CN107201178B - A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder - Google Patents
A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder Download PDFInfo
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- CN107201178B CN107201178B CN201710389350.5A CN201710389350A CN107201178B CN 107201178 B CN107201178 B CN 107201178B CN 201710389350 A CN201710389350 A CN 201710389350A CN 107201178 B CN107201178 B CN 107201178B
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- carbonate
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- roasting
- polishing powder
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- 238000005498 polishing Methods 0.000 title claims abstract description 63
- 239000000843 powder Substances 0.000 title claims abstract description 46
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 38
- JSKUQVBNGZGWIN-UHFFFAOYSA-N [Ce].[Pr] Chemical compound [Ce].[Pr] JSKUQVBNGZGWIN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims abstract description 16
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims abstract description 14
- 238000000975 co-precipitation Methods 0.000 claims abstract description 14
- XIRHLBQGEYXJKG-UHFFFAOYSA-H praseodymium(3+);tricarbonate Chemical compound [Pr+3].[Pr+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O XIRHLBQGEYXJKG-UHFFFAOYSA-H 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052777 Praseodymium Inorganic materials 0.000 abstract description 4
- 239000005304 optical glass Substances 0.000 abstract description 4
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052684 Cerium Inorganic materials 0.000 abstract description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000005245 sintering Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 230000032683 aging Effects 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- -1 rare earth zirconium oxide Chemical class 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000165940 Houjia Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention discloses a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, comprise the following steps：Zirconium carbonate, cerous carbonate, praseodymium carbonate are mixed with hydrochloric acid solution, obtain mixed solution；The mixed solution is added into aqueous slkali under stirring, precipitation reaction occurs, obtains the co-precipitation of zirconium oxycarbonate cerium praseodymium；Zirconium oxycarbonate cerium praseodymium co-precipitation is subjected to first time roasting, crushing successively, is calcined for second, obtains cerium praseodymium stabilizing zirconia polishing powder.The present invention in zirconium oxide polishing powder by adulterating two kinds of cerium, praseodymium elements, and by first time roasting, crush, be calcined obtained polishing powder for the second time there is higher removal speed and relatively low micro- scuffing rank, the polishing performance of polishing powder is improved, meets market to high accuracy, the demand of large-aperture optical glass lens.
Description
Technical field
The present invention relates to the preparation method of polishing material preparation field, more particularly to cerium praseodymium stabilizing zirconia polishing powder.
Background technology
With the development of science and technology market is increasing to the demand of high accuracy, large-aperture optical glass lens, to high hard
The demand of degree polishing product is also growing day by day.Chemically mechanical polishing is the novel polishing for being combined chemical attack and mechanical grinding
Technology, acted synergistically by polishing the chemical attack of slurry and the grinding of ultramicron, polishing workpiece surface is planarized
Processing.Therefore, a kind of good polishing powder of combination property is selected for being met the products such as glass of market needs to closing weight
Will.
For glass polishing, currently used polishing powder has cerium oxide, zirconium oxide and iron oxide.Wherein cerium oxide polishing speed
Rate is high, surface of polished easy cleaning, is to apply most polishing powders, but polishing powder from rare earth is expensive, and stock number is increasingly
Reduce, therefore, it is significant to develop non-polishing powder from rare earth.Rather than in polishing powder from rare earth zirconium oxide polishing performance relatively
It is good, but polishing performance is less than the polishing performance of polishing powder from rare earth, therefore, how zirconium oxide polishing powder to be adjusted, is optimized
As the subject matter studied at this stage.
The preparation technology of Fe2O3 doping zirconium oxide polishing fluid, obtained polishing fluid are disclosed in patent document CN103450813A
Defective products rate have dropped 1%, reach and imported product identical defective products rate；Open what thunder etc. was delivered《Fe2O3 doping oxygen is used in polishing
Change preparation and the sign of zirconium powder》In, in order to improve the polishing performance of zirconium oxide polishing powder, the doping iron member in zirconium oxide polishing powder
Element.It is to improve the polishing performance of polishing powder by the way that ferro element is doped into zirconium oxide polishing powder in the prior art above,
But the removal speed of polishing powder is made about in 3.3-3.5 μm/min in it, less than imported product removal speed (3.6-3.8 μm/
min)。
The content of the invention
It is an object of the invention to provide a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, system provided by the invention
The cerium praseodymium stabilizing zirconia polishing powder that Preparation Method obtains has higher removal speed, improves the processing efficiency of polishing powder.
The invention provides a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, comprise the following steps：
(1) zirconium carbonate, cerous carbonate, praseodymium carbonate are mixed with hydrochloric acid solution, obtains mixed solution；
(2) mixed solution is added into aqueous slkali under stirring, precipitation reaction occurs, obtains zirconium oxycarbonate cerium
Praseodymium is co-precipitated；
(3) zirconium oxycarbonate cerium praseodymium co-precipitation is subjected to first time roasting, crushing successively, be calcined for second, obtained
Cerium praseodymium stabilizing zirconia polishing powder.
Preferably, also include after second of roasting：Product of roasting is classified, obtains the product of different median particle diameters.
Preferably, the impurity content of the zirconium carbonate, cerous carbonate and praseodymium carbonate is less than 100ppm.
Preferably, the mass ratio of the zirconium carbonate, cerous carbonate and praseodymium carbonate is 180~480：15-20：1.
Preferably, the frequency of the stirring is 20-30Hz, and the temperature of mixed solution is 50-60 DEG C when adding aqueous slkali.
Preferably, the alkali in the aqueous slkali is the mass ratio 1- of sodium hydroxide and sodium carbonate, sodium hydroxide and sodium carbonate
2:1。
Preferably, the addition speed of the aqueous slkali is 80-120ml/min；Sodium hydroxide and carbonic acid in the aqueous slkali
The total mass concentration of sodium is 100-130g/L.
Preferably, the temperature of roasting is 620-660 DEG C, time 2-8h for the first time, is warming up to roasting final value temperature for the first time
The speed of degree is 100-150 DEG C/h.
Preferably, the first time product of roasting is crushed to median particle diameter as 1.0-1.3 μm.
Preferably, the temperature of second of roasting is 680~720 DEG C, time 2-8h, is warming up to second of roasting final value temperature
The speed of degree is 80-100 DEG C/h.
Beneficial effect：The application compensate for aoxidizing by adding two kinds of a small amount of cerium, praseodymium elements in zirconium oxide polishing powder
The performance deficiency of zirconium polishing powder one-component, and the higher oxide of activity is obtained by first time calcination procedure, then by it
Crushing obtains the big little particle of surface-active, then is calcined by second, obtains active high and crystal phase structure and more completely polishes
Powder particles, so as to improve the removal speed of polishing powder, and reduce the larger glass of abrasion degree and ultra-thin glass is processed
Micro- scuffing in journey simultaneously improves the yields of polishing powder.The preparation method is simple, cost is low.Therefore, the cerium that the application provides
Praseodymium stabilizing zirconia polishing powder meets market to high accuracy, the demand of large-aperture optical glass lens.
Embodiment
The invention provides a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, comprise the following steps：
(1) zirconium carbonate, cerous carbonate, praseodymium carbonate are mixed with hydrochloric acid solution, obtains mixed solution；
(2) mixed solution is added into aqueous slkali under stirring, precipitation reaction occurs, obtains zirconium oxycarbonate cerium
Praseodymium is co-precipitated；
(3) zirconium oxycarbonate cerium praseodymium co-precipitation is subjected to first time roasting, crushing successively, be calcined for second, obtained
Cerium praseodymium stabilizing zirconia polishing powder.
In the present invention, the source of raw material, which does not have, to be limited, and only need to ensure that the impurity of zirconium carbonate, cerous carbonate and praseodymium carbonate contains
Amount is less than 100ppm.
In the present invention, the mass ratio of zirconium carbonate, cerous carbonate and praseodymium carbonate is preferably 180~480：15-20：1, more preferably
180~200:19:1.
In the present invention, after preferably mixing zirconium carbonate, cerous carbonate, praseodymium carbonate with water, hydrochloric acid is added, obtains mixing molten
Liquid；The addition of the water be zirconium carbonate, cerous carbonate, 8-11 times of praseodymium carbonate gross mass.
In the present invention, the mass concentration of the hydrochloric acid is 5-10%；Addition is preferably can be by zirconium carbonate, cerous carbonate and carbon
1.05-1.1 times of the theoretical molar amount that sour praseodymium is completely dissolved.
After obtaining mixed solution, the present invention heats the mixed solution, and adds under stirring into mixed solution
Enter aqueous slkali.In the present invention, the alkali in the aqueous slkali is preferably sodium hydroxide and sodium carbonate；The sodium hydroxide and sodium carbonate
Mass ratio be preferably 1-2:1, more preferably 1:1.In the present invention, the temperature of mixed solution is preferably when adding aqueous slkali
50-60℃；The frequency of the stirring is preferably 20-30Hz, more preferably 20-25Hz；
In the present invention, the total mass concentration of sodium hydroxide and sodium carbonate is 100-130g/L in the aqueous slkali, is preferably
120g/L, the addition speed of the aqueous slkali is 80-120ml/min, preferably 80-100ml/min, when the pH of mixed liquor is
During 5.5-7, stop adding aqueous slkali.In the present invention, after mixed solution and the aqueous slkali mixing, it is small to be preferably aged 8-12
When, obtain the co-precipitation of zirconium oxycarbonate cerium praseodymium.
In the present invention, after obtaining the co-precipitation of zirconium oxycarbonate cerium praseodymium, it is preferably used into deionized water washing by soaking, washed every time
Wash be calculated as co-precipitation by volume with the amount of deionized water 3 times, washing by soaking 4~5 times；With centrifuge by alkali after the completion of washing
The co-precipitation of formula zirconium carbonate cerium praseodymium dries.
Dried zirconium oxycarbonate cerium praseodymium co-precipitation after, the present invention by described zirconium oxycarbonate cerium praseodymium be co-precipitated into
Row is calcined for the first time.In the present invention, the temperature of the first time roasting is preferably 620-660 DEG C, more preferably 630-650 DEG C,
Time is 2-8h；The speed for being warming up to roasting final observation for the first time is preferably 100-150 DEG C/h.
After the first time roasting, the present invention crushes obtained product, and product is preferably through gas after the first time roasting
Stream pulverizer is crushed to median particle diameter as 1.0-1.3 μm.
After obtaining crushed products, the product after the crushing is carried out second and is calcined by the present invention.In the present invention, described
The temperature of after baking is preferably 680~720 DEG C, more preferably 700~720 DEG C, time 2-8h；It is warming up to second of roasting
The speed of final observation is preferably 80-100 DEG C/h.
In the present invention, the calciner of roasting and second of roasting is unrestricted for the first time.
In the present invention, also include after second of roasting：Product of roasting is classified, obtains the production of different median particle diameters
Product；Preferably, grading is classified from Jet Classifier for Super, by the product of three kinds of different median particle diameters of production sharing.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.It is aobvious
So, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the reality in the present invention
Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, is all belonged to
In the scope of protection of the invention.
The impurity content of oxide spinel zirconium, cerous carbonate and the praseodymium carbonate selected in embodiment is less than 100ppm.Divide after roasting
The product that level obtains judges micro- scuffing rank according to grinding value, specifically refers to《MILSTD (MIL-PRF-
13830B)》；According to《Polishing powder from rare earth country examination criteria》(GB/T20165-2012) the removal speed of test product.
Embodiment 1
20kg deionized waters are added in a kettle, stir lower addition 1.8kg zirconium carbonates, 0.19kg cerous carbonates and 0.01kg
Carbonic acid is composed, and is then added the hydrochloric acid solution that mass concentration is 5% and is dissolved, until raw material is completely dissolved, then heated solution
To 50 DEG C, in the case where stirring frequency is 20Hz stirring, hydroxide of the concentration as 120g/L is added using 90ml/min speed
The mass ratio of the mixed solution of sodium and sodium carbonate, sodium hydroxide and sodium carbonate is 1:1, until the pH of solution is 6.5, obtain alkali formula
Zirconium carbonate cerium praseodymium is co-precipitated, room temperature ageing 8H；By the zirconium oxycarbonate cerium praseodymium co-precipitation deionized water washing by soaking 4 after ageing
Secondary, the dosage of each deionized water is 3 times of precipitation volume, after entering centrifuge drying after the completion of washing, by the coprecipitated of drying
Form sediment and load kiln progress first time roasting, sintering temperature is 620 DEG C, time 3h, is warming up to the speed of first time sintering temperature
For 100 DEG C/h, roasting for the first time is crushed product with airslide disintegrating mill after terminating, until it is 1.0-1.3 μ to be crushed to median particle diameter
During m, stop crushing, carry out second with crushed products are placed in kiln and be calcined, the temperature of roasting is 680 DEG C, and the time is
4h, the speed for being warming up to second of sintering temperature are 80 DEG C/h, roasting cooled down after terminating it is standby, by second of product of roasting with penetrating
Current classifier is classified to it, obtains the cerium praseodymium stabilizing zirconia polishing powder of three kinds of different median particle diameters, its median particle diameter point
Wei not be 0.4-0.6 μm, 0.9-1.1 μm and 1.4-1.7 μm.
The performance of three kinds of obtained different median particle diameter polishing powders refers to table 1.
Embodiment 2
Add 20kg deionized waters in a kettle, stir it is lower add 2.4kg zirconium carbonates, 0.095kg cerous carbonates and
0.005kg carbonic acid is composed, and is then added the hydrochloric acid solution that mass concentration is 6% and is dissolved, until raw material is completely dissolved, Ran Houjia
Hot solution is to 60 DEG C, and in the case where stirring frequency is 25Hz stirring, concentration is added as 110g/L's using 100ml/min speed
The mass ratio of the mixed solution of sodium hydroxide and sodium carbonate, sodium hydroxide and sodium carbonate is 2:1, until the pH of solution is 6.0, obtain
It is co-precipitated to zirconium oxycarbonate cerium praseodymium, room temperature ageing 10H；Zirconium oxycarbonate cerium praseodymium co-precipitation after ageing is soaked with deionized water
Foam washing is washed 5 times, and the dosage of each deionized water is 3 times of precipitation volume, after entering centrifuge drying after the completion of washing, will be dried
Co-precipitation load kiln carry out first time roasting, sintering temperature be 660 DEG C, time 4h, be warming up to first time sintering temperature
Speed be 150 DEG C/h, roasting is crushed product with airslide disintegrating mill after terminating for the first time, until being crushed to median particle diameter and being
At 1.0-1.3 μm, stop crushing, with crushed products are placed in kiln be calcined for the second time, the temperature of roasting is 700
DEG C, time 4h, the speed for being warming up to second of sintering temperature is 80 DEG C/h, and roasting cools down standby, second of roasting of general after terminating
Burn product to be classified it with Jet Classifier for Super, obtain the cerium praseodymium stabilizing zirconia polishing powder of three kinds of different median particle diameters, its
Median particle diameter is respectively 0.4-0.6 μm, 0.9-1.1 μm and 1.4-1.7 μm.
The performance of three kinds of obtained different median particle diameter polishing powders refers to table 1.
Embodiment 3
20kg deionized waters are added in a kettle, stir lower addition 2.0kg zirconium carbonates, 0.19kg cerous carbonates and 0.01kg
Carbonic acid is composed, and is then added the hydrochloric acid solution that mass concentration is 10% and is dissolved, until raw material is completely dissolved, then heated solution
To 50 DEG C, in the case where stirring frequency is 30Hz stirring, hydroxide of the concentration as 130g/L is added using 120ml/min speed
The mass ratio of the mixed solution of sodium and sodium carbonate, sodium hydroxide and sodium carbonate is 1:1, until the pH of solution is 6.5, obtain alkali formula
Zirconium carbonate cerium praseodymium is co-precipitated, room temperature ageing 12H；By the zirconium oxycarbonate cerium praseodymium co-precipitation deionized water washing by soaking after ageing
4 times, the dosage of each deionized water is 3 times of precipitation volume, after entering centrifuge drying after the completion of washing, by the coprecipitated of drying
Form sediment and load the roasting of kiln progress first, sintering temperature is 660 DEG C, time 2.5h, is warming up to the speed of first time sintering temperature
For 120 DEG C/h, roasting for the first time is crushed product with airslide disintegrating mill after terminating, until it is 1.0-1.3 μ to be crushed to median particle diameter
During m, stop crushing, carry out second with crushed products are placed in kiln and be calcined, the temperature of roasting is 720 DEG C, and the time is
3h, the speed for being warming up to second of sintering temperature are 100 DEG C/h, and roasting cools down standby after terminating, second product of roasting is used
Jet Classifier for Super is classified to it, obtains the cerium praseodymium stabilizing zirconia polishing powder of three kinds of different median particle diameters, its median particle diameter
Respectively 0.4-0.6 μm, 0.9-1.1 μm and 1.4-1.7 μm.
The performance of three kinds of obtained different median particle diameter polishing powders refers to table 1.
Table 1
The result described in table 1, cerium praseodymium stabilizing zirconia polishing powder made from the application, it removes speed in 3.9-
4.2 μm/min, micro- scuffing rank can reach 0 grade, either removes speed or micro- scuffing rank is superior to domestic existing polishing
Product and import polishing powder, achieve definitely technological progress, meet market to high accuracy, the need of large-aperture optical glass lens
Ask.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (2)
1. a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, comprises the following steps：
(1) zirconium carbonate, cerous carbonate, praseodymium carbonate are mixed with hydrochloric acid solution, obtain mixed solution, the zirconium carbonate, cerous carbonate and
The impurity content of praseodymium carbonate is less than 100ppm, and the mass ratio of the zirconium carbonate, cerous carbonate and praseodymium carbonate is 180~480：15-20：
1；
(2) mixed solution is added into aqueous slkali under stirring, precipitation reaction occurs, obtains zirconium oxycarbonate cerium praseodymium and is total to
Precipitation, the frequency of the stirring is 20-30Hz, and the temperature of mixed solution is 50-60 DEG C when adding aqueous slkali, in the aqueous slkali
Alkali be sodium hydroxide and sodium carbonate, sodium hydroxide and sodium carbonate mass ratio 1-2:1, the addition speed of the aqueous slkali is
80-120ml/min；The total mass concentration of sodium hydroxide and sodium carbonate is 100-130g/L in the aqueous slkali；
(3) zirconium oxycarbonate cerium praseodymium co-precipitation is subjected to first time roasting, crushing successively, be calcined for second, obtain cerium praseodymium
Stabilizing zirconia polishing powder, the temperature of roasting is 620-660 DEG C, time 2-8h for the first time, is warming up to roasting final value for the first time
The speed of temperature is 100-150 DEG C/h, and the first time product of roasting is crushed to median particle diameter as 1.0-1.3 μm, second of roasting
The temperature of burning is 680~720 DEG C, time 2-8h, and the speed for being warming up to second of roasting final observation is 80-100 DEG C/h.
2. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：Second of roasting
Also include after burning：Product of roasting is classified, obtains the product of different median particle diameters.
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| CN102352188A (en) * | 2011-09-05 | 2012-02-15 | 上海华明高纳稀土新材料有限公司 | Precision cerium-zirconium-based solid solution rare earth polishing powder and preparation method thereof |
| CN102559064A (en) * | 2011-12-15 | 2012-07-11 | 上海华明高纳稀土新材料有限公司 | Cerium-zirconium praseodymium sosoloid and preparation method thereof |
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| CN102352188A (en) * | 2011-09-05 | 2012-02-15 | 上海华明高纳稀土新材料有限公司 | Precision cerium-zirconium-based solid solution rare earth polishing powder and preparation method thereof |
| CN102559064A (en) * | 2011-12-15 | 2012-07-11 | 上海华明高纳稀土新材料有限公司 | Cerium-zirconium praseodymium sosoloid and preparation method thereof |
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