CN113292928A - Preparation method of nano cerium dioxide polishing solution (powder) - Google Patents
Preparation method of nano cerium dioxide polishing solution (powder) Download PDFInfo
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- CN113292928A CN113292928A CN202110552387.1A CN202110552387A CN113292928A CN 113292928 A CN113292928 A CN 113292928A CN 202110552387 A CN202110552387 A CN 202110552387A CN 113292928 A CN113292928 A CN 113292928A
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- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 135
- 238000005498 polishing Methods 0.000 title claims abstract description 111
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000000843 powder Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000000725 suspension Substances 0.000 claims abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 31
- 238000001694 spray drying Methods 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 62
- 230000000052 comparative effect Effects 0.000 description 17
- 239000002002 slurry Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
本发明公开了一种纳米二氧化铈抛光液(粉)的制备方法。本发明采用分散剂聚乙烯吡咯烷酮和醇类溶剂，与湿法球磨相结合，球磨后分离液体得到纳米二氧化铈悬浊液；再用去离子水稀释得到纳米二氧化铈抛光液，抛光液在温度为80‑120℃下喷雾干燥，得到适合运输的纳米二氧化铈抛光粉。本发明解决了制备纳米二氧化铈抛光液时二氧化铈颗粒在溶剂中易沉降和团聚的问题，所制备的纳米二氧化铈抛光液(粉)具有良好的分散性和悬浮性，粒径分布窄，尺寸小，抛光性能显著。
The invention discloses a preparation method of nano-cerium oxide polishing liquid (powder). The present invention adopts dispersant polyvinylpyrrolidone and alcohol solvent, combined with wet ball milling, the liquid is separated after ball milling to obtain nano-cerium oxide suspension; then it is diluted with deionized water to obtain nano-cerium oxide polishing liquid, and the polishing liquid is in Spray drying at a temperature of 80-120° C. to obtain nano-cerium oxide polishing powder suitable for transportation. The invention solves the problem of easy sedimentation and agglomeration of ceria particles in the solvent when preparing nano-cerium oxide polishing liquid, and the prepared nano-cerium oxide polishing liquid (powder) has good dispersibility and suspension, and particle size distribution Narrow, small in size and outstanding in polishing performance.
Description
Technical Field
The invention relates to a preparation method of nano cerium dioxide polishing solution (powder), belonging to the technical field of preparation of inorganic powder materials.
Background
The reserve of rare earth ores in China is the first in the world, and the reserve of light rare earth cerium is higher. The cerium dioxide products produced in China are mainly exported and sold to countries such as Japan and Europe. China is the largest supply country of cerium dioxide raw materials in the domestic market of Japan, and about 78% of cerium dioxide imported from Japan is imported from China. The nano cerium dioxide can be used for high-end optical glass polishing solution, but because the domestic technology is still immature, the polishing solution prepared by the prior art has low polishing performance, and China still mainly depends on the import of nano cerium dioxide polishing solution finished products from Japan in the field of high-end cerium-based polishing solution (powder).
The preparation process of the nano cerium dioxide powder with controllable particle size and morphology has been researched more. The applicant also previously developed a green preparation method (CN201910249277.0) of cerium dioxide powder with controllable particle size morphology and large specific surface area, the morphology and particle size of the cerium dioxide are controlled by adjusting the proportion of a mixed solvent for preparing a precipitator and the concentration of rare earth feed liquid, the precipitator is prepared by using greenhouse gas carbon dioxide as a raw material in the preparation process, no acid or alkali is used, the mixed solvent can be recycled, the method is energy-saving, green and environment-friendly, and the prepared nano cerium dioxide powder can be used for catalyst carriers, polishing powder, automobile exhaust purification and the like. However, when the nano ceria powder is prepared into a polishing solution, ceria particles are very easy to settle and agglomerate in a solvent, and a nano ceria suspension with high dispersibility cannot be formed, so that the polishing performance of the nano ceria suspension is greatly influenced, and therefore, it is very important to develop a preparation technology of the nano ceria polishing solution (powder) with high dispersibility.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of nano cerium dioxide polishing solution (powder). The invention solves the problem that cerium dioxide particles are easy to settle and agglomerate in a solvent when preparing the nano cerium dioxide polishing solution (powder), and prepares the nano cerium dioxide polishing solution (powder) which has good dispersibility and does not settle for a long time. The invention has the advantages of simple preparation method, low cost, high stability, good polishing performance and the like.
The technical scheme of the invention is as follows: a preparation method of nano cerium dioxide polishing solution is characterized in that nano cerium dioxide powder is mixed with an alcohol solvent, then polyvinylpyrrolidone dispersing agent is added, ball milling is carried out after uniform mixing, and liquid is separated after ball milling to obtain nano cerium dioxide suspension; then diluting with deionized water to obtain the nano cerium dioxide polishing solution.
Preferably, the polyvinylpyrrolidone used is: one of PVPK30, PVPK60 and PVPK 90.
Preferably, the alcoholic solvents used are: one of methanol, ethanol, propanol, isopropanol, and n-butanol.
Preferably, the mass ratio of the nano cerium dioxide powder to the alcohol solvent is 1: 5-100 percent, the addition of the polyvinylpyrrolidone accounts for 1-15 percent of the total material mass, the ball milling time is 300-.
Preferably, the deionized water used for diluting the nano cerium dioxide suspension is added in an amount of: the mass percentage of the cerium dioxide in the diluted suspension is 1-10%.
In addition, in view of the fact that the polishing powder is easier to store or transport than the polishing solution, we have also developed a method for preparing nano-ceria polishing powder.
The technical scheme of the invention is as follows: a preparation method of nano cerium dioxide polishing powder is characterized in that the polishing solution prepared by the method is taken and spray-dried at the temperature of 80-120 ℃ to obtain the nano cerium dioxide polishing powder.
The invention has the beneficial effects that:
1) the polishing solution has good dispersibility, good suspension property and good polishing performance
Firstly, compared with the raw material nano cerium dioxide particles, the nano cerium dioxide polishing solution prepared by the invention has better dispersity and the agglomerated particle size D50The particle size is obviously reduced from 10 μm (raw material) to 0.072 μm, and accordingly, the agglomerated nano cerium dioxide particles become highly dispersed nano cerium dioxide particles as can be seen from the scanning electron microscope picture.
And secondly, the nano cerium dioxide polishing solution prepared by the invention does not substantially settle after standing for 120 hours.
Most importantly, the nano-ceria polishing solution prepared using the present invention has significantly better polishing performance (Ra ═ 25.207nm) than the nano-ceria polishing solution prepared in comparative example 1(Ra ═ 354.446nm) and comparative example 2(Ra ═ 212.971nm) using water as a solvent, without adding a polyvinylpyrrolidone dispersant.
2) Polishing solution prepared by polyvinylpyrrolidone dispersing agent which is obviously better than other dispersing agents
The aggregate particle diameter D of the cerium dioxide nanoparticles and the raw material50(10 μm) in comparison with the agglomerated particle diameter D obtained when polyvinylpyrrolidone was used50The dispersion effect was remarkable when the particle size was reduced to 0.072 μm, while the agglomerate particle size was not remarkably reduced when other dispersants were used.
After the polishing solution is placed for 1h, the nano cerium dioxide polishing solution prepared by using polyvinylpyrrolidone as a dispersing agent has good suspension property, and the polishing solutions prepared by using other dispersing agents are completely settled.
3) Spray drying to improve polishing performance
Compared with the common heating drying mode, the polishing powder prepared by spray drying obviously has better dispersibility and suspension property. Most importantly, the polishing performance (Ra 3.28nm) of the polishing powder prepared by spray drying is obviously better than that (Ra 73.5nm) of the polishing powder prepared by the common drying method.
Drawings
FIG. 1 is a graph showing the laser particle size of the nano-ceria slurry and the raw nano-ceria particles prepared in example 1; wherein, A is the nano-ceria polishing solution prepared in example 1, and B is the raw material nano-ceria particles;
FIG. 2 is a scanning electron microscope image of nano-ceria particles and raw nano-ceria particles in the nano-ceria polishing solution prepared in example 1; wherein, A is nano-ceria particles in the nano-ceria polishing solution prepared in example 1, and B is raw nano-ceria particles;
FIG. 3 is a graph of the nano-ceria slurry prepared in example 1, which was left for 1 hour and 120 hours; wherein, the picture A is a picture placed for 1h, and the picture B is a picture placed for 120 h;
FIG. 4 is an atomic force microscope photograph of the nano-ceria slurry prepared in example 1 after polishing quartz glass;
FIG. 5 is a graph of the initial and standing time of the nano-ceria polishing solution prepared in example 2 for 120 h; wherein, the A picture is an initial picture, and the B picture is a picture placed for 120 h;
FIG. 6 is an atomic force microscope photograph of the nano-ceria slurry prepared in example 2 after polishing quartz glass;
FIG. 7 is a graph of the nano-ceria slurries prepared in comparative example 1, which were left to stand for 1h and 120 h; wherein, the picture A is a picture placed for 1h, and the picture B is a picture placed for 120 h;
FIG. 8 is an atomic force microscope photograph of a quartz glass polished by the nano-ceria polishing solution prepared in comparative example 1;
FIG. 9 is a graph of the nano-ceria slurries prepared in comparative example 2, which were left to stand for 1h and 120 h; wherein, the picture A is a picture placed for 1h, and the picture B is a picture placed for 120 h;
FIG. 10 is an atomic force microscope photograph of a quartz glass polished by the nano-ceria polishing solution prepared in comparative example 2;
FIG. 11 is a photograph of a nano-ceria polishing solution prepared in comparative example 3, which was set for 48 hours initially; wherein, the A picture is an initial picture, and the B picture is a picture placed for 48 h;
FIG. 12 is an atomic force microscope photograph of a quartz glass polished by the nano-ceria polishing solution prepared in comparative example 3;
FIG. 13 is an initial picture of nano-ceria slurries prepared using different dispersants; wherein, a is polyvinylpyrrolidone; b sodium dodecyl benzene sulfonate; c hexadecyltrimethylammonium bromide; d polyvinyl alcohol; e sodium hexametaphosphate;
FIG. 14 is a photograph of nano-ceria slurries prepared using different dispersants left for 1 h; wherein, a is polyvinylpyrrolidone; b sodium dodecyl benzene sulfonate; c hexadecyltrimethylammonium bromide; d polyvinyl alcohol; e sodium hexametaphosphate.
Detailed Description
The effect is described below with reference to the following examples, in which the ball mill used in the examples of the present invention is a MITR-QM-QX ball mill (miqi technology), zirconia balls are used as a milling medium, and the ball ratio is 2: 1.
polishing liquid of nano cerium dioxide
Example 1
Mixing 1.0kg of nano cerium dioxide with 30.0L of methanol, putting 1.24kg (5 percent of total material) of polyvinylpyrrolidone (K30) into a ball milling tank, ball milling for 700min at the ball milling rotation speed of 300r/min, and separating balls and liquid after ball milling to obtain nano cerium dioxide suspension with good dispersibility. Then 10.0kg of the suspension is taken and added with 4.0L of deionized water to be diluted until the mass fraction of the cerium dioxide is 2.75 percent, and the nano cerium dioxide polishing solution is obtained.
Comparative example 1 (without addition of polyvinylpyrrolidone dispersant):
mixing 1.0kg of nano cerium dioxide with 30.0L of methanol, putting the mixture into a ball milling tank, ball milling for 700min at the ball milling rotation speed of 300r/min, and separating balls and liquid after ball milling to obtain a cerium dioxide suspension. Then 10.0kg of the solution is added with 4.0L of deionized water for dilution until the mass fraction of the cerium dioxide is 2.75 percent.
Comparative example 2 (using water instead of alcoholic solvent):
mixing 1.0kg of nano cerium dioxide with 30.0L of water, putting 1.24kg (5 percent of total materials) of polyvinylpyrrolidone (K30) into a ball milling tank, ball milling for 700min at the ball milling rotation speed of 300r/min, and separating balls and liquid after ball milling to obtain cerium dioxide suspension. Then 10.0kg of the solution is added with 4.0L of deionized water for dilution until the mass fraction of the cerium dioxide is 2.75 percent.
The laser particle size diagram of the nano-ceria polishing solution prepared in example 1 of the present invention is shown in fig. 1A, and compared with the raw nano-ceria particles (fig. 1B), the nano-ceria polishing solution prepared in the present invention (fig. 1A) has better dispersibility and an agglomerate size D50Becomes significantly smaller, decreasing from 10 μm to 0.072 μm, and correspondingly, it can be seen from the scanning electron microscope picture (FIG. 2): the raw material-agglomerated nano-ceria particles (fig. 2B) become highly dispersed nano-ceria particles (fig. 2A) after being prepared into a polishing solution by the method of the present invention.
The pictures of the nano-ceria polishing solution prepared in example 1 after being placed for 1h and 120h are shown in fig. 3, and it can be seen that: the nano cerium dioxide polishing solution prepared by the invention does not substantially settle after being placed for 120 h. And the nano-ceria slurries prepared in comparative example 1 (fig. 7) and comparative example 2 (fig. 9) settled after being left for 120 hours.
An atomic force microscope photograph of the quartz glass of example 1 after polishing is shown in FIG. 4. As can be seen from fig. 4: after polishing the quartz glass surface with the nano-ceria polishing solution and polishing with a polishing pad (rotating speed 100r/min) for 1h, the Ra of 25.207nm is significantly better than that of the nano-ceria polishing solutions prepared in comparative example l (Ra 354.446nm, fig. 8) and comparative example 2(Ra 212.971nm, fig. 10).
The present invention also provides comparative laser particle size data of nano-ceria slurries prepared by using sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide, polyvinyl alcohol, and sodium hexametaphosphate, respectively, instead of polyvinylpyrrolidone as a dispersant (other components, procedure same as example 1), as shown in table 1 below.
TABLE 1 comparison of laser particle size of nano-ceria polishing solutions prepared by adding different dispersants
As shown in table 1, in comparison with the particle size of the nano ceria polishing solution prepared using different dispersants, it is apparent that: compared with the agglomerate size D50(10 μm) of the raw nano-ceria particles, the agglomerate size D50 was reduced to 0.072 μm with polyvinylpyrrolidone, the dispersing effect was significant, while the agglomerate size was not significantly reduced with other dispersants. Fig. 13 and 14 are graphs of sedimentation experiments for initial and standing 1h of polishing solutions prepared using different dispersants, from which it can be seen that: after the polishing solution is placed for 1h, the nano cerium dioxide polishing solution prepared by using polyvinylpyrrolidone as a dispersing agent has the best suspension property (a), and the polishing solutions prepared by using other dispersing agents are completely settled. It can thus be seen that: the polyvinylpyrrolidone of the present invention cannot be replaced by other dispersants.
Preparation of nano cerium dioxide polishing powder
Example 2
1.0L of the nano-ceria polishing solution prepared in example 1 was sprayed and dried at 80 ℃ to obtain nano-ceria polishing powder. And adding deionized water again to dilute until the mass fraction of the cerium dioxide is 2.75 percent, thereby obtaining the nano cerium dioxide polishing solution.
Comparative example 3 (oven drying)
1.0L of the nano-ceria polishing solution prepared in example 1 was dried in a common oven at 80 ℃ to obtain nano-ceria polishing powder. And adding deionized water again to dilute until the mass fraction of the cerium dioxide is 2.75 percent, thereby obtaining the nano cerium dioxide polishing solution.
FIG. 5 shows the initial picture and the standing picture for 120h of the nano-ceria slurry prepared by using the polishing powder, and it can be seen that: the nano-ceria polishing solution prepared by the invention does not settle after standing for 120h, and the dispersibility and the suspensibility are obviously better than those of comparative example 3 (figure 11). Most importantly, the polishing performance (Ra 3.28nm, fig. 6) of the spray-dried polishing powder prepared in example 2 is significantly better than that of the polishing powder prepared by the conventional drying method (Ra 73.5nm, fig. 12).
Example 3
Mixing 1.0kg of nano cerium dioxide with 30.0L of methanol, putting 1.5kg of polyvinylpyrrolidone (K30) into a ball milling tank, ball milling for 600min at the ball milling rotating speed of 300r/min, and separating balls and liquid after ball milling to obtain nano cerium dioxide suspension with good dispersibility. Then 10.0kg of the suspension is taken and added with 4.0L of deionized water to be diluted until the mass fraction of the cerium dioxide is 2.75 percent, and the nano cerium dioxide polishing solution is obtained.
1.0L of the nano-ceria polishing solution prepared in example 3 was sprayed and dried at 85 ℃ to obtain nano-ceria polishing powder. And adding deionized water again to dilute until the mass fraction of the cerium dioxide is 2.75 percent, thereby obtaining the nano cerium dioxide polishing solution.
Example 4
Mixing 1.0kg of nano cerium dioxide with 30.0L of methanol, putting 1.0kg of polyvinylpyrrolidone (K30) into a ball milling tank, ball milling for 720min at a ball milling rotating speed of 300r/min, and separating balls and liquid after ball milling to obtain nano cerium dioxide suspension with good dispersibility. Then 10.0kg of the suspension is taken and added with 4.0L of deionized water to be diluted until the mass fraction of the cerium dioxide is 2.75 percent, and the nano cerium dioxide polishing solution is obtained.
1.0L of the nano-ceria polishing solution prepared in example 4 was sprayed and dried at 90 ℃ to obtain nano-ceria polishing powder. And adding deionized water again to dilute until the mass fraction of the cerium dioxide is 2.75 percent, thereby obtaining the nano cerium dioxide polishing solution.
Example 5
Mixing 1.0kg of nano cerium dioxide with 30.0L of methanol, putting 1.24kg of polyvinylpyrrolidone (K60) into a ball milling tank, ball milling for 700min at the ball milling rotating speed of 300r/min, and separating balls and liquid after ball milling to obtain nano cerium dioxide suspension with good dispersibility. Then 10.0kg of the suspension is taken and added with 4.0L of deionized water to be diluted until the mass fraction of the cerium dioxide is 2.75 percent, and the nano cerium dioxide polishing solution is obtained.
1.0L of the nano-ceria polishing solution prepared in example 5 was sprayed and dried at 85 ℃ to obtain nano-ceria polishing powder. And adding deionized water again to dilute until the mass fraction of the cerium dioxide is 2.75 percent, thereby obtaining the nano cerium dioxide polishing solution.
Claims (8)
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| CN114045153A (en) * | 2021-12-21 | 2022-02-15 | 清华大学 | Method for preparing cerium dioxide suspension, cerium dioxide suspension and polishing solution |
| CN114181629A (en) * | 2021-12-21 | 2022-03-15 | 清华大学 | A kind of polishing liquid and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114045153A (en) * | 2021-12-21 | 2022-02-15 | 清华大学 | Method for preparing cerium dioxide suspension, cerium dioxide suspension and polishing solution |
| CN114181629A (en) * | 2021-12-21 | 2022-03-15 | 清华大学 | A kind of polishing liquid and its preparation method and application |
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