Preparation method of spherical cerium-based abrasive material with high hardness and high Ce < 3 + > content

Abstract

The invention discloses a preparation method of a spherical cerium-based abrasive material with high hardness and high Ce < 3 + > content. The method comprises the following steps: 1, carrying out hydrothermal reaction on cerium salt and aluminum salt in an ethylene glycol solution to generate a cerium-based abrasive precursor; 2, firing the cerium-based abrasive precursor to obtain a cerium oxide spherical abrasive doped with aluminum oxide; and 3, reducing the cerium oxide spherical abrasive by sodium borohydride to obtain the spherical cerium-based abrasive with high hardness and high Ce < 3 + > content. According to the method, aluminum ions are doped into the cerium oxide spherical abrasive through a one-step hydration method, the hardness of the abrasive is improved, meanwhile, a large amount of Ce < 4 + > is efficiently and rapidly reduced into Ce < 3 + > ions through an in-situ reduction method, and the polishing efficiency of the abrasive is improved. The cerium-based abrasive synthesized by the method is uniform in granularity, good in morphology, high in hardness and high in Ce < 3 + > content, and the polishing rate of silicon carbide can be remarkably increased and the surface roughness can be remarkably reduced when the cerium-based abrasive is prepared into a silicon carbide polishing solution; and the preparation method is simple, good in repeatability, green and environment-friendly, and beneficial to industrial production.

Description

Technical Field

[0001] The present invention relates to the technical field of polishing materials, and in particular to a high hardness and high Ce 3+ The invention discloses a preparation method of spherical cerium-based abrasive with high content. Background Art

[0002] Since IBM first used the chemical mechanical polishing (CMP) process for chip manufacturing in 1983, CMP has become a key technology in advanced semiconductor processes. It has been widely used in silicon wafer manufacturing, wafer manufacturing and back-end packaging. Each wafer will go through several or even dozens of CMP polishing steps during the production process. Polishing liquid is one of the keys to chemical mechanical polishing technology, and its performance directly affects the surface quality of the workpiece being polished. Polishing liquid is mainly composed of abrasive particles (high-purity silica sol, nanoparticles such as aluminum oxide and cerium oxide) and various additives. The function of the abrasive is to remove the protrusions on the surface of the workpiece being polished to improve the flatness of the workpiece surface. Abrasive is an important component of polishing liquid. Its hardness, particle size, morphology and other properties directly affect the polishing rate and polishing quality, so the preparation of abrasive is very important.

[0003] Because cerium oxide powder has the advantages of fine particle size, good chemical activity, strong grinding ability and long service life, it is widely used in optical glass parts, TV tube glass shells, eyeglass lenses, flat glass, oscilloscopes and organic glass products. When used as a polishing material, cerium oxide powder is required to have good hardness and morphology. Studies have shown that the surface of cerium oxide nanoparticles Ce 3+ Ions play an important role in the chemical polishing process. Kim et al. studied the polishing performance of CeO2 abrasives with different specific surface areas and found that small-sized CeO2 abrasives have a high surface area. 3+ The higher the concentration, the higher the polishing rate; therefore, the defects on the surface of cerium oxide can enhance the chemical activity of the abrasive, thereby improving the polishing performance. Sabia et al. also believed that high Ce 3+ CeO2 abrasives with high CeO2 content will produce more available active sites at the particle / workpiece interface during polishing, which is more conducive to the chemical polishing process. 3+ CeO2 nanopowders with high content have outstanding advantages in the polishing process of integrated circuits. However, compared with aluminum oxide and polycrystalline diamond, the hardness of CeO2 particles is not high (Mohs hardness is 6), which limits its polishing rate and further limits its application in the polishing field.

[0004] Therefore, the size-controlled, high hardness and high Ce 3+ The content of cerium-based abrasive is of great significance. Summary of the invention

[0005] In order to solve the shortcomings of the prior art, the main purpose of the present invention is to provide a high hardness and high Ce 3+ The present invention combines the green hydrothermal reaction and the roasting oxidation method to synthesize a cerium-based abrasive with high hardness and Ce content. 3+ Spherical cerium-based abrasives with a high content of cerium and mixed with silicon carbide polishing liquid can significantly increase the polishing rate of silicon carbide and reduce the surface roughness.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises the following steps:

[0008] Step 1, dissolving cerium salt and aluminum salt in ethylene glycol solution, and then synthesizing cerium-based abrasive precursor through hydrothermal reaction;

[0009] Step 2: placing the cerium-based abrasive precursor into a muffle furnace for calcination to obtain cerium oxide spherical abrasive doped with aluminum oxide, namely, cerium-based nanoparticles;

[0010] Step 3: Evenly mix the cerium-based nanoparticles and sodium borohydride, place them in a tube furnace, heat the mixture in the presence of argon, clean the reactants after the reaction, and finally dry them to obtain a high hardness and high Ce 3+ Spherical cerium-based abrasive with high content.

[0011] Preferably, in step 1, 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 chloride or aluminum sulfate.

[0013] Further preferably, the cerium salt is one of cerium nitrate hexahydrate and cerium chloride heptahydrate.

[0014] Further preferably, the aluminum salt is aluminum nitrate nonahydrate.

[0015] Preferably, the molar ratio of the cerium salt to the aluminum salt in step 1 is 1:0.08-0.5.

[0016] More preferably, the molar ratio of the cerium salt to the aluminum salt in step 1 is 1:0.08, 1:0.05, 1:0.1, 1:0.2, 1:0.3 and 1:0.5.

[0017] Preferably, in step 1, the hydrothermal temperature is 150-200° C., and the hydrothermal time is 8-12 h. Under such reaction conditions, the hydrothermal reaction is fully promoted.

[0018] Preferably, step one further comprises, after the reaction is completed, centrifuging the reactants to collect the precipitate, washing them with water and ethanol respectively, and drying them to obtain a cerium-based abrasive precursor.

[0019] After extensive research, the inventors found that the hardness of the spherical cerium-based abrasive can be changed by adjusting the dosage and reaction conditions of cerium salt and aluminum salt, and by selecting appropriate dosage and reaction conditions of cerium salt and aluminum salt, a spherical cerium-based abrasive with high hardness can be obtained.

[0020] A trace amount of aluminum element is introduced into the cerium-based abrasive of the present invention, thereby increasing the hardness of the abrasive and thus improving the polishing performance of the abrasive.

[0021] Preferably, in step 2, the calcination temperature is 300-600° C., and the calcination time is 1-3 h. By calcining the cerium-based abrasive precursor, the prepared nanoparticles have good dispersibility, making the spherical cerium-based abrasive crystal 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 flow rate of argon gas is 30scc, the temperature of the tube furnace is 200-300°C, the reaction time is 1-3h, the heating rate is 3-7°C / min, and the slow heating makes the spherical structure develop more completely.

[0025] After extensive research, the inventors found that the Ce content of spherical cerium-based abrasives can be changed by adjusting the amount of cerium-based nanoparticles and sodium borohydride and the reaction conditions. 3+ Content, choose the appropriate amount of sodium borohydride, can obtain high Ce 3+ The content of spherical cerium-based abrasive can improve the polishing performance of the cerium-based abrasive.

[0026] Preferably, in step three, the cleaning is to clean the reactant with water and ethanol respectively for 3-5 times.

[0027] Further preferably, in the cleaning process, the water is deionized water, the ethanol is anhydrous ethanol, the oven drying temperature is 50-70° C., and the drying time is 1.5-2.5 h.

[0028] The invention obtains a spherical abrasive material of cerium oxide doped with aluminum oxide through hydrothermal reaction and calcination treatment, thereby improving the hardness of the abrasive material; then, the CeO2 is reduced in situ. 4+ Oxidized to Ce 3+ , thereby increasing Ce 3+The content of , when used in the preparation of polishing liquid, can significantly improve the polishing performance of the polishing liquid.

[0029] The invention obtains cerium-based abrasive with suitable size and spherical structure by precisely controlling the amount of raw materials, reaction temperature and time of the reaction, and can significantly improve the polishing performance of the cerium-based abrasive. The particle size of the obtained spherical structure is 130-170nm.

[0030] The present invention also provides the high hardness and high Ce 3+ Application of spherical cerium-based abrasives with high content in chemical mechanical polishing.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] 1. The present invention synthesizes cerium oxide spherical abrasives doped with different aluminum oxide contents by a one-step hydrothermal method. The prepared spherical abrasives not only have uniform size (130-170nm) and good morphology, but also have significantly improved hardness, which is beneficial to improving the polishing efficiency of the abrasives.

[0033] 2. The present invention uses sodium borohydride as a reducing agent. Sodium borohydride will decompose and produce hydrogen at high temperature, which can produce a lot of Ce on the surface of cerium-based abrasives. 3+ ions, which is beneficial to improving the polishing performance of the abrasive; the reduction method is practical and simple, and is conducive to large-scale industrial production.

[0034] 3. The present invention combines the hydrothermal method with the roasting method, has a simple preparation process, good repeatability, a wide source of raw materials, low energy consumption, and is conducive to large-scale industrial production.

[0035] 4. The spherical cerium-based abrasive of the present invention is used to prepare silicon carbide polishing liquid, which can significantly improve the polishing performance of the silicon carbide polishing liquid, so that the polishing rate of silicon carbide is as high as 5um / h and the surface roughness is as low as 0.059nm. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] The present invention will be further described below in conjunction with the accompanying drawings and embodiments:

[0037] Figure 1 is a SEM image of Example 5 of the present invention;

[0038] Figure 2 This is an AFM image of Example 6 of the present invention. DETAILED DESCRIPTION

[0039] In the following examples and comparative examples, the hardness of the cerium-based abrasive was measured by a Mohs hardness tester, the ratio of trivalent cerium ions to tetravalent cerium ions in the cerium-based abrasive was measured by X-ray photoelectron spectroscopy (XPS), the morphology of the cerium-based abrasive was measured by scanning electron microscopy (SEM), and the morphology of the cerium-based abrasive was measured by atomic force microscopy (AFM).

[0040] Embodiment 1:

[0041] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 to mix evenly; 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 hours, collect the precipitate by centrifugation after the reaction is completed, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0043] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 400° C. at a rate of 5° C. / min and calcining it for 2 h to obtain cerium-based nanoparticles doped with aluminum oxide;

[0044] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.01g of sodium borohydride, heat to 300°C at a rate of 5°C / min, react for 2h, wash the reactants with deionized water and anhydrous ethanol for 5 times, dry at 60°C for 2h, and finally dry to obtain a high hardness and high Ce 3+ Content cerium based abrasive.

[0045] Embodiment 2:

[0046] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 them evenly 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 above solution in a muffle furnace and heat it to 180° C. for hydrothermal reaction for 10 hours, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0048] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 500° C. at a rate of 5° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles doped with aluminum oxide;

[0049] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.05g of sodium borohydride, heat to 300°C at a rate of 5°C / min and react for 2h. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60°C for 2h to obtain high hardness and high Ce nanoparticles. 3+ Content cerium based abrasive.

[0050] Embodiment 3:

[0051] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 them evenly 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 above solution in a muffle furnace and heat it to 180° C. for hydrothermal reaction for 10 hours, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0053] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 500° C. at a rate of 5° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles;

[0054] Step 3: Mix 0.1 g of cerium-based nanoparticles and 0.1 g of sodium borohydride, heat to 250 ° C at a rate of 5 ° C / min and react for 2 hours. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60 ° C for 2 hours to obtain high hardness and high Ce 3+ Content cerium based abrasive.

[0055] Embodiment 4:

[0056] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 them evenly 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 above solution in a muffle furnace and heat it to 180° C. for hydrothermal reaction for 10 hours, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0058] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 500° C. at a rate of 5° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles;

[0059] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.05g of sodium borohydride, heat to 250°C at a rate of 5°C / min and react for 2h. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60°C for 2h to obtain high hardness and high Ce nanoparticles. 3+ Content cerium based abrasive.

[0060] Embodiment 5:

[0061] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises the following steps:

[0062] Step 1, add 0.5mL of acetic acid and 0.5mL of deionized water to 15mL of ethylene glycol, and mix them evenly by magnetic stirring; then add 0.5g of cerium nitrate hexahydrate and 0.0864g of aluminum nitrate nonahydrate to the above solution and stir to dissolve, place the above solution in a muffle furnace and heat it to 180°C for hydrothermal reaction for 10h, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60°C drying oven for 8h to obtain a cerium-based abrasive precursor;

[0063] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 600° C. at a rate of 3° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles;

[0064] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.1g of sodium borohydride, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60℃ for 2h to obtain high hardness and high Ce nanoparticles. 3+ Content cerium based abrasive.

[0065] Embodiment 6:

[0066] A high hardness and high Ce 3+The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 them evenly 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 it to 180° C. for hydrothermal reaction for 10 hours, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0068] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 500° C. at a rate of 5° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles;

[0069] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.2g of sodium borohydride, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60℃ for 2h to obtain high hardness and high Ce nanoparticles. 3+ Content of cerium-based nanoparticles.

[0070] Embodiment 7:

[0071] A high hardness and high Ce 3+ The preparation method of the spherical cerium-based abrasive with a content of cerium comprises 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 them evenly 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 it to 180° C. for hydrothermal reaction for 10 hours, after the reaction is completed, collect the precipitate by centrifugation, wash the precipitate with water and ethanol three times respectively, and then put it in a 60° C. drying oven for 8 hours to obtain a cerium-based abrasive precursor;

[0073] Step 2: placing the cerium-based abrasive precursor into a muffle furnace, heating it to 300° C. at a rate of 2° C. / min and calcining it for 3 h to obtain cerium-based nanoparticles;

[0074] Step 3: Mix 0.1g of cerium-based nanoparticles and 0.1g of sodium borohydride, heat to 300℃ at a rate of 5℃ / min and react for 2h. After the reaction, wash the reactants with deionized water and anhydrous ethanol for 5 times, and dry them at 60℃ for 2h to obtain high hardness and high Ce nanoparticles. 3+ Content cerium based abrasive.

[0075] Comparative Example 1:

[0076] Based on Example 5, the molar ratio of the cerium salt to the aluminum salt in step 1 was changed to 1:0.005, and the rest was the same as Example 5.

[0077] Comparative Example 2:

[0078] Based on Example 5, the molar ratio of the cerium salt to the aluminum salt in step 1 was changed to 1:0.6, and the rest was the same as Example 5.

[0079] Comparative Example 3:

[0080] Based on Example 5, the molar ratio of the cerium salt to the aluminum salt in step 1 was changed to 1:0.8, and the rest was the same as Example 5.

[0081] Comparative Example 4:

[0082] Based on Example 6, the mass ratio of cerium-based abrasive to sodium borohydride in step 3 was changed to 1:0.05, and the rest was the same as 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, and the rest was the same as Example 6.

[0085] The hardness and content of the cerium-based abrasives prepared in Examples 1-7 and Comparative Examples 1-5 were measured. 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, from Examples 1-7 and Comparative Examples 1-3, it can be seen that with the increase in the amount of aluminum salt doping, the hardness of the cerium-based abrasive gradually increases, indicating that aluminum salt can increase the hardness of cerium oxide, but when the aluminum salt reaches a certain content, the hardness of cerium oxide decreases; from Examples 1-7 and Comparative Examples 4-5, it can be seen that with the increase in the amount of sodium borohydride, the content of trivalent cerium ions in the cerium-based abrasive increases, but excessive sodium borohydride will cause sodium ions to be doped into the cerium-based abrasive, resulting in a decrease in the content of trivalent cerium ions. It can be seen that the hardness and trivalent cerium ion content of the cerium-based abrasive can be ensured by selecting the appropriate amount of aluminum salt and sodium borohydride.

[0090] Polishing experiment:

[0091] The cerium-based abrasives of the above-mentioned embodiment and comparative example were respectively prepared into polishing liquids, and a polishing experiment of silicon carbide was carried out: 1% of the abrasive by mass was dispersed in deionized water, a surfactant was added, homogenized, and then a 6% by mass potassium permanganate solution was added to prepare a polishing liquid. After polishing, the surface roughness of the silicon carbide sheet was detected using AFM, and the results are shown in Table 2.

[0092] Polishing conditions: polishing machine FD-4603X single-sided polishing machine, polishing one 6-inch silicon carbide wafer each time; polishing pressure 100 kPa; polishing disc and polishing head speed 90 rpm; polishing time 2 min; polishing pad Suba 800; polishing liquid flow rate 100 mL / min; polishing temperature 25 °C.

[0093] Polishing rate: The polishing removal rate is calculated by calculating the change in silicon wafer mass before and after silicon carbide polishing. The formula is as follows:

[0094] MRR(nm / min)=(ΔM) / (ρ×S×T)×10 7 .

[0095] Table 2 Polishing effect of the polishing liquid configured in the embodiment and the comparative example

[0096]

[0097]

[0098] According to the polishing experiments of Examples 1-7 and Comparative Examples 1-5, the polishing rate of silicon carbide is as high as 5um / h, and the surface roughness is as low as 0.059nm. It can be seen that the increase of abrasive hardness and trivalent cerium ion content significantly improves the polishing performance of the abrasive.

[0099] The above embodiments are only preferred technical solutions of the present invention and should not be regarded as limiting the present invention. The protection scope of the present invention shall be the technical solutions recorded in the claims, including equivalent replacement solutions of the technical features in the technical solutions recorded in the claims. That is, equivalent replacement improvements within this scope are also within the protection scope of the present invention.

Claims

1. A high hardness and high Ce 3+ The method for preparing a spherical cerium-based abrasive with a content of The following steps are involved: Step 1, dissolving cerium salt and aluminum salt in ethylene glycol solution, and synthesizing cerium-based abrasive precursor through hydrothermal reaction; Step 2: placing the cerium-based abrasive precursor into a muffle furnace for calcination to obtain cerium oxide spherical abrasive doped with aluminum oxide, namely, cerium-based nanoparticles; Step 3: Evenly mix the cerium-based nanoparticles and sodium borohydride, place them in a tube furnace, heat the mixture in the presence of argon, wash the reactants after the reaction is complete, and dry them to obtain a high-hardness and high-Ce 3+ Spherical cerium-based abrasive with high content.

2. According to claim 1, a high hardness and high Ce 3+ The method for preparing a spherical cerium-based abrasive with a content of In step 1, 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 chloride or aluminum sulfate.

3. According to claim 1, a high hardness and high Ce 3+ The method for preparing a spherical cerium-based abrasive with a content of In step 1, the molar ratio of the cerium salt to the aluminum salt is 1:0.08-0.

5.

4. According to claim 1, a high hardness and high Ce 3+ The method for preparing a spherical cerium-based abrasive with a content of In step 1, the hydrothermal temperature is 150-200° C., and the hydrothermal time is 8-12 hours.

5. A high hardness and high Ce according to claim 1 3+ The method for preparing a spherical cerium-based abrasive with a content of In step 2, the calcination temperature is 300-600° C., and the calcination time is 1-3 hours.

6. A high hardness and high Ce according to claim 1 3+ The method for preparing a spherical cerium-based abrasive with a content of In step three, the mass ratio of the cerium oxide spherical abrasive to sodium borohydride is 1:0.1-2.

7. A high hardness and high Ce according to claim 1 3+ The method for preparing a spherical cerium-based abrasive with a content of In step 3, the flow rate of argon gas is 30 scc, the temperature of the tube furnace is 200-300°C, the reaction time is 1-3h, and the heating rate is 3-7°C / min.

8. A high hardness and high Ce according to claim 1 3+ The method for preparing a spherical cerium-based abrasive with a content of In step three, the water in the cleaning process is deionized water, the ethanol is anhydrous ethanol, the oven drying temperature is 50-70° C., and the drying time is 1.5-2.5 hours.

9. A high hardness and high Ce compound as claimed in any one of claims 1 to 8 3+ The spherical cerium-based abrasive is characterized by: The particle size of the cerium-based abrasive is 130-170 nm.

10. A high hardness and high Ce according to claim 9. 3+ Application of spherical cerium-based abrasives with high content in chemical mechanical polishing.

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