CN101550318B - Ce3+ -contained rare-earth polishing powder and preparation method thereof - Google Patents
Ce3+ -contained rare-earth polishing powder and preparation method thereof Download PDFInfo
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- CN101550318B CN101550318B CN2008101033793A CN200810103379A CN101550318B CN 101550318 B CN101550318 B CN 101550318B CN 2008101033793 A CN2008101033793 A CN 2008101033793A CN 200810103379 A CN200810103379 A CN 200810103379A CN 101550318 B CN101550318 B CN 101550318B
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Abstract
The invention provides a Ce3+-contained rare-earth polishing powder and a preparation method thereof. The Ce3+/Ce (mol ratio) of the rare-earth polishing powder is 0.5 percent to 20 percent. Low-valency Ce contained in cerium oxide crystal lattice promotes conversion between Ce4+ and Ce3+, and strengthens the formation of a hydroxide hydrate softening layer between the polishing powder and glass in the polishing process as well as the polishing performance of the powder. The rare-earth polishing powder contains the Ce3+, thus having good suspension properties, high dispersivity, large cutting force when being applied to glass polishing, few scratches on the glass polishing surface, and high polishing planeness. The Ce3+-contained rare-earth polishing powder has simple as well as easily controlled preparation process and is easy for industrialized production.
Description
Technical field
The present invention relates to a kind of Ce of containing
3+Polishing powder from rare earth and preparation method thereof, belong to rare earth powder body material chemistry and preparing technical field.
Background technology
Polishing powder from rare earth is mainly used in the polishing of goods such as glass, crystal, is mainly the cerium base oxide powder, generally is divided into low cerium polishing powder (CeO by cerium content
2/ TREO＜50%), middle cerium polishing powder (CeO
2/ TREO=50%-70%) with high cerium polishing powder (CeO
2/ TREO＞70%.The research proof, mainly being polished to of polishing powder from rare earth is divided into CeO
2, pure trivalent rare earth oxide compound does not have polishing performance, but the existence of trivalent rare earth oxide compound can improve CeO in the polishing powder from rare earth greatly
2Polishing performance.Many commercially available polishing powder from rare earth contain trivalent rare earth oxide compound, for example lanthanum trioxide.Lanthanum trioxide and cerium oxide can not form sosoloid, and it exists with the form of independent phase, therefore when polishing powder is mixed with polishing slurries, usually are partly dissolved, and make the particle of polishing powder the cavity occur, and particle diminishes, and in polishing process, causes the polishing ability to weaken to some extent.CeO
2The based relief polishing powder polishing mechanism is a chemical mechanical polishing, and mechanical polishing receives the influence of powder particle size, uniform particles degree and pellet hardness, and the structurally associated of the composition of chemical rightenning and powder, surface property and powder.CeO
2The chemical rightenning of based relief polishing powder is that trivalent cerium and ceric redox reaction are destroyed the lattice of being thrown material on the one hand, and through chemisorption, makes the material that is in contact with it oxidized or form complex compound and be removed; Be that cerium oxide forms hydrate on the other hand in polishing fluid, hydrate hydroxyl and glazed surface form soften layer, thereby increase the cutting force of polishing powder.Ce
3+Existence, make the cerium oxide lattice of fluorite phase produce defective, Ce
4+And Ce
3+On the lattice position, transform each other, it is active to have increased the Ce ionic, has promoted the formation of hydroxy water compound, has improved the polishing performance of powder.
At present, the researchist has recognized the effect of trivalent cerium in polishing, does not contain Ce but also have patent or bibliographical information to cross
3+Polishing powder from rare earth and preparation method thereof.
Summary of the invention
The purpose of this invention is to provide a kind of Ce of containing
3+Polishing powder from rare earth and preparation technology thereof, utilize the present invention to contain Ce
3+Polishing powder from rare earth, can increase the polishing performance of polishing powder, improve the polishing ability and the quality of finish of polishing powder.
For reaching the foregoing invention purpose, the present invention adopts following technical scheme:
A kind of Ce that contains provided by the invention
3+Polishing powder from rare earth, the cerium in the polishing powder is mainly Ce
4+, Ce wherein
3+With the mol ratio of total Ce at 0.5%-20%.
The Ce that contains provided by the present invention
3+The principal constituent of polishing powder from rare earth be cerium oxide and other rare earth oxide.
The Ce that contains provided by the present invention
3+Polishing powder from rare earth, the mol ratio of cerium and total rare earth (TRE) is 50%-99.9%, other rare earth is one or more in lanthanum, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, the yttrium, the content of other rare earth is 0.1-50%.
A kind of Ce that contains of the present invention
3+Polishing powder from rare earth, its median particle diameter is at 0.005 μ m-3 μ m.
Above-mentioned a kind of Ce that contains
3+The preparation method of polishing powder from rare earth: adopt chemical precipitation method to prepare the presoma of polishing powder from rare earth, with Ce
3+Soluble salt solution and the soluble salt solution of other rare earth ion; With one or more precipitation agent precipitating rare earth and other metals ions in bicarbonate of ammonia, yellow soda ash, oxalic acid, ammonium oxalate, urea, ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide, Neutral ammonium fluoride, Sodium Fluoride, the Sodium Silicofluoride 98min, the presoma that obtains is for containing Ce
3+Rare earth carbonate, oxalate or oxyhydroxide in one or more.With the presoma of the polishing powder from rare earth that obtains, under air or reducing atmosphere, carry out roasting, maturing temperature is 600 ℃-1200 ℃, roasting time is 1-10 hour, can make through aftertreatment then to contain Ce
3+Polishing powder from rare earth.
As with the roasting or add the compound of fluorine-containing or boron simultaneously under reducing atmosphere of the presoma of the polishing powder from rare earth that obtains, the dividing potential drop of oxygen is controlled at 100-10000Pa, and maturing temperature is controlled at 650-1000 ℃.
Presoma during roasting, adds the compound of fluorine-containing or boron in air, maturing temperature is controlled at 650-1000 ℃.
A kind of Ce that contains of the present invention
3+The preparation method of polishing powder from rare earth, when roasting, add compound fluorine-containing or boron and be in hydrofluoric acid and hydrofluoride, silicofluoric acid, silicofluoride, boric acid and the borate one or more.
A kind of Ce that contains of the present invention
3+The preparation method of polishing powder from rare earth, last handling process comprises at least two steps in grinding, washing, screening, oven dry, the classification.
Ce
3+And Ce
4+Adopt the XPS photoelectron spectrograph to test.According to analyses such as micro-area composition, XPS-ESCA, Auger electronic spectrum (XAES), SEAD and high-resolution electron microscopes, obtain this two states ionic ratio.
Advantage of the present invention is: contain Ce in the polishing powder from rare earth
3+, the suspension property of polishing powder is good, and is dispersed strong, and it is big to be applied in the glass polishing cutting force, and few to glass polishing face cut, the polishing planeness is high.Contain Ce
3+Polishing powder from rare earth preparation technology simple, technology is controlled easily, is easy to suitability for industrialized production.It is low that preparation consumes few cost.
Description of drawings
Fig. 1: the X diffracting spectrum of the polishing powder that the embodiment of the invention 1,2,3 is prepared.Abscissa is 2 θ/degree among Fig. 1, i.e. 2 θ/degree.
Fig. 2: the SEM picture of the polishing powder presoma of the embodiment of the invention 5 preparations.
Embodiment
Embodiment 1
Polishing powder presoma cerous carbonate (wherein the mol ratio of cerium and total rare earth (TRE) is 99.5%) is put into 700 ℃ high temperature kiln roasting 2 hours, in stoving oven, feed N
2, the maximum dividing potential drop of oxygen is 100Pa in the CA controlled atmosphere, is finally contained cerous polishing powder from rare earth product after the ball milling screening, and its median particle diameter is 0.07um, and x-ray photoelectron spectroscopy (XPS) is measured polishing powder Ce
3+/ Σ Ce=18.8%.
To contain trivalent cerium polishing powder and comparative sample and process 5% slurries, and under identical condition, liquid-crystalline glasses polished, containing trivalent cerium polishing powder product cutting force is 0.010mm/h, and the range estimation cut is 0/m
2
Embodiment 2
Polishing powder presoma Sedemesis (wherein the mol ratio of cerium and total rare earth (TRE) is 99.5%) is put into 650 ℃ high temperature kiln roasting 4 hours, in stoving oven, feed N
2, the maximum dividing potential drop of oxygen is 300Pa in the CA controlled atmosphere, and finally being contained cerous its median particle diameter of polishing powder from rare earth product after the ball milling screening is 0.36um, and XPS measures polishing powder Ce
3+/ Ce=15.6%.
Polishing powder and comparative sample are processed 10% slurries, under identical condition, laser glass is polished, polishing powder product cutting force is 0.014mm/h, and the range estimation cut is 1/m
2
Embodiment 3
The mixture (wherein the mol ratio of cerium and total rare earth (TRE) is 99.9%) of polishing powder presoma Sedemesis and cerous carbonate put into 850 ℃ high temperature kiln roasting 6 hours; In stoving oven, add Neutral ammonium fluoride (account for polishing powder from rare earth content 4%); Finally contained cerous polishing powder from rare earth product after the ball milling screening; Its median particle diameter is 0.98um, and XPS measures polishing powder Ce
3+/ Σ Ce=5.6%.
Polishing powder and comparative sample are processed 10% slurries, under identical condition, zf glass is polished, polishing powder product cutting force is 0.020mm/h, and the range estimation cut is 1/m
2
Embodiment 4
The mixture of polishing powder presoma Phosbloc cerium (wherein the mol ratio of cerium and total rare earth (TRE) is 70%) put into 850 ℃ high temperature kiln roasting 4 hours; In stoving oven, add boric acid (account for polishing powder from rare earth content 5%); Finally contained cerous polishing powder from rare earth product after the ball milling screening; Its median particle diameter is 1.11um, and XPS measures polishing powder Ce
3+/ Σ Ce=2.5%.
Other conditions are identical, and above-mentioned precursor is roasting 4h under competent oxygen, obtain parallel comparative sample (wherein cerium all is a tetravalence) after the ball milling screening.
Polishing powder and comparative sample are processed 20% slurries, under identical condition, K9 glass is polished, polishing powder product cutting force is 0.010mm/h, and the range estimation cut is 1/m
2Comparative sample cutting force is 0.009mm/h, and the range estimation cut is 3/m
2
Embodiment 5
With the cerous salt 0.5molL that is made into soluble in water
-1Solution (wherein the mol ratio of cerium and total rare earth (TRE) is 99%) put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent oxalic acid of 150g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, the nodulizing agent Neutral ammonium fluoride that adds the polishing powder weight percent and be 3% dispersion agent ammonium chloride and 2% is in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the presoma powder.
At 900 ℃ of roasting 4h, the maximum dividing potential drop of oxygen is 10000Pa in the CA controlled atmosphere with precursor powder, obtains the polishing powder from rare earth product after the ball milling screening, and its median particle diameter is 0.75um, and XPS measures polishing powder Ce
3+/ Σ Ce=7.4%; Polishing powder is processed 15% slurries, high-accuracy opticglass is polished, polishing powder product cutting force is 0.013mm/h, and the range estimation cut is 1/m
2
Embodiment 6
With the cerous salt 0.6molL that is made into soluble in water
-1Solution (wherein the mol ratio of cerium and total rare earth (TRE) is 99.9%) put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent ammonium bicarbonate soln of 150g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, the nodulizing agent Neutral ammonium fluoride that adds the polishing powder weight percent and be 4% dispersion agent ammonium chloride and 5% is in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the presoma powder of white.
Presoma powder art at 1000 ℃ of roasting 5h, is obtained the polishing powder from rare earth product after the ball milling screening, and its median particle diameter is 1.2um, Ce
3+/ Σ Ce=6.6%.
Embodiment 7
With cerous salt and the praseodymium salt 0.3olL that is made into soluble in water
-1Solution (wherein the mol ratio of cerium and total rare earth (TRE) is 65%) put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent ammonium bicarbonate soln of 150g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, the nodulizing agent Neutral ammonium fluoride that adds the polishing powder weight percent and be 2% dispersion agent ammonium chloride and 2% is in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the presoma powder.
It is 5% Sodium Silicofluoride 98min that precursor powder is added weight percent, at 700 ℃ of roasting 10h, obtains final pink polishing powder from rare earth product after the ball milling screening, and its median particle diameter is 0.83um, Ce
3+/ Σ Ce=10.7%.
Embodiment 8
With the rich cerium rare earth chloride salt 0.5molL that is made into soluble in water
-1Solution (wherein the mol ratio of cerium and total rare earth (TRE) is 85%) put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent ammonium bicarbonate soln of 150g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, add the polishing powder weight percent and be 2% dispersion agent ammonium chloride and 5% nodulizing agent Neutral ammonium fluoride in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the presoma powder.
Precursor powder at 1100 roasting 4h, is fed N in stoving oven
2, the maximum dividing potential drop of oxygen is 500Pa in the CA controlled atmosphere, obtains the polishing powder from rare earth product after the ball milling screening, its median particle diameter is 1.5um, Ce
3+/ Σ Ce=9.2%.
Embodiment 9
Lanthanum cerium re chloride (wherein the mol ratio of cerium and total rare earth (TRE) is 65%) is made into 0.7molL
-1Solution put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent ammonium bicarbonate soln of 200g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, add the polishing powder weight percent and be 2% nodulizing agent Neutral ammonium fluoride in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the polishing powder presoma.
Precursor powder at 1000 roasting 4h, is obtained the polishing powder from rare earth product after the ball milling screening, and its median particle diameter is 1.3um, Ce
3+/ Σ Ce=1.5%.
With the cerous salt 0.5molL that is made into soluble in water
-1Solution (wherein the mol ratio of cerium and total rare earth (TRE) is 95%) put into reactor drum, be heated to 60 ℃.With the concentration for preparing is the precipitation agent oxalic acid of 150g/L, joins in the end liquid with the speed of 2L/min; After treating reinforced the completion, stir 10min, add the polishing powder weight percent and be 3% dispersion agent ammonium chloride in mixing solutions; To mix mother liquor and be warming up to 90 ℃ of following continuation stirring reactions 5 hours, and react fully and carry out, and obtain deposition; Be deposited in 80 ℃ of following ageings 4 hours with what obtain; With precipitate and separate, collection, washing, drying, promptly obtain the presoma powder.
Precursor powder is added 5% (polishing powder weight percent) Sodium Fluoride, at 900 ℃ of roasting 4h, obtain the polishing powder from rare earth product after the ball milling screening, its median particle diameter is 1.33um, and XPS measures polishing powder Ce
3+/ Σ Ce=5.4%; Polishing powder is processed 12% slurries, zf glass is polished, polishing powder product cutting force is 0.019mm/h, and the range estimation cut is 2/m
2
Claims (10)
1. one kind contains Ce
3+Polishing powder from rare earth, it is characterized in that the cerium that contains in the polishing powder is mainly Ce
4+, Ce wherein
3+With the mol ratio of total Ce at 7.4%-20%.
2. a kind of Ce that contains according to claim 1
3+Polishing powder from rare earth, it is characterized in that the polishing powder principal constituent is cerium oxide and other rare earth oxide.
3. polishing powder from rare earth according to claim 2; The mol ratio that it is characterized in that cerium and total rare earth (TRE) is 50%-99.9%; Other rare earth is one or more in lanthanum, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, the yttrium, and other total amount of rare earth is 0.1-50%.
4. according to claim 1 or 2 or 3 described a kind of Ce that contain
3+Polishing powder from rare earth, it is characterized in that the median particle diameter of polishing powder is 0.005 μ m-3 μ m.
5. one kind prepares the described Ce of containing of claim 1
3+The method of polishing powder from rare earth, it is characterized in that, at first with Ce
3+Soluble salt solution and the soluble salt solution of other rare earth ion; With one or more precipitation agent precipitating rare earth and other metals ions in bicarbonate of ammonia, yellow soda ash, oxalic acid, ammonium oxalate, urea, ammoniacal liquor, sodium hydroxide, Pottasium Hydroxide, Neutral ammonium fluoride, Sodium Fluoride, the Sodium Silicofluoride 98min; Obtain the presoma of polishing powder from rare earth, it is for containing Ce
3+Rare earth carbonate, oxalate, oxyhydroxide in one or more.
6. 5 described Ce that contain as requested
3+The preparation method of polishing powder from rare earth, it is characterized in that, the presoma of polishing powder from rare earth is carried out roasting under reducing atmosphere; Control oxygen partial pressure simultaneously at 100-10000Pa; Maturing temperature is 600 ℃-1200 ℃, and roasting time is 1-10 hour, can make through aftertreatment then to contain Ce
3+Polishing powder from rare earth.
7. a kind of Ce that contains according to claim 6
3+The preparation method of polishing powder from rare earth, it is characterized in that, the roasting or add the compound of fluorine-containing or boron simultaneously under reducing atmosphere of the presoma of said polishing powder from rare earth, maturing temperature is controlled at 650-1000 ℃.
8. a kind of Ce that contains according to claim 5
3+The preparation method of polishing powder from rare earth, it is characterized in that the presoma of said polishing powder from rare earth during roasting, adds the compound of fluorine-containing or boron in air, maturing temperature is controlled at 650-1000 ℃.
9. according to claim 7 or 8 described a kind of Ce that contain
3+The preparation method of polishing powder from rare earth, it is characterized in that said compound salt fluorine-containing or boron is one or more in hydrofluoric acid, hydrofluoride, silicofluoric acid, silicofluoride, boric acid and the borate thereof.
10. a kind of Ce that contains according to claim 5
3+The preparation method of polishing powder from rare earth, it is characterized in that said post-processing step comprises at least two steps in grinding, washing, screening, oven dry, the classification.
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| CN101550318B true CN101550318B (en) | 2012-11-14 |
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