CN115259205B - Preparation method and application of nano cerium oxide - Google Patents

Preparation method and application of nano cerium oxide Download PDF

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CN115259205B
CN115259205B CN202211028207.0A CN202211028207A CN115259205B CN 115259205 B CN115259205 B CN 115259205B CN 202211028207 A CN202211028207 A CN 202211028207A CN 115259205 B CN115259205 B CN 115259205B
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cerium
cerium oxide
surfactant
nano cerium
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CN115259205A (en
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徐艳
侯晓刚
朱生能
谢小明
施本义
王卫军
陈玉娴
王佳蕊
施辉
曾能
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Lanzhou Lanshi Zhongke Nano Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224—Oxides or hydroxides of lanthanides
    • C01F17/235—Cerium oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/10—Preparation or treatment, e.g. separation or purification
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention belongs to the technical field of nano materials, and discloses a preparation method and application of nano cerium oxide. The preparation method comprises the following steps: feeding cerium salt solution, precipitant and surfactant into a multiphase interface reactor in parallel flow, and reacting in a stirring state; then aging, centrifuging and washing the slurry obtained by the reaction to obtain a nano cerium carbonate precursor; roasting the nano cerium carbonate precursor to obtain; ce in solution 3+ The molar concentration of (2) is 0.5-1.8mol/L; ce in cerium salt solution 3+ The molar concentration ratio of the surfactant to the precipitant is 1: (1-2.0): (0.3% -3%). The cerium dioxide prepared by the invention is sphere-like, has controllable morphology and particle size, good dispersibility and good product batch stability. The polishing powder can be used for improving polishing efficiency and polishing quality. The preparation method has the advantages of short reaction time, high efficiency, good repeatability, simple process and easy industrialization.

Description

Preparation method and application of nano cerium oxide
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method and application of nano cerium oxide.
Background
Cerium oxide (CeO) 2 ) As polishing powder, the polishing powder has high polishing rate and rough surface to be polishedThe polishing agent has the advantages of smaller degree and surface microscopic waviness, weaker damage to the polished surface and the like, and therefore, the polishing agent has wide application in the polishing of optical glass, very large scale integrated circuits, monocrystalline silicon wafers and semiconductor substrate materials. Traditional CeO 2 The polishing powder still has great challenges and limitations in polishing selectivity, surface precision, slurry stability and the like, so the nano-scale CeO is used 2 As a polishing material, there is a necessary trend.
The existing preparation methods of cerium oxide mainly comprise a precipitation method, a hydrothermal method, a sol-gel method and the like. Yang Rong cerium oxide nano-sheets are prepared by adopting a precipitation method by taking cerium nitrate and sodium hydroxide/potassium hydroxide as raw materials, wherein the equivalent diameter of the cerium oxide nano-sheets is 0.15-1.2 mu m, and noble metal catalysts can be loaded on the cerium oxide nano-sheets to improve the catalytic efficiency, but the method requires non-oxidizing gas for atmosphere protection during precipitation reaction, so that the process complexity is increased. Tian Zhimin and the like take cerium nitrate and sodium hydroxide as raw materials, the nano cerium oxide is prepared by a two-step hydrothermal method, and the nano cerium oxide has good biological safety when being used as an ultraviolet protective agent, but the reaction conditions are harsh, a plurality of hydrothermal reactions are often required, the temperature is 100-180 ℃, the high-temperature and high-pressure reaction lasts for more than 20 hours, and the products are required to be centrifugally separated at high speed after the reaction, so that the industrial production is difficult to realize.
Generally, the existing preparation method of the cerium oxide has a relatively complex process, and the prepared cerium oxide has irregular shapes such as a flake shape or a plate shape or nonuniform particle size. When cerium oxide with irregular shape, non-uniform shape or large grain size is used as polishing powder, the polishing efficiency is low, and serious scratches and poor flatness can be generated on the surface of a polished workpiece, so that the quality of the polished workpiece is affected.
Therefore, it is needed to provide a preparation method which is simple in process, mild in condition and easy to industrialize, and can prepare nano cerium oxide with similar spheres and uniform particle size.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a preparation method and application of nano cerium oxide, and the preparation method has simple process, mild condition and easy industrialization; and can prepare the nano cerium dioxide with similar sphere shape and uniform particle size; the polishing powder is used as polishing powder, the polishing efficiency is high, and the workpiece flatness after polishing is high.
The first aspect of the invention provides a preparation method of nano cerium oxide.
Specifically, the preparation method of the nano cerium oxide comprises the following steps:
feeding cerium salt solution, precipitant and surfactant into a multiphase interface reactor in parallel flow, and reacting in a stirring state; then aging, centrifuging and washing the slurry obtained by the reaction to obtain a nano cerium carbonate precursor; roasting the nano cerium carbonate precursor to obtain nano cerium oxide;
ce in the cerium salt solution 3+ The molar concentration of (2) is 0.5-1.8mol/L;
ce in the cerium salt solution 3+ The molar concentration ratio of the surfactant to the precipitant is 1: (1-2.0): (0.3% -3%).
Preferably, the precipitant is at least one selected from sodium carbonate solution, sodium hydroxide solution, sodium bicarbonate solution.
Preferably, the surfactant is at least one selected from polyethylene glycol solution, cetyltrimethylammonium bromide solution, sodium oleate solution and citric acid solution.
Preferably, ce in the cerium salt solution 3+ The molar concentration of (C) is 0.5-1.75mol/L.
Preferably, ce in the cerium salt solution 3+ The molar concentration ratio of the surfactant to the precipitant is 1: (1-1.5): (0.3% -3%).
Preferably, the reaction raw material co-current fed with the cerium salt solution, the precipitant, and the surfactant further comprises a dispersant.
Preferably, the dispersant is polyvinylpyrrolidone.
Preferably, the stirring speed in the stirring process is 1000-5000rpm; further preferably, the rotational speed of stirring during the stirring is 2500-4000rpm.
Preferably, the flow rate of the cerium salt solution, the precipitator and the surfactant which are parallelly fed into the multiphase interface reactor is 100-500mL/min respectively; further preferably, the flow rates of the cerium salt solution, the precipitator and the surfactant which are fed into the multiphase interface reactor in parallel flow are respectively 250-400mL/min.
Preferably, the temperature of the reaction is 10-50 ℃; further preferably, the temperature of the reaction is 15-40 ℃.
Preferably, the aging time is 1 to 4 hours.
Preferably, the roasting process is to heat the nano cerium carbonate precursor from room temperature (5-40 ℃) to 450-750 ℃ at a heating rate of 0.5-5 ℃/min, and then keeping for 1-3 hours; further preferably, the roasting process is to raise the temperature of the nano cerium carbonate precursor from room temperature (5-40 ℃) to 500-750 ℃ at a heating rate of 1-3 ℃/min, and then maintain for 1-2 hours.
In a second aspect, the present invention provides a nano-ceria.
In particular to nano cerium oxide which is spherical and has the particle size of 10-60nm.
Further preferably, the particle size of the nano cerium oxide is 20-50nm.
In a third aspect, the present invention provides a polishing powder.
Specifically, the polishing powder comprises the nano cerium oxide.
The multiphase interface reactor has the advantages of good product batch stability, high production efficiency and the like. However, in the preparation of nano cerium oxide, the morphology of the nano cerium oxide is difficult to control by utilizing a multiphase interface reactor, and irregular cerium oxide with non-uniform particle size is extremely easy to generate. The invention strictly controls Ce in cerium salt solution 3+ The molar concentration ratio of the material to the precipitant and the surfactant, and the selection of the special surfactant can lead the material to form a rich and fine bubble liquid film when reacting in the microreactor, micro-area precipitation is carried out in the bubble liquid film, thus preventing the growth and agglomeration of particles,so that the prepared precursor is nano particles; in the subsequent roasting process, the agglomeration and growth of particles can be further reduced by controlling the roasting temperature, so that the finally prepared nano cerium oxide is spherical-like, and has uniform particle size distribution and good dispersibility.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention strictly controls Ce in cerium salt solution 3+ The molar concentration ratio of the nano cerium oxide to the precipitant and the surfactant, and selecting a special surfactant, and preparing the nano cerium oxide by adopting a multiphase interface reactor. The cerium dioxide prepared by the method is spherical, and has the advantages of controllable morphology and particle size, good dispersibility, good product batch stability and the like. The nano cerium dioxide prepared by the method is used as polishing powder, and can improve polishing efficiency and polishing quality.
(2) The preparation method provided by the invention has the advantages of short reaction time, high efficiency, good repeatability, simple process and easiness in industrialization.
Drawings
FIG. 1 is an XRD pattern of a nano cerium carbonate precursor prepared in example 1;
FIG. 2 is an XRD pattern of the nano cerium oxide prepared in example 1;
FIG. 3 is an SEM image of the nano-ceria prepared in example 1;
FIG. 4 is an SEM image of cerium oxide obtained in comparative example 1;
FIG. 5 is an SEM image of cerium oxide obtained in comparative example 2;
FIG. 6 is an SEM image of cerium oxide obtained in comparative example 3;
FIG. 7 is an SEM image of cerium oxide obtained in comparative example 3.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The multiphase interfacial reactor used in the following examples or comparative examples was obtained according to International publication No. WO 2021/2175550 A1. The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
A method for preparing nano cerium oxide, which comprises the following steps:
(1) Preparing a sodium carbonate solution with the concentration of 1.75mol/L, a cerium chloride solution with the concentration of 1.75mol/L, a surfactant solution with the concentration of 0.006mol/L (the surfactant in the embodiment is Cetyl Trimethyl Ammonium Bromide (CTAB)), and a polyvinylpyrrolidone solution with the concentration of 0.00014mol/L for later use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1:0.34％。
(2) And (3) conveying the four solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for aging, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 600 ℃, keeping the temperature for 2 hours at a heating rate of 2 ℃/min, cooling to room temperature after roasting is finished, and taking out to obtain spherical nano cerium oxide, wherein the yield of the nano cerium oxide is 99.5% and the purity is 99.9% through calculation and test.
The XRD pattern of the nano cerium carbonate prepared in the embodiment is shown in figure 1, and the diffraction peak of the XRD pattern is identical to the standard spectrum PDF#30-0295 of cerium carbonate hexahydrate, and no other impurity peak exists, so that the pure-phase nano cerium carbonate is prepared. The appearance of the nano cerium oxide prepared in the embodiment is light yellow powder, the XRD spectrum is shown in figure 2, and diffraction peaks of the XRD spectrum are well matched with the standard spectrum PDF#34-0394 of the cerium oxide, which shows that the pure-phase nano cerium oxide with good crystallinity is prepared. Microscopic morphology analysis was performed on the nano-ceria by using a scanning electron microscope, and SEM images are shown in fig. 3, in which a is an SEM image at a scale of 20nm and b is an SEM image at a scale of 100nm in fig. 3. As can be seen from FIG. 3 a, the nano cerium oxide is spherical, and the particle size is about 20 nm; from fig. 3 b, it can be seen that the nano cerium oxide has a uniform particle size distribution and good dispersibility.
Example 2
A method for preparing nano cerium oxide, which comprises the following steps:
(1) Preparing a sodium carbonate solution with the concentration of 1.0mol/L, a cerium chloride solution with the concentration of 0.8mol/L and a surfactant solution with the concentration of 0.0178mol/L (the surfactant in the embodiment is sodium oleate) for later use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1.25:2.23％。
(2) And (3) conveying the three solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for ageing, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 750 ℃, preserving heat for 2 hours, heating at a rate of 2 ℃/min, cooling to room temperature after roasting, and taking out to obtain the light yellow spherical nano cerium dioxide with the particle size of about 30nm. The yield of the nano cerium oxide is 99.0% and the purity is 99.8% through calculation and test.
Example 3
A method for preparing nano cerium oxide, which comprises the following steps:
(1) Preparing a sodium carbonate solution with the concentration of 1.75mol/L, a cerium chloride solution with the concentration of 1.16mol/L and a surfactant solution with the concentration of 0.010mol/L (the surfactant is polyethylene glycol in the embodiment) for later use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1.5:0.86％。
(2) And (3) conveying the three solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3500rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for ageing, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 750 ℃, preserving heat for 2 hours, heating at a rate of 2 ℃/min, cooling to room temperature after roasting, and taking out to obtain the light yellow spherical nano cerium dioxide with the particle size of about 50nm. The yield of the nano cerium oxide is 98.5% and the purity is 99.6% through calculation and test.
Comparative example 1
A method for preparing cerium oxide, comprising the steps of:
(1) A sodium carbonate solution having a concentration of 1.75mol/L, a cerium chloride solution having a concentration of 0.58mol/L, and a surfactant solution having a concentration of 0.002mol/L (the surfactant in this example is cetyltrimethylammonium bromide (CTAB)), a polyvinylpyrrolidone solution having a concentration of 0.00014mol/L were prepared for use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:3.02:0.34％。
(2) And (3) conveying the four solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for aging, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 600 ℃, keeping the temperature for 2 hours at a heating rate of 2 ℃/min, cooling to room temperature after roasting is finished, and taking out to obtain cerium dioxide, wherein the yield of the cerium dioxide is 97.0% and the purity is 98.0% through calculation and test.
Microscopic morphology analysis of ceria was performed using a scanning electron microscope, and SEM images of ceria prepared in this comparative example are shown in fig. 4, in which a is an SEM image at a scale of 4 μm and b is an SEM image at a scale of 5 μm in fig. 4. As can be seen from FIG. 4, the cerium oxide particles prepared in this comparative example have a particle diameter of more than 1 μm and are not uniform in particle size and irregular in morphology. This may be due to the relatively high concentration of the precipitant sodium carbonate, which makes the local concentration too high.
Comparative example 2
A method for preparing cerium oxide, comprising the steps of:
(1) Preparing a sodium carbonate solution with the concentration of 1.75mol/L, a cerium chloride solution with the concentration of 1.75mol/L and a surfactant solution with the concentration of 0.006mol/L (the surfactant in the embodiment is sodium dodecyl benzene sulfonate) and a polyvinylpyrrolidone solution with the concentration of 0.00014mol/L for later use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1:0.34％。
(2) And (3) conveying the four solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for aging, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 600 ℃, keeping the temperature for 2 hours at a heating rate of 2 ℃/min, cooling to room temperature after roasting is finished, and taking out to obtain spherical nano cerium oxide, wherein the yield of the nano cerium oxide is 97.5% and the purity is 98.5% through calculation and test.
Microscopic morphology analysis was performed on ceria using a scanning electron microscope, and an SEM image of the ceria prepared in this comparative example is shown in fig. 5. As can be seen from fig. 5, the cerium oxide prepared in this comparative example has a regular morphology and a uniform size, the size of the cerium oxide in the form of a sheet is several micrometers, and the cerium oxide in the form of a sheet is used as polishing powder, which causes scratches on the surface of a workpiece to be polished, and has a large particle size and low polishing efficiency.
Comparative example 3
A method for preparing cerium oxide, comprising the steps of:
(1) A sodium carbonate solution having a concentration of 2.0mol/L, a cerium chloride solution having a concentration of 2.0mol/L, and a surfactant solution having a concentration of 0.006mol/L (the surfactant in this example is cetyltrimethylammonium bromide (CTAB)), a polyvinylpyrrolidone solution having a concentration of 0.00014mol/L were prepared for use. In the present embodiment, cerium ions (Ce 3+ ) The molar concentration ratio of the precipitant (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1:0.3％。
(2) And (3) conveying the four solutions to a continuous multiphase interface reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for aging, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 600 ℃, keeping the temperature for 2 hours at a heating rate of 2 ℃/min, cooling to room temperature after roasting is finished, and taking out to obtain spherical nano cerium oxide, wherein the yield of the nano cerium oxide is 97.2% and the purity is 98.3% through calculation and test.
Microscopic morphology analysis was performed on ceria using a scanning electron microscope, and an SEM image of the ceria prepared in this comparative example is shown in fig. 6. As can be seen from FIG. 6, the large cerium oxide particles prepared in this comparative example have a particle size of about several microns, small particles having a particle size of 300 to 500nm, a non-uniform particle size and irregular morphology, and are used as polishing powder with low polishing efficiency and poor flatness of the surface of the workpiece being polished.
Comparative example 4
(1) A sodium carbonate solution having a concentration of 1.75mol/L, a cerium chloride solution having a concentration of 1.75mol/L, and a surfactant solution having a concentration of 0.006mol/L (the surfactant in this example is cetyltrimethylammonium bromide (CTAB)), a polyvinylpyrrolidone solution having a concentration of 0.00014mol/L were prepared for use. In the present embodiment, cerium ions (Ce 3+ ) Sinking and depositingThe molar concentration ratio of the starch agent (P) to the surfactant (S) is as follows: n (Ce) 3+ ):n(P - ):n(S)＝1:1:0.35％。
(2) And (3) conveying the four solutions to a continuous micro-reactor in parallel flow and equal volume through a metering pump, starting a stirring motor of the reactor to perform continuous synthesis reaction, wherein the flow rate of each solution is 300mL/min, and the stirring rotating speed is 3000rpm.
(3) Standing the slurry obtained in the step (2) for 2 hours for aging, centrifuging, washing and drying to obtain a nano cerium carbonate precursor, placing the nano cerium carbonate precursor into a muffle furnace for roasting at 900 ℃, keeping the temperature for 2 hours at a heating rate of 2 ℃/min, cooling to room temperature after roasting is finished, and taking out to obtain spherical nano cerium oxide, wherein the yield of the nano cerium oxide is 96.5% and the purity is 96.8% through calculation and test.
Microscopic morphology analysis was performed on ceria using a scanning electron microscope, and an SEM image of the ceria prepared in this comparative example is shown in fig. 7. As can be seen from FIG. 7, the cerium oxide particles prepared in this comparative example are severely agglomerated, and have non-uniform particle size, irregular morphology, and other impurities attached to the surface of the cerium oxide particles, and the purity is lowered; in addition, when the temperature is too high, the hardness of the cerium oxide is large, so that the application of the cerium oxide in polishing powder is limited.

Claims (6)

1. The preparation method of the polishing powder is characterized in that the polishing powder is nano cerium oxide and comprises the following steps:
feeding cerium salt solution, precipitant and surfactant into a multiphase interface reactor in parallel flow, and reacting in a stirring state; then aging, centrifuging and washing the slurry obtained by the reaction to obtain a nano cerium carbonate precursor; roasting the nano cerium carbonate precursor, heating to 450-750 ℃, and then keeping for 1-3 hours to obtain nano cerium oxide;
ce in the cerium salt solution 3+ The molar concentration of (2) is 0.8-1.8mol/L;
ce in the cerium salt solution 3+ The molar concentration ratio of the surfactant to the precipitant is 1: (1-2.0): (0.3% -3%);
the surfactant is selected from sodium oleate solution;
the precipitant is at least one of sodium carbonate solution and sodium bicarbonate solution;
the nano cerium oxide is in a sphere-like shape, and the particle size of the nano cerium oxide is 10-60nm.
2. The method according to claim 1, wherein Ce in the cerium salt solution 3+ The molar concentration of (C) is 0.8-1.75mol/L.
3. The method according to claim 1, wherein the rotation speed of stirring during the stirring is 1000 to 5000rpm.
4. A method of preparing according to claim 3, wherein the rotational speed of stirring during the stirring is 2500-4000rpm.
5. The method according to claim 3, wherein the flow rates of the cerium salt solution, the precipitant and the surfactant which are co-currently fed into the multiphase interfacial reactor are 100-500mL/min, respectively.
6. The method according to claim 1, wherein the calcination is performed by heating the nano cerium carbonate precursor at a temperature rising rate of 0.5 to 5 ℃/min from 5 to 40 ℃.
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