CN107556922A - A kind of polishing powder from rare earth containing samarium and its preparation technology - Google Patents
A kind of polishing powder from rare earth containing samarium and its preparation technology Download PDFInfo
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Abstract
A kind of polishing powder from rare earth containing samarium, its composition is according to the molar ratio：Sm2O3/TREO=1.4×10‑4~0.014, La2O3/ TREO=0.06~0.12, Pr7O11/TREO=8.6×10‑6~0.0047, Nd2O3/TREO=2.97×10‑5~0.0074, surplus CeO2/ TREO=0.27~0.46.The polishing powder from rare earth adds fluorine-containing precipitant solution into raw material using the rare-earth salt solution containing samarium as primary raw material, by adjusting the Oil repellent in the control product of the fluorinion concentration in precipitating reagent, then the process acquisition such as scrubbed, drying, calcining, broken classification.The process distinction introduces samarium element in being mainly shown as other production technologies in rare earths material, and fluorine element is introduced in precipitating reagent, has the advantages that preparation technology is simple, and raw material sources are extensive.Prepared polishing powder from rare earth crystal grain is uniform, corner angle are obvious, and cutting speed is fast.
Description
Technical field
The present invention relates to rare earth material technical field, and in particular to a kind of polishing powder from rare earth containing samarium and its preparation technology.
Background technology
Rare earth grinding-material is widely used as the grinding of glass material with material.Particularly in recent years mobile phone glass and
The Fast Growth in the electric/electronic device fields such as liquid crystal display (LCD), photomask, the grinding material as their glass substrates
Expect increase in demand.With the continuous development of industry manufacturing technology, the grinding for glass such as substrates requires higher grind
Grind speed and more preferable surface accuracy.Require that grinding-material has higher recycling performance and reduces fluorine element possibility simultaneously
Caused by environmental problem.
Patent CN201310403538.2 discloses a kind of polishing powder from rare earth fluorine doped technique of use using cerium as main component.
The technique adds rare-earth salt solution, precipitant solution, fluorination agent solution in reactor simultaneously, in system pH 6-9, temperature
30-90 DEG C and with the conditions of strong mixing carry out polishing powder from rare earth synthesis.The technique compares other techniques to a certain degree
On improve the situation pockety of fluorine element in polishing powder from rare earth, but fluorization agent and being separately added into for precipitating reagent easily cause
Local concentration is too high, the uneven situation of fluorine element occurs.System pH maintains 6-9 in precipitation process so that a large amount of impurity
Element precipitation enters in polishing powder from rare earth, and product quality can be had undesirable effect.It can be formed under the conditions of strong mixing simultaneously big
Non-breakable foam is measured, is allowed to be restricted in commercial Application.Patent CN200310116366.7 discloses a kind of glass
The manufacture method of abrasive material, it is mainly characterized by after carbonated rare earth is calcined carrying out wet ball grinding with rare earth fluoride, made by calcining
Generation solid phase reaction, reach the purpose that fluorine element spreads in particle.This method is uneven in fluorine element distribution, high fluorine-containing
The particle of amount can form excrescent oversize grain under the high temperature conditions, influence product quality.And the complex technical process, if
It is standby to require high, it is unfavorable for the production of product.It is mainly lanthanum cerium system in the manufacture raw material of existing patent document middle rare earth polishing powder
Row, La-Ce-Pr series, LaCePrNd series, pure cerium series, and the polishing powder from rare earth of part adulterated al, zirconium, and in existing element
The polishing powder from rare earth of middle samarium doped element has not been reported.High-purity samarium element is mainly used in SmCo in market application aspect and closed
Gold and light sensation, catalysis material field, it is small to the market demand.The samarium element of low-purity be not only worth it is low and also can not be formed market pin
Sell, cause ample resources to overstock.Samarium element is added in cerium-based rare earth polishing powder and grinds performance without it can be improved, raising follows
Ring service efficiency, and resource can be made full use of.
In order to solve the above problems, present inventor to the rare earth grinding-material of various particle diameters conscientiously study to improve
Grinding rate.As a result find, when the particle diameter of cerium based abrasive material is in prescribed limit, agglomerated particle corner angle it is sharp advantageously in
Grinding rate is improved, while less crystallite dimension can ensure more preferable surface quality, with the continuous stripping of small grains,
Particle fresh surface is all the time present, effective time of the particle in process of lapping can be extended, improve the circulation of grinding-material
Performance.
The content of the invention
It is an object of the invention to provide a kind of polishing powder from rare earth containing samarium and its preparation technology, obtained polishing powder from rare earth are brilliant
Grain is uniform, corner angle are obvious, and cutting speed is fast.
The technical solution adopted in the present invention is：
A kind of polishing powder from rare earth containing samarium, its composition is according to the molar ratio： Sm2O3/TREO=1.4×10-4~0.014, La2O3/TREO
=0.06~0.12, Pr7O11/TREO=8.6×10-6~0.0047, Nd2O3/TREO=2.97×10-5~0.0074, surplus is
CeO2/ TREO=0.27~0.46.
A kind of preparation technology of polishing powder from rare earth containing samarium, its production technology are:
A, the compound of rare earth is formulated as salting liquid, the molar concentration of the rare-earth salt solution is 0.59~1.78mol/L；
B, fluorine-containing precipitating reagent is prepared, after precipitating reagent is prepared as into solution, fluorization agent is slowly added into precipitant solution, stirring is equal
It is even, sediment is filtered to remove, takes supernatant；Adjust 1.5~4.5 times that precipitant concentration is rare-earth salt solution molar concentration, fluorine
Ion concentration is 0.4~1.0 times of rare-earth salt solution molar concentration；
C, material liquid is added into reaction vessel, is warming up to 90~96 DEG C；
D, fluorine-containing precipitating reagent is added into reaction vessel；
E, fluorine-containing precipitating reagent is added until system pH is 7.0, whole building-up process control time is 0.5~5h；
F, by sediment washing and filtering, 4~36h is dried at 300~650 DEG C；
G, material drying is calcined into 6~12h at 960~1150 DEG C；
H, polishing powder from rare earth containing samarium of the present invention can be obtained by calcined product being crushed into classification.
The present invention adds fluorine-containing precipitant solution into raw material, passed through using the rare-earth salt solution containing samarium as primary raw material
Adjust the Oil repellent in the fluorinion concentration control product in precipitating reagent, then the process such as scrubbed, drying, calcining, broken classification
Obtain.The present invention introduced in rare earths material samarium element make gained the corner angle of polishing powder from rare earth containing samarium it is sharper, crystal grain is uniform
Closely, grinding rate is fast.Fluorization agent is added in precipitating reagent, while ensureing that fluorine element is equally distributed, avoids high concentration fluorine
Particle corner angle caused by element are passivated, and particle is kept having preferable grinding efficiency and is recycled performance.Carry simultaneously
Comprehensive utilization of resources level is risen, simple with preparation technology, raw material sources are extensive, and pollution is small, is easy to industrialized production etc.
Advantage.
Brief description of the drawings
Fig. 1 is the powder SEM figures prepared by the embodiment of the present invention 1；
Fig. 2 is the powder SEM figures prepared by the embodiment of the present invention 2；
Fig. 3 is the powder SEM figures prepared by the embodiment of the present invention 3；
Fig. 4 is the powder SEM figures prepared by the embodiment of the present invention 4；
Fig. 5 is the powder SEM figures prepared by the embodiment of the present invention 5；
Fig. 6 is the powder SEM figures prepared by comparative example 1 of the present invention；
Fig. 7 is the powder SEM figures prepared by comparative example 2 of the present invention；
Fig. 8 is the embodiment of the present invention 3（Optimised process）And its powder XRD prepared by the content of border.
Embodiment
Embodiment 1
The compound of rare earth is formulated as salting liquid, salting liquid composition is Sm for calculation in the molar ratio2O3/TREO=1.4×10-4,
La2O3/ TREO=0.104, Pr7O11/ TREO=0.0022, Nd2O3/ TREO=0.0045, surplus CeO2/ TREO=0.36, salt are molten
Liquid molar concentration is 0.59mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 96 DEG C.Ammonium hydrogen carbonate is formulated as
0.885mol/L solution, ammonium fluoride is added into ammonium bicarbonate soln, makes the fluorinion concentration in ammonium bicarbonate soln be
0.236mol/L.By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.Fluorine-containing ammonium bicarbonate soln is added into reactor,
Until system pH is 7.0, building-up process control time is 5 hours.By sediment washing and filtering, dried 36 hours at 300 DEG C,
Material drying is calcined into 6h at 1150 DEG C.Calcined product is crushed and is classified to D50：It is 1.0 ± 0.2 μm, as of the present invention
Polishing powder from rare earth containing samarium.
Embodiment 2
The compound of rare earth is formulated as salting liquid, salting liquid composition is Sm for calculation in the molar ratio2O3/ TREO=0.014,
La2O3/ TREO=0.104, Pr7O11/TREO=8.6×10-6, Nd2O3/TREO=2.97×10-4, surplus CeO2/TREO=
0.28, salting liquid molar concentration is 1.78mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 90 DEG C.By bicarbonate
Ammonium is formulated as 2.67mol/L solution, and ammonium fluoride is added into ammonium bicarbonate soln, makes fluorinion concentration in ammonium bicarbonate soln
For 0.712mol/L.By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.It is molten that fluorine-containing ammonium hydrogen carbonate is added into reactor
Liquid, until system pH is 7.0, building-up process control time is 0.5 hour.By sediment washing and filtering, 6 are dried at 650 DEG C
Hour, material drying is calcined into 12h at 960 DEG C.Calcined product is crushed and is classified to D50：1.0 ± 0.2 μm, be the present invention
Described polishing powder from rare earth containing samarium.
Embodiment 3
The compound of rare earth is formulated as salting liquid, salting liquid composition is Sm for calculation in the molar ratio2O3/ TREO=0.014,
La2O3/ TREO=0.06, Pr7O11/ TREO=0.0022, Nd2O3/ TREO=0.0045, surplus CeO2/ TREO=0.37, salting liquid
Molar concentration is 0.59mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 93 DEG C.Sodium carbonate is formulated as
2.655mol/L solution, sodium fluoride is added into ammonium bicarbonate soln, makes the fluorinion concentration in ammonium bicarbonate soln be
0.59mol/L.By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.Fluorine-containing ammonium bicarbonate soln is added into reactor, directly
It is 7.0 to system pH, building-up process control time is 2.5 hours.By sediment washing and filtering, dried 12 hours at 600 DEG C,
Material drying is calcined into 8h at 1080 DEG C.Calcined product is crushed and is classified to D50：It is 1.0 ± 0.2 μm, as of the present invention
Polishing powder from rare earth containing samarium.
Embodiment 4
The compound of rare earth is formulated as salting liquid, salting liquid composition is Sm for calculation in the molar ratio2O3/TREO=1.4×10-4,
La2O3/ TREO=0.06, Pr7O11/TREO=8.6×10-6, Nd2O3/TREO=2.97×10-5, surplus CeO2/ TREO=0.46,
Salting liquid molar concentration is 1.16mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 94 DEG C.Sodium carbonate is formulated as
2mol/L solution, sodium fluoride is added into ammonium bicarbonate soln, and it is 0.7mol/L to make fluorinion concentration in ammonium bicarbonate soln.
By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.Fluorine-containing ammonium bicarbonate soln is added into reactor, until system pH
For 7.0, building-up process control time is 4.5 hours.Dry 6 hours, sediment washing and filtering by material drying at 500 DEG C
10h is calcined at 1000 DEG C.Calcined product is crushed and is classified to D50：1.0 ± 0.2 μm, rare earth containing samarium as of the present invention
Polishing powder.
Embodiment 5
The compound of rare earth is formulated as salting liquid, salting liquid composition is Sm for calculation in the molar ratio2O3/ TREO=0.014,
La2O3/ TREO=0.12, Pr7O11/ TREO=0.0047, Nd2O3/ TREO=0.0074, surplus CeO2/ TREO=0.27, salting liquid
Molar concentration is 1.22mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 94 DEG C.Sodium carbonate is formulated as
1.83mol/L solution, sodium fluoride is added into ammonium bicarbonate soln, makes the fluorinion concentration in ammonium bicarbonate soln be
1.1mol/L.By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.Fluorine-containing ammonium bicarbonate soln is added into reactor, directly
It is 7.0 to system pH, building-up process control time is 1.5 hours.By sediment washing and filtering, dried 24 hours at 450 DEG C,
Material drying is calcined into 11h at 980 DEG C.Calcined product is crushed and is classified to D50：It is 1.0 ± 0.2 μm, as of the present invention
Polishing powder from rare earth containing samarium.
Comparative example 1
The compound of rare earth is formulated as salting liquid, salting liquid composition is CeO for calculation in the molar ratio2/ TREO=0.58, salt are molten
Liquid molar concentration is 1.19mol/L.1m is added into reaction vessel3Material liquid, it is warming up to 94 DEG C.Sodium carbonate is formulated as
2.0mol/L solution, sodium fluoride is added into ammonium bicarbonate soln, and it is 0.7mol/ to make fluorinion concentration in ammonium bicarbonate soln
L.By fluorine-containing ammonium bicarbonate soln press filtration, clear liquid is taken.Fluorine-containing ammonium bicarbonate soln is added into reactor, until system pH
It is worth for 7.0, building-up process control time is 2.6 hours.Dry 12 hours, sediment washing and filtering by drying object at 600 DEG C
Material calcines 8h at 1060 DEG C.Calcined product is crushed and is classified to D50：1.0±0.2μm.
Comparative example 2
The compound of rare earth is formulated as salting liquid, salting liquid composition is La for calculation in the molar ratio2O3/ TREO=0.06,
CeO2/TREO=0.418, Pr7O11/ TREO=0.0047, Nd2O3/ TREO=0.0074, salting liquid molar concentration are 1.36mol/
L.1m is added into reaction vessel3Material liquid, it is warming up to 94 DEG C.Ammonium hydrogen carbonate is formulated as to 3.15mol/L solution, to carbonic acid
Ammonium fluoride is added in hydrogen ammonium salt solution, it is 1.1mol/L to make fluorinion concentration in ammonium bicarbonate soln.Fluorine-containing ammonium hydrogen carbonate is molten
Hydraulic pressure is filtered, and takes clear liquid.Fluorine-containing ammonium bicarbonate soln is added into reactor, until system pH is 7.0, building-up process control
Time is 1.5 hours.By sediment washing and filtering, dried 8 hours at 550 DEG C, material drying is calcined into 11h at 1000 DEG C.
Calcined product is crushed and is classified to D50：1.0±0.2μm.
Evaluation is ground on M200 type precisive plane grinders to each embodiment and comparative example.Polishing powder is prepared as
10% consistency pulp, using Φ 70mm flat glass as grinding-material, glass is thrown using polyurethane polishing pad
Light.Polishing disk rotating speed is 200 turns/min, number of oscillations 30 times/min, grinding pressure 0.2MPa.By before and after weighing glass polishing
Weight measure grinding rate, per 24h determine a glass weight, average measure polishing powder recycle performance.Grinding
Glass surface cut quantity is counted, is repeated, it is good to calculate glass in 70 times of lower sight glass surfaces using image measurer afterwards
Product rate.
Polishing powder grinding efficiency contrast table prepared by table 1
Polishing powder grinding yields contrast table prepared by table 2
By the contrast of the table 2 of table 1 it can be found that embodiment 3 has higher grinding efficiency, while has more preferable recycling
Can, speculate with reference to SEM figures and promote crystal grain refinement with the increase of samarium content, but structure can also become loose simultaneously, show to grind
Grind that speed is fast but the phenomenon of service life reduction, as the increase crystal grain of neodymium content combines even closer, powder is non-breakable, grinding
During lack fresh surface, show that grinding rate is not high but the phenomenon of service life cycle length.Comparative example 1 initially have compared with
High grinding efficiency, but as the extension of circulation time, its grinding efficiency reduce significantly after 72h, comparative example 2 by
In larger and hard particle be present, grinding-material is caused fully to be contacted with glass surface, it is relatively low to be allowed to grinding efficiency, thick
The presence of particle also result in being greatly reduced for its yields.
Claims (4)
- A kind of 1. polishing powder from rare earth containing samarium, it is characterised in that：Its composition is according to the molar ratio：Sm2O3/TREO=1.4×10-4~ 0.014, La2O3/ TREO=0.06~0.12, Pr7O11/TREO=8.6×10-6~0.0047, Nd2O3/TREO=2.97×10-5~ 0.0074, surplus CeO2/ TREO=0.27~0.46.
- A kind of 2. preparation technology of polishing powder from rare earth containing samarium, it is characterised in that：Its production technology is:A, the compound of rare earth is formulated as salting liquid, the molar concentration of the rare-earth salt solution is 0.59~1.78mol/L；B, fluorine-containing precipitating reagent is prepared, after precipitating reagent is prepared as into solution, fluorization agent is slowly added into precipitant solution, stirring is equal It is even, sediment is filtered to remove, takes supernatant；Adjust 1.5~4.5 times that precipitant concentration is rare-earth salt solution molar concentration, fluorine Ion concentration is 0.4~1.0 times of rare-earth salt solution molar concentration；C, material liquid is added into reaction vessel, is warming up to 90~96 DEG C；D, fluorine-containing precipitating reagent is added into reaction vessel；E, fluorine-containing precipitating reagent is added until system pH is 7.0, whole building-up process control time is 0.5~5h；F, by sediment washing and filtering, 4~36h is dried at 300~650 DEG C；G, material drying is calcined into 6~12h at 960~1150 DEG C；H, polishing powder from rare earth containing samarium of the present invention can be obtained by calcined product being crushed into classification.
- A kind of 3. preparation technology of polishing powder from rare earth containing samarium according to claim 2, it is characterised in that：By rare earth compound It is formulated as the salting liquid of rare earth nitrades, rare earth sulfate, rare earth-iron-boron or rare earth carbonate.
- A kind of 4. preparation technology of polishing powder from rare earth containing samarium according to claim 2, it is characterised in that：Fluorine-containing precipitating reagent is Ammonium hydrogen carbonate, sodium carbonate or ammonium carbonate and fluorization agent ammonium fluoride, sodium fluoride, ammonium acid fluoride or hydrogen fluoride solution any appoint More than one mixed solution.
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| CN109111856A (en) * | 2018-08-24 | 2019-01-01 | 甘肃稀土新材料股份有限公司 | A kind of lanthanum cerium yttrium element polishing powder and its preparation process |
| CN111252798A (en) * | 2020-01-21 | 2020-06-09 | 包头稀土研究院 | Method for preparing rare earth fluoride particles under alkaline condition and application of alkaline substance |
| CN111252798B (en) * | 2020-01-21 | 2022-05-24 | 包头稀土研究院 | Method for preparing rare earth fluoride particles under alkaline condition and use of alkaline substance |
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