A high hardness and high Ce 3+ Preparation method of spherical cerium-based abrasive with high content
High-hardness, high-Ce3+ content spherical cerium-based abrasives were prepared by hydrothermal reaction and calcination oxidation methods, which solved the problems of insufficient hardness and insufficient Ce3+ content in cerium oxide abrasives, improved polishing performance and polishing rate of silicon carbide, and are suitable for industrial production.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- HUBEI SINOPHORUS ELECTRONIC MATERIALS CO LTD
- Filing Date
- 2024-07-30
- Publication Date
- 2026-05-15
AI Technical Summary
Existing cerium oxide abrasives have low hardness, which limits their application in the polishing field, and insufficient Ce3+ content affects polishing performance.
By combining green hydrothermal reaction and calcination oxidation methods, spherical cerium-based abrasives with high hardness and high Ce3+ content were prepared. Cerium salt and aluminum salt were dissolved in ethylene glycol solution for hydrothermal reaction, followed by calcination in a muffle furnace and reaction with sodium borohydride. The reaction conditions were controlled to improve the hardness and Ce3+ content of the abrasive.
It significantly improves the polishing performance of abrasives, increases the polishing rate of silicon carbide, and reduces surface roughness, making it suitable for large-scale industrial production.
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Figure CN119081650B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of polishing materials technology, specifically to a high-hardness and high-Ce material. 3+ A method for preparing spherical cerium-based abrasives with a high content of cerium. Background Technology
[0002] Since IBM first applied chemical mechanical polishing (CMP) to chip manufacturing in 1983, CMP has become a key technology in advanced semiconductor processes, with extremely wide applications in silicon wafer manufacturing, wafer fabrication, and back-end packaging. Each wafer undergoes several or even dozens of CMP polishing steps during production. Polishing slurry is one of the key components of CMP technology, and its performance directly affects the surface quality of the workpiece being polished. Polishing slurry mainly consists of abrasive particles (high-purity silica sol, alumina, and cerium oxide nanoparticles, etc.) and various additives. The role of the abrasive is to remove protrusions from the surface of the workpiece, thereby improving the surface smoothness. The abrasive is an important component of the polishing slurry; its hardness, particle size, morphology, and other properties directly affect the polishing rate and quality, therefore, the preparation of the abrasive is crucial.
[0003] Cerium oxide powder is widely used in optical glass parts, television picture tube shells, eyeglass lenses, flat glass, oscilloscope tubes, and acrylic products due to its advantages such as fine particle size, good chemical activity, strong grinding ability, and long service life. When used as a polishing material, cerium oxide powder is required to have good hardness and morphology. Studies have shown that the Ce2O3 surface of cerium oxide nanoparticles... 3+ Ions play an important role in chemical polishing. Kim et al. studied the polishing performance of CeO2 abrasives with different specific surface areas and concluded that small-sized CeO2 abrasives have a higher surface area due to the presence of Ce on their surface. 3+ Higher cerium oxide concentrations result in higher polishing rates; therefore, defects on the cerium oxide surface can enhance the chemical activity of the abrasive, thereby improving polishing performance. Sabia et al. also believe that high Ce... 3+ High-CeO2 abrasives generate more usable active sites at the particle / workpiece interface during polishing, which is more conducive to the chemical polishing process. Therefore, high-CeO2 abrasives... 3+ Cerium oxide nanoparticles with high content have significant advantages in the polishing process of integrated circuits. However, compared with alumina and polycrystalline diamond, the hardness of CeO2 particles is not high (Mohs hardness is 6), which limits their polishing rate and further restricts their application in the polishing field.
[0004] Therefore, materials with controllable dimensions, high hardness, and high Ce were prepared. 3+ The content of cerium-based abrasives is of great significance. Summary of the Invention
[0005] To address the shortcomings of existing technologies, the main objective of this invention is to provide a high-hardness and high-Ce material. 3+ This invention relates to cerium-based abrasives with high hardness and cerium content, and their preparation method. The invention combines a green hydrothermal reaction with a calcination oxidation method to synthesize a cerium-based abrasive with high hardness and cerium content. 3+ Spherical cerium-based abrasives with a high content of cerium, when formulated into a silicon carbide polishing slurry, can significantly improve the polishing rate of silicon carbide and reduce surface roughness.
[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0007] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0008] Step 1: Dissolve cerium salt and aluminum salt in ethylene glycol solution, and then synthesize cerium-based abrasive precursor through hydrothermal reaction;
[0009] Step 2: Place the cerium-based abrasive precursor into a muffle furnace for calcination to obtain cerium oxide spherical abrasive doped with alumina, i.e., cerium-based nanoparticles.
[0010] Step 3: Mix cerium-based nanoparticles with sodium borohydride evenly, place the mixture in a tube furnace, and heat the mixture in the presence of argon. After the reaction is complete, wash the reactants and finally dry them to obtain high hardness and high Ce content. 3+ Spherical cerium-based abrasive with high content.
[0011] Preferably, in step one, the cerium salt is at least one of cerium nitrate hexahydrate, cerium chloride heptahydrate, cerium chloride, cerium acetate, or cerium sulfate.
[0012] The aluminum salt is at least one of aluminum nitrate nonahydrate, aluminum trichloride, or aluminum sulfate.
[0013] More preferably, the cerium salt is one of cerium nitrate hexahydrate and cerium chloride heptahydrate.
[0014] More preferably, the aluminum salt is aluminum nitrate nonahydrate.
[0015] Preferably, the molar ratio of cerium salt to aluminum salt in step one is 1:0.08-0.5.
[0016] More preferably, the molar ratio of cerium salt and aluminum salt in step one is 1:0.08, 1:0.05, 1:0.1, 1:0.2, 1:0.3 and 1:0.5.
[0017] Preferably, in step one, the hydrothermal temperature is 150-200℃ and the hydrothermal time is 8-12h; under these reaction conditions, the hydrothermal reaction is promoted to proceed fully.
[0018] Preferably, step one further includes centrifuging the reactants to collect the precipitate after the reaction is complete, washing it with water and ethanol respectively, and drying it to obtain the cerium-based abrasive precursor.
[0019] Through extensive research, the inventors discovered that the hardness of spherical cerium-based abrasives can be altered by adjusting the amount of cerium and aluminum salts and the reaction conditions. By selecting appropriate amounts of cerium and aluminum salts and reaction conditions, high-hardness spherical cerium-based abrasives can be obtained.
[0020] The present invention introduces trace amounts of aluminum into the cerium-based abrasive, which increases the hardness of the abrasive and thus improves its polishing performance.
[0021] Preferably, in step two, the calcination temperature is 300-600℃ and the calcination time is 1-3h; by calcining the cerium-based abrasive precursor, the prepared nanoparticles have good dispersibility, making the spherical cerium-based abrasive crystal form more perfect.
[0022] Preferably, in step three, the mass ratio of the cerium-based nanoparticles to sodium borohydride is 1:0.1-2.
[0023] More preferably, in step three, the mass ratio of the cerium-based nanoparticles to sodium borohydride is 1:0.1, 1:0.5, 1:1, and 1:2.
[0024] Preferably, in step three, the argon flow rate is 30 scc, the tube furnace temperature is 200-300℃, the reaction time is 1-3 h, and the heating rate is 3-7℃ / min. Slow heating allows the spherical structure to develop more completely.
[0025] Through extensive research, the inventors discovered that by adjusting the amounts of cerium-based nanoparticles and sodium borohydride, as well as the reaction conditions, the Ce content of spherical cerium-based abrasives can be altered. 3+ By selecting an appropriate amount of sodium borohydride, high Ce content can be obtained. 3+ The content of spherical cerium-based abrasive improves the polishing performance of cerium-based abrasives.
[0026] Preferably, in step three, the cleaning involves washing the reactants 3-5 times with water and ethanol, respectively.
[0027] More preferably, the water used in the cleaning process is deionized water, the ethanol is anhydrous ethanol, the oven drying temperature is 50-70℃, and the drying time is 1.5-2.5h.
[0028] This invention obtains cerium oxide spherical abrasives doped with alumina through hydrothermal reaction and calcination, thereby improving the hardness of the abrasive; subsequently, in-situ reduction is used to remove Ce... 4+ Oxidized to Ce 3+ This will improve Ce 3+The content of [specific ingredient] can be used to prepare polishing slurry, which can significantly improve the polishing performance of the slurry.
[0029] This invention obtains cerium-based abrasives with suitable size and spherical structure by precisely controlling the amount of raw materials, reaction temperature and time, which can significantly improve the polishing performance of cerium-based abrasives. The obtained spherical structure has a particle size of 130-170 nm.
[0030] The present invention also provides the aforementioned high hardness and high Ce. 3+ Application of high-content spherical cerium-based abrasives in chemical mechanical polishing.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] 1. This invention synthesizes cerium oxide spherical abrasives with different alumina contents through a one-step hydrothermal method. The prepared spherical abrasives are not only uniform in size (130-170nm) and have good morphology, but also have significantly improved hardness, which is beneficial to improving the polishing efficiency of the abrasive.
[0033] 2. This invention uses sodium borohydride as a reducing agent. Sodium borohydride decomposes at high temperatures to produce hydrogen gas, which can generate a large amount of Ce on the surface of cerium-based abrasives. 3+ Ions can improve the polishing performance of abrasives; this reduction method is practical and simple, which is conducive to large-scale industrial production.
[0034] 3. This invention combines hydrothermal and calcination methods, resulting in a simple preparation process with good repeatability, wide availability of raw materials, and low energy consumption, which is conducive to large-scale industrial production.
[0035] 4. Applying the spherical cerium-based abrasive of the present invention to the preparation of silicon carbide polishing slurry can significantly improve the polishing performance of silicon carbide polishing slurry, making the polishing rate of silicon carbide as high as 5 μm / h and the surface roughness as low as 0.059 nm. Attached Figure Description
[0036] The present invention will be further described below with reference to the accompanying drawings and embodiments:
[0037] Figure 1 This is a SEM image of Embodiment 5 of the present invention;
[0038] Figure 2 This is the AFM diagram of Embodiment 6 of the present invention. Detailed Implementation
[0039] In the following examples and comparative examples, the hardness of the cerium-based abrasive was determined using a Mohs hardness tester, the ratio of trivalent cerium ions to tetravalent cerium ions in the cerium-based abrasive was determined using X-ray photoelectron spectroscopy (XPS), the morphology of the cerium-based abrasive was determined using scanning electron microscopy (SEM), and the morphology was determined using atomic force microscopy (AFM).
[0040] Example 1:
[0041] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0042] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and stir until well mixed. Then add 0.5 g of cerium nitrate hexahydrate and 0.004 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the above solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is complete, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0043] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 400℃ at a rate of 5℃ / min and calcine it for 2 hours to obtain cerium-based nanoparticles doped with alumina.
[0044] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.01g of sodium borohydride until homogeneous, and heat to 300℃ at a rate of 5℃ / min. React for 2 hours. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2 hours. Finally, dry to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0045] Example 2:
[0046] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0047] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring. Then add 0.5 g of cerium nitrate hexahydrate and 0.0216 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is complete, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0048] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 500°C at a rate of 5°C / min and calcine it for 3 hours to obtain cerium-based nanoparticles doped with alumina.
[0049] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.05g of sodium borohydride until homogeneous, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0050] Example 3:
[0051] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0052] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring. Then add 0.5 g of cerium nitrate hexahydrate and 0.0432 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is complete, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0053] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 500°C at a rate of 5°C / min, and calcine it for 3 hours to obtain cerium-based nanoparticles.
[0054] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.1g of sodium borohydride until homogeneous, heat to 250℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0055] Example 4:
[0056] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0057] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring. Then add 0.5 g of cerium nitrate hexahydrate and 0.0432 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is complete, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0058] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 500°C at a rate of 5°C / min, and calcine it for 3 hours to obtain cerium-based nanoparticles.
[0059] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.05g of sodium borohydride until homogeneous, heat to 250℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0060] Example 5:
[0061] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0062] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring. Then add 0.5 g of cerium nitrate hexahydrate and 0.0864 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is complete, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0063] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 600℃ at a rate of 3℃ / min, and calcine it for 3 hours to obtain cerium-based nanoparticles.
[0064] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.1g of sodium borohydride until homogeneous, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0065] Example 6:
[0066] A high hardness and high Ce 3+The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0067] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring; then add 0.5 g of cerium nitrate hexahydrate and 0.1296 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the above solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is completed, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0068] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 500°C at a rate of 5°C / min, and calcine it for 3 hours to obtain cerium-based nanoparticles.
[0069] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.2g of sodium borohydride until homogeneous, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Content: Cerium-based nanoparticles.
[0070] Example 7:
[0071] A high hardness and high Ce 3+ The method for preparing spherical cerium-based abrasives with a high cerium content includes the following steps:
[0072] Step 1: Add 0.5 mL of acetic acid and 0.5 mL of deionized water to 15 mL of ethylene glycol and mix thoroughly by magnetic stirring; then add 0.5 g of cerium nitrate hexahydrate and 0.216 g of aluminum nitrate nonahydrate to the above solution and stir to dissolve. Place the above solution in a muffle furnace and heat to 180 °C for hydrothermal reaction for 10 h. After the reaction is completed, centrifuge to collect the precipitate. Wash the precipitate three times with water and ethanol respectively, and then dry it in a drying oven at 60 °C for 8 h to obtain the cerium-based abrasive precursor.
[0073] Step 2: Place the cerium-based abrasive precursor into a muffle furnace, heat it to 300℃ at a rate of 2℃ / min, and calcine it for 3 hours to obtain cerium-based nanoparticles.
[0074] Step 3: Mix 0.1g of cerium-based nanoparticles with 0.1g of sodium borohydride until homogeneous, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants five times each with deionized water and anhydrous ethanol, and dry at 60℃ for 2h to obtain high hardness and high Ce content. 3+ Cerium-based abrasive.
[0075] Comparative Example 1:
[0076] Based on Example 5, the molar ratio of cerium salt and aluminum salt in step one was changed to 1:0.005, while other aspects remained the same as in Example 5.
[0077] Comparative Example 2:
[0078] Based on Example 5, the molar ratio of cerium salt and aluminum salt in step one was changed to 1:0.6, and the rest was the same as in Example 5.
[0079] Comparative Example 3:
[0080] Based on Example 5, the molar ratio of cerium salt and aluminum salt in step one was changed to 1:0.8, while other aspects remained the same as in Example 5.
[0081] Comparative Example 4:
[0082] Based on Example 6, the mass ratio of cerium-based abrasive to sodium borohydride in step three was changed to 1:0.05, while other aspects remained the same as in Example 6.
[0083] Comparative Example 5:
[0084] Based on Example 6, the mass ratio of cerium-based abrasive to sodium borohydride in step 3 was changed to 1:5, while other aspects remained the same as in Example 6.
[0085] The hardness and content of the cerium-based abrasives prepared in Examples 1-7 and Comparative Examples 1-5 were determined, and the results are shown in Table 1.
[0086] Table 1. Hardness and content determination of cerium-based abrasives
[0087]
[0088]
[0089] As shown in Table 1, Examples 1-7 and Comparative Examples 1-3 demonstrate that the hardness of cerium-based abrasives gradually increases with increasing aluminum salt doping content, indicating that aluminum salts can increase the hardness of cerium oxide. However, once a certain aluminum salt content is reached, the hardness of cerium oxide decreases. Examples 1-7 and Comparative Examples 4-5 show that the content of trivalent cerium ions in cerium-based abrasives increases with increasing sodium borohydride dosage. However, excessive sodium borohydride can cause sodium ions to be incorporated into the cerium-based abrasive, leading to a decrease in the content of trivalent cerium ions. Therefore, selecting appropriate amounts of aluminum salt and sodium borohydride is crucial to ensuring both the hardness and trivalent cerium ion content of cerium-based abrasives.
[0090] Polishing experiment:
[0091] The cerium-based abrasives from the above examples and comparative examples were prepared into polishing slurries for silicon carbide polishing experiments: 1% by mass of the abrasive was dispersed in deionized water, a surfactant was added, and the mixture was homogenized. Then, a 6% by mass potassium permanganate solution was added to prepare the polishing slurry. After polishing, the surface roughness of the silicon carbide wafer was measured using AFM, and the results are shown in Table 2.
[0092] Polishing conditions: FD-4603X single-sided polishing machine, polishing one 6-inch silicon carbide wafer at a time; polishing pressure 100 kPa; polishing disc and polishing head rotation speed 90 rpm; polishing time 2 min; polishing pad Suba 800; polishing fluid flow rate 100 mL / min; polishing temperature 25℃.
[0093] Polishing rate: The polishing removal rate is calculated by calculating the change in silicon wafer mass before and after silicon carbide polishing, using the following formula:
[0094] MRR(nm / min)=(ΔM) / (ρ×S×T)×10 7 .
[0095] Table 2 shows the polishing effects of the polishing slurries prepared in the examples and comparative examples.
[0096]
[0097]
[0098] Polishing experiments conducted in Examples 1-7 and Comparative Examples 1-5 show that silicon carbide achieves a polishing rate as high as 5 μm / h and a surface roughness as low as 0.059 nm. This demonstrates that increasing the abrasive hardness and trivalent cerium ion content significantly improves the polishing performance of the abrasive.
[0099] The above embodiments are merely preferred technical solutions of the present invention and should not be considered as limitations on the present invention. The scope of protection of the present invention should be limited to the technical solutions described in the claims, including equivalent substitutions of the technical features described in the claims. That is, equivalent substitutions and improvements within this scope are also within the scope of protection of the present invention.
Claims
1. A high-hardness and high-Ce 3+ A method for preparing spherical cerium-based abrasives with a high cerium content, characterized in that... Includes the following steps: Step 1: Dissolve cerium salt and aluminum salt in ethylene glycol solution and synthesize cerium-based abrasive precursors through hydrothermal reaction; Step 2: Place the cerium-based abrasive precursor into a muffle furnace for calcination to obtain cerium oxide spherical abrasive doped with alumina, i.e., cerium-based nanoparticles. Step 3: Mix cerium-based nanoparticles with sodium borohydride evenly, place the mixture in a tube furnace, and heat the mixture in the presence of argon. After the reaction is complete, wash the reactants and dry them to obtain high hardness and high Ce content. 3+ Spherical cerium-based abrasives with high content; In step one, the cerium salt is at least one of cerium nitrate hexahydrate, cerium chloride heptahydrate, cerium chloride, cerium acetate, or cerium sulfate; the aluminum salt is at least one of aluminum nitrate nonahydrate, aluminum trichloride, or aluminum sulfate. The molar ratio of the cerium salt to the aluminum salt is 1:0.08-0.5; The hydrothermal temperature is 150-200℃, and the hydrothermal time is 8-12 hours; In step two, the calcination temperature is 300-600℃, and the calcination time is 1-3 hours. In step three, the mass ratio of the cerium-based nanoparticles to sodium borohydride is 1:0.1-2; The argon gas flow rate is 30 scc, the tube furnace temperature is 200-300℃, the reaction time is 1-3 h, and the heating rate is 3-7℃ / min.
2. The high hardness and high Ce content according to claim 1 3+ A method for preparing spherical cerium-based abrasives with a high cerium content, characterized in that... In step three, the cleaning process involves sequentially cleaning with deionized water and anhydrous ethanol, drying in an oven at a temperature of 50-70°C for 1.5-2.5 hours.
3. The high hardness and high Ce content of claim 1 3+ The method for preparing spherical cerium-based abrasives with a certain content is characterized by the following: The particle size of the spherical cerium-based abrasive is 130-170 nm.
4. The application of the spherical cerium-based abrasive as described in claim 3 in chemical mechanical polishing.