CN102585708A - Rare earth polishing material and preparation method thereof - Google Patents
Rare earth polishing material and preparation method thereof Download PDFInfo
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- CN102585708A CN102585708A CN2012100655907A CN201210065590A CN102585708A CN 102585708 A CN102585708 A CN 102585708A CN 2012100655907 A CN2012100655907 A CN 2012100655907A CN 201210065590 A CN201210065590 A CN 201210065590A CN 102585708 A CN102585708 A CN 102585708A
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Abstract
The invention aims to disclose a rare earth polishing material and a preparation method thereof. The rare earth polishing material comprises the following components by weight part: 65 to 98 parts of rare earth polishing powder, 1 to 5 parts of dispersant, 5 to 30 parts of suspension, and 0.05 to 0.3 part of pH regulator. Compared with the conventional product, the invention has the advantages as follows: the polishing powder is a crystalline homogeneous solid solution composed of oxyfluoride rare earth and cubic phase rare earth oxide; the suspension property of the prepared rare earth polishing material is good, and the polishing powder product is good in wear resistance, high in polishing speed and easy to control in polishing accuracy; and the product is good in homogeneity, high in production efficiency and low in cost, is free from contamination, and is applicable to surface polishing of precise devices in the electronic information industry, such as integrated circuits, two-dimensional displays and optical glass, so as to achieve the purposes of the invention.
Description
Technical field
The present invention relates to a kind of rare-earth polishing material and preparation method thereof, particularly a kind ofly be applicable to that unicircuit, plane show and the cerium base mishmetal polishing material of the surface finish of electronics and information industry accurate devices such as opticglass and preparation method thereof.
Background technology
At present, various glass materials are widely used, and these materials all need pass through necessary surface finish before being employed.The early stage main materials such as zirconium white, red stone or silicon-dioxide that use polish various glass surfaces; In recent years; Consider that from polishing efficiency and precision aspect rare earth oxide (particularly cerium oxide) is considered to be more suitable for the surface finish in glass material for the polishing material of staple.
Fast development along with electronic information technology; The demand of glass baseplates such as lens, sheet glass, liquid-crystal display (LCD), glasses, optical element and stupalith increases greatly; Precision and polishing speed for polishing material are also had higher requirement; This just impels manufacturer to improve constantly product specification, the rare earth application product that to adapt to the requirement of new technology product innovation, that polishing powder from rare earth has become is applied widely now, consumption is big, with high content of technology.
It is raw material that early stage polishing powder from rare earth adopts hamartite; Like the Chinese patent patent publication No. is that the patent of invention of CN101215446A discloses the method that a kind of rare earth ore concentrate prepares high cerium nanometer scale polishing powder from rare earth, from rare earth ore concentrate concentrated sulfuric acid roasting, infusion, directly makes mixed rare earth carbonate with hydrogen-carbonate by the precipitator method; Mixed rare earth carbonate mixes with alkali, is heated to fusion, and is incubated 1-4 hour in molten state, cools off, pulverizes, adds industrial hydrofluoric acid then, obtains fluorine rare earth oxide enriched substance; The rare enriched substance of fluorine oxidation is pulverized, washing; Drainage, even in stirrer for mixing, in the band sieve high energy ball mill of packing into then; Charge into nitrogen, carry out the wet-milling high-energy ball milling, the below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel; Undersized powder dries processing to the moisture of powder under high velocity air promotes, dry again handle polishing powder from rare earth.
The Chinese patent patent publication No. is that the patent of invention of CN101899281A discloses a kind of polishing powder from rare earth and preparation method thereof, and this invention polishing powder contains cerium oxide, lanthanum trioxide, Praseodymium trioxide, and its total amount of rare earth TERO is more than 90wt%.For guaranteeing necessary polishing speed, in the wet method synthesis procedure, allocate the fluorine element that chemically reacts into, and controlled beginning to take shape of product granularity, make 877-3 type polishing powder from rare earth.
In the market, the more use of preparation method of rare-earth polishing material be the heavy back of first carbon flaorination process, promptly add bicarbonate of ammonia earlier and precipitate, add hydrofluoric acid after the washing again and fluoridize.
Like the Chinese patent patent publication No. is the working method that the patent of invention of CN100497508C discloses a kind of high-cerium rare-earth polishing powder, adds hydrofluoric acid behind the preparation Phosbloc cerium earlier and fluoridizes, and roasting gets high-cerium rare-earth polishing powder.
The polishing powder that adopts above-mentioned existing production technique to produce; Because what adopt is disposable fluoridizing; Have the inhomogeneous or local fluorizated situation of fluoridation, can influence on the one hand the crystal phase structure of product after the roasting, the free state fluorion of can exert an influence on the other hand polishing precision and speed; The agglomerating particles size and the intensity that form after the roasting also have very big difference; And the polishing precision of polishing powder and polishing speed mainly are to be determined by the coacervate particulate size and the agglomeration strength that form behind the high temperature sintering, can cause a series of problems like this, and for example the glass surface in polishing produces cut or polishing speed reduction fast in the very short time; Particularly when throwing the hard glass surface, it is fatal that polishing speed reduces rapidly; The fluorine carbonated rare earth granularity that obtains in the fluorination process simultaneously is less, and the dehydration difficulty has caused output lower.
The polishing powder product that just need pick out certain agglomeration strength, certain particle size in order to satisfy condition, and these characteristics are to be difficult to control, and complex manufacturing, cost increases and introduces foreign ion, causes quality fluctuation.
In addition, be that the patent of invention of CN101010402A discloses rare earth oxide is mixed with rare earth fluoride like the Chinese patent patent publication No., prepare the method for polishing powder from rare earth through grinding, drying, roasting, classification.The rare earth fluoride particle is thinner, and aftertreatment technology is complicated; Use the also more complicated of technology that is mixed of fluorochemical and oxide compound simultaneously; This method can produce the phenomenon of particle double sintering, and the part particle produces unusual growth through re-baking, forms partial big particle, thereby in polishing process, causes scuffing.
Simultaneously, the polishing powder from rare earth true density is bigger, causes polishing powder in use to precipitate easily, causes the utilization ratio of polishing powder lower.
Therefore, need a kind of rare-earth polishing material and preparation method thereof especially, solved the problem of above-mentioned existing existence.
Summary of the invention
The object of the present invention is to provide a kind of rare-earth polishing material and preparation method thereof, overcome prior art and have above-mentioned problem, have that median size is little, narrow particle size distribution, suspension is good, polishing speed is fast and characteristics such as polishing precision height.
To achieve these goals, technical scheme of the present invention is following:
On the one hand, the present invention provides a kind of rare-earth polishing material, it is characterized in that, it comprises the component of following weight part: polishing powder from rare earth: 65-98 part, dispersion agent: 1-5 part, suspensoid: 5-30 part and pH regulator agent: 0.05-0.3 part.
In one embodiment of the invention, said polishing powder from rare earth is by the crystal formation homogeneous sosoloid that to be the oxyfluoride rare earth form with rare earth oxide cube mutually.
In one embodiment of the invention, said dispersion agent is an acrylic polymers, is selected from Vestolen PP 7052, ZX-I a kind of.
In one embodiment of the invention, said suspensoid is a polysaccharide polymer, is selected from Microcrystalline Cellulose, agaropectin, guar gum, my glue, carrageenin, the one or more combination of Schardinger dextrins.
In one embodiment of the invention, said pH regulator agent is selected from sodium hydrogencarbonate, yellow soda ash, the one or more combination of sodium hydroxide.
On the other hand, the present invention provides a kind of preparation method of rare-earth polishing material, it is characterized in that, it comprises the steps:
(1) preparation of polishing powder from rare earth:
Fluoridize: carbonated rare earth is mixed with water; Be heated to 30-50 ℃; Under agitation condition, drip a certain amount of 20% hydrofluoric acid solution, drip and finish the back and add the ammonium bicarbonate aqueous solution that uses 10-15% and be adjusted to pH and be 6.5-7, be heated to 70-90 ℃; Insulation 5-10h obtains partially fluorinated carbonated rare earth slurry;
Dehydration and dry: will partially fluorinated carbonated rare earth slurry after dewatering, at 120-200 ℃ of dry 10-20h;
Roasting: above-mentioned product at 950-1100 ℃ of roasting 4-6h, is obtained rare earth oxyfluoride;
Pulverize and classification: the rare earth oxyfluoride that obtains through pulverizing, classification, is got the polishing powder from rare earth of meso-position radius D50:0.8-3.0 μ m;
(2) preparation of rare-earth polishing material:
With the polishing powder from rare earth that obtains and dispersion agent, suspensoid, pH regulator agent thorough mixing proportionally, obtain described rare-earth polishing material.
In one embodiment of the invention, said carbonated rare earth is selected from a kind of in Phosbloc cerium or the carbonic acid La-Ce-Pr.
In one embodiment of the invention, the consumption of said 20% hydrofluoric acid solution is a 80-160kg/ ton carbonated rare earth.
In one embodiment of the invention, the grinding mode of said pulverizing is selected from fluidized bed airflow pulverizing or mechanical disintegration; Said hierarchical approaches is dry classification or wet classification.
Rare-earth polishing material of the present invention and preparation method thereof is compared with existing product, and it is the oxyfluoride rare earth and the homogeneous sosoloid of rare earth oxide composition cube mutually that polishing powder adopts crystal formation; The suspension of the rare-earth polishing material that makes is good, and the wear resistance of product polishing powder is good, and polishing speed is fast, and the polishing precision is controlled easily; The homogeneity of product is good, and production efficiency is high, and cost is low, pollution-free, is applicable to the surface finish processing of the accurate close device of electronics and information industries such as unicircuit, plane demonstration, opticglass, realizes the object of the invention.
Characteristics of the present invention can consult this case graphic and below better embodiment detailed description and obtain to be well understood to.
Description of drawings
Fig. 1 is the XRD synoptic diagram of embodiments of the invention 1 gained mishmetal polishing powder;
Fig. 2 is the XRD synoptic diagram of embodiments of the invention 2 gained mishmetal polishing powders;
Fig. 3 is the XRD synoptic diagram of Comparative Examples 1 gained mishmetal polishing powder of the present invention.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, further set forth the present invention below in conjunction with specific embodiment.
On the one hand, rare-earth polishing material of the present invention, it comprises the component of following weight part: polishing powder from rare earth: 65-98 part, dispersion agent: 1-5 part, suspensoid: 5-30 part and pH regulator agent: 0.05-0.3 part.
In the present invention, said polishing powder from rare earth is by the crystal formation homogeneous sosoloid that to be the oxyfluoride rare earth form with rare earth oxide cube mutually.
In the present invention, said dispersion agent is an acrylic polymers, is selected from Vestolen PP 7052, ZX-I a kind of.
In the present invention, said suspensoid is a polysaccharide polymer, is selected from Microcrystalline Cellulose, agaropectin, guar gum, my glue, carrageenin, the one or more combination of Schardinger dextrins.
In the present invention, said pH regulator agent is selected from sodium hydrogencarbonate, yellow soda ash, the one or more combination of sodium hydroxide.
On the other hand, the preparation method of rare-earth polishing material of the present invention, it comprises the steps:
(1) preparation of polishing powder from rare earth:
Fluoridize: carbonated rare earth is mixed with water; Be heated to 30-50 ℃; Under agitation condition, drip a certain amount of 20% hydrofluoric acid solution, drip and finish the back and add the ammonium bicarbonate aqueous solution that uses 10-15% and be adjusted to pH and be 6.5-7, be heated to 70-90 ℃; Insulation 5-10h obtains partially fluorinated carbonated rare earth slurry;
Dehydration and dry: will partially fluorinated carbonated rare earth slurry after dewatering, at 120-200 ℃ of dry 10-20h;
Roasting: above-mentioned product at 950-1100 ℃ of roasting 4-6h, is obtained rare earth oxyfluoride;
Pulverize and classification: the rare earth oxyfluoride that obtains through pulverizing, classification, is got meso-position radius D
50: the polishing powder from rare earth of 0.8-3.0 μ m;
(2) preparation of rare-earth polishing material:
With the polishing powder from rare earth that obtains and dispersion agent, suspensoid, pH regulator agent thorough mixing proportionally, obtain described rare-earth polishing material.
In the present invention, said carbonated rare earth is selected from a kind of in Phosbloc cerium or the carbonic acid La-Ce-Pr.
In the present invention, the consumption of said 20% hydrofluoric acid solution is a 80-160kg/ ton carbonated rare earth.
In the present invention, the grinding mode of said pulverizing is selected from fluidized bed airflow pulverizing or mechanical disintegration; Said hierarchical approaches is dry classification or wet classification.
Embodiment 1
1000kg Phosbloc cerium is mixed with 1000kg water, is heated to 30 ℃, drip 20% hydrofluoric acid 80kg, drip and finish post-heating to 70 ℃, insulation 10h, partially fluorinated Phosbloc cerium slurries; With the partially fluorinated Phosbloc cerium slurries that obtain through centrifuge dehydration, 200 ℃ of dry 10h, 1100 ℃ of roasting 4h.Through comminution by gas stream and classification, get polishing powder from rare earth then.Through laser particle analyzer test, product D
50=0.81 μ m, XRD result sees Fig. 1.
With 98 parts of polishing powder from rare earth, 1 part of ROHM, 1 part of Microcrystalline Cellulose, 0.05 part of sodium hydrogencarbonate thorough mixing, get described rare-earth polishing material.
1000kg carbonic acid La-Ce-Pr is mixed with 1000kg water, is heated to 50 ℃, drip 20% hydrofluoric acid 160kg, drip and finish post-heating to 90 ℃, insulation 5h, partially fluorinated carbonic acid La-Ce-Pr slurries; With the partially fluorinated carbonic acid La-Ce-Pr slurries that obtain through centrifuge dehydration, 120 ℃ of dry 20h, 950 ℃ of roasting 6h; Through comminution by gas stream and classification, get polishing powder from rare earth then.Through laser particle analyzer test, product D
50=2.98 μ m, XRD result sees Fig. 2.
With 65 parts of rare polishing powder from rare earth, 5 parts of ROHM, 10 parts of agaropectins, 15 parts of guar gums, 5 parts of my glue, 0.3 part of yellow soda ash thorough mixing, described rare-earth polishing material.
Embodiment 3
1000kg carbonic acid La-Ce-Pr is mixed with 1000kg water, is heated to 400 ℃, drip 20% hydrofluoric acid 100kg, drip and finish post-heating to 80 ℃, insulation 4h, partially fluorinated carbonic acid La-Ce-Pr slurries; With the partially fluorinated carbonic acid La-Ce-Pr slurries that obtain through centrifuge dehydration, 160 ℃ of dry 12h, 990 ℃ of roasting 5h, then through comminution by gas stream and classification, polishing powder from rare earth.Through laser particle analyzer test, product D
50=1.80 μ m.
With rare 79.98 parts of polishing powder from rare earth, 5 parts of ROHM, 15 parts of Schardinger dextrins, 0.2 part of sodium hydroxide thorough mixing, get described rare-earth polishing material.
Embodiment 4
The polishing performance appreciation condition and the evaluation result of polishing material are following:
Get rare-earth polishing material 500g, add deionized water to 5L, getting concentration is the polishing fluid slurries of 100g/L.Adopt UNIPOL802 (Shenyang section is brilliant) precise grinding polisher that K9 glass is polished, automatic stirring to pulp, filtration cycle is used, and polishing arbor rotating speed is 100 rev/mins, and pressure is 660N/cm
2, the polishing skin is KSP66B-1.25, polishing time is 6.5 hours, tests the granularity and the dried weight of glass of record washing of slurries at regular intervals.Mass Calculation according to the polished front and back of take by weighing polishing element goes out difference, and this difference is the erosion amount of throwing divided by polishing time.Polishing performance calculates with relative polishing speed, counts 100, average throwing erosion amount * 100% of average throwing erosion amount/Comparative Examples 1 of the relative polishing speed=embodiment of all the other products with the average throwing erosion amount of the polishing material of Comparative Examples 1 gained
Comparative Examples 1
1000kg Phosbloc cerium is mixed with 1000kg water, is heated to 30 ℃, drip 20% hydrofluoric acid 80kg, drip and finish post-heating to 70 ℃, insulation 10h, partially fluorinated Phosbloc cerium slurries; With the partially fluorinated Phosbloc cerium slurries that obtain through centrifuge dehydration, 200 ℃ of dry 10h, 1100 ℃ of roasting 4h.Through comminution by gas stream and classification, get polishing powder from rare earth then.Through laser particle analyzer test, product D
50=0.82 μ m, XRD result sees Fig. 3.
The data contrast of embodiment and Comparative Examples is referring to table 1
Table 1
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; The present invention is not restricted to the described embodiments; What describe in the foregoing description and the specification sheets is principle of the present invention; The present invention also has various changes and modifications under the prerequisite that does not break away from spirit and scope of the invention, and these variations and improvement all fall in the scope of the present invention that requires protection.The protection domain that the present invention requires is defined by appending claims and equivalent thereof.
Claims (9)
1. a rare-earth polishing material is characterized in that, it comprises the component of following weight part: polishing powder from rare earth: 65-98 part, dispersion agent: 1-5 part, suspensoid: 5-30 part and pH regulator agent: 0.05-0.3 part.
2. rare-earth polishing material according to claim 1 is characterized in that, said polishing powder from rare earth is by the crystal formation homogeneous sosoloid that to be the oxyfluoride rare earth form with rare earth oxide cube mutually.
3. rare-earth polishing material according to claim 1 is characterized in that said dispersion agent is an acrylic polymers, is selected from Vestolen PP 7052, ZX-I a kind of.
4. rare-earth polishing material according to claim 1 is characterized in that said suspensoid is a polysaccharide polymer, is selected from Microcrystalline Cellulose, agaropectin, guar gum, my glue, carrageenin, the one or more combination of Schardinger dextrins.
5. rare-earth polishing material according to claim 1 is characterized in that, said pH regulator agent is selected from sodium hydrogencarbonate, yellow soda ash, the one or more combination of sodium hydroxide.
6. the preparation method of a rare-earth polishing material is characterized in that, it comprises the steps:
(1) preparation of polishing powder from rare earth:
Fluoridize: carbonated rare earth is mixed with water; Be heated to 30-50 ℃; Under agitation condition, drip a certain amount of 20% hydrofluoric acid solution, drip and finish the back and add the ammonium bicarbonate aqueous solution that uses 10-15% and be adjusted to pH and be 6.5-7, be heated to 70-90 ℃; Insulation 5-10h obtains partially fluorinated carbonated rare earth slurry;
Dehydration and dry: will partially fluorinated carbonated rare earth slurry after dewatering, at 120-200 ℃ of dry 10-20h;
Roasting: above-mentioned product at 950-1100 ℃ of roasting 4-6h, is obtained rare earth oxyfluoride;
Pulverize and classification: the rare earth oxyfluoride that obtains through pulverizing, classification, is got meso-position radius D
50: the polishing powder from rare earth of 0.8-3.0 μ m;
(2) preparation of rare-earth polishing material:
With the polishing powder from rare earth that obtains and dispersion agent, suspensoid, pH regulator agent thorough mixing proportionally, obtain described rare-earth polishing material.
7. preparation method according to claim 6 is characterized in that, said carbonated rare earth is selected from a kind of in Phosbloc cerium or the carbonic acid La-Ce-Pr.
8. preparation method according to claim 6 is characterized in that, the consumption of said 20% hydrofluoric acid solution is a 80-160kg/ ton carbonated rare earth.
9. preparation method according to claim 6 is characterized in that, the grinding mode of said pulverizing is selected from fluidized bed airflow and pulverizes or mechanical disintegration; Said hierarchical approaches is dry classification or wet classification.
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| CN104017500A (en) * | 2014-06-11 | 2014-09-03 | 泰安麦丰新材料科技有限公司 | Preparation method of rare earth polishing powder |
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Application publication date: 20120718 |