Method for preparing erbium / erbium oxide composite film on steel plate

Abstract

The invention relates to the technical field of erbium oxide film preparation, and discloses a method for preparing an erbium / erbium oxide composite film on a steel plate, and the preparation method comprises the following steps: fixing a steel substrate on a base, and putting the steel substrate into a cavity of a magnetron sputtering system; the cavity is vacuumized, the steel substrate is heated to a first preset temperature, then argon is introduced, a metal Er target is sputtered on the steel substrate, and therefore a metal Er layer is formed on the surface of the steel substrate; after the metal Er layer is cooled, the steel substrate with the metal Er layer formed on the surface is heated to a second preset temperature, mixed gas with the flow ratio of oxygen to argon being 1: 20-40 is introduced, a metal Er target continues to be sputtered on the surface of the metal Er layer to form an Er2O3 film, then annealing treatment is conducted in the nitrogen atmosphere, and therefore the erbium / erbium oxide composite film is prepared on the steel substrate. The thin film is prepared through magnetron sputtering, high binding force between the Er2O3 thin film and the steel substrate is achieved, and the uniformity, compactness and stability of the thin film are improved.

Description

Technical Field

[0001] The invention belongs to the technical field of erbium oxide film preparation, and particularly relates to a method for preparing an erbium / erbium oxide composite film on a steel plate. Background Art

[0002] Due to the advantages of erbium oxide such as high resistivity and high tritium permeation reduction factor (PRF), the application of erbium oxide coating in nuclear fusion reactor blanket coating has attracted people's attention. In addition, as an important optical and electronic material, erbium oxide coating has a wide range of applications in lasers, fiber optic communications, displays and other fields. However, the bonding force between erbium oxide coating and metal steel substrate is weak, which easily leads to coating shedding or performance degradation, limiting its application in certain specific fields. Therefore, how to improve the bonding force between erbium oxide coating and steel substrate while maintaining the excellent performance of the film has become a problem that needs to be solved urgently.

[0003] Therefore, the prior art still needs to be improved and developed. Summary of the invention

[0004] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing an erbium / erbium oxide composite film on a steel plate, aiming to solve the problem that the bonding force between the erbium oxide coating prepared by the prior art and the steel substrate is weak, which easily leads to the coating falling off.

[0005] The technical solution of the present invention is as follows:

[0006] A method for preparing an erbium / erbium oxide composite film on a steel substrate, comprising the steps of:

[0007] preparing a steel substrate;

[0008] The steel substrate is fixed on a base and placed in a cavity of a magnetron sputtering system;

[0009] The chamber is evacuated, the steel substrate is heated to a first predetermined temperature, and then argon gas is introduced, and a metal Er target is sputtered on the steel substrate, thereby forming a metal Er layer on the surface of the steel substrate;

[0010] After the metal Er layer is cooled, the steel substrate with the metal Er layer formed on the surface is heated to a second predetermined temperature and a mixed gas with a flow ratio of oxygen and argon of 1:20-40 is introduced. The metal Er target is continued to be sputtered on the surface of the metal Er layer to form an Er2O3 film, and then annealing treatment is performed in a nitrogen atmosphere to obtain an erbium / erbium oxide composite film on the steel substrate.

[0011] The method for preparing an erbium / erbium oxide composite thin film on a steel substrate, wherein the step of preparing the steel substrate comprises:

[0012] Cutting a low-activity martensitic steel plate to obtain a steel sheet, grinding the surface of the steel sheet with sandpaper, and then polishing the surface of the steel sheet with a diamond polishing paste to obtain a mirror-finished steel sheet;

[0013] The mirror steel sheet is ultrasonically cleaned with deionized water and alcohol, and dried with N2 to obtain the steel substrate.

[0014] The method for preparing an erbium / erbium oxide composite film on a steel plate, wherein the first predetermined temperature is 450-550°C; and the second predetermined temperature is 450-550°C.

[0015] The method for preparing an erbium / erbium oxide composite film on a steel plate comprises the following steps: the annealing temperature is 700-900° C. and the annealing time is 1-3 hours.

[0016] The method for preparing an erbium / erbium oxide composite film on a steel plate, wherein in the step of evacuating the cavity, the cavity is evacuated to a vacuum of 2.0×10 -4 Pa-4.0×10 -4 Pa.

[0017] The method for preparing an erbium / erbium oxide composite film on a steel plate comprises the following steps: after argon gas is introduced, the vacuum degree of the cavity is maintained at 0.6-0.8 Pa.

[0018] The method for preparing an erbium / erbium oxide composite film on a steel plate comprises the following steps: sputtering a metal Er target on the steel substrate for 20-40 minutes.

[0019] The method for preparing an erbium / erbium oxide composite film on a steel plate comprises the following steps: the time for continuously sputtering the metal Er target on the surface of the metal Er layer to form an Er2O3 film is 40-80 minutes.

[0020] Beneficial effects: The present invention adopts magnetron sputtering technology to first deposit an Er intermediate layer on a steel substrate, and then prepare an Er2O3 composite film on this basis. The present invention prepares the film by magnetron sputtering, realizes a high bonding force between the Er2O3 film and the steel substrate, and improves the uniformity, density and stability of the film. The process of the present invention is simple and efficient, suitable for large-scale production, and the prepared Er2O3 composite film has broad application prospects in the fields of optics, electronics and magnetic materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A flow chart of a method for preparing an erbium / erbium oxide composite film on a steel plate according to the present invention is shown.

[0022] Figure 2 The SEM images of the erbium / erbium oxide composite film prepared in Example 2 of the present invention at different magnification scales are shown.

[0023] Figure 3 The SEM images of the erbium oxide thin film prepared in Comparative Example 1 at different magnification scales. DETAILED DESCRIPTION

[0024] The present invention provides a method for preparing an erbium / erbium oxide composite film on a steel plate. In order to make the purpose, technical solution and effect of the present invention clearer and more specific, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0025] See also Figure 1 , Figure 1 A flow chart of a method for preparing an erbium / erbium oxide composite film on a steel plate provided by the present invention is shown in the figure, which comprises the steps of:

[0026] S10, preparing a steel substrate;

[0027] S20, fixing the steel substrate on a base and placing it into a cavity of a magnetron sputtering system;

[0028] S30, evacuating the chamber, heating the steel substrate to a first predetermined temperature, then introducing argon gas, and sputtering a metal Er target on the steel substrate, thereby forming a metal Er layer on the surface of the steel substrate;

[0029] S40. After the metal Er layer is cooled, the steel substrate with the metal Er layer formed on the surface is heated to a second predetermined temperature and a mixed gas with a flow ratio of oxygen and argon of 1:20-40 is introduced, and the metal Er target is continued to be sputtered on the surface of the metal Er layer to form an Er2O3 film, and then annealing treatment is performed in a nitrogen atmosphere, so as to obtain an erbium / erbium oxide composite film on the steel substrate.

[0030] The present invention adopts magnetron sputtering technology to first deposit an Er intermediate layer on a steel substrate, and then prepare an Er2O3 composite film on this basis, thereby achieving a high bonding force between the Er2O3 film and the steel substrate, and improving the uniformity, density and stability of the film. The present invention has a simple and efficient process and is suitable for large-scale production. The prepared Er2O3 composite film has broad application prospects in the fields of optics, electronics and magnetic materials.

[0031] In some embodiments, the preparation steps of the steel substrate include: cutting a low-activity martensitic steel plate (CLAM) to obtain a steel sheet, grinding the surface of the steel sheet with sandpaper, and then polishing the surface of the steel sheet with diamond polishing paste to obtain a mirror steel sheet; ultrasonically cleaning the mirror steel sheet with deionized water and alcohol, and drying with N2 to obtain the steel substrate.

[0032] In some embodiments, the first predetermined temperature is 450-550° C.; the second predetermined temperature is 450-550° C., but is not limited thereto.

[0033] In some embodiments, the annealing treatment is performed at a temperature of 700-900° C. for 1-3 hours, but is not limited thereto. For example, the annealing treatment is performed at a temperature of 800° C. for 2 hours.

[0034] In some embodiments, in the step of evacuating the cavity, the cavity is evacuated to a vacuum of 2.0×10 -4 Pa-4.0×10 -4 Pa, but not limited to this.

[0035] In some embodiments, after the argon gas is introduced, the vacuum degree of the chamber is maintained at 0.6-0.8 Pa, but it is not limited thereto.

[0036] In some embodiments, the time for sputtering the metal Er target on the steel substrate is 20-40 minutes, but is not limited thereto.

[0037] In some embodiments, the time for continuously sputtering the metal Er target on the surface of the metal Er layer to form the Er2O3 film is 40-80 minutes, but is not limited thereto.

[0038] The present invention will be further explained below by means of specific embodiments:

[0039] Example 1

[0040] A method for preparing an erbium / erbium oxide composite thin film on a steel substrate comprises the following steps:

[0041] Steel substrate pretreatment: Cut the Chinese low-activity martensitic (CLAM) steel plate to obtain a 1cm×1cm×0.5cm CLAM steel sheet, and polish its surface with 800#, 1000#, 1200#, 1500# and 2000# sandpaper in turn, and then polish its surface with 2.0 and 1.0μm diamond polishing paste to obtain a mirror surface. Before use, it was ultrasonically cleaned with deionized water and alcohol, and immediately fixed on the base after N2 drying, and placed in the cavity for film preparation.

[0042] Er / Er2O3 composite films were prepared on the cut CLAM steel substrate using a 40kHz pulsed magnetron sputtering system: the vacuum was pumped to 2.0×10 -4Pa, the substrate is heated to 450°C, and then 90sccm Ar (purity is 999.99%) is introduced, the vacuum degree is maintained at 0.6Pa, and a metal Er target (purity is 99.9wt%, size is Φ50mm×3mm) is sputtered in a pure Ar atmosphere for 20min to obtain a metal Er layer. When the sample is cooled sufficiently, it is reheated to the corresponding process temperature of 450°C and a mixed gas with an oxygen-argon flow ratio of 1:20 is introduced, the sputtering power is 90W, and the deposition is carried out for 40min to prepare an Er2O3 composite film (CLAM / Er / Er2O3) containing an Er intermediate layer; the prepared composite film is kept warm in a nitrogen atmosphere at 800°C for 3h, and the sample is taken out after it is naturally cooled to room temperature in the furnace.

[0043] Example 2

[0044] A method for preparing an erbium / erbium oxide composite thin film on a steel substrate comprises the following steps:

[0045] Steel substrate pretreatment: Cut the Chinese low-activity martensitic (CLAM) steel plate to obtain a 1cm×1cm×0.5cm CLAM steel sheet, and polish its surface with 800#, 1000#, 1200#, 1500# and 2000# sandpaper in turn, and then polish its surface with 2.0 and 1.0μm diamond polishing paste to obtain a mirror surface. Before use, it was ultrasonically cleaned with deionized water and alcohol, and immediately fixed on the base after N2 drying, and placed in the cavity for film preparation.

[0046] Er / Er2O3 composite films were prepared on the cut CLAM steel substrate using a 40kHz pulsed magnetron sputtering system: the vacuum was pumped to 3.0×10 -4 Pa, the substrate is heated to 500°C, and then 90sccm Ar (purity is 999.99%) is introduced, the vacuum degree is maintained at 0.7Pa, and a metal Er target (purity is 99.9wt%, size is Φ50mm×3mm) is sputtered in a pure Ar atmosphere for 0.5h to obtain a metal Er layer. When the sample is cooled enough, it is reheated to the corresponding process temperature of 500°C and a mixed gas with an oxygen-argon flow ratio of 1:30 is introduced, the sputtering power is 90W, and the deposition power is 1h to prepare an Er2O3 composite film (CLAM / Er / Er2O3) containing an Er intermediate layer; the prepared composite film is kept warm in a nitrogen atmosphere at 700°C for 2h, and the sample is taken out after it is naturally cooled to room temperature in the furnace.

[0047] Example 3

[0048] A method for preparing an erbium / erbium oxide composite thin film on a steel substrate comprises the following steps:

[0049] Steel substrate pretreatment: Cut the Chinese low-activity martensitic (CLAM) steel plate to obtain a 1cm×1cm×0.5cm CLAM steel sheet, and polish its surface with 800#, 1000#, 1200#, 1500# and 2000# sandpaper in turn, and then polish its surface with 2.0 and 1.0μm diamond polishing paste to obtain a mirror surface. Before use, it was ultrasonically cleaned with deionized water and alcohol, and immediately fixed on the base after N2 drying, and placed in the cavity for film preparation.

[0050] Er / Er2O3 composite films were prepared on the cut CLAM steel substrate using a 40kHz pulsed magnetron sputtering system: the vacuum was pumped to 4.0×10 -4 Pa, the substrate is heated to 550°C, and then 90sccm Ar (purity is 999.99%) is introduced, the vacuum degree is maintained at 0.8Pa, and a metal Er target (purity is 99.9wt%, size is Φ50mm×3mm) is sputtered in a pure Ar atmosphere for 40min to obtain a metal Er layer. When the sample is cooled sufficiently, it is reheated to the corresponding process temperature of 550°C and a mixed gas with an oxygen-argon flow ratio of 1:40 is introduced, the sputtering power is 90W, and the deposition is performed for 80min to obtain an Er2O3 composite film (CLAM / Er / Er2O3) containing an Er intermediate layer; the prepared composite film is kept warm in a nitrogen atmosphere at 900°C for 1h, and the sample is taken out after it is naturally cooled to room temperature in the furnace.

[0051] Comparative Example 1

[0052] A method for preparing an erbium oxide thin film on a steel substrate comprises the following steps:

[0053] Steel substrate pretreatment: Cut the Chinese low-activity martensitic (CLAM) steel plate to obtain a 1cm×1cm×0.5cm CLAM steel sheet, and polish its surface with 800#, 1000#, 1200#, 1500# and 2000# sandpaper in turn, and then polish its surface with 2.0 and 1.0μm diamond polishing paste to obtain a mirror surface. Before use, it was ultrasonically cleaned with deionized water and alcohol, and immediately fixed on the base after N2 drying, and placed in the cavity for film preparation.

[0054] Er / Er2O3 composite films were prepared on the cut CLAM steel substrate using a 40kHz pulsed magnetron sputtering system: the vacuum was pumped to 3.0×10 -4 Pa, the substrate was heated to 500°C, and then a mixed gas with an oxygen-argon flow ratio of 1:30 was introduced, the sputtering power was 90 W, and the deposition was performed for 1 h to prepare the Er2O3 film (CL AM / Er2O3); the prepared film was kept at 700°C for 2 h in a nitrogen atmosphere, and the sample was taken out after naturally cooling to room temperature in the furnace.

[0055] Test Case

[0056] The erbium / erbium oxide composite film prepared in Example 2 and the Er2O3 film prepared in Comparative Example 1 were tested by scanning electron microscopy (SEM) at different magnification scales. The results are as follows: Figure 2 and Figure 3 As shown, from Figure 2 It can be seen that a high density of irregular particles are found attached to the surface of the erbium / erbium oxide composite film sample, which indicates that the introduction of the Er intermediate layer improves the adhesion of the film to the substrate. Figure 3 Fish-scale-like protrusions appeared on the surface of the Er2O3 film sample without Er intermediate layer, and the original obvious laminar morphology disappeared; this shows that the Er2O3 / Er surface is uniformly deposited and well bonded to the steel substrate, which can eliminate residual stress in the film, improve crystallinity and performance stability.

[0057] It should be understood that the application of the present invention is not limited to the above examples. For ordinary technicians in this field, improvements or changes can be made based on the above description. All these improvements and changes should fall within the scope of protection of the claims attached to the present invention.

Claims

1. A method for preparing an erbium / erbium oxide composite thin film on a steel substrate, characterized in that: Includes steps: preparing a steel substrate; The steel substrate is fixed on a base and placed in a cavity of a magnetron sputtering system; The chamber is evacuated, the steel substrate is heated to a first predetermined temperature, and then argon gas is introduced, and a metal Er target is sputtered on the steel substrate, thereby forming a metal Er layer on the surface of the steel substrate; After the metal Er layer is cooled, the steel substrate with the metal Er layer formed on the surface is heated to a second predetermined temperature and a mixed gas with a flow ratio of oxygen and argon of 1:20-40 is introduced. The metal Er target is continued to be sputtered on the surface of the metal Er layer to form an Er2O3 film, and then annealing treatment is performed in a nitrogen atmosphere to obtain an erbium / erbium oxide composite film on the steel substrate.

2. The method for preparing an erbium / erbium oxide composite thin film on a steel substrate according to claim 1, characterized in that: The steps of preparing the steel substrate include: Cutting a low-activity martensitic steel plate to obtain a steel sheet, grinding the surface of the steel sheet with sandpaper, and then polishing the surface of the steel sheet with a diamond polishing paste to obtain a mirror-finished steel sheet; The mirror steel sheet is ultrasonically cleaned with deionized water and alcohol, and dried with N2 to obtain the steel substrate.

3. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: The first predetermined temperature is 450-550°C; the second predetermined temperature is 450-550°C.

4. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: The annealing temperature is 700-900°C and the time is 1-3h.

5. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: In the step of evacuating the cavity, the cavity is evacuated to a vacuum of 2.0×10 -4 Pa-4.0×10 -4 Pa.

6. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: After introducing argon gas, the vacuum degree of the cavity is maintained at 0.6-0.8Pa.

7. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: The time for sputtering metal Er target on steel substrate is 20-40min.

8. The method for preparing an erbium / erbium oxide composite thin film on a steel plate according to claim 1, characterized in that: The time for continuing to sputter the metal Er target on the surface of the metal Er layer to form the Er2O3 film is 40-80 minutes.

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