CN112266730B - Preparation method of fluorinated cerium dioxide polishing powder under microwave condition - Google Patents
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Abstract
The invention discloses a preparation method of cerium fluoride dioxide polishing powder under microwave condition, belonging to the technical field of preparation of nano rare earth materials, and comprising the following steps: adding Ce (NO)3)3·6H2Dissolving O in deionized water, preheating by microwave, adding NH4F; reacting NH4HCO3Dissolved in deionized water, and preheated Ce (NO3) is added thereto3·6H2O and NH4F mixed solution is subjected to constant temperature precipitation reaction under the microwave condition to generate Ce2(CO3)3Precursor and continuing aging; filtering the precursor reaction solution to obtain a precipitate, drying at constant temperature, and grinding into powder; roasting the precursor powder to prepare fluorinated cerium dioxide polishing powder; the cerium dioxide powder prepared by the method has high particle crystallinity, regular shape and spherical shape, uniform particle size distribution and good dispersibility, and further improves the polishing efficiency and the polishing precision of the fluorinated cerium dioxide powder.
Description
Technical Field
The invention belongs to the technical field of preparation of nano rare earth materials, and particularly relates to a preparation method of fluoridized cerium dioxide polishing powder under the microwave condition.
Background
The polishing principle of the rare earth cerium oxide polishing powder is chemical mechanical polishing, and the surface is continuously subjected to chemical reaction while being physically ground, so that the cerium oxide polishing powder has high polishing efficiency and excellent polishing quality which are difficult to achieve by the traditional polishing powder. In addition, the cerium oxide polishing powder has moderate hardness, long service life and little pollution to the polished surface, so that the cerium oxide becomes the best choice among a plurality of polishing materials in the polishing fields of optical instrument glass, magnetic disk glass substrates, optical instrument glass, kinescopes and the like. With the progress of science and technology, the requirements on the roughness of the surface of a component used on high-precision equipment are continuously improved, and correspondingly, the requirements on the performance and the type of the rare earth cerium oxide polishing powder are higher and higher. The preparation method and the production process conditions can be used for preparing the cerium oxide polishing powder with more excellent polishing performance, and the cerium oxide polishing powder becomes the focus of attention at home and abroad.
Many ceria materials are currently fluorinated to improve polishing performance. When preparing cerium oxide polishing powder by precipitation-calcination liquid-phase reaction method, various fluorinating agents such as H are added in the synthesis of precursor of the polishing powder2SiF6HF or NH4F, and the like, thereby introducing fluorine ions into the polishing powder. The addition of fluorine does not change the structure of the cerium dioxide cubic fluorite, but changes the morphology of the cerium dioxide polishing powder particles, presents a sphere-like shape, and obviously improves the polishing performance of the polishing powder. But still has obvious agglomeration phenomenon, and the polishing powder particles have grape-like shape and uneven particle size distribution. In the prior art, a mode of adding an auxiliary reagent into a precipitation reaction system is often adopted to improve the agglomeration condition. This approach tends to involve additional costs and operating steps, with the risk of time consuming, equipment increase and product purity reduction.
Disclosure of Invention
Aiming at the defect of the existing liquid phase precipitation method in controlling the morphology of cerium oxide particles, the invention provides a preparation method for synthesizing spherical nano cerium dioxide with uniform particle size and better dispersibility in a microwave environment.
The technical scheme adopted by the invention is as follows: a preparation method of fluoridized cerium dioxide polishing powder under the microwave condition comprises the following steps:
(1) taking Ce (NO)3)3·6H2O、NH4HCO3And NH4Dissolving F in deionized water to prepare an aqueous solution;
(2) microwave preheating: taking Ce (NO)3)3·6H2Preheating an O aqueous solution to 55-75 ℃ in a microwave mode; taking NH4F aqueous solution to Ce (NO)3)3·6H2Stirring the solution O uniformly;
(3) precipitation reaction: taking NH4HCO3Adding the aqueous solution into the mixed solution prepared in the step (2); then, under the condition of continuous stirring, carrying out constant temperature reaction for 60-90 min in a microwave mode to generate a precursor Ce2(CO3)3(ii) a The constant temperature of the microwave is 55-75 ℃;
(4) aging: stopping stirring in the step (3), and obtaining a precursor Ce2(CO3)3Continuing aging in a microwave constant temperature; the aging time is 45-75 min, and the constant temperature of the microwave is 70-90 ℃;
(5) precursor powder preparation: the precursor Ce aged in the step (4) is2(CO3)3Carrying out vacuum filtration to obtain a precipitate, drying the precipitate at constant temperature, and grinding the precipitate into nano powdery particles; wherein the drying temperature is 100-140 ℃, and the drying time is 20-28 h;
(6) roasting: roasting the particles prepared in the step (5), wherein the roasting temperature is 850-950 ℃, and the roasting time is 4-6 h; cooling along with the furnace to room temperature after roasting;
(7) grinding: and (4) carrying out secondary grinding on the finished product powder prepared in the step (6) to obtain the finished product of the fluorinated cerium dioxide polishing powder.
Further, NH4The amount of F is 5-7% of the mass of the fluorine element in the final finished product; furthermore, NH4F may be replaced by a fluoride such as HF, NaF or KF.
Further, NH4HCO3And Ce (NO)3)3·6H2The molar ratio of O is 4.5:1 or more.
Further, the sections that play a role in the above process with respect to the unique set of microwave conditions are described below: under microwave condition, electromagnetic radiationTo Ce (NO)3)3Inside the solution, the heating is generated by utilizing the dielectric loss of the polar medium, and the molecular motion and collision are aggravated in a very short time, so that the temperature rise speed in the preheating process is high. After the polar medium taking part in the reaction absorbs the microwave, the activation energy of the reaction is reduced, the progress of the precipitation reaction is promoted, and the reaction efficiency is improved. The microwave condition realizes uniform heating on the molecular level, the temperature of each part in the reaction system is uniform, all crystal grains synchronously grow into uniform particles in the aging process, and a uniform dispersion system is formed; and precursor crystal grains with higher crystallinity are obtained. The above conclusions are verified in the following detailed description.
Compared with the prior art, the invention has the following beneficial effects:
1. precursor Ce of the invention2(CO3)3The precipitation reaction is carried out under the microwave condition, so that the agglomeration of precipitated particles is weakened, and the particle size of the product is refined; compared with the prior art, the method has the advantages of more convenient and simplified process flow, more environmental protection and easier obtaining of high-purity products.
2. The roasting temperature of the precursor after microwave treatment is reasonably controlled, micron-sized spherical cerium oxide particles with uniform particle size, round and smooth surface and better dispersibility can be prepared, and the defects of scratches and the like on the surface of a polished part can be reduced.
Drawings
FIG. 1 is an SEM image of a precursor cerium carbonate under water bath conditions, obtained in example 1 of the present invention.
FIG. 2 is an SEM image of a precursor cerium carbonate under microwave conditions, obtained in example 2 of the present invention.
FIG. 3 is an SEM photograph of fluorinated ceria under water bath conditions as prepared in example 1 of the present invention.
FIG. 4 is an SEM photograph of fluorinated ceria under microwave conditions prepared in example 2 of the present invention.
FIG. 5 is an X-ray diffraction (XRD) pattern of the fluorinated ceria particles obtained in examples 1 and 2 of the present invention.
FIG. 6 is a graph of the particle size of fluorinated ceria under water bath conditions as prepared in example 1 of the present invention.
FIG. 7 is a graph showing the particle size of fluorinated ceria under microwave conditions, obtained in example 2 of the present invention.
FIG. 8 is an SEM photograph of fluorinated ceria prepared according to example 3 of the present invention.
FIG. 9 is a graph showing the width R of the particle size distribution of fluorinated ceria obtained under the same conditions and other microwave intensities in example 3.
FIG. 10 is an SEM photograph of fluorinated ceria prepared according to example 4 of the present invention.
FIG. 11 is an SEM photograph of fluorinated ceria prepared according to example 5 of the present invention.
FIG. 12 is an X-ray diffraction (XRD) pattern of the fluorinated ceria particles obtained in examples 2, 4 and 5 of the present invention.
FIG. 13 is a graph of the particle size of fluorinated ceria prepared according to example 4 of the present invention.
FIG. 14 is a graph of particle size for fluorinated ceria prepared according to example 5 of the present invention.
FIG. 15 shows median particle size D of fluorinated ceria prepared in examples 2, 4, and 5 of the present invention50A line graph; three pieces of key coordinate data information are (850,8.308), (900,6.964), (1000, 43.5).
FIG. 16 is a line graph showing the width R of the particle size distribution of fluorinated ceria prepared according to examples 2, 4 and 5 of the present invention; the three pieces of key coordinate data information are (850,3.87), (900,2.10), (1000, 1.87).
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following description is provided with specific examples and drawings, but the examples are not intended to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and raw materials are commercially available, unless otherwise specified.
Example 1 (control without microwave)
A method for preparing fluorinated cerium dioxide polishing powder under the condition of water bath comprises the following steps:
(1) taking Ce (NO)3)3·6H2O、NH4HCO3And NH4Dissolving F in deionized water, and preparing 500mL of 0.0582mol/L cerium nitrate aqueous solution, 125mL of 1.047mol/L ammonium bicarbonate aqueous solution and 125mL of 0.126mol/L ammonium fluoride aqueous solution; the invention mainly researches the influence of conditions such as microwave, roasting and the like on the preparation of the polishing powder, does not research the influence of the content of the components on the polishing powder, and the use amount of the components is a preferable scheme in the research process of the invention, and the selection range of the components meets the following conditions:
A.NH4the amount of F is 5-7% of the mass of the fluorine element in the final finished product;
B.NH4HCO3and Ce (NO)3)3·6H2The molar ratio of O is more than 4.5: 1;
C.NH4f can be replaced by fluoride such as HF, NaF or KF;
the following examples all used the same concentrations and amounts;
(2) putting the cerium nitrate solution prepared in the step (1) into a water bath tank, heating the cerium nitrate solution in the water bath tank to 65 ℃, adding the ammonium fluoride solution in the step (1), and magnetically stirring the ammonium fluoride solution uniformly;
(3) adding the ammonium bicarbonate solution prepared in the step (1) into the mixed solution of cerium nitrate and ammonium fluoride obtained in the step (2), magnetically stirring, and reacting for 75min at the constant temperature of 65 ℃ in a water bath manner;
preparing a precursor through the three steps;
(4) stopping stirring after the reaction in the step (3) is finished, and aging the mixed suspension in the step (3) for 60min at a constant temperature of 80 ℃ in a water bath manner;
(5) after the aging in the step (4) is finished, taking the suspension liquid for vacuum filtration, and separating out a solid precipitate product;
(6) taking the solid precipitate product obtained in the step (5), and placing the solid precipitate product in a forced air drying oven, wherein the drying temperature is 120 ℃, and the drying time is 24 hours;
(7) taking the dried precipitate product obtained in the step (6), and grinding the precipitate product into nano powdery particles by agate;
(8) placing the powder (7) in a muffle furnace to be roasted at 900 ℃, wherein the roasting time is 5h, and cooling the powder along with the furnace to room temperature after the roasting is finished;
(9) and (4) taking the product in the step (8), and further grinding the product into powdery particles by agate to obtain the finished product of the fluorinated cerium dioxide polishing powder.
Example 2
A preparation method of fluoridized cerium dioxide polishing powder under the microwave condition comprises the following steps:
(1) taking Ce (NO)3)3·6H2O、NH4HCO3And NH4Dissolving F in deionized water, and preparing 500mL of 0.0582mol/L cerium nitrate aqueous solution, 125mL of 1.047mol/L ammonium bicarbonate aqueous solution and 125mL of 0.126mol/L ammonium fluoride aqueous solution;
(2) putting the cerium nitrate solution prepared in the step (1) into a microwave reactor for microwave heating, heating the temperature to 65 ℃, adding the ammonium fluoride solution in the step (1), and magnetically stirring the mixture uniformly;
(3) taking the ammonium bicarbonate solution prepared in the step (1), adding the mixed solution of cerium nitrate and ammonium fluoride obtained in the step (2), magnetically stirring, and reacting for 75min at a constant temperature of 65 ℃ in a microwave manner;
the microwave heating temperature in the steps (2) and (3) is the same, and a precursor is prepared through the three steps;
(4) stopping stirring after the reaction in the step (3) is finished, and aging the mixed suspension in the step (3) for 60min at a constant temperature of 80 ℃ in a microwave manner;
(5) after the aging in the step (4) is finished, taking the suspension liquid for vacuum filtration, and separating out a solid precipitate product;
(6) taking the solid precipitate product obtained in the step (5), and placing the solid precipitate product in a forced air drying oven, wherein the drying temperature is 120 ℃, and the drying time is 24 hours;
(7) taking the dried precipitate product obtained in the step (6), and grinding the precipitate product into nano powdery particles by agate;
(8) placing the powder (7) in a muffle furnace to be roasted at 900 ℃, wherein the roasting time is 5h, and cooling the powder along with the furnace to room temperature after the roasting is finished;
(9) and (4) taking the product in the step (8), and further grinding the product into powdery particles by agate to obtain the finished product of the fluorinated cerium dioxide polishing powder.
Examples 1, 2 were analyzed in comparison as follows:
(1) fig. 1 is an SEM image of a precursor cerium carbonate under water bath conditions obtained in example 1, and fig. 2 is an SEM image of a precursor cerium carbonate under microwave conditions obtained in example 2; as can be seen by comparing two SEM images, the cerium carbonate particles prepared under the microwave condition are more round and have better particle dispersibility.
(2) FIG. 3 is a SEM photograph of the fluorinated ceria under the water bath condition obtained in example 1, and FIG. 4 is a SEM photograph of the fluorinated ceria under the microwave condition obtained in example 2; the comparison shows that the cerium dioxide particles prepared under the water bath condition have large-scale agglomeration, while the cerium dioxide particles prepared under the microwave condition have better dispersibility, which shows that the microwave condition has obvious inhibition effect on the agglomeration of the polishing powder particles; and the microwave condition can refine the grain diameter of the polishing powder.
(3) As shown in FIG. 5, which is an X-ray diffraction (XRD) pattern of the fluorinated cerium oxide particles obtained in examples 1 and 2, it can be seen that the characteristic peak positions of the XRD profiles were the same as those of CeO under different reaction conditions2The standard card PDF #43-1002 is consistent, which shows that the product still keeps the cubic fluorite crystal structure under the microwave reaction condition; the intensity of X-ray diffraction peak is stronger under the microwave condition, which shows that the microwave improves the crystallinity of the product.
(4) FIG. 6 is a graph showing the particle size of the fluorinated ceria under the water bath condition obtained in example 1, and FIG. 7 is a graph showing the particle size of the fluorinated ceria under the microwave condition obtained in example 2; as can be seen from the comparison of the two figures, the particle size distribution of the cerium dioxide particles prepared under the water bath condition is extremely uneven, and double peaks appear; the cerium dioxide particles prepared under the microwave condition have narrow and uniform particle size distribution; it can be seen that the microwave reaction conditions act to homogenize the particle size.
Example 3
A preparation method of fluoridized cerium dioxide polishing powder under the microwave condition comprises the following steps:
(1) taking Ce (NO)3)3·6H2O、NH4HCO3And NH4Dissolving F in deionized water, and preparing 500mL of 0.0582mol/L cerium nitrate aqueous solution, 125mL of 1.047mol/L ammonium bicarbonate aqueous solution and 125mL of 0.126mol/L ammonium fluoride aqueous solution;
(2) putting the cerium nitrate solution prepared in the step (1) into a microwave reactor for microwave heating, heating the temperature to 45 ℃, adding the ammonium fluoride solution in the step (1), and magnetically stirring the mixture uniformly;
(3) taking the ammonium bicarbonate solution prepared in the step (1), adding the mixed solution of cerium nitrate and ammonium fluoride obtained in the step (2), magnetically stirring, and reacting for 75min at a constant temperature of 45 ℃ in a microwave manner;
the microwave heating temperature in the steps (2) and (3) is the same, and a precursor is prepared through the three steps;
(4) stopping stirring after the reaction in the step (3) is finished, and aging the mixed suspension in the step (3) for 60min at a constant temperature of 60 ℃ in a microwave manner;
(5) and (4) after the aging is finished, taking the suspension, carrying out vacuum filtration, and separating out a solid precipitate product.
(6) Taking the solid precipitate product obtained in the step (5), and placing the solid precipitate product in a forced air drying oven, wherein the drying temperature is 120 ℃, and the drying time is 24 hours;
(8) and (3) taking the powder (7), placing the powder in a muffle furnace, roasting at 900 ℃ for 5 hours, and cooling the powder along with the furnace to room temperature after roasting is finished.
(9) And (4) taking the product in the step (8), and further grinding the product into powdery particles by agate to obtain the finished product of the fluorinated cerium dioxide polishing powder.
Examples 2, 3 were analyzed in comparison as follows:
example 3 is mainly used for studying the influence of microwaves with different intensities on the preparation performance of polishing powder, and compared with example 2, the variables are different microwave temperatures in different steps, specifically, in example 2, the microwave temperatures in steps (2) and (3) are 65 ℃, and the microwave temperature in step (4) is 80 ℃; in the embodiment 3, the microwave temperature in the steps (2) and (3) is 45 ℃, and the microwave temperature in the step (4) is 60 ℃;
as shown in fig. 8, which is an SEM image of the fluorinated ceria obtained in example 3, it can be seen from comparison with fig. 4 that the product particles obtained under the reaction condition of weak microwave intensity have non-uniform particle size and some particles are agglomerated, and compared with fig. 3, the case is better than that without microwave; this fully explains that the intensity of the microwave is an important factor to achieve a good effect;
therefore, the invention also focuses on the research of the precipitation reaction under different microwave temperature conditions of 50 ℃, 55 ℃, 65 ℃, 75 ℃ and 80 ℃, namely, the experimental research is carried out by changing the microwave temperatures of the steps (2) and (3) in the embodiment 3 into 50 ℃, 55 ℃, 65 ℃, 75 ℃ and 80 ℃; correspondingly, the microwave temperatures during the aging process of the step (4) in example 3 were changed to 65 ℃, 70 ℃, 80 ℃, 90 ℃ and 95 ℃; wherein SEM pictures of the fluorinated cerium dioxide powder particles prepared at 50 ℃ and 80 ℃ precipitation reaction microwave temperatures are similar to SEM pictures at 45 ℃ (FIG. 8), product particles are locally agglomerated, and dispersibility at 55 ℃, 65 ℃ and 75 ℃ is good; FIG. 9 is a graph showing the distribution of the distribution width R of the fluorinated ceria particles at different precipitation microwave reaction temperatures, wherein it can be seen from the distribution of the R lines that the distribution width R of the product particles is kept at a low level by the corresponding microwave radiation intensity when the precipitation reaction temperature is 55-75 ℃.
Example 4
A method for preparing a fluorinated ceria polishing powder under microwave conditions, the steps are the same as example 2, except that the firing temperature is 850 ℃.
Example 5
A method for preparing a fluorinated ceria polishing powder under microwave conditions, the steps are the same as example 2, except that the firing temperature is 1000 ℃.
Examples 2, 4, 5 were analyzed in comparison as follows:
examples 2, 4 and 5 were mainly studied to examine the influence of the calcination temperature on the performance of the polishing powder;
(1) as shown in FIGS. 10 and 11, which are SEM images of the fluorinated ceria prepared in examples 4 and 5, respectively, and as compared with FIG. 4, it can be seen that the particle size of the product particles is increased with the increase of the calcination temperature; when the firing temperature is low (850 ℃), the polishing powder particles are locally agglomerated.
(2) As shown in FIG. 12, which is an X-ray diffraction (XRD) pattern of the fluorinated cerium oxide particles obtained in examples 2, 4 and 5, when the calcination temperature is 850 to 900 deg.C, the intensity of the X-ray diffraction peak of the product is strong, indicating that the crystallinity of cerium oxide is good.
(3) As shown in FIGS. 13 and 14, which are particle size diagrams of the fluorinated ceria prepared in examples 4 and 5, respectively, and a comparison analysis with FIG. 7 shows that the particle size distribution of the product is relatively uniform when the calcination temperature is 900-1000 ℃.
(4) FIG. 15 shows the median particle diameter D of the fluorinated ceria prepared in examples 2, 4 and 550A line drawing shows that when the roasting temperature is 850-900 ℃, the median particle diameter D of the product50All keep a small level; and as the roasting temperature is further increased, the median particle diameter D50And increases sharply.
(5) As shown in FIG. 16, which is a line graph showing the particle size distribution width R of the fluorinated ceria prepared in examples 2, 4, and 5, the particle size distribution width R sharply decreases with increasing temperature at low temperature, and the particle size distribution width R of the product is maintained at a low level when the firing temperature is 900 to 1000 ℃.
In conclusion, the precursor cerium carbonate particles generated under the microwave condition are roasted at a proper temperature of 850-950 ℃, so that the fluorinated cerium dioxide polishing powder with high crystallinity, small particle size, uniform particle size distribution and good dispersibility can be prepared.
Summary of the invention
According to the method, the following core conditions are controlled to realize that the cerium dioxide fluoride polishing powder maintains the crystal structure of cubic fluorite, and the median particle size (6.964-8.308 mu m), the particle size distribution width (1.87-2.10) and the like of particles are improved; the prepared particles have higher crystallinity, are more mellow and have better dispersibility.
(1) In the steps (2) and (3), microwave regulation is involved twice in the preparation of the precursor;
(2) regulating and controlling by microwave in the aging process;
(3) the roasting temperature is strictly controlled.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. This need not be, nor should it be exhaustive of all embodiments. Such modifications and improvements are within the scope of the invention as defined in the claims and their equivalents.
Claims (6)
1. A preparation method of fluorinated cerium dioxide polishing powder under microwave condition is characterized by comprising the following steps:
(1) taking Ce (NO)3)3·6H2O、NH4HCO3And NH4F are respectively dissolved in deionized water to prepare aqueous solution; NH (NH)4The amount of F is 5-7% of the mass of the fluorine element in the final finished product; NH (NH)4HCO3And Ce (NO)3)3·6H2The molar ratio of O is more than 4.5: 1;
(2) microwave preheating: taking Ce (NO)3)3·6H2Preheating an O aqueous solution to 55-75 ℃ in a microwave mode; taking NH4F aqueous solution to Ce (NO)3)3·6H2Stirring the solution O uniformly;
(3) precipitation reaction: taking NH4HCO3Adding the aqueous solution into the mixed solution prepared in the step (2); then, under the condition of continuous stirring, the precursor Ce is generated by constant temperature reaction in a microwave mode2(CO3)3(ii) a The constant temperature of the microwave is 55-75 ℃;
(4) aging: stopping stirring in the step (3), and obtaining a precursor Ce2(CO3)3Continuing aging in a microwave constant temperature; the constant temperature of the microwave is 70-90 ℃;
(5) precursor powder preparation: the precursor Ce aged in the step (4) is2(CO3)3To carry outVacuum filtering to obtain precipitate, drying the precipitate at constant temperature, and grinding into nanometer powder particles;
(6) roasting: roasting the particles prepared in the step (5) at the roasting temperature of 850-950 ℃; cooling along with the furnace to room temperature after roasting;
(7) grinding: and (4) carrying out secondary grinding on the finished product powder prepared in the step (6) to obtain the finished product of the fluorinated cerium dioxide polishing powder.
2. The method of claim 1, wherein the step of preparing the fluorinated ceria polishing powder under microwave conditions comprises: NH (NH)4F may be replaced by HF or NaF or KF.
3. The method of claim 1, wherein the step of preparing the fluorinated ceria polishing powder under microwave conditions comprises: and (4) carrying out constant temperature reaction for 60-90 min in a microwave mode in the step (3) to generate a precursor.
4. The method of claim 1, wherein the step of preparing the fluorinated ceria polishing powder under microwave conditions comprises: the aging time in the step (4) is 45-75 min.
5. The method of claim 1, wherein the step of preparing the fluorinated ceria polishing powder under microwave conditions comprises: in the step (5), the drying temperature is 100-140 ℃, and the drying time is 20-28 h.
6. The method of claim 1, wherein the step of preparing the fluorinated ceria polishing powder under microwave conditions comprises: the roasting time in the step (6) is 4-6 h.
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| CN113969108B (en) * | 2021-11-18 | 2023-04-25 | 东北大学 | Method for preparing polishing solution for optical glass by taking cerium concentrate as raw material |
| CN114394578A (en) * | 2021-12-06 | 2022-04-26 | 武汉科技大学 | Vanadium nitride precursor and preparation method thereof |
| CN115449345B (en) * | 2022-08-29 | 2023-08-22 | 内蒙古科技大学 | Preparation method of mesoporous cerium oxide coated polystyrene nano-composite abrasive under microwave condition |
| CN115448354B (en) * | 2022-09-16 | 2023-10-31 | 包头稀土研究院 | Cerium oxide particles and method for preparing same |
| CN115403064B (en) * | 2022-09-20 | 2023-10-13 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
| CN115785818B (en) * | 2022-11-10 | 2023-06-20 | 湖北五方光电股份有限公司 | Polishing solution and preparation method and application thereof |
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