Rare earth oxide coating with adjustable and controllable components and preparation method of rare earth oxide coating

Abstract

The invention relates to a rare earth oxide coating with adjustable and controllable components and a preparation method thereof, and the method comprises the following steps: adding rare earth acetate into ethanol, then adding a proper amount of complexing agent to promote the dissolution of the rare earth acetate and generate complexing reaction to generate sol, and preparing the coating on a metal substrate through a spin coating process and a heat treatment process. Through a universal wet chemical method, the sol containing yttrium, scandium and all lanthanide series rare earth can be prepared, the corresponding rare earth oxide coating can be prepared through a related coating preparation process, and in addition, the n-element rare earth oxide coating (n is more than or equal to 1 and less than or equal to 17) can be prepared through any kind of mixed sol. The adjustable scheme of the rare earth oxide coating is enriched, and the practicable field of the rare earth oxide coating is widened.

Description

Technical Field

[0001] The invention relates to the field of rare earth materials, in particular to a rare earth oxide coating with adjustable components and a preparation method thereof. Background Art

[0002] Rare earth elements are a special class of elements in the periodic table, with a total of 17 elements, including 15 lanthanides, scandium and yttrium. Rare earth raw metals and oxides have excellent electronic, optical, optoelectronic, mechanical, magnetic and chemical properties, which are very promising in modern advanced industrial applications. As an important form of rare earth elements, rare earth oxides play an indispensable role in many fields such as smartphones, semiconductors, computer storage, nuclear fusion, fluorescent materials, electronic displays, battery electrodes and advanced weapon systems. And preparing the corresponding coating and applying it to the substrate material can greatly broaden its application range.

[0003] In view of the excellent performance that rare earth oxide coatings may present in various fields, we need a universal process for preparing all rare earth oxide coatings, and through this process, we can increase or change the type of elements to make the rare earth oxide coatings achieve the desired performance. However, there is currently no universal preparation process to obtain all rare earth oxide coatings, let alone to adjust the elements in the rare earth oxide coatings to obtain multi-component rare earth oxide coatings. Summary of the invention

[0004] The purpose of the present invention is to provide a component-adjustable rare earth oxide coating and a preparation method thereof, wherein all rare earth oxide coatings are prepared using a general wet chemical method combined with a homogenization process, that is, the rare earth sol is uniformly covered on the metal substrate through the homogenization process, and the n-element rare earth oxide coating can be obtained through the sol mixing scheme. This scheme not only achieves the purpose of using a process scheme to achieve all rare earth oxide coatings, but also can conveniently obtain n-element rare earth oxide coatings, greatly enhancing the controllability of the rare earth oxide coating.

[0005] To achieve the above objectives, the present invention adopts the following technical solutions:

[0006] A method for preparing a rare earth oxide coating with adjustable components, comprising:

[0007] 1) Preparation of rare earth sol: 1%-10% by mass of rare earth acetate and 55%-65% by mass of ethanol are mixed, and then 25%-35% by mass of a complexing agent is added to promote the dissolution of the rare earth acetate, and stirred for 5-10 minutes in a water bath heating environment to obtain a clear and transparent rare earth sol;

[0008] 2) Preparation of n-ary rare earth oxide sol: mixing the rare earth sol obtained in step 1) in any type and desired proportion to obtain an n-ary sol, wherein 1≤n≤17;

[0009] 3) Preparation of rare earth oxide coating: The rare earth sol prepared in step 2) is evenly coated on 321 steel using a homogenization process to obtain a sample, the sample is placed on a heating plate at a temperature of 100 to 500° C. for drying, the sample is then placed in a muffle furnace at 500 to 800° C. for heat treatment, and finally the sample is sintered at a high temperature of 800 to 1000° C. to obtain an n-element rare earth oxide coating.

[0010] Furthermore, the rare earth acetate includes one or a combination of scandium acetate, yttrium acetate, lanthanum acetate, lanthanum acetate, cerium acetate, praseodymium acetate, neodymium acetate, promethium acetate, samarium acetate, europium acetate, gadolinium acetate, terbium acetate, dysprosium acetate, holmium acetate, erbium acetate, thulium acetate, ytterbium acetate and lutetium acetate.

[0011] Furthermore, the complexing agent is an amine complexing agent, which can promote the dissolution of rare earth acetate and make the system sol.

[0012] Furthermore, in step 1), the water bath temperature is 30-90°C.

[0013] Furthermore, the required ratio of the n-component sol is an equimolar ratio.

[0014] A novel wet chemical rare earth oxide coating prepared by the method as described above.

[0015] The beneficial effects of the present invention are:

[0016] 1. Process uniformity and high efficiency: The present invention successfully realizes the preparation of all rare earth oxide coatings by introducing a universal wet chemical method combined with a coating process. This innovative method breaks the limitation of using different processes for different rare earth oxides in the traditional preparation process, greatly simplifies the preparation process, and improves production efficiency.

[0017] 2. Significant improvement in coating controllability: By precisely controlling the mixing scheme of the sol, the present invention can conveniently prepare n-ary rare earth oxide coatings, which means that the composition, structure and performance of the coating can be precisely controlled within a wider range. This high degree of controllability not only provides unprecedented freedom in the design of rare earth oxide coatings, but also enables the coatings to be customized and optimized for specific application scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 CeO2, La2O3, Pr6O 11, optical images of coatings of Tm2O3, Sm2O3, Yb2O3, Eu2O3 and Er2O3;

[0019] Figure 2 CeO2, La2O3, Pr6O 11 , SEM morphology of Tm2O3, Sm2O3, Yb2O3, Eu2O3 and Er2O3 coatings;

[0020] Figure 3 CeO2, La2O3, Pr6O 11 Quaternary rare earth oxide coating Ce with equal molar ratio of Tm2O3 0.25 La 0.25 Pr 0.25 Tm 0.25 O 1.39 coating;

[0021] Figure 4 CeO2, La2O3, Pr6O 11 、Tm2O3、Sm2O3、Eu2O 3、 Eight-element rare earth oxide coating Ce with equal molar ratio of Yb2O3 and Er2O3 0.25 La 0.25 Pr 0.25 Tm 0.25 Sm 0.25 Yb 0.25 Eu 0.25 Er 0.25 O 2.89 coating. DETAILED DESCRIPTION

[0022] The technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings of the present invention.

[0023] The present invention provides a method for preparing a rare earth oxide coating with adjustable components, wherein rare earth acetate is dissolved in ethanol, an appropriate amount of amine complexing agent is added to promote the dissolution of the acetate, and the system is sol-formed in a water bath environment, and the coating is prepared on a substrate through a homogenization process and a heat treatment process. The scheme of the present invention is described below with specific embodiments:

[0024] Embodiment 1:

[0025] 1) Prepare a sol according to the mass ratio of rare earth acetate (cerium acetate, lanthanum acetate, praseodymium acetate, thulium acetate, samarium acetate, ytterbium acetate, europium acetate and erbium acetate): ethanol: amine complexing agent = 1:55:34, stir in a 40°C water bath for 10 minutes and set aside.

[0026] 2) The sol was coated on 321 steel by a coating process to obtain a sample, the coating speed was 2000 rpm, and the coating time was 10 s.

[0027] 3) Place the sample on a heating plate at 300°C for drying for 15 minutes, then place the sample in a muffle furnace at 650°C for heat treatment for 15 minutes, and repeat steps 2) and 3) three times.

[0028] 4) The substrate is sintered at 800℃ for 1h to obtain CeO2, La2O3, Pr6O 11 , Tm2O3, Sm2O3, Yb2O3, Eu2O3 and Er2O3 coatings.

[0029] Embodiment 2:

[0030] 1) Prepare a sol according to the mass ratio of rare earth acetate (cerium acetate, lanthanum acetate, praseodymium acetate and thulium acetate): ethanol: amine complexing agent = 10:60:30, stir in a 70°C water bath for 8 minutes and set aside.

[0031] 2) Mix the sol obtained in 1) with an equal molar ratio of rare earth elements

[0032] 3) The sol prepared in 2) was coated on 321 steel by a coating process to obtain a sample, the coating speed was 3000 rpm, and the coating time was 15 s.

[0033] 4) Place the sample on a heating plate at 400°C for drying for 15 minutes, then place the sample in a muffle furnace at 700°C for heat treatment for 15 minutes, and repeat steps 2) and 3) three times.

[0034] 5) The sample was sintered at 900℃ for 1.5h to obtain Ce 0.25 La 0.25 Pr 0.25 Tm 0.25 O 1.39 coating.

[0035] Embodiment 3:

[0036] 1) Prepare a sol by mixing rare earth acetate (cerium acetate, lanthanum acetate, praseodymium acetate, thulium acetate, samarium acetate, ytterbium acetate, europium acetate and erbium acetate): ethanol: amine complexing agent in a ratio of 8:65:27, and stir in a water bath at 90° C. for 15 min for later use.

[0037] 2) Mix the sol obtained in 1) with an equal molar ratio of rare earth elements

[0038] 3) The sol prepared in 2) was coated on 321 steel by a coating process to obtain a sample, the coating speed was 4000 rpm, and the coating time was 10 s.

[0039] 4) Place the substrate on a heating plate at 500° C. and dry it for 15 min. Place the substrate in a muffle furnace at 800° C. and heat treat it for 5 min. Repeat steps 2) and 3) 3 times.

[0040] 5) The substrate is sintered at 1000℃ for 1.5h to obtain Ce 0.25 La 0.25 Pr 0.25 Tm 0.25 Sm 0.25 Yb 0.25 Eu 0.25 Er 0.25 O 2.89 coating.

[0041] Figure 1 and Figure 2 They are CeO2, La2O3, Pr6O prepared in Example 1 11 Optical photos and SEM morphology of Tm2O3, Sm2O3, Yb2O3, Eu2O3 and Er2O3 coatings. From the macroscopic image, the coating is evenly coated on the surface of the substrate; from the microscopic morphology (SEM) of the coating, the coating is uniform and complete, without cracks and holes, and the rare earth elements are evenly distributed on the coating surface.

[0042] Figure 3 To prepare Ce for Example 2 0.25 La 0.25 Pr 0.25 Tm 0.25 O 1.39 Optical photo of quaternary rare earth composite coating. From the macroscopic image, it can be seen that the coating prepared by rare earth sol obtained by mixing four sols with equal rare earth molar ratios can be evenly coated on the surface of the substrate.

[0043] Figure 4 For the Ce prepared in Example 3 0.25 La 0.25 Pr 0.25 Tm 0.25 Sm 0.25 Yb 0.25 Eu 0.25 Er 0.25 O 2.89 Optical photo of eight-element rare earth composite coating. From the macroscopic image, it can be seen that the coating prepared by the rare earth sol obtained by mixing eight kinds of sols with equal rare earth molar ratios can be evenly coated on the surface of the substrate.

[0044] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed by the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A method for preparing a rare earth oxide coating with adjustable components, characterized in that: include: 1) Preparation of rare earth sol: 1%-10% by mass of rare earth acetate and 55%-65% by mass of ethanol are mixed, and then 25%-35% by mass of a complexing agent is added to promote the dissolution of the rare earth acetate, and stirred for 5-10 minutes in a water bath heating environment to obtain a clear and transparent rare earth sol; 2) Preparation of n-ary rare earth oxide sol: mixing the rare earth sol obtained in step 1) in any type and desired proportion to obtain an n-ary sol, wherein 1≤n≤17; 3) Preparation of rare earth oxide coating: The rare earth sol prepared in step 2) is evenly coated on 321 steel using a homogenization process to obtain a sample, the sample is placed on a heating plate at a temperature of 100 to 500° C. for drying, the sample is then placed in a muffle furnace at 500 to 800° C. for heat treatment, and finally the sample is sintered at a high temperature of 800 to 1000° C. to obtain a single n-element rare earth oxide coating.

2. The method for preparing a new type of rare earth oxide coating by wet chemical method according to claim 1, characterized in that: The rare earth acetate includes one or a combination of scandium acetate, yttrium acetate, lanthanum acetate, lanthanum acetate, cerium acetate, praseodymium acetate, neodymium acetate, promethium acetate, samarium acetate, europium acetate, gadolinium acetate, terbium acetate, dysprosium acetate, holmium acetate, erbium acetate, thulium acetate, ytterbium acetate and lutetium acetate.

3. The method for preparing a new type of rare earth oxide coating by wet chemical method according to claim 1, characterized in that: The complexing agent is an amine complexing agent.

4. The novel wet chemical method for preparing rare earth oxide coating according to claim 1, characterized in that: In the step 1), the water bath temperature is 30-90°C.

5. The novel wet chemical method for preparing rare earth oxide coating according to claim 1, characterized in that: The required ratio of the n-component sol is an equimolar ratio.

6. A novel wet chemical rare earth oxide coating prepared by the method according to any one of claims 1 to 5.

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