering target) with <D80mm, thickness of 5mm and purity of 99.99%, and microslide (25.4x76.2mm) as the substrate to prepare aluminum film by radio frequency sputtering;
S102, clean the substrate with anhydrous ethanol for 20min before placing it into the vacuum chamber, dry it and place it on the rotating sample stage;
S103, adjust the target-substrate distance to 100mm, and the base pressure of the sputtering device is up to 5.0x10-4Pa by vacuum pumping; introduce argon with purity of 99.999% and flow of 40sccm, at room temperature, sputtering time: 600s;
S104, adjust negative bias voltage, RF power and working gas pressure, and discuss the effects of the three parameters on film deposition rate by orthogonal experiment.
Further, a measurement method is provided for the preparation of nanometer aluminum film by RF magnetron sputtering, as follows:
The film thickness is measured by field emission scanning electron microscope (SEM, TESCANVEGA3SBH, Czech), the surfaces of two samples of the same group are coated with a certain amount of erosion agent and then glued together to measure the total film thickness of the two samples, and the deposition rate is obtained by the ratio of the thickness of a single sample to the deposition time; optical metallographic microscope (OM, AxioVert.Al, Germany) is used to observe the film surface morphology; low-angle (1.5°) X-ray diffractometer (XRD, RigakuD/max2500PCXRD, Japan) is used to determine the phase structure of the coating (Cu target, 40kV, 150mA); the full width at half maximum and diffraction angle of diffraction peak of aluminum film sample are obtained by X-ray diffraction, thus obtaining the grain size of the film through the Scherrerformula, where, D is the grain size of the aluminum film; k is the experimental instrument coefficient; X is X-ray wavelength; 0 is the diffraction angle; P is full width half maximum of diffraction peak.
Further, in S104, the table of orthogonal test parameters is shown in Table 1:
Table 1 Head of Orthogonal Test Table
Description
Level Negative Bias Voltage (V) Power (W) Working Gas Pressure (Pa) 1 0 100 0.5 2 20 150 0.7 3 40 200 0.9 4 60 250 1.1 5 80 300 1.3
The purpose of the invention is to design an aluminum film with higher deposition rate, better film quality, thicker film and fine grain size by selecting the appropriate process parameters based on the existing magnetron sputtering technology. The thickness and surface morphology of thin films have important effects on the microstructure and intrinsic properties, such as optical properties and dielectric properties. The invention adopts radio frequency magnetron sputtering technology to prepare nanometer aluminum film on the surface of microslide with high purity aluminum as the target material. In the process of preparing aluminum film, it is important to select process parameters. The effects of RF power, working gas pressure and negative bias voltage on aluminum film surface morphology and deposition rate are analyzed. FIG. 2 is the surface morphology of 6 groups of thin film samples under different process parameters.
As can be seen from FIG. 2(a), there are large particle aggregates on the surface of the film, and particles of small size are scattered randomly, with a large difference in size, among which the largest particle is up to 473 pm long. In FIG. 2(b), dense island-like structures appear, with similar size, accompanied by fusion of the structures. In FIG. 2(c), the islands are denser than those in FIG. 2(b), with smaller gaps between the islands, which become elongated gully clusters. The surface morphology of FIG. 2(d) includes both large cluster aggregates in FIG. 2(a) and island-shaped dense structures in FIG. 2(b). The process parameters in FIG. 2(d) indicate that the deposition rate of the film is very high at this time, and some of the particles may be covered by particles deposited behind before they have time to migrate on the surface, resulting in large clusters in 1, 2 and 3 in FIG. 2(d). The black areas in FIG. 2(e) represent clusters and island structures of aluminum, while the remaining areas represent those not covered by aluminum particles. The undeposited areas are not evenly distributed, and there are large undeposited areas in the middle and around, with different areas and shapes. The islands in FIG. 2(f) are denser than those in FIG. 2(b) and flatter than those in FIG. 2(c), with roughly the same size. The process parameters in FIG. 2(f) indicate that the particles deposited on the surface have a high energy, with few particles per unit time, resulting in sufficient time for the particles to migrate on the surface and grow and aggregate at the appropriate location. Therefore, the film becomes more uniform and the surface becomes densified. Moreover, at this time, the film thickness is 4.1pm, which is smaller in the whole experiment, indicating that
Description
relatively flat surface morphology can be obtained with high energy and low deposition rate.
Table 2 shows the film thickness and grain size of several groups of crystal films in the orthogonal test.
Table 2 Grain Sizes of Aluminum Films with Different Thickness
Process Parameters Film Thickness Deposition Rate Grain Size pm nm/s nm Negative Bias Voltage Power Working Gas Pressure V W Pa 20 200 1.1 4.3 7.17 22.05 20 300 0.5 5.7 9.50 16.60 40 300 0.7 4.9 8.17 20.70 60 200 0.5 4.1 6.83 20.35 80 300 1.1 4.5 7.50 19.73
According to the analysis of the orthogonal test results in FIG. 3, the difference between the ranges of negative bias voltage, RF power and working gas pressure is not large. According to the results of range analysis, the process parameters affecting the film thickness are negative bias voltage, RF power and working gas pressure in turn. With the increase of the negative bias voltage, the deposition rate of the film increases first and then decreases. The deposition rate of the film is the largest at 40V, reaching 0.77 pm/min. With the increase of sputtering power, the film thickness first increases, then drops sharply, and then rises. The deposition rate of the film is the maximum at 150W, reaching 0.75ptm/min. With the increase of working gas pressure, the deposition rate of the film does not change significantly at the beginning, and then increases rapidly, reaching the maximum 0.69pm/min at 1.3Pa.
The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modifications, alternatives and improvements made within the spirit and principles of the present invention shall fall within the scope of the appended claims.
Claims (4)
1. A method of preparing nanometer aluminum film by radio frequency magnetron sputtering is characterized in the fact that it uses microslide as substrate to prepare aluminum film by radio frequency sputtering, with negative bias voltage of -60v, RF power of 100-150w, and working gas pressure of 0.7-0.9 Pa.
2. A measurement method for the method of preparing nanometer aluminum film by radio frequency magnetron sputtering is characterized in the fact that the film thickness is measured by field emission scanning electron microscope, the surfaces of the samples are coated with erosion agent to measure the total film thickness of the two samples, and the deposition rate is obtained by the ratio of the thickness of a single sample to the deposition time; optical metallographic microscope is used to observe the film surface morphology; low-angle X-ray diffractometer is used to determine the phase structure of the coating (Cu target, 40kV, 150mA); the full width at half maximum and diffraction angle of diffraction peak of aluminum film sample are obtained by X-ray diffraction, thus obtaining the grain size of the film.
3. The measurement method as described in claim 2 is characterized by the calculation formula of the grain size of the film:
D=U flcos6 .
D is the grain size of the aluminum film; k is the experimental instrument coefficient; ) is X-ray wavelength; 0 is the diffraction angle; P is full width half maximum of diffraction peak.
4. A nanometer aluminum film prepared by the method of preparing nanometer aluminum film by radio frequency magnetron sputtering as described in claim 1.
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