CN104673100A - Preparation technology of cerium oxide-based polishing powder - Google Patents

Preparation technology of cerium oxide-based polishing powder Download PDF

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Publication number
CN104673100A
CN104673100A CN201510072921.3A CN201510072921A CN104673100A CN 104673100 A CN104673100 A CN 104673100A CN 201510072921 A CN201510072921 A CN 201510072921A CN 104673100 A CN104673100 A CN 104673100A
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China
Prior art keywords
cerium
preparation technology
polishing powder
powder
technology according
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Pending
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CN201510072921.3A
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Chinese (zh)
Inventor
易鉴荣
林荔琍
唐臻
吴坚
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Liuzhou Haoxiangte Technology Co Ltd
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Liuzhou Haoxiangte Technology Co Ltd
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Priority to CN201510072921.3A priority Critical patent/CN104673100A/en
Publication of CN104673100A publication Critical patent/CN104673100A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention relates to the field of preparing polishing powder, and particularly relates to a preparation technology of cerium oxide-based polishing powder. The preparation technology comprises the following steps: mixing cerium carbonate hydrate and zirconium oxychloride hydrate, adding concentrated ammonia water and stirring into slurry, and milling in a ball mill; performing press-filtering and drying to the milled product to obtain cerium-zirconia oxide hydrate; roasting the cerium-zirconia oxide hydrate, to obtain cerium-zirconia oxide composite powder. According to the preparation technology, mechanical ball milling is firstly performed, ammonia water is volatilized through heat generated during ball milling, and the inner pressure of a ball milling tank is increased, so that the milled materials in the tank can have hydrothermal reaction, small-particle size and weak-agglomeration precursor can be favorably generated, and then the precursor is roasted to obtain the cerium-zirconia oxide composite powder. Not only is the polishing powder prepared by the technology uniform in particle size, but also the preparation technology is simple to operate and low in cost and the polishing powder is applicable to polishing of high-grade products.

Description

The preparation technology of cerium oxide base polishing powder
Technical field
The present invention relates to polishing powder preparation field, is the preparation technology of cerium oxide base polishing powder specifically.
Background technology
Polishing powder is mainly used in the polishing of the article of the glossy requirements such as jewel, opticglass, artistic glass, TV and graphoscope, medicine equipment and component of machine.Its effect body is by the absorption between polished die and polished part and grinding, improves the smooth finish of surface to be machined, is mainly used in the polishing of workpiece fine grinding.Polishing powder is made up of metal oxide components such as cerium oxide, aluminum oxide, silicon oxide, ferric oxide, zirconium white, chromic oxide usually.At present, domestic polishing powder based on low throwing, its production technology and market all comparative maturities.But produce at the polishing powder that higher gears is secondary and still have larger gap compared with abroad, to special optical camera lens and the higher device of ask for something is precise polished still must dependence on import polishing powder, these device added values are high, profit large and be closely related with high-new utilisation technology.Therefore, accelerating the high-grade wide aperture polishing powder from rare earth of development, has been our very urgent task.
Summary of the invention
For above-mentioned technical problem, the invention provides that a kind of work particle diameter is less, simple to operate, the preparation technology of the cerium oxide base polishing powder of being convenient to suitability for industrialized production.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation technology of cerium oxide base polishing powder, and it comprises the following steps:
(1) by cerium carbonate hydrate and the mixing of hydration basic zirconium chloride, add strong aqua and stir into pulpous state, grind in ball mill;
(2) product after grinding is obtained hydration cerium Zirconium oxide after press filtration, oven dry;
(3) again by the roasting of hydration cerium Zirconium oxide, cerium zirconium compound oxide powder is obtained.
As preferably, the mol ratio that cerium and zirconium calculate pressed by cerium carbonate hydrate and hydration basic zirconium chloride is (0.2 ~ 1): 1.
As preferably, using agate ball as grinding medium during grinding, material ball ratio is 1:5.
As preferably, grinding rate is 180 ~ 200r/min, and milling time is 2 ~ 4h.
As preferably, oven dry carries out in the baking oven of 80 ~ 100 DEG C, time 2 ~ 3h
As preferably, maturing temperature is 900 ~ 1100 DEG C
As preferably, roasting time is 2 ~ 3h.
As can be known from the above technical solutions, first the present invention carries out mechanical ball milling, the heat produced in mechanical milling process makes ammoniacal liquor volatilize, ball grinder internal pressure raises, the grinding material in tank can be made to carry out hydro-thermal reaction, be conducive to generating little, the weakly agglomerated precursor of particle diameter, then roasting precursor can obtain cerium zirconium compound oxide powder.The polishing powder prepared of this technique not only uniform particle sizes, particle diameter is little, and simple to operate, cost is low, is applicable to polishing expensive goods.
Embodiment
Introduce the preparation technology of cerium oxide base polishing powder of the present invention in detail below in conjunction with embodiment, it comprises the following steps:
First, by cerium carbonate hydrate and hydration basic zirconium chloride by certain mixed in molar ratio, then add excessive strong aqua and stir into pulpous state, grind in ball mill; The mol ratio that cerium and zirconium calculate pressed by cerium carbonate hydrate and hydration basic zirconium chloride is (0.2 ~ 1): 1; Using agate ball as grinding medium during grinding, material ball ratio is 1:5, with 180 ~ 200r/min ball milling, 2 ~ 4h,
Again the product after grinding is obtained hydration cerium Zirconium oxide after press filtration, oven dry; Dry and have material impact to follow-up roasting process, if precursor is completely not dry, internal residual has moisture easily will be formed liquid phase bridge in powder inside by the process of killing, produce huge capillary force, under the effect of this power, particle interphase interaction strengthens, and particle shrinks, is agglomerated into harmful hard agglomeration; Temperature is too high, and precursor Direct Resolution can be made to obtain oxide compound.Therefore, drying of the present invention carries out in the baking oven of 80 ~ 100 DEG C, time 2 ~ 3h.
Finally, by the roasting of hydration cerium Zirconium oxide, cerium zirconium compound oxide powder is obtained; Maturing temperature is 900 ~ 1100 DEG C, and roasting time is 2 ~ 3h.
Embodiment 1
The mol ratio being 0.2:1 by cerium and zirconium gets cerium carbonate hydrate and hydration basic zirconium chloride mixes, and adds excessive strong aqua and stirs into pulpous state, then is placed in ball mill and grinds, and using agate ball as grinding medium, material ball ratio is 1:5, with 180r/min ball milling 4h; Again by the product press filtration after grinding, the baking oven being placed in 80 DEG C carries out 3h oven dry; Subsequently at 900 DEG C of roasting 3h; Obtain composite cerium-zirconium oxide polishing powder.By analysis, better, median size about 1.1 μm, reaches as high as 367nm/min to the throwing erosion speed of glass in powder distribution.
Embodiment 2
The mol ratio being 1:1 by cerium and zirconium gets cerium carbonate hydrate and hydration basic zirconium chloride mixes, and adds excessive strong aqua and stirs into pulpous state, then is placed in ball mill and grinds, and using agate ball as grinding medium, material ball ratio is 1:5, with 190r/min ball milling 3h; Again by the product press filtration after grinding, the baking oven being placed in 90 DEG C carries out 3h oven dry; Subsequently at 1000 DEG C of roasting 3h; Obtain composite cerium-zirconium oxide polishing powder.By analysis, better, median size about 0.68 μm, reaches as high as 395nm/min to the throwing erosion speed of glass in powder distribution.
Embodiment 3
The mol ratio being 0.6:1 by cerium and zirconium gets cerium carbonate hydrate and hydration basic zirconium chloride mixes, and adds excessive strong aqua and stirs into pulpous state, then is placed in ball mill and grinds, and using agate ball as grinding medium, material ball ratio is 1:5, with 200r/min ball milling 2h; Again by the product press filtration after grinding, the baking oven being placed in 100 DEG C carries out 2h oven dry; Subsequently at 1100 DEG C of roasting 2h; Obtain composite cerium-zirconium oxide polishing powder.By analysis, better, median size about 0.83 μm, reaches as high as 381nm/min to the throwing erosion speed of glass in powder distribution.
Above-mentioned embodiment is used for illustrative purposes only, and be not limitation of the present invention, the those of ordinary skill of relevant technical field, without departing from the spirit and scope of the present invention, can also make various change and modification, therefore all equivalent technical schemes also should belong to category of the present invention.

Claims (7)

1. the preparation technology of cerium oxide base polishing powder, it comprises the following steps:
(1) by cerium carbonate hydrate and the mixing of hydration basic zirconium chloride, add strong aqua and stir into pulpous state, grind in ball mill;
(2) product after grinding is obtained hydration cerium Zirconium oxide after press filtration, oven dry;
(3) again by the roasting of hydration cerium Zirconium oxide, cerium zirconium compound oxide powder is obtained.
2. preparation technology according to claim 1, is characterized in that: cerium carbonate hydrate and hydration basic zirconium chloride are (0.2 ~ 1) by the mol ratio that cerium and zirconium calculate: 1.
3. preparation technology according to claim 1, is characterized in that: using agate ball as grinding medium during grinding, and material ball ratio is 1:5.
4. preparation technology according to claim 1, is characterized in that: grinding rate is 180 ~ 200r/min, and milling time is 2 ~ 4h.
5. preparation technology according to claim 1, is characterized in that: oven dry carries out in the baking oven of 80 ~ 100 DEG C, time 2 ~ 3h.
6. preparation technology according to claim 1, is characterized in that: maturing temperature is 900 ~ 1100 DEG C.
7. preparation technology according to claim 6, is characterized in that: roasting time is 2 ~ 3h.
CN201510072921.3A 2015-02-12 2015-02-12 Preparation technology of cerium oxide-based polishing powder Pending CN104673100A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106916567A (en) * 2015-12-25 2017-07-04 安集微电子科技(上海)有限公司 A kind of cerium oxide abrasives preparation method and its CMP planarization application

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827721A (en) * 2005-02-28 2006-09-06 宜兴新威集团有限公司 Process for preparing high-performance rare-earth precise polishing materials
CN101284983A (en) * 2007-04-12 2008-10-15 北京有色金属研究总院 Superfine and spheroidizing rare-earth polish and preparing process thereof
CN101550318A (en) * 2008-04-03 2009-10-07 北京有色金属研究总院 Ce<3+>-contained rare-earth polishing powder and preparation method thereof
CN102250552A (en) * 2011-08-19 2011-11-23 永州皓志稀土材料有限公司 Preparation method for cerium doped zirconium composite polishing powder
CN102337085A (en) * 2011-10-10 2012-02-01 上海华明高纳稀土新材料有限公司 Preparation method of composite cerium-zirconium oxide polishing powder
CN102936461A (en) * 2012-11-14 2013-02-20 内蒙古科技大学 Rich cerium rare earth polishing powder and preparation method thereof
CN102965026A (en) * 2012-11-12 2013-03-13 上海华明高纳稀土新材料有限公司 Rare-earth polishing powder and preparation method thereof
CN103013444A (en) * 2011-09-23 2013-04-03 上海华明高纳稀土新材料有限公司 Precision-type mischmetal polishing powder and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827721A (en) * 2005-02-28 2006-09-06 宜兴新威集团有限公司 Process for preparing high-performance rare-earth precise polishing materials
CN101284983A (en) * 2007-04-12 2008-10-15 北京有色金属研究总院 Superfine and spheroidizing rare-earth polish and preparing process thereof
CN101550318A (en) * 2008-04-03 2009-10-07 北京有色金属研究总院 Ce<3+>-contained rare-earth polishing powder and preparation method thereof
CN102250552A (en) * 2011-08-19 2011-11-23 永州皓志稀土材料有限公司 Preparation method for cerium doped zirconium composite polishing powder
CN103013444A (en) * 2011-09-23 2013-04-03 上海华明高纳稀土新材料有限公司 Precision-type mischmetal polishing powder and preparation method thereof
CN102337085A (en) * 2011-10-10 2012-02-01 上海华明高纳稀土新材料有限公司 Preparation method of composite cerium-zirconium oxide polishing powder
CN102965026A (en) * 2012-11-12 2013-03-13 上海华明高纳稀土新材料有限公司 Rare-earth polishing powder and preparation method thereof
CN102936461A (en) * 2012-11-14 2013-02-20 内蒙古科技大学 Rich cerium rare earth polishing powder and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106916567A (en) * 2015-12-25 2017-07-04 安集微电子科技(上海)有限公司 A kind of cerium oxide abrasives preparation method and its CMP planarization application
CN106916567B (en) * 2015-12-25 2020-10-09 安集微电子科技(上海)股份有限公司 Cerium oxide abrasive preparation method and CMP polishing application thereof

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Application publication date: 20150603