Dispersed yttrium oxide powder as well as preparation method and application thereof
By using polyethylene oxide as a dispersant, the yttrium oxide powder is dispersed, and the problem of agglomeration of yttrium oxide powder in vacuum cold spraying is solved, and the good dispersion of yttrium oxide powder is achieved and the service life of the equipment is extended.
Patent Information
- Application Number
- CN202411606050.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-12
- Publication Date
- 2025-02-18
AI Technical Summary
In the vacuum cold spraying process, the small particle size of the yttrium oxide powder leads to agglomeration, increasing the risk of equipment damage, and the prior art is difficult to effectively solve this problem.
Polyethylene oxide is used as a dispersant, and the yttrium oxide powder and polyethylene oxide are mixed in distilled water through an ultrasonic disperser to form a suspension, and the polyethylene oxide and water are removed by vacuum drying to prepare a dispersed yttrium oxide powder.
It effectively reduces the agglomeration of yttrium oxide powder, reduces the risk of equipment damage, extends the service life of the equipment, and meets the application needs of cold spray coatings.
Smart Images
Figure CN119461452A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of powder preparation, and in particular to a dispersed yttrium oxide powder and a preparation method and application thereof. Background Art
[0002] Yttria coating has the functions of high temperature resistance, wear resistance and corrosion resistance. At present, yttria coating is mainly used for the anti-corrosion protection of plasma etching equipment to protect the body, extend the service life of the equipment and improve the working accuracy. Alumina and zirconium oxide coatings are more commonly used anti-corrosion coatings, but they cannot meet the requirements of the technical progress in this field and will be gradually replaced by yttria coatings.
[0003] Yttria coatings are usually prepared by vacuum cold spraying, which is an advanced spraying technology that sprays materials in a vacuum environment. It is widely used in aerospace, automotive manufacturing, and the electronics industry. The working principle of vacuum cold spraying is based on two key steps: vacuum environment and cold spraying technology. First, the vacuum environment is created to eliminate the interference of gas molecules between the coating and the substrate; by reducing the presence of gas, the adhesion and quality of the coating can be improved. Secondly, the cold spraying technology uses supersonic gas jets to accelerate yttria powder particles to high speeds and deposit them on the surface of the substrate to form a uniform coating. The working principle of this technology and its unique advantages make it an efficient, environmentally friendly spraying method with good coating quality.
[0004] In the process of preparing yttrium oxide coating by vacuum cold spraying, submicron (100-1000nm) yttrium oxide powder is usually selected to be deposited on the substrate surface to form a coating. This is because the smaller the particle size of the yttrium oxide powder, the better its plastic deformation, which is conducive to forming a uniform and dense coating on the substrate surface. However, the smaller the particle size of the yttrium oxide powder, the larger its specific surface area, and the greater the probability of agglomeration; and the surface energy interactions such as the charge, moisture, and van der Waals force carried by the powder particles will cause the powder to form agglomerates, which are easy to clog the nozzle during the cold spraying process and cause damage to the equipment.
[0005] Therefore, it is urgent to propose a preparation method for reducing the agglomeration of yttrium oxide powder, so as to improve the interaction forces of van der Waals force, charge, etc. on the surface of yttrium oxide powder and obtain dispersed yttrium oxide powder. Summary of the invention
[0006] In view of the deficiencies in the prior art, the present invention discloses a dispersed yttrium oxide powder and a preparation method and application thereof, thereby solving or at least alleviating one or more of the above-mentioned problems and other problems in the prior art.
[0007] The present invention discloses a method for preparing dispersed yttrium oxide powder, comprising the following steps:
[0008] S1. Weigh the raw materials: by mass percentage, yttrium oxide powder is 0.5%, and the balance is distilled water; the amount of polyethylene oxide added is 0.5-1.5% of the mass of the yttrium oxide powder;
[0009] S2, mixing the weighed yttrium oxide powder and polyethylene oxide in distilled water to form a suspension, and dispersing the suspension using an ultrasonic disperser;
[0010] S3, placing the suspension into a culture dish, and then placing the culture dish in an oven for vacuum drying to volatilize the polyethylene oxide and water;
[0011] S4. The culture dish is taken out of the oven and naturally cooled to room temperature to obtain dispersed yttrium oxide powder in the culture dish.
[0012] Preferably, in step S1, the amount of polyethylene oxide added is 0.5-1.0% of the mass of the yttrium oxide powder.
[0013] Preferably, in step S1, the molecular weight M of polyethylene oxide is 800,000-1.5 million.
[0014] Preferably, in step S1, the molecular weight M of polyethylene oxide is 800,000-1,000,000.
[0015] Preferably, in step S1, the molecular weight M of polyethylene oxide is 1-1.5 million.
[0016] Preferably, in step S1, the particle size of the yttrium oxide powder is 0.3-0.5 μm.
[0017] Preferably, in step S2, the ultrasonic disperser disperses the suspension for 5-10 minutes.
[0018] Preferably, in step S3, the drying temperature of the vacuum drying is 140-180°C.
[0019] In addition, the present invention provides yttrium oxide powder prepared by the method for preparing dispersed yttrium oxide powder as described above.
[0020] The yttrium oxide powder prepared by the present invention has an excellent dispersion state, meets the application requirements of cold spray coatings, is not easy to cause nozzle blockage during the cold spraying process, greatly reduces the damage to the equipment caused by this, and prolongs the service life of the equipment.
[0021] Furthermore, the present invention also provides the use of the yttrium oxide powder as described above in cold spray coatings.
[0022] The present invention has the following beneficial effects:
[0023] After the polyethylene oxide particles are dissolved in water, the polyethylene oxide forms an adsorption layer on the surface of the yttrium oxide particles, and its molecules repel each other, similar to the arrangement of spheres, thereby preventing the yttrium oxide particles from approaching each other; at the same time, the adsorption layer increases the charge on the surface of the yttrium oxide particles to increase the reaction force between the particles that form a three-dimensional barrier, further preventing the agglomeration of yttrium oxide; in addition, a double-layer structure is formed on the surface of the yttrium oxide particles, and the polar end of the outer dispersant has a strong affinity with water, which increases the degree to which the yttrium oxide particles are wetted by water, and adjacent yttrium oxide particles are kept away from each other due to electrostatic repulsion; thereby reducing the surface charge of the yttrium oxide particles and the effect of van der Waals force, and subsequently removing the polyethylene oxide and water by vacuum drying; the above combined effects achieve the effect of dispersing the powder, realize the purpose of removing soft agglomerates and dispersing the powder, and finally prepare a fluffy yttrium oxide powder with excellent dispersion effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] In order to more clearly illustrate the specific embodiments of the present disclosure, the following briefly introduces the drawings required for use in the specific embodiments. In all the drawings, each element or part is not necessarily drawn according to the actual scale.
[0025] Figure 1 is a process flow chart of Examples 1-9 of the present invention;
[0026] Figure 2 The SEM morphology of the yttrium oxide powder prepared in Examples 1-9 of the present invention;
[0027] Figure 3 This is the SEM morphology of the yttrium oxide powder prepared in Comparative Example 1;
[0028] Figure 4 This is the SEM morphology of the yttrium oxide powder prepared in Comparative Example 2;. DETAILED DESCRIPTION
[0029] The following embodiments of the technical solution of the present disclosure are described in detail in conjunction with the accompanying drawings. The following embodiments are only used to more clearly illustrate the technical solution of the present disclosure, and are therefore only used as examples, and cannot be used to limit the protection scope of the present disclosure.
[0030] It should be noted that, unless otherwise specified, the technical terms or scientific terms used in this application should have the common meanings understood by those skilled in the art to which the present invention belongs.
[0031] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.
[0032] In addition, the terms "first", "second", etc. are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.
[0033] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0034] In the present application, unless otherwise clearly specified and limited, a first feature being “above” or “below” a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being “above”, “above”, and “above” a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being “below”, “below”, and “below” a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.
[0035] The preparation method of a dispersed yttrium oxide powder provided in Examples 1-9 of the present invention, and the specific parameters of the preparation process for reducing the agglomeration of the yttrium oxide powder are shown in Table 1.
[0036] like Figure 1 As shown, a method for preparing dispersed yttrium oxide powder comprises:
[0037] S1. Weigh the raw materials, and the yttrium oxide powder is 0.5% by mass, and the balance is distilled water; the amount of polyethylene oxide added is 0.5-1.5% of the mass of the yttrium oxide powder; polyethylene oxide is used as a dispersant, and the molecular weight M of polyethylene oxide is 800,000-1.5 million; the particle size of the yttrium oxide powder is 0.3-0.5 μm;
[0038] S2, mixing the weighed yttrium oxide powder and polyethylene oxide in distilled water to form a suspension, and dispersing the suspension using an ultrasonic disperser; the dispersion time t is 5-10min;
[0039] S3, the suspension is placed in a culture dish, and the culture dish is placed in an oven for vacuum drying to volatilize the polyethylene oxide and water; the drying temperature T is 140-180°C, and the drying time is not less than 3 hours;
[0040] S4. The culture dish is taken out of the oven and naturally cooled to room temperature to obtain dispersed yttrium oxide powder in the culture dish.
[0041] Comparative Example 1
[0042] Sodium polyacrylate (molecular weight of 15000) is used as a dispersant. By mass percentage, yttrium oxide powder is 0.5%, and the remainder is distilled water; the addition amount of sodium polyacrylate (molecular weight of 15000) is 1.5% of the mass of yttrium oxide powder, yttrium oxide powder and sodium polyacrylate are mixed in distilled water to form a suspension, and the pH value of the suspension is adjusted to 8-9 with ammonia water. The suspension is ground by planetary ball milling, and the planetary ball uses zirconium oxide grinding balls for 30 minutes. The ground suspension is placed in a culture dish, and the culture dish is placed in an oven for vacuum drying and heated to 100°C. Subsequently, the suspension is gradually heated from 100°C to 400°C at a heating rate of 3°C / min; after heating to 400°C, it is kept warm for 5 minutes to remove the dispersant in the suspension. Finally, the culture dish is taken out of the oven and naturally cooled to room temperature to obtain yttrium oxide powder.
[0043] Comparative Example 2
[0044] By volume percentage, the yttrium oxide powder is 5% and the calcium chloride powder is 95%. The weighed calcium chloride powder and yttrium oxide powder are placed in the chamber of a powder mixer and fully mixed to obtain a powder mixture. Among them, calcium chloride is used as a dispersant, and the particle size of the calcium chloride powder is larger than that of the yttrium oxide powder. When the calcium chloride powder and the yttrium oxide powder are mixed by a powder mixer, the yttrium oxide particles adhere to the calcium chloride particles, that is, a single calcium chloride particle is attached with multiple yttrium oxide particles. By mass percentage, the powder mixture is 0.5%, and the remainder is distilled water. The weighed powder mixture is added to distilled water to form a mixed solution, the calcium chloride is dissolved in water, and multiple yttrium oxide particles attached to the calcium chloride particles form a hollow state. The mixed solution is then loaded into a culture dish and the culture dish is centrifuged at a speed of 3000rpm / min for 10 minutes by a centrifuge to allow the yttrium oxide particles in the mixed solution to settle, and then the supernatant in the culture dish is poured out. Then, the culture dish with the supernatant poured out was placed in an oven at 100° C. for vacuum drying for 4 hours; then, the culture dish was taken out of the oven and naturally cooled to room temperature to obtain yttrium oxide powder.
[0045] Comparative Examples 1-2 are all preparation methods for reducing agglomeration of yttrium oxide powder in the prior art. In Examples 1-9 and Comparative Examples 1-2, the height of the suspension or mixed solution in the culture dish is uniformly set to 2 mm, so as to facilitate comparative analysis of the yttrium oxide powder prepared in each embodiment and each comparative example through SEM morphology images.
[0046] Table 1
[0047]
[0048] like Figure 2 As shown, Figure 2 (b) Figure 2 (c) and Figure 2 (d) are SEM images of yttrium oxide powders prepared in Example 1, Example 2 and Example 3, respectively. Figure 2 (b1), Figure 2 (c1) and Figure 2 (d1) are SEM images of yttrium oxide powders prepared in Example 4, Example 5 and Example 6, respectively. Figure 2 (b2), Figure 2 (c2) and Figure 2 (d2) are SEM images of yttrium oxide powders prepared in Example 7, Example 8 and Example 9, respectively. Figure 2 (a) Figure 2 (a1), Figure 2 (a2), Figure 3 (a) and Figure 4(a) The same picture is used, that is, the SEM morphology of the original yttrium oxide powder particles (without any dispersion process) for comparative analysis with Examples 1-9 and Comparative Examples 1-2.
[0049] observe Figure 2 (a) Figure 2 (a1) and Figure 2 (a2) It can be seen that when no dispersant is added, the agglomeration of the original yttrium oxide powder particles is very obvious. Figure 2 (b) Figure 2 (c) and Figure 2 (d) Figure 2 (b1), Figure 2 (c1) and Figure 2 (d1), and Figure 2 (b2), Figure 2 (c2) and Figure 2 (d2), from the comparison of Examples 1-9, it can be seen that after adding the polyethylene oxide dispersant, the agglomeration phenomenon of the prepared yttrium oxide powder is significantly improved; and when the mass of the added polyethylene oxide is equal to 0.5-1.5% of the mass of the yttrium oxide powder, as the amount of polyethylene oxide added increases, the prepared yttrium oxide powder gradually shows partial agglomeration phenomenon, and the agglomeration phenomenon becomes more and more obvious. When the amount of polyethylene oxide added is 0.5% of the mass of the yttrium oxide powder, the molecular weight M of the polyethylene oxide is 800,000-1.5 million, and the dispersion state of the prepared yttrium oxide powder reaches the best, such as Figure 2 (b) Figure 2 (b1) and Figure 2 As shown in (b2).
[0050] observe Figure 2 (b) Figure 2 (b1) and Figure 2 (b2), Figure 2 (c) Figure 2 (c1) and Figure 2 (c2), and Figure 2 (d) Figure 2 (d1) and Figure 2(d2), from the comparison of Examples 1-9, it can be seen that when the molecular weight M of polyethylene oxide is 1 million, the dispersion state of the prepared yttrium oxide powder reaches the best; this is due to the physical and chemical properties of polyethylene oxide. If its molecular weight is too large, the viscosity of the suspension solution will increase, the fluidity will be weakened, which is not conducive to powder dispersion and has the risk of increasing powder agglomeration; at the same time, when the molecular weight of polyethylene oxide is too small, it is impossible to form a complete hydrophilic-hydrophobic layer in the aqueous solution to wrap the powder particles, so that the effect of dispersing the powder cannot be achieved. Therefore, in the actual preparation and application of yttrium oxide powder, it is preferred that the molecular weight M of polyethylene oxide is 1 million and the amount of polyethylene oxide added is 0.5% of the mass of the yttrium oxide powder to obtain yttrium oxide powder with the best fluffy dispersion effect.
[0051] This technical solution uses polyethylene oxide as a dispersant, which is a polymer with good water solubility. When polyethylene oxide particles are dissolved in water, polyethylene oxide forms an adsorption layer on the surface of yttrium oxide particles. Its molecules repel each other, similar to the arrangement of spheres, thereby hindering the yttrium oxide particles from approaching each other; at the same time, the adsorption layer increases the charge on the surface of the yttrium oxide particles to increase the reaction force between the particles that form a steric barrier, further preventing the agglomeration of yttrium oxide; in addition, a bilayer structure is formed on the surface of the yttrium oxide particles, and the polar end of the outer layer dispersant has a strong affinity with water, which increases the degree of wetting of the yttrium oxide particles by water, and the adjacent yttrium oxide particles are kept away from each other due to electrostatic repulsion; thereby reducing the surface charge of the yttrium oxide particles and the effect of van der Waals force, and subsequently removing polyethylene oxide and water through vacuum drying, the above combined effects achieve the effect of dispersing the powder, achieving the purpose of removing soft agglomerates and dispersing the powder, this principle is similar to Figure 2 The actual phenomenon is consistent.
[0052] like Figure 3 As shown, Figure 3 (a) is the SEM morphology of the original yttrium oxide powder particles (without any dispersion process). Figure 3 (b) is the SEM morphology of the yttrium oxide powder prepared in Comparative Example 1. Figure 3 (a) and Figure 3 (b) It can be seen that the addition of sodium polyacrylate significantly reduces the agglomeration of yttrium oxide powder. As a polymer electrolyte, sodium polyacrylate has hydrophilic and hydrophobic groups, can be dissolved in water, and is stable to temperature changes. When sodium polyacrylate is dissolved in water, it will ionize to form polymer anions and sodium ions (Na+). These polymer anions and small molecular ions are tightly adsorbed on the surface of the dispersed yttrium oxide particles, making the yttrium oxide particles carry the same charge; because the same charges repel each other, electrostatic repulsion is formed, which effectively prevents the particles from agglomerating in the water medium and achieves dispersion.
[0053] like Figure 4 As shown, Figure 4 (a) is the SEM morphology of the original yttrium oxide powder particles (without any dispersion process). Figure 4 (b) is the SEM morphology of the yttrium oxide powder prepared in Comparative Example 2. Figure 4 (a) and Figure 4 (b) It can be seen that the addition of calcium chloride powder significantly reduces the agglomeration of yttrium oxide powder. When calcium chloride powder and yttrium oxide powder are mixed in a mixer, yttrium oxide particles adhere to calcium chloride particles, that is, multiple yttrium oxide particles adhere to a single calcium chloride particle; after the powder mixture is added with distilled water, calcium chloride is dissolved in water, and multiple yttrium oxide particles attached to the surface of calcium chloride particles form a hollow state. After centrifugation to remove the supernatant and drying, dispersed yttrium oxide powder can be obtained.
[0054] observe Figure 2 (d) Figure 2 (d1), Figure 2 (d2) and Figure 3 (b) By comparing Examples 3, 6 and 9 with Comparative Example 1, it can be seen that when the amount of polyethylene oxide added is 1.5% of the mass of the yttrium oxide powder, the molecular weight M of polyethylene oxide is 800,000-1.5 million, and the dispersion state of the prepared yttrium oxide powder is almost the same as the dispersion state of the yttrium oxide powder prepared using sodium polyacrylate as a dispersant. Figure 2 (b) Figure 2 (b1) and Figure 2 (b2), Figure 2 (c) Figure 2 (c1) and Figure 2 (c2), and Figure 3 (b) By comparing Examples 1-3, Examples 4-6 and Comparative Example 1, it can be seen that when the addition amount of polyethylene oxide is 0.5-1% of the mass of the yttrium oxide powder, the molecular weight M of polyethylene oxide is 800,000-1.5 million, and the dispersion state of the prepared yttrium oxide powder is significantly better than the dispersion state of the yttrium oxide powder prepared using sodium polyacrylate as a dispersant.
[0055] observe Figure 2 (d) Figure 2 (d1), Figure 2 (d2) and Figure 4 (b) By comparing Examples 3, 6 and 9 with Comparative Example 2, it can be seen that when the amount of polyethylene oxide added is 1.5% of the mass of the yttrium oxide powder, the molecular weight M of polyethylene oxide is 800,000-1.5 million, and the dispersion state of the prepared yttrium oxide powder is almost the same as the dispersion state of the yttrium oxide powder prepared using calcium chloride as a dispersant. Figure 2 (b) Figure 2 (b1) and Figure 2 (b2), Figure 2 (c) Figure 2 (c1) and Figure 2 (c2), and Figure 4 (b) By comparing Examples 1-3, Examples 4-6 and Comparative Example 2, it can be seen that when the addition amount of polyethylene oxide is 0.5-1% of the mass of the yttrium oxide powder, the molecular weight M of polyethylene oxide is 800,000-1.5 million, and the dispersion state of the prepared yttrium oxide powder is significantly better than the dispersion state of the yttrium oxide powder prepared using calcium chloride as a dispersant.
[0056] In summary, the technical solution adopts polyethylene oxide with a molecular weight M of 800,000-1.5 million. When the addition amount of polyethylene oxide is 0.5-1% of the mass of the yttrium oxide powder, the dispersion state of the prepared yttrium oxide powder is significantly better than the dispersion state of the yttrium oxide powder prepared using sodium polyacrylate or calcium chloride particles as dispersants.
[0057] The above embodiments are only used to illustrate the technical solutions of the present disclosure, rather than to limit them. Although the present disclosure has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present disclosure, and they should all be included in the scope of the claims and specification of the present disclosure.
Claims
1. A method for preparing dispersed yttrium oxide powder, characterized in that: The steps include: S1. Weigh the raw materials: by mass percentage, yttrium oxide powder is 0.5%, and the balance is distilled water; the amount of polyethylene oxide added is 0.5-1.5% of the mass of the yttrium oxide powder; S2, mixing the weighed yttrium oxide powder and polyethylene oxide in distilled water to form a suspension, and dispersing the suspension using an ultrasonic disperser; S3, placing the suspension into a culture dish, and then placing the culture dish in an oven for vacuum drying to volatilize the polyethylene oxide and water; S4. The culture dish is taken out of the oven and naturally cooled to room temperature to obtain dispersed yttrium oxide powder in the culture dish.
2. The method for preparing dispersed yttrium oxide powder according to claim 1, characterized in that: In step S1, the amount of polyethylene oxide added is 0.5-1.0% of the mass of the yttrium oxide powder.
3. The method for preparing dispersed yttrium oxide powder according to claim 1, characterized in that: In step S1, the molecular weight M of polyethylene oxide is 800,000-1.5 million.
4. The method for preparing dispersed yttrium oxide powder according to claim 3, characterized in that: In step S1, the molecular weight M of polyethylene oxide is 800,000-1,000,000.
5. The method for preparing dispersed yttrium oxide powder according to claim 3, characterized in that: In step S1, the molecular weight M of polyethylene oxide is 1-1.5 million.
6. The method for preparing dispersed yttrium oxide powder according to claim 1, characterized in that: In step S1, the particle size of the yttrium oxide powder is 0.3-0.5 μm.
7. The method for preparing dispersed yttrium oxide powder according to claim 1, characterized in that: In step S2, the ultrasonic disperser disperses the suspension for 5-10 minutes.
8. The method for preparing dispersed yttrium oxide powder according to claim 1, characterized in that: In step S3, the drying temperature of the vacuum drying is 140-180°C.
9. Yttrium oxide powder prepared by the method for preparing dispersed yttrium oxide powder according to any one of claims 1 to 8.
10. Use of the yttrium oxide powder according to claim 9 in cold spray coating.