CN112142088A - Method for preparing cerium dioxide polishing powder by roasting method - Google Patents

Method for preparing cerium dioxide polishing powder by roasting method Download PDF

Info

Publication number
CN112142088A
CN112142088A CN202010671309.9A CN202010671309A CN112142088A CN 112142088 A CN112142088 A CN 112142088A CN 202010671309 A CN202010671309 A CN 202010671309A CN 112142088 A CN112142088 A CN 112142088A
Authority
CN
China
Prior art keywords
putting
corundum crucible
degrees
crystal
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202010671309.9A
Other languages
Chinese (zh)
Inventor
冯平仓
梅燕
夏烨
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sichuan Ruichi Tuowi Machinery Manufacturing Co ltd
Beijing University of Technology
Original Assignee
Sichuan Ruichi Tuowi Machinery Manufacturing Co ltd
Beijing University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sichuan Ruichi Tuowi Machinery Manufacturing Co ltd, Beijing University of Technology filed Critical Sichuan Ruichi Tuowi Machinery Manufacturing Co ltd
Priority to CN202010671309.9A priority Critical patent/CN112142088A/en
Publication of CN112142088A publication Critical patent/CN112142088A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224Oxides or hydroxides of lanthanides
    • C01F17/235Cerium oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/10Preparation or treatment, e.g. separation or purification
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/60Compounds characterised by their crystallite size
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Landscapes

  • 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

A method for preparing cerium dioxide polishing powder by a roasting method belongs to the field of preparation of micron-sized crystal form and particle size controllable powder. Putting the cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 400-1050 ℃ at the heating rate of 2-10 ℃/min, then preserving the heat for 2-8 hours, and naturally cooling to room temperature to obtain the cerium dioxide polishing powder. Cerium dioxide is prepared by adopting a cerium carbonate raw material roasting method, and micron-sized cerium dioxide polishing powder with controllable crystal form and controllable particle size is prepared by changing factors such as roasting temperature, heating rate, heat preservation time and the like2Different process products of the polishing powder.

Description

Method for preparing cerium dioxide polishing powder by roasting method
One, the technical field
The invention relates to a preparation method of micron-sized powder, in particular to a method for preparing micron-sized cerium dioxide by a roasting method, specifically to a method for preparing micron-sized cerium dioxide polishing powder by roasting cerium carbonate, and belongs to the technical field of crystal form and particle size control of micron-sized powder.
Second, background Art
Cerium oxide (CeO)2) The compound is the most abundant and widely used compound in rare earth oxides, is generally light yellow or even pink to reddish brown powder, and is a difficultly soluble oxide. CeO (CeO)2The crystal belongs to a face-centered cubic system, a space group Fm3m and is CaF2The typical structure of the type eight ligand is that the three-dimensional structure is that 8 equidistant oxygen ions are arranged around a cerium ion, and 4 cerium ions are arranged around the oxygen ion, so that the coordination numbers of positive and negative ions are Ce4+:O2-8:4, and Ce4+Ion radius of
Figure BDA0002582402480000011
O2-Ion radius of
Figure BDA0002582402480000012
The sum of the two is
Figure BDA0002582402480000013
Bond length with Ce-O
Figure BDA0002582402480000014
Substantially identical, Ce and O are closely arranged.
CeO2The crystal mainly comprises a (200) crystal plane and a (111) crystal plane, wherein the (200) crystal plane spacing is far smaller than the (111) crystal plane spacing, and the longitudinal growth speed of the crystal surface is increased due to the fact that the smaller the crystal plane spacing is, the larger the attraction force between adjacent crystal grains is, so that the longitudinal growth speed of the (200) crystal plane is larger than that of the (111) crystal plane. The larger the growth rate of the crystal plane, the smaller the area of the crystal plane in the surface layer, so that CeO is generally used2The crystal surface is mostly (111) crystal plane.
Ceria is well known as a polishing abrasive, the first used to polish glass, in combination with SnO2、TiO2、Cr2O3、Al2O3、Y2O3、La2O3In the comparison of the equal abrasive materials, CeO belongs to the same category under the same conditions2The polishing rate is highest. In addition, CeO2The abrasive has moderate Mohs hardness (7.0), is lighter for scratches formed on the surface of a precision workpiece, has more excellent polishing performance, and can be widely applied to the high-tech fields of optical glass, mechanical polishing, electronic products and the like.
According to the self-limitation of the crystal, all the crystals have a tendency of spontaneously forming a closed geometric polyhedral shape for CeO2For the crystal polishing process, when CeO is used2When the crystal grains on the outermost layer of the crystal are small, the surface is more easily in a smooth spherical shape, and basically no polishing capability exists; when CeO is used2After the crystal grains are enlarged, the surfaces of the crystal grains become uneven from smooth, and edges and corners are generated on the convex parts, so that the polishing capacity of the grains is increased; when CeO is used2When the crystal grains are too large, the degree of closeness between the crystal grains becomes low, and instead, the crystal grains easily fall off during polishing, thereby reducing the polishing ability of the crystal grains. Therefore, in the actual production, the research on the preparation conditions of the cerium dioxide polishing powder and the polishing performance rule of the cerium dioxide polishing powder not only has a theoretical guidance function, but also has the practical significance of large-scale industrialization.
Third, the invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a preparation method of cerium dioxide polishing powder with simple process, controllable crystal form and grain size.
The technical scheme adopted by the invention is as follows: the preparation method of the cerium dioxide polishing powder comprises the following steps: putting the cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 400-1050 ℃ at the heating rate of 2-10 ℃/min, then preserving heat for 2-8 hours, and cooling to obtain the cerium carbonate material. The invention adopts a cerium carbonate raw material roasting method to prepare micron-sized cerium dioxide, firstly, temperature-changing roasting is carried out by controlling the temperature-rising rate, then, constant-temperature roasting is carried out by combining the control of the roasting and heat-preserving time, and micron-sized cerium dioxide polishing powder with controllable crystal form and particle size can be obtained by matching two sections of processes.
The invention adopts a cerium carbonate raw material roasting method to prepare micron-sized cerium dioxide, and provides a preparation method for obtaining micron-sized cerium dioxide polishing powder with controllable crystal form and controllable particle size by adopting different heating rates (variable temperature roasting) and different roasting heat preservation times (constant temperature roasting) within the temperature range of 400-1050 ℃.
The method for preparing the micron-sized cerium dioxide polishing powder with the controllable crystal form and the controllable particle size by using the cerium carbonate as the raw material and changing factors such as the roasting temperature, the temperature rise rate, the heat preservation time and the like has strong operability, simple roasting process and accurate control of the roasting temperature, the heat preservation time and the temperature rise rate, and can obtain the micron-sized CeO with the controllable crystal form and the controllable particle size from the cerium carbonate as the raw material2Different process products of the polishing powder.
1. A method for preparing cerium dioxide polishing powder by a roasting method is characterized by comprising the following steps: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 400-1050 ℃ at a heating rate of 2-10 ℃/min, preserving heat for 2-8h, preparing micron-sized cerium dioxide polishing powder with controllable crystal form and controllable particle size by changing one or more factors of roasting temperature, heating rate and heat preservation time, and then naturally cooling.
2. Further, putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, raising the temperature to 400 ℃ at the temperature rise rate of 2 ℃/min, preserving the temperature for 2 hours, and naturally cooling to room temperature to obtain yellow cerium dioxide polishing powder with a cubic crystal structure, wherein the crystal face 2theta of the main peak (111) is positioned at 28.542 DEG, and the lattice constant is
Figure BDA0002582402480000021
Interplanar spacing of
Figure BDA0002582402480000022
The particle size is 11.90nm, and the calculated value of the Sherle formula is 8.7393 nm.
3. Further, putting the cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 500-700 ℃ at the heating rate of 3 ℃/min, preserving heat for 3 hours, and naturally cooling to room temperature to obtain the cerium dioxide polishing powder with a light yellow, yellow-white and earthy yellow cubic crystal system structure, wherein the crystal face 2theta of the main peak (111) is 2thetaRespectively positioned at 28.557 degrees, 28.552 degrees and 28.542 degrees, and the lattice constants are respectively
Figure BDA0002582402480000023
Interplanar spacings of respectively
Figure BDA0002582402480000031
4. Further, putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 750-800 ℃ at a heating rate of 5 ℃/min, preserving heat for 4 hours, naturally cooling to room temperature to obtain the yellowish-brown and pink-earth cerium dioxide polishing powder with a cubic crystal system structure, wherein the crystal face 2theta of a main peak (111) is respectively positioned at 28.577 degrees and 28.572 degrees, and the lattice constants are respectively 28.577 degrees and 28.572 degrees
Figure BDA0002582402480000032
And
Figure BDA0002582402480000033
interplanar spacings of respectively
Figure BDA0002582402480000034
And
Figure BDA0002582402480000035
the particle sizes are respectively 30.95nm and 37.25nm, and the calculated values of the Sherle formula are respectively 38.2580nm and 48.2896 nm.
5. Further, putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 850-900 ℃ at the heating rate of 6 ℃/min, preserving the temperature for 5 hours, naturally cooling to room temperature to obtain the soil-pink cerium dioxide polishing powder with the cubic crystal system structure, wherein the crystal faces 2theta of the main peaks (111) are respectively positioned at 28.56 degrees and 28.576 degrees, and the lattice constants are respectively
Figure BDA0002582402480000036
And
Figure BDA0002582402480000037
interplanar spacings of respectively
Figure BDA0002582402480000038
And
Figure BDA0002582402480000039
the particle sizes are 52.90nm and 47.05nm respectively, and the calculated values of the Sherle formula are 60.9804nm and 67.5884nm respectively.
6. Further, putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 950-1000 ℃ at the heating rate of 8 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature to obtain the cerium dioxide polishing powder with a light pink cubic crystal structure, wherein the crystal face 2theta of a main peak (111) is respectively positioned at 28.556 degrees and 28.563 degrees, and the lattice constants are respectively 28.556 degrees and 28.563 degrees
Figure BDA00025824024800000310
And
Figure BDA00025824024800000311
interplanar spacings of respectively
Figure BDA00025824024800000312
And
Figure BDA00025824024800000313
the particle sizes are 69.02nm and 69.71nm respectively, and the calculated values of the Sherle formula are 77.9839nm and 81.9237nm respectively.
7. Further, putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, raising the temperature to 1050 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 8 hours, and naturally cooling to room temperature to obtain the ceric oxide polishing powder with a light pink cubic crystal system structure, wherein the crystal face 2theta of a main peak (111) is positioned at 28.553 DEG, and the lattice constant is
Figure BDA00025824024800000314
Interplanar spacing of
Figure BDA00025824024800000315
The particle size is 81.95nm, and the calculated value of the Sherle formula is 86.2794 nm.
Products obtained by roasting at different heating rates (variable temperature roasting) and different roasting heat preservation times (constant temperature roasting) to the temperature range of 400-1050 ℃ are respectively yellow, light yellow, yellow-white, earthy yellow, earth pink and light pink powders, and XRD proves that all the products are cerium dioxide powders with cubic crystal forms and different particle sizes.
Compared with the prior art, the preparation method of the micron-sized cerium dioxide polishing powder has the beneficial effects that: the invention provides a method for preparing cerium dioxide with controllable crystal form and grain size by different heating rates and different roasting heat preservation times. The method for preparing the micron-sized cerium dioxide polishing powder with the controllable crystal form and the controllable particle size by using the cerium carbonate as the raw material and changing factors such as the roasting temperature, the temperature rise rate, the heat preservation time and the like has strong operability, simple roasting process and accurate control of the roasting temperature, the heat preservation time and the temperature rise rate, and can obtain the micron-sized CeO with the controllable crystal form and the controllable particle size from the cerium carbonate as the raw material2Different process products of the polishing powder.
Table 1 shows the yields of cerium oxide powder obtained by calcining cerium oxide powders at 400 ℃, 500 ℃, 600 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, and shows that: the average yield of the polishing powder was 55.54%.
TABLE 1 yield of cerium oxide powder at different temperatures
Figure BDA0002582402480000041
Table 2 shows XRD crystal parameters of the main peak (111) plane of cerium oxide crystal obtained by calcination at 400 deg.C, 500 deg.C, 600 deg.C, 700 deg.C, 750 deg.C, 800 deg.C, 850 deg.C, 900 deg.C, 950 deg.C, 1000 deg.C, 1050 deg.C, including the 2theta position, main peak height, full width at half maximum, interplanar spacing (d value), peak area, particle size, etc. of the (111) plane, and the particle size calculated by Scherrer's formula was compared with the particle size read by XRD, and specific surface area (BET) values at 700 deg.C and above were measured.
Main peak- -main peak (most intense peak) around 28.6 ℃ on XRD spectrum was identified as CeO2Crystal (111)Crystal face, and along with the temperature rise, crystal grains grow gradually, and the crystal form is gradually perfected.
Lattice constant — a change in the basic structure of a crystal, and the composition and stress state in the crystal, is related to the bonding energy between atoms. Standard CeO2The crystal lattice constant was 0.5411nm (see PDF card #81-0792), as seen in Table 2: when the roasting temperature is at least 850 ℃ and above, the lattice constant value can reach or approach the standard value, which shows that the lattice distortion gradually reduces and tends to be stable along with the rise of the temperature, so that the product distortion of the roasting temperature of 850 ℃ and above is theoretically determined to be small and the crystal form is good;
interplanar spacing- -standard CeO2The interplanar spacing d of the (111) crystal face of the crystal is
Figure BDA0002582402480000042
(refer to PDF card #81-0792), as can be seen from Table 2, the interplanar spacings at the baking temperature of 400-1050 ℃ are all equal to the standard values
Figure BDA0002582402480000043
The difference is not much, and the total is slightly increased because of Ce3+The ionic radius of 0.1034nm is larger than that of Ce4+Ionic radius of 0.092nm, if Ce3+Ion solid solution into CeO2In the crystal, the increase of the value of the interplanar spacing d inevitably occurs, so that CeO can be inferred2In the crystal there is Ce3+、Ce4+Coexistence phenomena.
Specific surface area-refers to the amount of surface area of an object per unit mass. Generally, the larger the specific surface area, the more particles contained in the substance, the smaller the particle size. As can be seen in table 2: the specific surface shows a decreasing trend with increasing temperature, indicating a gradual increase in particle size, possibly associated with grain agglomeration at increasing temperature, consistent with the trend of XRD reading of particle size to be equal to the grain size calculated by the scherrer equation.
TABLE 2 XRD parameters and BET values of (111) crystal face of cerium dioxide crystal at different temperatures
Figure BDA0002582402480000051
Through the analysis of lattice constant, interplanar spacing, grain size, specific surface and the like in the above table 2, the roasting temperature is determined to be at least above 850 ℃ so as to ensure that CeO can be obtained2The polishing powder achieves the purposes of small distortion, complete crystal form and the like, and can provide theoretical basis and technical support for large-scale industrialization.
Drawings
FIG. 1 is an XRD spectrum of the powder in example 1 of the present invention.
FIG. 2 is an XRD spectrum of the powder in example 2 of the present invention.
FIG. 3 is an XRD spectrum of the powder in example 3 of the present invention.
FIG. 4 is an XRD spectrum of the powder in example 4 of the present invention.
FIG. 5 is an XRD spectrum of the powder of example 5 of the present invention.
FIG. 6 is an XRD spectrum of the powder of example 6 of the present invention.
FIG. 7 is an XRD spectrum of the powder of example 7 of the present invention.
FIG. 8 is an XRD spectrum of the powder of example 8 of the present invention.
FIG. 9 is an XRD spectrum of the powder of example 9 of the present invention.
FIG. 10 is an XRD spectrum of the powder of example 10 of the present invention.
FIG. 11 is an XRD spectrum of the powder of example 11 of the present invention.
FIG. 12 is an XRD summation spectrum of the powders of examples 1 to 11 of the present invention.
Detailed Description
Comparative example: accurately weighing 9.9-10.5g of cerium carbonate raw material, placing the cerium carbonate raw material into a 30mL corundum crucible, placing the corundum crucible into a muffle furnace, raising the temperature to 400-1050 ℃ at a heating rate of 2-10 ℃/min, then preserving the heat for 2-8 hours, naturally cooling to room temperature, taking out the cerium carbonate raw material, obtaining cerium dioxide polishing powder products with controllable particle size from the raw material cerium carbonate to micron-sized crystal form, weighing and measuring the yield of the products by using an analytical balance, analyzing the phase structure of the products by using X-ray diffraction, and confirming that the strongest peak near 28.6 ℃ on an XRD spectrogram is determined to be CeO2Crystal (111)) Crystal plane, several parameters defining the (111) crystal plane of the cerium oxide crystals.
Example 1: referring to attached figure 1, 10.041g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is raised to 400 ℃ at the temperature rise rate of 2 ℃/min, the temperature is kept for 2h, the obtained yellow powder XRD proves that the yellow powder is cubic crystal cerium dioxide, the crystal face 2theta of a main peak (111) is located at 28.542 degrees, and the lattice constant is 28.542 DEG
Figure BDA0002582402480000061
Interplanar spacing of
Figure BDA0002582402480000062
The particle size is 11.90nm, and the calculated value of the Sherle formula is 8.7393 nm.
Example 2: referring to the attached figure 2, 9.997g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 500 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 3h, the obtained light yellow powder XRD proves that the light yellow powder is cubic crystal cerium dioxide, the crystal face 2theta of a main peak (111) is located at 28.557 degrees, and the lattice constant is 28.557 degrees
Figure BDA0002582402480000071
Interplanar spacing of
Figure BDA0002582402480000072
The particle size is 11.50nm, and the calculated value of the Sherle formula is 10.1635 nm.
Example 3: referring to attached figure 3, 10.308g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is raised to 600 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 3h, the obtained yellow-white powder XRD is proved to be cubic crystal ceric oxide, the crystal face 2theta of the main peak (111) is located at 28.552 degrees, and the lattice constant is 28.552 degrees
Figure BDA0002582402480000073
Interplanar spacing of
Figure BDA0002582402480000074
The particle size is 16.35nm, and the calculated value of the Sherle formula is 14.3296 nm.
Example 4: referring to the attached figure 4, 10.020g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 700 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 3h, the obtained khaki powder XRD proves that the powder is cubic crystal cerium dioxide, the crystal face 2theta of the main peak (111) is positioned at 28.542 degrees, and the lattice constant is 28.542 degrees
Figure BDA0002582402480000075
Interplanar spacing of
Figure BDA0002582402480000076
The particle size is 23.90nm, calculated by the Sherle formula, is 27.6844 nm.
Example 5: referring to the attached figure 5, 9.988g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 750 ℃ at the temperature rising rate of 5 ℃/min, the temperature is kept for 4h, the obtained khaki powder XRD proves that the cerium dioxide is cubic crystal form cerium dioxide, the crystal face 2theta of the main peak (111) is positioned at 28.577 degrees, and the lattice constant is 28.577 DEG
Figure BDA0002582402480000077
Interplanar spacing of
Figure BDA0002582402480000078
The particle size is 30.95nm, and the calculated value of the Sherle formula is 38.2580 nm.
Example 6: referring to the attached figure 6, 10.124g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 800 ℃ at the temperature rising rate of 5 ℃/min, the temperature is kept for 4 hours, the obtained soil powder body XRD proves to be cubic crystal ceric oxide, the crystal face 2theta of the main peak (111) is located at 28.572 degrees, and the lattice constant is 28.572 degrees
Figure BDA0002582402480000079
Interplanar spacing of
Figure BDA00025824024800000710
The particle size is 37.25nm, and the calculated value of the Sherle formula is 48.2896 nm.
Example 7: referring to FIG. 7, 10.473g of cerium carbonate raw material was accurately weighed and placed in a 30mL corundum cruciblePlacing the powder into a muffle furnace, heating to 850 ℃ at a heating rate of 6 ℃/min, and keeping the temperature for 5 hours to obtain a soil powder body XRD which proves that the obtained soil powder body is cubic crystal cerium dioxide, the crystal face 2theta of a main peak (111) is positioned at 28.56 degrees, and the lattice constant is
Figure BDA00025824024800000711
Interplanar spacing of
Figure BDA00025824024800000712
The particle size is 52.90nm, calculated by the Sherle formula, is 60.9804 nm.
Example 8: referring to the attached figure 8, 10.472g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 900 ℃ at the temperature rising rate of 6 ℃/min, the temperature is kept for 5 hours, the obtained soil powder body XRD proves to be cubic crystal ceric oxide, the crystal face 2theta of the main peak (111) is located at 28.576 degrees, and the lattice constant is 28.576 degrees
Figure BDA0002582402480000081
Interplanar spacing of
Figure BDA0002582402480000082
The particle size is 47.05nm, calculated by the Sherle formula, is 67.5884 nm.
Example 9: referring to the attached figure 9, 10.112g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 950 ℃ at the temperature rising rate of 8 ℃/min, the temperature is kept for 6h, the obtained light pink powder XRD proves that the light pink powder is cubic crystal cerium dioxide, the crystal face 2theta of the main peak (111) is located at 28.556 degrees, and the lattice constant is 28.556 degrees
Figure BDA0002582402480000083
Interplanar spacing of
Figure BDA0002582402480000084
The particle size is 69.02nm, calculated by the Sherle formula, is 77.9839 nm.
Example 10: referring to the attached figure 10, 10.007g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the corundum crucible is placed into a muffle furnace, the temperature is raised to 1000 ℃ at the heating rate of 8 ℃/min, then the temperature is kept for 6h,XRD of the obtained light pink powder proves that the powder is cubic crystal cerium dioxide, the crystal face 2theta of a main peak (111) is positioned at 28.563 degrees, and the lattice constant is
Figure BDA0002582402480000085
Interplanar spacing of
Figure BDA0002582402480000086
The particle size is 69.71nm, calculated by the Sherle formula, is 81.9237 nm.
Example 11: referring to the attached figure 11, 10.094g of cerium carbonate raw material is accurately weighed and placed into a 30mL corundum crucible, the mixture is placed into a muffle furnace, the temperature is increased to 1050 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 8 hours, the obtained light pink powder XRD is proved to be cubic crystal cerium dioxide, the crystal face 2theta of the main peak (111) is located at 28.553 degrees, and the lattice constant is that
Figure BDA0002582402480000087
Interplanar spacing of
Figure BDA0002582402480000088
The particle size is 81.95nm, and the calculated value of the Sherle formula is 86.2794 nm.
Referring to the XRD addition diagram in the attached figure 12, it is seen that, from 850 ℃, the peak value of the (111) crystal face of the main peak is obviously higher than that of a calcined sample product below 850 ℃, according to the self-limiting theory of crystals, the crystal grains grow up, the number of sub-crystal grains in the crystal grains is gradually reduced, unevenness is easily generated on the surface, the polishing capacity of cerium dioxide is increased, and the condition for preparing polishing powder by the calcined powder at the temperature of 850 ℃ and above is demonstrated.
As can be seen from the above examples, the method of the present invention can prepare cubic crystal cerium dioxide, the color of the product changes with the temperature rise, and finally, the micron-sized cerium dioxide polishing powder product of 17-46um can be obtained.

Claims (7)

1. A method for preparing cerium dioxide polishing powder by a roasting method is characterized by comprising the following steps: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 400-1050 ℃ at a heating rate of 2-10 ℃/min, preserving heat for 2-8h, obtaining several prepared micron-sized cerium dioxide polishing powders with controllable crystal forms and controllable particle sizes by changing one of factors of roasting temperature, heating rate and heat preservation time, and then naturally cooling.
2. The method of claim 1, wherein: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 400 ℃ at the heating rate of 2 ℃/min, preserving heat for 2 hours, and naturally cooling to room temperature to obtain yellow cerium dioxide polishing powder with a cubic crystal structure, wherein the crystal face 2theta of a main peak (111) is positioned at 28.542 DEG, and the lattice constant is
Figure FDA0002582402470000011
Interplanar spacing of
Figure FDA0002582402470000012
The particle size is 11.90nm, and the calculated value of the Sherle formula is 8.7393 nm.
3. The method of claim 1, wherein: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 500-700 ℃ at a heating rate of 3 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain cerium dioxide polishing powder with a light yellow, yellow-white and earthy yellow cubic crystal system structure, wherein crystal faces 2theta of main peaks (111) are respectively located at 28.557 degrees, 28.552 degrees and 28.542 degrees, and lattice constants are respectively
Figure FDA0002582402470000013
Interplanar spacings of respectively
Figure FDA0002582402470000014
Figure FDA0002582402470000015
4. The method of claim 1, wherein: putting the cerium carbonate raw material into a corundum crucible, and putting the corundum crucible into a muffle furnace at the temperature of 5 ℃/minRaising the temperature to 750-800 ℃ at a speed rate, preserving the temperature for 4h, and then naturally cooling to room temperature to obtain the ceria polishing powder with earthy yellow and earthy pink cubic crystal system structures, wherein the crystal face 2theta of the main peak (111) is respectively positioned at 28.577 degrees and 28.572 degrees, and the lattice constants are respectively
Figure FDA0002582402470000016
And
Figure FDA0002582402470000017
interplanar spacings of respectively
Figure FDA0002582402470000018
And
Figure FDA0002582402470000019
the particle sizes are respectively 30.95nm and 37.25nm, and the calculated values of the Sherle formula are respectively 38.2580nm and 48.2896 nm.
5. The method of claim 1, wherein: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 850-900 ℃ at the heating rate of 6 ℃/min, preserving heat for 5 hours, and naturally cooling to room temperature to obtain the ceria polishing powder with a pink cubic crystal system structure, wherein the crystal faces 2theta of main peaks (111) are respectively positioned at 28.56 degrees and 28.576 degrees, and the lattice constants are respectively
Figure FDA0002582402470000021
And
Figure FDA0002582402470000022
interplanar spacings of respectively
Figure FDA0002582402470000023
And
Figure FDA0002582402470000024
the particle sizes are 52.90nm and 47.05nm respectively, and the calculated values of the Sherle formula are 60.9804nm and 67.5884nm respectivelynm。
6. The method of claim 1, wherein: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 950-1000 ℃ at the heating rate of 8 ℃/min, preserving heat for 6 hours, and naturally cooling to room temperature to obtain the ceric oxide polishing powder with a light pink cubic crystal system structure, wherein the crystal face 2theta of a main peak (111) is respectively positioned at 28.556 degrees and 28.563 degrees, and the lattice constants are respectively 28.556 degrees and 28.563 degrees
Figure FDA0002582402470000025
And
Figure FDA0002582402470000026
interplanar spacings of respectively
Figure FDA0002582402470000027
And
Figure FDA0002582402470000028
the particle sizes are 69.02nm and 69.71nm respectively, and the calculated values of the Sherle formula are 77.9839nm and 81.9237nm respectively.
7. The method of claim 1, wherein: putting a cerium carbonate raw material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 1050 ℃ at a heating rate of 10 ℃/min, preserving heat for 8 hours, and naturally cooling to room temperature to obtain the ceric oxide polishing powder with a light pink cubic crystal system structure, wherein the crystal face 2theta of a main peak (111) is positioned at 28.553 DEG, and the lattice constant is
Figure FDA0002582402470000029
Interplanar spacing of
Figure FDA00025824024700000210
The particle size is 81.95nm, and the calculated value of the Sherle formula is 86.2794 nm.
CN202010671309.9A 2020-07-13 2020-07-13 Method for preparing cerium dioxide polishing powder by roasting method Withdrawn CN112142088A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010671309.9A CN112142088A (en) 2020-07-13 2020-07-13 Method for preparing cerium dioxide polishing powder by roasting method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010671309.9A CN112142088A (en) 2020-07-13 2020-07-13 Method for preparing cerium dioxide polishing powder by roasting method

Publications (1)

Publication Number Publication Date
CN112142088A true CN112142088A (en) 2020-12-29

Family

ID=73888785

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010671309.9A Withdrawn CN112142088A (en) 2020-07-13 2020-07-13 Method for preparing cerium dioxide polishing powder by roasting method

Country Status (1)

Country Link
CN (1) CN112142088A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113772713A (en) * 2021-08-26 2021-12-10 北京工业大学 Roasting preparation method of rare earth fluoride lanthanum cerium polishing powder
CN113845847A (en) * 2021-08-02 2021-12-28 北京工业大学 Method for preparing lanthanum-cerium solid solution polishing powder with controllable particle size by roasting method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102559066A (en) * 2011-12-23 2012-07-11 河南省联合磨料磨具有限公司 Production method of ceria powder polishing size
CN103571334A (en) * 2013-11-05 2014-02-12 上海华明高纳稀土新材料有限公司 Cerium oxide polishing powder and preparation method thereof
CN104261454A (en) * 2014-08-22 2015-01-07 郑州市甫明新材料有限公司 A producing process for preparing cerium oxide polishing powder
CN105712399A (en) * 2016-01-20 2016-06-29 淄博晶泽光学材料科技有限公司 Method for preparing zirconium dioxide polishing powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102559066A (en) * 2011-12-23 2012-07-11 河南省联合磨料磨具有限公司 Production method of ceria powder polishing size
CN103571334A (en) * 2013-11-05 2014-02-12 上海华明高纳稀土新材料有限公司 Cerium oxide polishing powder and preparation method thereof
CN104261454A (en) * 2014-08-22 2015-01-07 郑州市甫明新材料有限公司 A producing process for preparing cerium oxide polishing powder
CN105712399A (en) * 2016-01-20 2016-06-29 淄博晶泽光学材料科技有限公司 Method for preparing zirconium dioxide polishing powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杨国胜等: "无氟铈基稀土抛光粉制备过程的研究", 《稀土》 *
杨来东: "焙烧温度对铈基稀土抛光粉抛光性能影响的研究", 《陇东学院学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113845847A (en) * 2021-08-02 2021-12-28 北京工业大学 Method for preparing lanthanum-cerium solid solution polishing powder with controllable particle size by roasting method
CN113772713A (en) * 2021-08-26 2021-12-10 北京工业大学 Roasting preparation method of rare earth fluoride lanthanum cerium polishing powder

Similar Documents

Publication Publication Date Title
CN112142088A (en) Method for preparing cerium dioxide polishing powder by roasting method
CN110342556A (en) A kind of low sodium high activity special type α-Al2O3The preparation method of micro mist
Wang Growth and characterization of spinel single crystals for substrate use in integrated electronics
US5304226A (en) Abrasive grain and manufacture for the same
CN111533556B (en) Preparation method of grain-oriented strontium sodium niobate leadless ferroelectric ceramic
CN109678506A (en) A kind of preparation method of erbium oxide crystalline ceramics
US4350559A (en) Process for the manufacture of polycrystalline garnet and corresponding monocrystal
US2360841A (en) Aluminous material
KR101141816B1 (en) Method for producing ?-alumina powder
CN115745573A (en) Preparation method of fine-grain IZO target material
CN113353973B (en) Preparation method of calcium-doped barium titanate powder
CN114032034A (en) CeO for chemical mechanical polishing2Method for producing abrasive particles and use thereof
EP0409991B1 (en) Abrasive grain and method of producing same
CN113845847A (en) Method for preparing lanthanum-cerium solid solution polishing powder with controllable particle size by roasting method
CN108130595A (en) A kind of method that control climate prepares alumina whisker
JP2000026840A (en) Abrasive
JP2013091585A (en) Zirconia powder, method for producing the same, and its application
CN114988469A (en) Preparation of piezoelectric material Pb (Zr, Ti) O 3 Method for single-phase fine-grained powder
JP4178224B2 (en) Method for producing yttrium oxide powder
CN113353974A (en) Method for preparing barium titanate powder by solid-phase synthesis
CN113772713A (en) Roasting preparation method of rare earth fluoride lanthanum cerium polishing powder
Mashkovtcev et al. Synthesis and luminescence properties of yttrium oxide ceramics with a variable europium content
CN116217216B (en) Lanthanum ferrite ceramic powder with variable solar absorptivity, and preparation method and application thereof
CN115140754B (en) Preparation method of low-temperature sintered alumina ceramic abrasive
CN115710008B (en) Modified rare earth oxide and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20201229

WW01 Invention patent application withdrawn after publication