CN101993662B - Preparation method of cerium-based polishing powder suspension - Google Patents
Preparation method of cerium-based polishing powder suspension Download PDFInfo
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- CN101993662B CN101993662B CN2010105838483A CN201010583848A CN101993662B CN 101993662 B CN101993662 B CN 101993662B CN 2010105838483 A CN2010105838483 A CN 2010105838483A CN 201010583848 A CN201010583848 A CN 201010583848A CN 101993662 B CN101993662 B CN 101993662B
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- Prior art keywords
- polishing powder
- cerium based
- cerium
- powder suspension
- preparation
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- 238000005498 polishing Methods 0.000 title claims abstract description 69
- 239000000843 powder Substances 0.000 title claims abstract description 66
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 41
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000725 suspension Substances 0.000 title abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- QYNAIIBQNXVXCP-UHFFFAOYSA-N tetracosan-8-yloxybenzene Chemical compound C1(=CC=CC=C1)OC(CCCCCCC)CCCCCCCCCCCCCCCC QYNAIIBQNXVXCP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000013019 agitation Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000000274 adsorptive effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000009736 wetting Methods 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 abstract 1
- 230000003670 easy-to-clean Effects 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 metals ion Chemical class 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention relates to a preparation method of a cerium-based polishing powder suspension, which comprises the following steps of: 1, sieving cerium-based polishing powder with particle diameter of 0.1-1.5mu m; 2, weighting a ml of pure water, weighting b g of sodium dodecyl benzene sulfonate and c g of hexadecyl octyl phenyl ether and dissolving into the pure water, wherein b=0.01-0.03a, and c=0.03-0.05a; 3, taking d g of screened cerium-based polishing powder to be added in the solution of the step 2, magnetically stirring uniformly, wherein d=0.05a; and 4, ultrasonically vibrating a powder suspension formed in the step 3 for 5-15min. By using the dispersing function, the wetting function of a surface active agent and the ultrasound function of ultrasonic, the method can effectively improve the dispersing property of the polishing powder suspension, obtains good dispersing effect, and is simple and practical; meanwhile, the invention is beneficial to the post-treatment technology by using the function of reducing the adsorptive power of particles on the surface of a part by the surface active agent to ensure that the surface of the part is easy to clean with less residues.
Description
[technical field]
The present invention relates to the polishing technology field, particularly a kind of preparation method of cerium based relief polishing powder suspension-s.
[background technology]
In the super-smooth surface complete processing, the quality of polishing powder slurries directly influences super-smooth surface defective, damage, cleaning and stress.Because the suspension of cerium based relief polishing powder is poor at present; Coagulation be prone to take place in particle, makes in the polishing slurries size distribution inhomogeneous on the one hand, produces agglomerating particles; Make finished surface cut occur; Also make simultaneously the population of actual participation polishing reduce, reduced polishing speed, thereby affected the quality of polishing efficiency and super-smooth surface.Make in the cleaning process of back polishing powder particle absorption back clean difficulty on the other hand and have problem such as metals ion contamination, cause that cleaning performance is poor, the yield rate of device can't improve.
[summary of the invention]
The preparation method who the purpose of this invention is to provide a kind of cerium based relief polishing powder suspension-s, this method can suppress the reunion trend of polishing powder, effectively improve the suspended dispersed performance of cerium based relief polishing powder, thereby improve quality of finish; Can reduce the adsorptive power of polishing powder particle again, the cleaning after helping polishing at piece surface.
To achieve these goals, the utility model adopts following technical scheme:
A kind of preparation method of cerium based relief polishing powder suspension-s may further comprise the steps:
1), filters out the cerium based relief polishing powder that particle diameter is 0.1-1.5um;
2), measure pure water a milliliter, take by weighing X 2073 b gram and also be dissolved in fully in the said a ml pure water with hexadecyl octyl phenyl ether c gram; B=0.01～0.03a wherein, c=0.03～0.05a;
3), get the cerium based relief polishing powder d gram that has screened in the step 1) and be added into step 2) in solution in, magnetic agitation evenly forms suspension-s; D=0.05a wherein;
4) the powder suspension-s ultrasonic vibration 5-15min that, adopts Ultrasonic Cleaners that step 3) is formed.
Particle diameter is that the cerium based relief polishing powder of 0.1-1.5um filters out through hydraulic elutria-tion method in the step 1).
Step 2) temperature of said pure water is room temperature～60 ℃.
Step 2) temperature of said pure water is 40 ℃.
The frequency of Ultrasonic Cleaners is 40kHz in the said step 4).
The time of magnetic agitation is 10min in the said step 3).
Compared with prior art; The present invention has the following advantages: the inventive method is utilized dispersion, wetting action and hyperacoustic ultrasonication of tensio-active agent; Can effectively improve the dispersing property of polishing powder suspension-s, dispersion effect is good, and method is simple, practical; Utilize tensio-active agent to have simultaneously and reduce particle cleaning technique after the effect of piece surface adsorptive power helps, make that piece surface is prone to clean, residue is few.In sum, the cerium based relief polishing powder suspension-s of the inventive method preparation can improve the suspension property of polishing powder, thereby obtains to pollute less, be prone to the super-smooth surface of cleaning.
[embodiment]
Below in conjunction with specific embodiment the present invention is done and to describe in further detail.
Instance one:
1, the 50g cerium based relief polishing powder is mixed stirring with the 1000ml pure water, adopt hydraulic elutria-tion method that cerium based relief polishing powder is screened, filter out the cerium based relief polishing powder that particle diameter is 0.1-1.5um, and adopt laser particle analyzer that the particle diameter of selected polishing powder is carried out analysis and characterization;
2, be that 1% X 2073 and mass percent are 3% hexadecyl octyl phenyl ether to 500ml, 40 ℃ pure water China and foreign countries admixture amount percentage ratio, and be stirred to abundant dissolving;
3, get the polishing powder 25g that has screened in the step 1 and be added in the solution in the step 2, carry out magnetic agitation 10min, process suspension-s;
4, adopt Ultrasonic Cleaners to the suspension-s ultrasonic vibration 5min in the step 3, take out and obtain cerium based relief polishing powder suspension-s of the present invention, under 25 ℃, leave standstill 5h, with the absorbancy of polishing powder suspension-s under the certain wavelength of spectrophotometric determination, absorbancy is 0.92.
Cleaning performance is following:
The optical element that the polishing powder that adopts different dispersion effects polishes is detected with Talysurf CCI Lite white light three-dimensional topography measurement appearance through ZYGO New View white light interferometer; The optical element surface roughness that the cerium based relief polishing powder suspension-s that adopts present embodiment to make is polished can reach 0.3nm, and the dispersive polishing powder optical element surface roughness of being polished can not reach 0.8nm.
Instance two:
1, the 50g cerium based relief polishing powder is mixed stirring with the 1000ml pure water; Adopt hydraulic elutria-tion method that cerium based relief polishing powder is screened; Filter out the cerium based relief polishing powder that particle diameter is 0.1-1.5um, and adopt laser particle analyzer that the particle diameter of selected cerium based relief polishing powder is carried out analysis and characterization;
2, be that 2% X 2073 and mass percent are 4% hexadecyl octyl phenyl ether to 500ml, 40 ℃ pure water China and foreign countries admixture amount percentage ratio, and be stirred to abundant dissolving;
3, get the cerium based relief polishing powder 25g that has screened in the step 1 and be added in the solution in the step 2, carry out magnetic agitation 10min, process suspension-s;
4, adopt Ultrasonic Cleaners to the suspension-s ultrasonic vibration 10min in the step 3, take out and obtain cerium based relief polishing powder suspension-s of the present invention, under 25 ℃, leave standstill 5h, with the absorbancy of polishing powder suspension-s under the certain wavelength of spectrophotometric determination, absorbancy is 0.94.
Cleaning performance is following:
The optical element that the polishing powder that adopts different dispersion effects polishes is detected with Talysurf CCI Lite white light three-dimensional topography measurement appearance through ZYGO New View white light interferometer; The optical element surface roughness that the cerium based relief polishing powder suspension-s that adopts embodiment to make is polished can reach 0.2nm, and the dispersive polishing powder optical element surface roughness of being polished can not reach 0.8nm.
Instance three:
1, the 50g polishing powder is mixed stirring with the 1000ml pure water, adopt hydraulic elutria-tion method that polishing powder is screened, filter out the cerium based relief polishing powder that particle diameter is 0.1-1.5um, and adopt laser particle analyzer that the particle diameter of selected cerium based relief polishing powder is carried out analysis and characterization;
2, be that 3% X 2073 and mass percent are 5% hexadecyl octyl phenyl ether to 500ml, 40 ℃ pure water China and foreign countries admixture amount percentage ratio, and be stirred to abundant dissolving;
3, get the polishing powder 25g that has screened in the step 1 and be added in the solution in the step 2, carry out magnetic agitation 10min, process suspension-s;
4, adopt Ultrasonic Cleaners to the polishing powder suspension-s ultrasonic vibration 15min in the step 3, obtain cerium based relief polishing powder suspension-s of the present invention, under 25 ℃, leave standstill 5h, with the absorbancy of polishing powder suspension-s under the certain wavelength of spectrophotometric determination, absorbancy is 0.95.
Cleaning performance is following:
The optical element that the polishing powder that adopts different dispersion effects polishes is detected with Talysurf CCI Lite white light three-dimensional topography measurement appearance through ZYGO New View white light interferometer; The optical element surface roughness that the cerium based relief polishing powder suspension-s that adopts embodiment to make is polished can reach 0.1nm, and the dispersive polishing powder optical element surface roughness of being polished can not reach 0.8nm.
Grain size screening is that the method for the cerium based relief polishing powder of 0.1-1.5um can be used screening method commonly used in other industry in the step 1 of the present invention.
The temperature of pure water can be ambient temperature～60 ℃ in the step 2 of the present invention; Two kinds of additive X 2073es and hexadecyl octyl phenyl ether dissolution rate are lower during ambient temperature～40 ℃; The performance of two kinds of additive X 2073es and hexadecyl octyl phenyl ether will be affected when being higher than 60 ℃, and pure water temperature is preferred 40 ℃ in the step 2 of the present invention.The quality of the X 2073 that adds in the step 2 is the 1-3% of pure water quality in the step 2, and the quality of the hexadecyl octyl phenyl ether of adding is the 3-5% of pure water quality in the step 2.
The ultrasonic frequency of Ultrasonic Cleaners is 40kHz in the step 4 of the present invention; Ultrasonic time is 5～15min; Cerium based relief polishing powder is uniformly dispersed, and it is inhomogeneous to be lower than suspension-s dispersion in 5 minutes, has little significance greater than 15 minutes supersound process that have been uniformly dispersed again.
Claims (6)
1. the preparation method of a cerium based relief polishing powder suspension-s is characterized in that, may further comprise the steps:
1), filters out the cerium based relief polishing powder that particle diameter is 0.1-1.5 μ m;
2), measure pure water a milliliter, take by weighing X 2073 b gram and also be dissolved in fully in the said a ml pure water with hexadecyl octyl phenyl ether c gram; B=0.01～0.03a wherein, c=0.03～0.05a;
3), get the cerium based relief polishing powder d gram that has screened in the step 1) and be added into step 2) in solution in, magnetic agitation evenly forms suspension-s; D=0.05a wherein;
4) the powder suspension-s ultrasonic vibration 5-15min that, adopts Ultrasonic Cleaners that step 3) is formed.
2. a kind of according to claim 1 preparation method of cerium based relief polishing powder suspension-s is characterized in that: particle diameter is that the cerium based relief polishing powder of 0.1-1.5 μ m filters out through hydraulic elutria-tion method in the step 1).
3. a kind of according to claim 1 preparation method of cerium based relief polishing powder suspension-s is characterized in that: step 2) temperature of said pure water is room temperature～60 ℃.
4. like the preparation method of the said a kind of cerium based relief polishing powder suspension-s of claim 3, it is characterized in that: step 2) temperature of said pure water is 40 ℃.
5. a kind of according to claim 1 preparation method of cerium based relief polishing powder suspension-s, it is characterized in that: the frequency of Ultrasonic Cleaners is 40kHz in the said step 4).
6. a kind of according to claim 1 preparation method of cerium based relief polishing powder suspension-s, it is characterized in that: the time of magnetic agitation is 10min in the said step 3).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105838483A CN101993662B (en) | 2010-12-13 | 2010-12-13 | Preparation method of cerium-based polishing powder suspension |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105838483A CN101993662B (en) | 2010-12-13 | 2010-12-13 | Preparation method of cerium-based polishing powder suspension |
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| Publication Number | Publication Date |
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| CN101993662A CN101993662A (en) | 2011-03-30 |
| CN101993662B true CN101993662B (en) | 2012-11-07 |
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| CN105255368B (en) * | 2015-10-09 | 2018-02-09 | 同济大学 | A kind of Ultraprecise polished screening technique with micron-submicron polishing fluid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453328A (en) * | 2002-04-22 | 2003-11-05 | Jsr株式会社 | Aqueous dispersion body for chemical mechanical grinding |
| CN1807540A (en) * | 2006-01-18 | 2006-07-26 | 北京工业大学 | Rare earth polishing liquor for organic alkaline corrosive medium |
| CN1831076A (en) * | 2005-03-09 | 2006-09-13 | Jsr株式会社 | Chemical mechanical polishing aqueous dispersion, chemical mechanical polishing method, and kit for preparing chemical mechanical polishing aqueous dispersion |
| CN1948418A (en) * | 2005-10-14 | 2007-04-18 | 花王株式会社 | Polishing composition for a semiconductor substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5482194B2 (en) * | 2009-03-31 | 2014-04-23 | 東レ株式会社 | Carbon nanotube aqueous dispersion, conductive composite, and method for producing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453328A (en) * | 2002-04-22 | 2003-11-05 | Jsr株式会社 | Aqueous dispersion body for chemical mechanical grinding |
| CN1831076A (en) * | 2005-03-09 | 2006-09-13 | Jsr株式会社 | Chemical mechanical polishing aqueous dispersion, chemical mechanical polishing method, and kit for preparing chemical mechanical polishing aqueous dispersion |
| CN1948418A (en) * | 2005-10-14 | 2007-04-18 | 花王株式会社 | Polishing composition for a semiconductor substrate |
| CN1807540A (en) * | 2006-01-18 | 2006-07-26 | 北京工业大学 | Rare earth polishing liquor for organic alkaline corrosive medium |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2010-254546A 2010.11.11 |
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| CN101993662A (en) | 2011-03-30 |
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