CN107201178A - 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
- Publication number
- CN107201178A CN107201178A CN201710389350.5A CN201710389350A CN107201178A CN 107201178 A CN107201178 A CN 107201178A CN 201710389350 A CN201710389350 A CN 201710389350A CN 107201178 A CN107201178 A CN 107201178A
- Authority
- CN
- China
- Prior art keywords
- praseodymium
- polishing powder
- carbonate
- preparation
- cerium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 72
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000000843 powder Substances 0.000 title claims abstract description 54
- JSKUQVBNGZGWIN-UHFFFAOYSA-N [Ce].[Pr] Chemical compound [Ce].[Pr] JSKUQVBNGZGWIN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052726 zirconium Inorganic materials 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
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000000975 co-precipitation Methods 0.000 claims abstract description 15
- 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 15
- 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
- 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 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 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
- 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
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
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, mixed solution is obtained；The mixed solution is added into aqueous slkali under stirring, occurs precipitation reaction, the co-precipitation of zirconium oxycarbonate cerium praseodymium is obtained；Zirconium oxycarbonate cerium praseodymium co-precipitation is subjected to first time roasting, crushing successively, is calcined for second, cerium praseodymium stabilizing zirconia polishing powder is obtained.The present invention passes through cerium, the two kinds of elements of praseodymium of being adulterated in zirconium oxide polishing powder, and be calcined, crushed by first time, being calcined obtained polishing powder for the second time with higher removal speed and relatively low micro- scuffing rank, the polishing performance of polishing powder is improved, market is met 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, it is hard to height
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, is acted synergistically by polishing the chemical attack of slurry and the grinding of ultramicron, polishing workpiece surface is planarized
Processing.Therefore, a kind of products such as the glass of the good polishing powder of combination property for being met market needs are selected to closing weight
Will.
For glass polishing, the polishing powder commonly used at present has cerium oxide, zirconium oxide and iron oxide.Wherein cerium oxide polishing is fast
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, develop non-polishing powder from rare earth significant.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 the system that a kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder, the present invention are provided
The cerium praseodymium stabilizing zirconia polishing powder that Preparation Method is obtained 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, occurs precipitation reaction, obtain 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.
It is preferred that, also include after second of roasting：Product of roasting is classified, the product of different median particle diameters is obtained.
It is preferred that, the impurity content of the zirconium carbonate, cerous carbonate and praseodymium carbonate is less than 100ppm.
It is preferred that, the mass ratio of the zirconium carbonate, cerous carbonate and praseodymium carbonate is 180~480：15-20：1.
It is preferred that, the frequency of the stirring is 20-30Hz, and the temperature of mixed solution is 50-60 DEG C when adding aqueous slkali.
It is preferred that, the alkali in the aqueous slkali is the mass ratio 1- of sodium hydroxide and sodium carbonate, sodium hydroxide and sodium carbonate
2:1。
It is preferred that, 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.
It is preferred that, the temperature of roasting is 620-660 DEG C for the first time, and the time is 2-8h, is warming up to roasting final value temperature for the first time
The speed of degree is 100-150 DEG C/h.
It is preferred that, the first time product of roasting is crushed to median particle diameter for 1.0-1.3 μm.
It is preferred that, the temperature of second of roasting is 680~720 DEG C, and the time is 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 oxidation by adding a small amount of cerium, two kinds of elements of praseodymium 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 the active high and more complete polishing of crystal phase structure
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 and the yields for improving polishing powder.The preparation method is simple, cost is low.Therefore, the cerium that the application is provided
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, occurs precipitation reaction, obtain 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, mixing is obtained 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.
Obtain after mixed solution, the present invention heats the mixed solution, and add 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, preferably it is aged 8-12 small
When, obtain the co-precipitation of zirconium oxycarbonate cerium praseodymium.
In the present invention, obtain after the co-precipitation of zirconium oxycarbonate cerium praseodymium, it is preferably used to 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 is dried.
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 for 1.0-1.3 μm.
Obtain after 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, and more preferably 700~720 DEG C, the time is 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, the production of different median particle diameters is obtained
Product；It is preferred that, 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 a part of embodiment of the 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 all belongs 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 is obtained 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., and stirring is lower to add 1.8kg zirconium carbonates, 0.19kg cerous carbonates and 0.01kg
Carbonic acid is composed, and is then added mass concentration and is dissolved for 5% hydrochloric acid solution, up to 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 consumption of each deionized water is 3 times of precipitation volume, is entered after the completion of washing after centrifuge drying, by the coprecipitated of drying
Form sediment and load kiln progress first time roasting, sintering temperature is 620 DEG C, and the time is 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 being crushed to median particle diameter for 1.0-1.3 μ
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, the time is
4h, the speed for being warming up to second of sintering temperature is 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., stirring is lower add 2.4kg zirconium carbonates, 0.095kg cerous carbonates and
0.005kg carbonic acid is composed, and is then added mass concentration and is dissolved for 6% hydrochloric acid solution, until raw material is completely dissolved, Ran Houjia
Hot solution is to 60 DEG C, in stirring frequency under 25Hz stirring, the speed addition concentration using 100ml/min is 110g/L's
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
To the co-precipitation of 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 consumption of each deionized water is 3 times of precipitation volume, is entered after the completion of washing after centrifuge drying, will be dried
Co-precipitation load kiln carry out first time roasting, sintering temperature be 660 DEG C, the time is 4h, is 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, the time is 4h, and the speed for being warming up to second of sintering temperature is 80 DEG C/h, and roasting cools down standby after terminating, second will roast
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., and stirring is lower to add 2.0kg zirconium carbonates, 0.19kg cerous carbonates and 0.01kg
Carbonic acid is composed, and is then added mass concentration and is dissolved for 10% hydrochloric acid solution, up to 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 consumption of each deionized water is 3 times of precipitation volume, is entered after the completion of washing after centrifuge drying, by the coprecipitated of drying
Form sediment and load the roasting of kiln progress first, sintering temperature is 660 DEG C, and the time is 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 being crushed to median particle diameter for 1.0-1.3 μ
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, the time is
3h, the speed for being warming up to second of sintering temperature is 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 (10)
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, obtains mixed solution；
(2) mixed solution is added into aqueous slkali under stirring, occurs precipitation reaction, obtained zirconium oxycarbonate cerium praseodymium and be total to
Precipitation；
(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.
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, the product of different median particle diameters is obtained.
3. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：The zirconium carbonate,
The impurity content of cerous carbonate and praseodymium carbonate is less than 100ppm.
4. the preparation method of the cerium praseodymium stabilizing zirconia polishing powder as described in claim 1 or 3, it is characterised in that：The carbonic acid
The mass ratio of zirconium, cerous carbonate and praseodymium carbonate is 180~480：15-20：1.
5. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：The frequency of the stirring
Rate is 20-30Hz, and the temperature of mixed solution is 50-60 DEG C when adding aqueous slkali.
6. the preparation method of the cerium praseodymium stabilizing zirconia polishing powder as described in claim 1 or 5, it is characterised in that：The alkali soluble
Alkali in liquid is the mass ratio 1-2 of sodium hydroxide and sodium carbonate, sodium hydroxide and sodium carbonate:1.
7. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 6, it is characterised in that：The aqueous slkali
Addition speed is 80-120ml/min；The total mass concentration of sodium hydroxide and sodium carbonate is 100-130g/L in the aqueous slkali.
8. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：Roasting for the first time
Temperature is 620-660 DEG C, and the time is 2-8h, and the speed for being warming up to roasting final observation for the first time is 100-150 DEG C/h.
9. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：The first time roasting
Burn product and be crushed to median particle diameter for 1.0-1.3 μm.
10. the preparation method of cerium praseodymium stabilizing zirconia polishing powder as claimed in claim 1, it is characterised in that：Second of roasting
Temperature be 680~720 DEG C, the time is 2-8h, be warming up to second of roasting final observation speed be 80-100 DEG C/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710389350.5A CN107201178B (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710389350.5A CN107201178B (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107201178A true CN107201178A (en) | 2017-09-26 |
| CN107201178B CN107201178B (en) | 2018-03-06 |
Family
ID=59905455
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710389350.5A Active CN107201178B (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107201178B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724836A (en) * | 2020-12-24 | 2021-04-30 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
| CN113897177A (en) * | 2021-09-03 | 2022-01-07 | 永州市湘江稀土有限责任公司 | Composite oxide abrasive particle and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006025614A1 (en) * | 2004-09-03 | 2006-03-09 | Showa Denko K.K. | Mixed rare earth oxide, mixed rare earth fluoride, cerium-based abrasive using the materials and production processes thereof |
| 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 |
-
2017
- 2017-05-27 CN CN201710389350.5A patent/CN107201178B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006025614A1 (en) * | 2004-09-03 | 2006-03-09 | Showa Denko K.K. | Mixed rare earth oxide, mixed rare earth fluoride, cerium-based abrasive using the materials and production processes thereof |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724836A (en) * | 2020-12-24 | 2021-04-30 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
| CN112724836B (en) * | 2020-12-24 | 2022-03-29 | 德米特（苏州）电子环保材料有限公司 | Cerium-zirconium-doped polishing solution and preparation method and application thereof |
| CN113897177A (en) * | 2021-09-03 | 2022-01-07 | 永州市湘江稀土有限责任公司 | Composite oxide abrasive particle and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107201178B (en) | 2018-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101899281B (en) | Rare earth polishing powder and production method thereof | |
| CN103571334B (en) | Cerium oxide polishing powder and preparation method thereof | |
| CN112080207B (en) | Preparation method of rare earth polishing powder | |
| CN107201178B (en) | A kind of preparation method of cerium praseodymium stabilizing zirconia polishing powder | |
| CN102850938A (en) | Preparation method of spherical composite rare earth polishing powder | |
| CN105461311B (en) | Sol-gel methods prepare NaNbO3The method that powder and sintering obtain monocrystalline | |
| CN107935007A (en) | The method that after baking prepares alumina with high temperature and low sodium | |
| CN111454666A (en) | High-suspension polishing powder and preparation method thereof | |
| CN108998658A (en) | A method of roasting vanadium extraction | |
| TWI293981B (en) | ||
| CN109704403A (en) | A kind of high tenacity oxidation zirconium base composite powder and preparation method thereof | |
| CN109704759A (en) | A kind of compound rare-earth modified zirconia ceramic powder and preparation method thereof | |
| CN111393998B (en) | Preparation method of lanthanum-cerium modified aluminum oxide composite polishing powder | |
| CN103450813A (en) | Preparation method of iron-doped zirconium oxide polishing solution | |
| CN102337085B (en) | Preparation method of composite cerium-zirconium oxide polishing powder | |
| CN108083333A (en) | It is a kind of to be given up the method that zirconium prepares zirconium aluminium composite granule using solid | |
| CN102329571B (en) | Rare earth and silicon compound precision type rare earth polishing powder and preparation method thereof | |
| CN102775958A (en) | Cerium oxide polishing material for stone grinding tool and preparation method thereof | |
| CN104003707A (en) | Preparing method of barium permanent-magnetic ferrite materials | |
| CN107603491A (en) | Polishing powder from rare earth and preparation method thereof | |
| CN107973332A (en) | A kind of method for preparing high rare-earth content basic carbonate cerium | |
| CN110885637A (en) | Preparation method of rare earth fluoride polishing powder and rare earth fluoride polishing solution | |
| CN102531427A (en) | Steel slag cement for road and preparation method thereof | |
| CN107364884B (en) | A kind of nano zirconium oxide powder preparation method | |
| CN102061108A (en) | Process for whitening pyrophyllite micro powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180131 Address after: 271600 Tai'an City, Shandong Province, Feicheng hi tech Zone West pay Village Industrial Park North Applicant after: TAIAN MAIFENG NEW MATERIAL TECHNOLOGY CO.,LTD. Address before: 271600 Tai'an City, Shandong Province, Feicheng hi tech Zone West pay Village Industrial Park North Applicant before: Yu Changjiang |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 271600 South of Kangwang West Road and North of Industrial Third Road, Feicheng High-tech Zone, Taian City, Shandong Province Patentee after: Shandong Maifeng New Material Science and Technology Co.,Ltd. Address before: 271600 North Head of Xifucun Industrial Park, Feicheng High-tech Zone, Taian City, Shandong Province Patentee before: TAIAN MAIFENG NEW MATERIAL TECHNOLOGY CO.,LTD. |
|
| CP03 | Change of name, title or address | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of cerium and praseodymium stabilized zirconia polishing powder Effective date of registration: 20190807 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2019370000004 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20200731 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2019370000004 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation of cerium praseodymium stabilized zirconia polishing powder Effective date of registration: 20200804 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2020980004690 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210809 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2020980004690 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of cerium praseodymium stabilized zirconia polishing powder Effective date of registration: 20210816 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2021980007746 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220815 Granted publication date: 20180306 Pledgee: Taian Bank Co.,Ltd. Feicheng Branch Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2021980007746 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of cerium praseodymium stabilized zirconia polishing powder Granted publication date: 20180306 Pledgee: Shandong Feicheng Rural Commercial Bank Co.,Ltd. Pledgor: Shandong Maifeng New Material Science and Technology Co.,Ltd. Registration number: Y2024980002191 |