CN109054655A - A kind of polishing powder from rare earth and preparation method thereof - Google Patents
A kind of polishing powder from rare earth and preparation method thereof Download PDFInfo
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- CN109054655A CN109054655A CN201811072617.9A CN201811072617A CN109054655A CN 109054655 A CN109054655 A CN 109054655A CN 201811072617 A CN201811072617 A CN 201811072617A CN 109054655 A CN109054655 A CN 109054655A
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Abstract
A kind of polishing powder from rare earth of disclosure of the invention and preparation method thereof, the polishing powder from rare earth includes following component and its mass percent: CeO2 content 60 80%, La2O3 content 30 40%, Pr6O11 content 0.1 5%, F content 4 6%, P2O5 content 1 3%；The preparation method of above-mentioned polishing powder from rare earth, including, the synthesis of modified carbonated rare earth presoma, modified carbonated rare earth presoma washing, the dehydration of modified carbonated rare earth presoma, roasting, crushing.Polishing powder from rare earth prepared by the present invention has wearability good, and polishing speed is fast, and polishing precision is easy to control；The homogeneity of product is good, high production efficiency, at low cost, pollution-free, shows suitable for integrated circuit, plane, the surface polishing processing of the electronics and information industries accurate device such as optical glass.
Description
Technical field
The present invention relates to a kind of polishing powder from rare earth and preparation method thereof, in particular to a kind of to be applied to integrated circuit, plane
The polishing powder from rare earth of surface polishing and preparation method thereof of the electronics and information industries accurate device such as display, optical glass.
Background technique
Currently, various glass materials are widely used, and these materials are all needed before application by necessary surface polishing.
Early stage mainly polishes various glass surfaces using materials such as zirconium oxide, iron oxide or silica, in recent years, from polishing
Efficiency and precision aspect consider that rare earth oxide (especially cerium oxide) polishing material as main component is considered being more suitable for
In the surface polishing of glass material.
With the fast development of electronic information technology, lens, plate glass, liquid crystal display (LCD), glasses, optics member
The demand of the glass baseplates such as part and ceramic material greatly increases, and the precision and polishing speed for polishing material also proposed higher
Requirement, this just promotes manufacturer that product specification is continuously improved, to adapt to the requirement of New Products, polishing powder from rare earth oneself
As current rare earth application product applied widely, dosage is big, with high content of technology.
The polishing powder from rare earth of early stage uses bastnaesite for raw material, and the invention if patent publication No. is CN101215446A is special
Benefit discloses a kind of method that rare earth ore concentrate prepares high cerium nanometer scale polishing powder from rare earth, smart from rare earth by the precipitation method with bicarbonate
Mixed rare earth carbonate is directly made in mine concentrated sulfuric acid roasting, infusion；Mixed rare earth carbonate is mixed with alkali, is heated to melting, and
1-4 hours are kept the temperature in molten condition, then industrial hydrofluoric acid is added in cooling, crushing, obtain fluorine rare earth oxide enriched substance；Fluorine oxygen
Change rareearth enriching material, crush, washing, drainage is uniform in stirrer for mixing, is then charged into band sieve high energy ball mill, is filled with
Nitrogen carries out wet-milling high-energy ball milling, and the lower section sieved behind high-energy ball milling room is with high pressure draught rotating channel, and the powder under sieving is in high speed
Under air-flow pushes, spin-drying is carried out to the moisture of powder, then carry out drying and processing and obtain polishing powder from rare earth.
CN101899281A discloses a kind of polishing powder from rare earth and preparation method thereof.The invention polishing powder contain cerium oxide,
Lanthana, praseodymium oxide, total amount of rare earth TERO is in 90wt% or more.To guarantee necessary grinding rate, in Moist chemical synthesis process
It has been incorporated the fluorine element to chemically react, and has controlled preliminarily forming for product granularity, 877-3 type polishing powder from rare earth is made.
It is more currently on the market to use the heavy rear flaorination process of first carbon, i.e., ammonium hydrogen carbonate is first added and is precipitated, washs
After add hydrofluoric acid fluorination.
Patent of invention if patent publication No. is CN100497508C discloses a kind of producer of high-cerium rare-earth polishing powder
Method, addition hydrofluoric acid is fluorinated after first preparing lanthanum carbonate cerium, roasts to obtain high-cerium rare-earth polishing powder.
The preparation of presoma is the prerequisite of the excellent polishing powder of processability.The performance and state of presoma determine
The size of polishing powder crystal grain, shape etc., the final application performance for influencing polishing powder.According to the production of current polishing powder, presoma
It prepares main purpose to be on the one hand to have carried out the control of particle, crystal form, pattern, further aspect is that introducing F to form fluorine
Carbonated rare earth.Wherein the control of particle and pattern includes chemical precipitation method control and two kinds of wet ball grinding；The factor of F element includes
It introduces when chemical precipitation and is introduced in the form of wet process or dry method hydrofluoric acid or high fluorine carbonated rare earth.
Fluorination can be had due to using disposable fluorination using the polishing powder of above-mentioned existing production technology production
The case where reaction is uneven or part is fluorinated, on the one hand will affect the crystal phase structure of product after roasting, on the other hand can generate shadow
The free state fluorine ion of polishing precision and rate is rung, the agglomerated particle size and intensity formed after roasting also has very big difference,
And the polishing precision and polishing speed of polishing powder are mainly the size by the agglomerate particle formed after high temperature sintering and reunite strong
Degree is determined, will lead to a series of problems in this way, such as generate scratch or polishing speed very short in the glass surface of polishing
Time in quickly reduce, especially when throwing Bohemian glass surface, it is fatal that polishing speed, which rapidly reduces,；Fluorination process simultaneously
Obtained in fluorine carbonated rare earth granularity it is smaller, dehydration is difficult, and it is lower to cause yield.
In order to meet the polishing powder product that condition just needs to pick out certain agglomeration strength, certain particle size, and these are special
Property be very rambunctious again, and production technology is complicated, increased costs and introduces foreign ion, causes quality fluctuation.
Rare earth oxide and rare earth fluoride are mixed in addition, such as patent publication No. has been the patent of invention public affairs Jian of CN101010402A
Close, it is ground, dry, roast, grading system for polishing powder from rare earth method.Rare earth fluoride particle is thinner, and aftertreatment technology is complicated；
Compounding process simultaneously using fluoride and oxide is also more complicated；This method can generate the phenomenon that particle double sintering, portion
Divide particle to generate abnormal growth by after baking, local big particle is formed, to cause to scratch during the polishing process.
In addition, it is that precipitating reagent prepares polishing powder from rare earth that presently disclosed patent, which is ammonium hydroxide, oxalic acid, ammonium hydrogen carbonate etc., this
There are cost and environmental protection pressures in terms of increasingly strict environmental requirement.
It is accordingly required in particular to which a kind of polishing powder from rare earth and preparation method thereof, has solved the problems, such as above-mentioned existing.
Summary of the invention
In view of the above drawbacks of the prior art, technical problem to be solved by the invention is to provide a kind of polishing powder from rare earth
And preparation method thereof.
To achieve the above object, the present invention provides a kind of polishing powder from rare earth, including following component and its mass percent；
CeO2 60〜80%
La2O3 30〜40%
Pr6O11 0.1〜5%
F(fluorine) 4 6%
P2O5 1〜3%。
The preparation method of above-mentioned polishing powder from rare earth, includes the following steps:
(1) synthesis of modified carbonated rare earth presoma: mixed chlorinated rare earth is dissolved in the water, is heated to 60 80 DEG C, is being stirred
It mixes under state, using the mixed solution of NaF and Na2CO3 as precipitating reagent, being precipitated to pH is 6.2 6.5, continues to stir 0.5 1.5h
Afterwards, a certain amount of phosphoric acid (content 85%) is added, Na2CO3 aqueous solution is then added, being precipitated to pH is 6.5 7, continues to stir
1 2h obtains modified carbonated rare earth precursor pulp.
Preferably, the REO of mixed chlorinated rare earth is 45 50%；
In mixed chlorinated rare earth, each component is calculated as on the basis of the REO of mixed chlorinated rare earth with the quality of oxide:
CeO2 60〜80%
La203 18〜40%
Pr6O11 0.1〜5%。
Term " REO " is ion phase total amount of the rare earth oxide, and by taking 100kg rare earth chloride as an example, rare earth oxide is
45kg, i.e. REO=45%, similarly hereinafter；
Preferably, the mixed chlorinated rare earth is dissolved in water, the ratio of mixed chlorinated rare earth and water, with mixed chlorinated rare earth with
Water quality summation meter, mixed chlorinated rare earth quality account for the 15 30% of mixed chlorinated rare earth and water quality summation；
Preferably, the mixed solution of the NaF and Na2CO3, in terms of mixed solution, the mass fraction of NaF is 2% 3%,
The mass fraction of Na2CO3 is 10% 15%；
Preferably, the phosphoric acid (content 85%) quality dosage is 7 20kg/ tons of rare earth chloride；
Preferably, the Na2CO3 aqueous solution, the mass fraction of Na2C03 are 10% 15%；
(2) by the modification carbonated rare earth precursor pulp in step (1), 2 3h modified carbonated rare earth presoma washing: are stood
Afterwards, upper layer clear aqueous solution is pumped, adds 50 85 DEG C of equivalent of hot water, after 0.5 1.5h of stirring stands 2 3h again, again
Upper layer clear aqueous solution is pumped, it is accumulative to add hot water and wash 35 times；
(3) slurry after washing in step (2) dehydration of modified carbonated rare earth presoma: is obtained into presoma through centrifugal dehydration
Solid Modified carbonated rare earth；
(4) it roasts: the modification carbonated rare earth in step (3) is fired, obtain modified RE oxide, maturing temperature is
900 950 DEG C, calcining time is 4 6h；
(5) it crushes: modified RE oxide is crushed, obtain polishing powder from rare earth, the polishing powder from rare earth, D50 0.8-
3.0 μm, D50≤2.5D50.
Preferably, the grinding mode is air-flow crushing or is mechanically pulverized one such or combinations thereof.
For polishing powder from rare earth of the invention compared with existing product, the present invention passes through the modification of fluorine (F) and phosphorus (P), so that
The polishing powder from rare earth of preparation has high wear intensity.The effect of fluorine (F) and phosphorus (P) is to play change crystal morphology, structure
And the effect of polishing performance.Change maturing temperature simultaneously, crystal grain refinement and generate distortion of lattice and form Lacking oxygen, favorably
In raising wear intensity.
The present invention first precipitates mixed chlorinated rare earth by precipitating reagent of the mixed solution of NaF and Na2CO3, solves fluorination not
The free state fluorine ion and fluoride for uniformly having an impact polishing precision and rate, do not generate local anomaly in roasting process
Coarse particle；The present invention is by being added phosphoric acid and being precipitated again with aqueous sodium carbonate, before the modification carbonated rare earth for making preparation
The grain size that body has certain size is driven, solves the disadvantage that the difficult dehydration of polishing powder from rare earth presoma and low output.
It is not related to the discharge such as ammonia nitrogen in production process of the present invention, environmental protection pressure is not present.And rare earth prepared by the present invention is thrown
Light powder has wearability good, and polishing speed is fast, and polishing precision is easy to control；The homogeneity of product is good, high production efficiency, cost
It is low, pollution-free, it is shown suitable for integrated circuit, plane, the surface polishing of the electronics and information industries accurate device such as optical glass adds
Work.
Containing other rare earth elements in addition to cerium oxide in polishing powder of the invention, these rare earth elements are not changing oxygen
Change cerium crystal structure under the premise of, change crystal form between fluorite type and hexagonal crystal system, in a certain range with cerium oxide shape
At solid solution, play a positive role to the wear intensity of polishing powder.By other elements such as doping F, P, change maturing temperature
Become, crystal grain refinement and generate distortion of lattice and form Lacking oxygen, is conducive to improve wear intensity.
Detailed description of the invention
Fig. 1 is the XRD schematic diagram of 1 gained polishing powder from rare earth of the embodiment of the present invention.
Fig. 2 is the XRD schematic diagram of 1 gained polishing powder from rare earth of the embodiment of the present invention.
Specific embodiment
Below with reference to embodiment, the invention will be further described:
Embodiment 1
In mixed chlorinated rare earth, the mass ratio of each component are as follows: total amount of rare earth REO is 45%；Cerium oxide 70%, lanthana are
19.9%, praseodymium oxide 0.1%；
Above-mentioned 1000kg rare earth chloride is mixed with 2500kg water, 60 DEG C are heated to after dissolution, is slowly added to NaF and Na2CO3
Mixed solution (mass fraction that wherein mass fraction of NaF is 2.25%, Na2C03 is that 10%), pH value to terminal is 6.5,
Continue after stirring 0.5h, be added 20kg phosphoric acid (content 85%), the Na2C03 aqueous solution that mass fraction is 10%, precipitating is then added
It is 7 to pH, continues to stir 2h, obtain modified carbonated rare earth precursor pulp.
After above-mentioned slurry is stood 2h, upper layer clear aqueous solution is pumped, adds 85 DEG C of equivalent of hot water, stirring 1.5h is quiet again
After setting 3h, upper layer clear aqueous solution is pumped again, and accumulative hot water of adding washs 3 times.
Slurry after washing obtains presoma solid through centrifugal dehydration, then in 950 DEG C of roasting 6h.
Product after roasting obtains the polishing powder from rare earth, the fluorine content of the polishing powder through air-flow crushing, air current classifying
It is 2.7% for 4%, content containing P2O5, laser particle analyzer test result: D50=0.82 μm, D90=1.7 μm.
Embodiment 2
In mixed chlorinated rare earth, the mass ratio of each component are as follows: total amount of rare earth REO is 45%；Cerium oxide 80%, lanthana are
19.9%, praseodymium oxide 0.1%；
Above-mentioned 1000kg rare earth chloride is mixed with 2500kg water, 80 DEG C are heated to after dissolution, is slowly added to NaF and Na2CO3
Mixed solution (mass fraction that wherein mass fraction of NaF is 3%, Na2CO3 is that 15%), pH value to terminal is 6.5, after
It after continuous stirring 0.5h, is added 7kg phosphoric acid (content 85%), the Na2CO3 aqueous solution that mass fraction is 10% is then added, is precipitated to
PH is 7, continues to stir 2h, obtains modified carbonated rare earth precursor pulp.
After above-mentioned slurry is stood 2h, upper layer clear aqueous solution is pumped, adds 50 DEG C of equivalent of hot water, stirring 0.5h is quiet again
After setting 2h, upper layer clear aqueous solution is pumped again, and accumulative hot water of adding washs 3 times.
Slurry after washing obtains presoma solid through centrifugal dehydration, then in 900 DEG C of roasting 6h.
Product after roasting obtains the polishing powder from rare earth through air-flow crushing, air current classifying, and the fluorine content of the polishing powder is
5.5%, content containing P2O5 is 1.1%, laser particle analyzer test result: D50=1.52 μm, D90=3.1 μm.
Embodiment 3
In mixed chlorinated rare earth, the mass ratio of each component are as follows: total amount of rare earth REO is 45%；Cerium oxide 60%, lanthana 35%,
Praseodymium oxide 3%；
Above-mentioned 1000kg rare earth chloride is mixed with 2500kg water, 80 DEG C are heated to after dissolution, is slowly added to NaF and Na2CO3
Mixed solution (mass fraction that wherein mass fraction of NaF is 3%, Na2CO3 is that 15%), pH value to terminal is 6.5, after
It after continuous stirring 0.5h, is added 14kg phosphoric acid (content 85%), the Na2CO3 aqueous solution that mass fraction is 10% is then added, is precipitated to
PH is 7, continues to stir lh, obtains modified carbonated rare earth precursor pulp.
After above-mentioned slurry is stood 2h, upper layer clear aqueous solution is pumped, adds 70 DEG C of equivalent of hot water, stirring lh is stood again
After 2h, upper layer clear aqueous solution is pumped again, and accumulative hot water of adding washs 3 times.
Slurry after washing obtains presoma solid through centrifugal dehydration, then in 950 DEG C of roasting 6h.
Product after roasting obtains the polishing powder from rare earth through air-flow crushing, air current classifying, and the fluorine content of the polishing powder is
5.5%, content containing P2O5 is 2.3%, laser particle analyzer test result: D50=2.8 μm, D90=6.5 μm.
In the present invention, D50 indicates that cumulative particle sizes distribution number reaches partial size corresponding when 50%, and D90 indicates cumulative particle sizes point
Cloth number reaches partial size corresponding when 90%.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of polishing powder from rare earth, which is characterized in that including following component and its mass percent:
CeO2 60〜80%
La2O3 30〜40%
Pr6Oll 0.1 〜5%
F 4 〜6%
P2O5 1〜3%。
2. a kind of method for preparing polishing powder from rare earth described in claim 1, which comprises the steps of:
(1) synthesis of modified carbonated rare earth presoma: mixed chlorinated rare earth is dissolved in the water, is heated to 60 80 DEG C, is being stirred
It mixes under state, using the mixed solution of NaF and Na2CO3 as precipitating reagent, being precipitated to pH is 6.2 6.5, continues to stir 0.5 1.5h
Afterwards, a certain amount of phosphoric acid (content 85%) is added, Na2CO3 aqueous solution is then added, being precipitated to pH is 6.5 7, continues to stir
1 2h obtains modified carbonated rare earth precursor pulp；
(2) by the modification carbonated rare earth precursor pulp in step (1), 2 3h modified carbonated rare earth presoma washing: are stood
Afterwards, upper layer clear aqueous solution is pumped, adds 50 85 DEG C of equivalent of hot water, after 0.5 1.5h of stirring stands 2 3h again, again
Pump upper layer clear aqueous solution；
(3) slurry after washing in step (2) dehydration of modified carbonated rare earth presoma: is obtained into forerunner through centrifugal dehydration
The Solid Modified carbonated rare earth of body；
(4) it roasts: the modification carbonated rare earth in step (3) is fired, obtain modified RE oxide, maturing temperature is
900 950 DEG C, calcining time is 4 6h；
(5) it crushes: modified RE oxide is crushed, obtain polishing powder from rare earth, the polishing powder from rare earth, D50 0.8-
3.0, D50≤2.5D50.
3. method according to claim 2, which is characterized in that in step (1), the REO of mixed chlorinated rare earth is 45 50%.
4. method as claimed in claim 2 or claim 3, which is characterized in that in mixed chlorinated rare earth, each component is with mixed chlorinated dilute
On the basis of the REO of soil, it is calculated as with the quality of oxide:
CeO2 60〜80%
La203 18〜40%
Pr6O11 0.1〜5%。
5. method according to claim 2, which is characterized in that the mixed chlorinated rare earth is dissolved in water, mixed chlorinated dilute
The ratio of soil and water, with mixed chlorinated rare earth and water quality summation meter, mixed chlorinated rare earth quality accounts for mixed chlorinated rare earth and water
The 15 30% of quality summation.
6. method according to claim 2, which is characterized in that the mixed solution of the NaF and Na2CO3, with mixed solution
Meter, the mass fraction of NaF are 2% 3%, and the mass fraction of Na2CO3 is 10% 15%.
7. method according to claim 2, which is characterized in that the phosphoric acid, content is 85% and quality dosage is 7
20kg/ tons of rare earth chlorides.
8. method according to claim 2, which is characterized in that the mass fraction of the Na2CO3 aqueous solution is 10%
15%。
9. method according to claim 2, which is characterized in that in step (4), the roasting, maturing temperature 900
950 DEG C, calcining time is 4 6h.
10. method according to claim 2, which is characterized in that in step (5), the polishing powder from rare earth, D50 is
0.8-3.0 μm, D50≤2.5D50.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978869A (en) * | 2020-09-16 | 2020-11-24 | 包头市昊锐稀土有限公司 | Preparation method of cerium-based polishing powder for optical glass and liquid crystal display glass |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
-
2018
- 2018-09-14 CN CN201811072617.9A patent/CN109054655A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978869A (en) * | 2020-09-16 | 2020-11-24 | 包头市昊锐稀土有限公司 | Preparation method of cerium-based polishing powder for optical glass and liquid crystal display glass |
| CN111978869B (en) * | 2020-09-16 | 2021-06-04 | 包头市昊锐稀土有限公司 | Preparation method of cerium-based polishing powder for optical glass and liquid crystal display glass |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
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