CN111441027A - Surface Modification of Fe70Nb10B20 Amorphous Alloy Thin Films - Google Patents

Abstract

The present application discloses a surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film, which includes the following steps: installing a target material on a target head of a magnetron sputtering equipment, the target material containing Fe, Nb and B elements; The experimental substrate is arranged on the board surface of the substrate; the position of the substrate is adjusted so that the experimental substrate faces the target head; the substrate is installed so that the substrate faces the target head; the temperature of the substrate is heated to reach the first preset temperature; The space is in a preset argon atmosphere; the target head is energized; the target is sputtered to the substrate in a preset sputtering state. The benefit of the present application is to provide a surface modification method capable of obtaining Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin films with better wear resistance.

Description

Surface Modification of Fe70Nb10B20 Amorphous Alloy Thin Films

technical field

The present application relates to a surface modification method of an amorphous alloy thin film, in particular to a surface modification method of an Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film.

Background technique

Amorphous alloys are different from traditional metal materials, and their internal atomic arrangement structure is disordered. Due to this complex structural feature, there are no defects in crystalline materials, so that they have good toughness, high strength, and excellent The anti-corrosion and wear-resistant properties of the alloy have gradually become a new type of material that has attracted much attention in aerospace, medical equipment and electronic products. With the development of electronic technology, amorphous alloy films have become a research boom in MEMS.

Amorphous alloys can be prepared into a magnetic thin film, which is mainly used in micro-electromechanical systems to protect passivation films and magnetic recording thin film media. Therefore, how to improve the hardness and wear resistance of this component thin film becomes a key to prolonging product life. The essential.

SUMMARY OF THE INVENTION

A surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film includes the following steps: installing a target material to a target head of a magnetron sputtering device, the target material containing Fe, Nb and B elements; The bottom is arranged on the board surface of the substrate; the position of the substrate is adjusted so that the experimental substrate faces the target head; the substrate is installed so that the experimental substrate faces the target head; its temperature reaches a first preset temperature; the space where the target material and the substrate are located is in a preset atmosphere state; the target head is energized; the target material is sputtered to the substrate in a preset sputtering state shoot.

Further, the target material is selected from Fe ₇₀ Nb ₁₀ B ₂₀ alloy material with the same atomic ratio.

Further, the target material is cylindrical, and its diameter ranges from 48mm to 50mm.

Further, the thickness of the target material ranges from 3 mm to 5 mm.

Further, the experimental substrate is rectangular, and its length ranges from 8 mm to 12 mm, and its width ranges from 8 mm to 12 mm.

Further, the experimental substrate includes a single crystal silicon wafer (thickness 1 mm) and a glass sheet (thickness 3 mm).

Further, the value range of the first preset temperature is 25 degrees Celsius to 200 degrees Celsius.

Further, the vacuum degree of the equipment is 4×10 ^-4 Pa.

Further, the pre-sputtering atmosphere is argon, and the sputtering gas pressure ranges from 0.5Pa to 1.2Pa.

The benefits of this application are:

Provided is a surface modification method capable of obtaining Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin films with better wear resistance.

Description of drawings

1 is a schematic structural diagram of a magnetron sputtering apparatus according to an embodiment of the application;

Fig. 2 is an information diagram obtained by XRD detection of the amorphous alloy film obtained by the method of the present application;

3 is a schematic diagram of nano-indentation load displacement of amorphous alloy thin films according to several embodiments of the present application;

Fig. 4 is the nanoindentation experiment result modulus and hardness statistics diagram of several embodiments of the application;

FIG. 5 is a statistical graph of the friction force on the needle tip during the nano-scratch process of several embodiments of the present application.

Explanation of reference numerals: 1- sample stage with thermocouple, 2- experimental substrate, 3- sample substrate, 4- glow during sputtering, 5- Fe ₇₀ Nb ₁₀ B ₂₀ alloy target, 6- equipment target.

Detailed ways

In order to make those skilled in the art better understand the solutions of the present application, the technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of the present application, not All examples. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the scope of protection of the present application.

FIG. 1 shows the magnetron sputtering apparatus employed in the present application.

When the present application is prepared, the following steps may be included:

The target is mounted on the target head of the magnetron sputtering equipment, and the target contains Fe, Nb and B elements. As a specific solution, the target material is selected from Fe ₇₀ Nb ₁₀ B ₂₀ alloy material with the same atomic ratio; the target material is cylindrical, and its diameter ranges from 48mm to 50mm; the target thickness ranges from 3mm to 5mm, preferably 4mm.

Adhere the experimental substrate to the surface of the base plate; adjust the position of the sample stage with the thermocouple so that the experimental substrate faces the target head. Specifically, the experimental substrate is pasted to the substrate. The experimental substrate is protected by a blue film during the preparation period. When the preparation period is over, the blue film is removed to ensure the surface roughness of the experimental substrate when sputtering is ready. As a specific solution, the experimental substrate is a rectangle with a length ranging from 8 mm to 12 mm and a width ranging from 8 mm to 12 mm, preferably a square sheet of 10 mm by 10 mm. The experimental substrate can choose single crystal silicon wafer and glass wafer, the thickness of single crystal silicon wafer is 1mm, and the thickness of glass wafer is 3mm.

Install the substrate on the sample stage so that the experimental substrate faces the target head, and adjust the corresponding position according to the specific situation and the instrument. It is advisable that the sputtering direction is perpendicular to the experimental substrate.

The substrate is heated to reach a first preset temperature. As a specific solution, the first preset temperature may be in a non-heated state, such as 25 degrees Celsius, and 100 degrees Celsius and 200 degrees Celsius in a heated state, corresponding to RT, 373K and 473K, respectively.

The space where the target and substrate are located is in a preset high vacuum state. As a specific scheme, the degree ^of vacuum is 4×10 ^-4 Pa.

The target head is energized and the target is sputtered to the substrate in a preset sputtering state. The preset atmosphere state is argon atmosphere, and the sputtering gas pressure ranges from 0.5Pa to 1.2Pa, preferably 0.7Pa.

The present application will be described in detail below with reference to the embodiments.

Example 1

The target in this embodiment is an alloy target with an atomic ratio of Fe ₇₀ Nb ₁₀ B _20. Before placing the target, the surface of the target needs to be ground with an angle grinder to remove the surface oxide layer. The substrate is a glass sheet covered with a blue film (size: 10*10*3mm) or a single crystal silicon wafer with a <100> crystal orientation (size: 10*10*1mm). Before the experiment, the substrate was ultrasonically cleaned with acetone for 3 minutes, and the acetone on the surface was quickly evaporated with a compressed air gun, and then the cleaned glass or single crystal silicon wafer was fixed on the sample stage with high-temperature tape.

After the preliminary preparation is completed, install the polished alloy target on the target head with the characteristics of the magnetic target. After installation, use a multimeter to check whether the target is connected to the shielding cover. If there is a short circuit, the shielding cover should be loosened. . Insert the substrate with the glued sample on the sample stage of the equipment. The temperature of the substrate is 373K. The sample needs to be installed on the sample stage with a thermocouple. Close the chamber and prepare for vacuuming.

When the vacuum degree is 4.0×10 ^-4 Pa, argon gas is introduced, and the molecular pump and the argon gas flux are adjusted to keep the vacuum degree at 2.0Pa. Turn on the DC power supply, adjust the power to 80W to start the target, and adjust the molecular pump channel to maintain the sputtering pressure at 0.7Pa. After the glow is stable, open the target baffle for half an hour and start sputtering. During pre-sputtering, the heating furnace plate can be opened to preheat to avoid excessive internal stress. The sputtering time was selected to be two hours. After heating the samples, the heat preservation was continued for half an hour. The surface of the film was more uniform, and all samples were cooled with the furnace.

Example 2

The target material in this embodiment is an alloy target material with an atomic ratio of Fe ₇₀ Nb ₁₀ B _20. Before securing the target material, the surface of the target material needs to be ground with an angle grinder to remove the surface oxide layer. The substrate is a glass sheet covered with a blue film (size: 10*10*3mm) and a monocrystalline silicon wafer with a <100> crystal orientation (size: 10*10*1mm). Before the experiment, the substrate was ultrasonically cleaned with acetone for 3 minutes, and the acetone on the surface was quickly evaporated with a compressed air gun, and then the cleaned glass wafer and single crystal silicon wafer were fixed on the sample stage with high-temperature tape.

After the preliminary preparation is completed, install the polished alloy target on the target head with the characteristics of the magnetic target. After installation, use a multimeter to check whether the target is connected to the shielding cover. If there is a short circuit, the shielding cover should be loosened. . Insert the sample stage with the glued sample into the designated position on the device. The substrate temperature is 473K. The sample needs to be installed on the sample stage with the thermocouple, close the chamber, and prepare to vacuumize.

When the vacuum degree is 4.0×10 ^-4 Pa, argon gas is introduced, and the molecular pump and the argon gas flux are adjusted to keep the vacuum degree at 2.0Pa. Turn on the DC power supply, adjust the power to 80W to start the target, and adjust the molecular pump channel to maintain the sputtering pressure at 0.7Pa. After the glow is stable, open the target baffle for half an hour and start sputtering. During pre-sputtering, the heating furnace plate can be opened to preheat to avoid excessive internal stress. The sputtering time was selected to be two hours. After heating the samples, the heat preservation was continued for half an hour. The surface of the film was more uniform, and all samples were cooled with the furnace.

Comparative ratio

The target material in this embodiment is an alloy target material with an atomic ratio of Fe ₇₀ Nb ₁₀ B _20. Before securing the target material, the surface of the target material needs to be ground with an angle grinder to remove the surface oxide layer. The substrate is a glass sheet covered with a blue film (size: 10*10*3mm) and a monocrystalline silicon wafer with a <100> crystal orientation (size: 10*10*1mm). Before the experiment, the substrate was ultrasonically cleaned with acetone for 3 minutes, and the acetone on the surface was quickly evaporated with a compressed air gun, and then the cleaned glass wafer and single crystal silicon wafer were fixed on the sample stage with high-temperature tape.

After the preliminary preparation is completed, install the polished alloy target on the target head with the characteristics of the magnetic target. After installation, use a multimeter to check whether the target is connected to the shielding cover. If there is a short circuit, the shielding cover should be loosened. . Insert the sample stage with the glued sample into the designated position on the equipment, the substrate temperature is room temperature, close the chamber, and prepare to vacuumize.

When the vacuum degree is 4.0×10 ^-4 Pa, argon gas is introduced, and the molecular pump and the argon gas flux are adjusted to keep the vacuum degree at 2.0Pa. Turn on the DC power supply, adjust the power to 80W to start the target, and adjust the molecular pump channel to maintain the sputtering pressure at 0.7Pa. After the glow is stable, open the target baffle for half an hour and start sputtering. During pre-sputtering, the heating furnace plate can be opened to preheat to avoid excessive internal stress. The sputtering time was selected to be two hours. After heating the samples, the heat preservation was continued for half an hour. The surface of the film was more uniform, and all samples were cooled with the furnace.

After the film samples prepared in the above examples were taken out, the samples on the glass substrate were tested by XRD, and the experimental results were all amorphous structures.

Figure 2 shows the experimental results. After the structural information is determined, Hysitron Inc, Minneapolis, MN nano-indentation tester is used to test the mechanical parameters of the modulus and hardness of the thin film sample. The nano-indentation experimental parameters use Berkvich indenter, and the maximum displacement resolution of the instrument is 0.05nm/s the following. In order to verify the repeatability of the experimental results, 9 points were measured under each parameter. The experimental conditions are as follows: the maximum load is 8mN, the loading rate is 1.6mN/s, the holding time is 5s, the unloading rate is 1.6mN/s, and the dot matrix is 3×3. The nano-scratch experiment adopts the ramp loading mode with a peak load of 1.5 mN and a loading rate of 10 μN/s.

The experimental results show that the modulus and hardness of the material increase with the increase of the substrate temperature. In the nanoindentation experiment, from the load-displacement curve, the film samples of the same composition and the film samples with the higher substrate temperature are The shallower the maximum indentation depth, from the modulus and hardness statistics, the modulus and hardness of the film will increase with the increase of the substrate. The lateral force on the amorphous alloy film, that is, the friction force, will become smaller, and the friction force is the product of the load and the friction coefficient. Since the test parameters are consistent, it means that the friction coefficient will become smaller, and the wear resistance of the material depends on The friction coefficient of the material itself, the smaller the friction coefficient, the better the wear resistance of the material.

It can be seen from the above that the principle of magnetron sputtering technology is vapor deposition, which can easily prepare amorphous alloys. The atomic structure of amorphous alloys is disordered. During the sputtering process, there will be local atomic clusters. There are vacancies around the clusters, which will induce the softening behavior of the film. This application is different from the traditional annealing process. The substrate is heated in real time and annealed in real time during the process of preparing the sample, which greatly homogenizes the atomic arrangement inside the film, thereby improving the material. hardness and wear resistance.

The foregoing has shown and described the rationale, main features and advantages of the present application. Those skilled in the art should understand that the above-mentioned embodiments do not limit the present application in any form, and all technical solutions obtained by means of equivalent replacement or equivalent transformation fall within the protection scope of the present application.

Claims (9)

1. a surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film, is characterized in that: The method includes the following steps: Mounting the target material to the target head of the magnetron sputtering equipment, the target material containing Fe, Nb and B elements; Adhering the experimental substrate to the surface of the substrate; Adjust the position of the heated sample stage to face the target head; mounting the substrate so that the substrate faces the target; heating the substrate so that its temperature reaches a first preset temperature; making the target and the substrate in a preset atmosphere state; energizing the target; The target is sputtered on the substrate in a preset sputtering state. 2. the surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, is characterized in that: The target material is selected from Fe ₇₀ Nb ₁₀ B ₂₀ alloy material with the same atomic ratio. 3. the surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 2, is characterized in that: The target material is cylindrical, and its diameter ranges from 48mm to 50mm. 4. the surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 3, is characterized in that: The thickness of the target material ranges from 3 mm to 5 mm. 5. the surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, is characterized in that: The experimental substrate is rectangular, its length ranges from 8 mm to 12 mm, and its width ranges from 8 mm to 12 mm. 6. The surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, characterized in that: The experimental substrate includes a single crystal silicon wafer and a glass wafer, the single crystal silicon wafer is 1 mm, and the glass wafer is 3 mm. 7. The surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, characterized in that: The values of the first preset temperature are 25 degrees Celsius, 100 degrees Celsius and 200 degrees Celsius. 8. The surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, characterized in that: The vacuum degree of the equipment during the experiment was 4×10 ^-4 Pa. 9. The surface modification method of Fe ₇₀ Nb ₁₀ B ₂₀ amorphous alloy thin film according to claim 1, characterized in that: The preset sputtering atmosphere is argon, and the sputtering gas pressure ranges from 0.5Pa to 1.2Pa.

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