CN101659850A - Modified nanometer cerium oxide and preparation and application thereof - Google Patents
Modified nanometer cerium oxide and preparation and application thereof Download PDFInfo
- Publication number
- CN101659850A CN101659850A CN200910196102A CN200910196102A CN101659850A CN 101659850 A CN101659850 A CN 101659850A CN 200910196102 A CN200910196102 A CN 200910196102A CN 200910196102 A CN200910196102 A CN 200910196102A CN 101659850 A CN101659850 A CN 101659850A
- Authority
- CN
- China
- Prior art keywords
- cerium oxide
- nano
- surface modifying
- reaction
- modifying method
- 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.)
- Pending
Links
Images
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention relates to a modified nanometer cerium oxide and preparation and an application thereof. In the invention, the silane coupling agent aminopropyl triethoxysilane is used for modifying nanometer cerium oxide powder. When the polishing solution prepared by the modified cerium oxide is used for polishing silicon dioxide interlayer dielectrics of ultra-large integrated circuits and optical disk glass, the surface roughness can be obviously reduced.
Description
Technical field
The invention belongs to the grinding medium for chemico-mechanical polishing technical field, what be specifically related to a kind of modification receives cerium oxide abrasive particle and method of modifying and application.
Background technology
Cerium oxide has had very long history as the polishing that polish abrasive is used for precision glass polishing and super large-scale integration silica dioxide medium layer, cerium oxide abrasives since its can with silicon oxide generation chemical reaction, under the same conditions, the polishing speed of cerium oxide approximately is three times of silicon oxide, especially in neutral polishing fluid, keep higher removal, and the polishing between silicon oxide and silicon nitride is selected than higher.But the performance of nano-cerium oxide polishing performance depends on its dispersion situation, nano-cerium oxide is the same as its high surface energy is easy to reunite with its other nanoparticle, cause polishing the damage of back workpiece surface, it is big to be embodied in the surface of polished roughness, numerous defectives such as cut.So the dispersion of cerium oxide at present becomes one of most critical technology of cerium oxide polishing slurry preparation, and do not appear in the newspapers as yet about cerium oxide surface modification and the research that is applied to chemically machinery polished.
Summary of the invention
The object of the invention is to provide a kind of modified nanometer cerium oxide, can reduce the reunion of cerium oxide abrasives, improve its in water dispersing property and be applied in the chemically machinery polished, improve the surface quality of polishing back workpiece.
The surface modifying method of nano-cerium oxide of the present invention comprises the following steps:
1) the water-soluble back of silane coupling agent KH550 (aminopropyl triethoxysilane) is mixed with nano cerium oxide powder, be configured to the cerium oxide weight percentage and be 1～10% dispersion liquid;
2) stir evenly with magnetic agitation then, and after the supersound process, make cerium oxide dispersion;
3) above-mentioned dispersion liquid is heated to 70～100 ℃ of temperature of reaction, back flow reaction 1～12 hour;
4) after reaction finished, centrifugation, purification, oven dry finally obtained the cerium oxide abrasive particle through the KH550 modification.
In the described step 1), the mass ratio of KH550 and ceria oxide powder is 1: 10～1: 2.Preferable, the water of dissolving silane coupling agent KH550 is deionized water in the step 1).
Preferable, described step 2) in, pH value to 3～6 regulated earlier.The method of regulating pH can be and adopts the acetic acid,diluted aqueous solution, aqueous hydrochloric acid or aqueous nitric acid to regulate.
Step 2) in, the supersound process time is 0.4-0.6 hour.
In the described step 3), temperature of reaction is preferably 80 ℃, and the reaction times is preferably 5 hours.
Method of purification in the described step 4) is centrifuge washing or ultrafiltration.
The invention provides a kind of modified nanometer cerium oxide, described nano-cerium oxide obtains through the aforesaid method modification.
The present invention also provides a kind of polishing fluid, contains above-mentioned modified nanometer cerium oxide.Preferable, the mass percent concentration of described nano-cerium oxide adopts polishing machine that the thermooxidizing silicon chip is polished between 0.5%～1%.Super large-scale integration silicon-dioxide interlayer medium and CD glass are polished, can obviously reduce the roughness on surface.
The present invention has adopted comparatively simple chemical technology that cerium oxide abrasives has been carried out surface modification, and the surface damage the when polishing fluid that the cerium oxide abrasives after the modification is mixed with can effectively improve polishing reduces roughness, improves polishing efficiency.Owing to need not complex apparatus, required chemical feedstocks kind is few simultaneously, and favorable repeatability has bigger industrial promotional value.
Description of drawings
Fig. 1: the SEM figure of unmodified cerium oxide
The SEM figure of Fig. 2: embodiment 1 cerium oxide
Fig. 3: the AFM figure after the polishing fluid of unmodified cerium oxide preparation polishes the thermooxidizing silicon chip
AFM figure after the polishing fluid of Fig. 4: embodiment 1 preparation polishes the thermooxidizing silicon chip
Embodiment
Below enumerate specific examples with further elaboration the present invention, should be understood that example is not to be used to limit protection scope of the present invention.
Embodiment 1:
Add 3g silane coupling agent KH550 in the 300mL deionized water, fully stirring and dissolving adds the 15g nano cerium oxide powder, dispersed with stirring again; Regulate pH value to 4 with rare acetic acid solution subsequently, stir evenly with magnetic agitation then, and after ultrasonic 0.5 hour, make cerium oxide dispersion.Above-mentioned dispersion liquid is heated to 80 ℃ of temperature of reaction, back flow reaction 5 hours.After reaction finished, centrifugation, purification, oven dry finally obtained the cerium oxide abrasive particle through the KH550 modification.
Getting cerium oxide powder after certain unmodified and modification respectively, to be mixed with mass concentration be 1% dispersion liquid, the CP-4 polishing machine that adopts U.S. CE TR company is after polishing the thermooxidizing silicon chip under the same process parameter, use the distilled water ultrasonic cleaning, utilize the roughness root-mean-square value RMS (RootMean Square) in AFM atomic force microscope tested glass surface 10 μ m * 10 μ m zones then.
The surface sweeping Electronic Speculum figure that presses the cerium oxide powder sample before and after embodiment 1 modification as shown in Figure 1 and Figure 2, cerium oxide powder is reunited seriously before the visible modification, dispersiveness makes moderate progress after the modification.Thermooxidizing silicon chip surface of polished atomic power microgram as shown in Figure 1 and Figure 2.The 3 dimensional drawing after the polishing fluid polishing that is mixed with for unmodified cerium oxide powder of Fig. 1 wherein, its RMS is 3.358nm, the 3 dimensional drawing after the polishing fluid polishing that Fig. 2 is mixed with for the cerium oxide powder after the modification, its RMS is 3.002nm.
Embodiment 2:
Add 0.4g silane coupling agent KH550 in the 300mL deionized water, fully stirring and dissolving adds the 4g nano cerium oxide powder, dispersed with stirring again; Regulate pH value to 3 with rare acetic acid solution subsequently, stir evenly with magnetic agitation then, and after ultrasonic 0.4 hour, make cerium oxide dispersion.Above-mentioned dispersion liquid is heated to 70 ℃ of temperature of reaction, back flow reaction 1 hour.After reaction finished, centrifugation, purification, oven dry finally obtained the cerium oxide abrasive particle through the KH550 modification.With compare before the modification, the cerium oxide powder dispersiveness makes moderate progress.
Embodiment 3:
Add 15g silane coupling agent KH550 in the 300mL deionized water, fully stirring and dissolving adds the 30g nano cerium oxide powder, dispersed with stirring again; Regulate pH value to 6 with rare acetic acid solution subsequently, stir evenly with magnetic agitation then, and after ultrasonic 0.6 hour, make cerium oxide dispersion.Above-mentioned dispersion liquid is heated to 100 ℃ of temperature of reaction, back flow reaction 8 hours.After reaction finished, centrifugation, purification, oven dry finally obtained the cerium oxide abrasive particle through the KH550 modification.With compare before the modification, the cerium oxide powder dispersiveness makes moderate progress.
Embodiment 5:
This example and embodiment 1 step are basic identical, different is need not be rare acetic acid solution regulate pH value, finally obtain passing through the cerium oxide abrasive particle of KH550 modification.With compare before the modification, the cerium oxide powder dispersiveness makes moderate progress.
Above-mentioned example is only in order to specifying of the present invention, and scope of the present invention do not done any restriction, and any personnel that are familiar with this technology can realize easily that modifications and variations include within the present invention and claims scope.With compare before the modification, the cerium oxide powder dispersiveness makes moderate progress.
Claims (8)
1. the surface modifying method of a nano-cerium oxide comprises the following steps:
1) the water-soluble back of silane coupling agent KH550 is mixed with nano cerium oxide powder, be configured to the cerium oxide weight percentage and be 1～10% dispersion liquid;
2) stir evenly with magnetic agitation then, and after the supersound process, make cerium oxide dispersion;
3) above-mentioned dispersion liquid is heated to 70～100 ℃ of temperature of reaction, back flow reaction 1～12 hour;
4) after reaction finished, centrifugation, purification, oven dry finally obtained the cerium oxide abrasive particle through the KH550 modification.
2. the surface modifying method of nano-cerium oxide according to claim 1 is characterized in that in the described step 1), the mass ratio of KH550 and ceria oxide powder is 1: 10～1: 2.
3. the surface modifying method of nano-cerium oxide according to claim 1 is characterized in that described step 2) also comprise and regulate pH value to 3～6.
4. the surface modifying method of nano-cerium oxide according to claim 1 is characterized in that, the method for described adjusting pH is regulated for adopting the acetic acid,diluted aqueous solution, aqueous hydrochloric acid or aqueous nitric acid.
5. the surface modifying method of nano-cerium oxide according to claim 1 is characterized in that described step 2) in, the supersound process time is 0.4-0.6 hour.
6. the surface modifying method of nano-cerium oxide according to claim 1 is characterized in that in the described step 3), temperature of reaction is 80 ℃, and the reaction times is 5 hours.
7. modified nanometer cerium oxide, the described method modification of described nano-cerium oxide arbitrary claim in claim 1-6 obtains.
8. a polishing fluid is characterized in that, contains mass percent concentration and be 0.5%～1% the described nano-cerium oxide of claim 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910196102A CN101659850A (en) | 2009-09-22 | 2009-09-22 | Modified nanometer cerium oxide and preparation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910196102A CN101659850A (en) | 2009-09-22 | 2009-09-22 | Modified nanometer cerium oxide and preparation and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101659850A true CN101659850A (en) | 2010-03-03 |
Family
ID=41788106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910196102A Pending CN101659850A (en) | 2009-09-22 | 2009-09-22 | Modified nanometer cerium oxide and preparation and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101659850A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775958A (en) * | 2012-08-16 | 2012-11-14 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing material for stone grinding tool and preparation method thereof |
| CN106590442A (en) * | 2017-01-22 | 2017-04-26 | 海城海美抛光材料制造有限公司 | Preparation method of cerium dioxide polishing powder liquid |
| CN106867411A (en) * | 2015-10-15 | 2017-06-20 | 三星电子株式会社 | For the paste compound, its preparation method, polishing method, the method for manufacture semiconductor devices and the polissoir that chemically-mechanicapolish polish |
| CN107827141A (en) * | 2017-11-03 | 2018-03-23 | 上海映智研磨材料有限公司 | Nano ceric oxide and preparation method thereof |
| CN109486240A (en) * | 2018-12-26 | 2019-03-19 | 江南大学 | A kind of preparation method of surface amine groups oxide nano rare earth |
| CN110713820A (en) * | 2019-10-29 | 2020-01-21 | 河南联合精密材料股份有限公司 | Preparation method of hydrophobic modified diamond abrasive |
| CN111471217A (en) * | 2020-05-12 | 2020-07-31 | 上海应用技术大学 | Modified nano cerium oxide and preparation method thereof, and modified nano cerium oxide flame-retardant polyformaldehyde and preparation method thereof |
| CN112094493A (en) * | 2020-08-14 | 2020-12-18 | 沈阳化工大学 | Nano-modified thermoplastic polyurethane elastomer polishing material and preparation method thereof |
| CN112662202A (en) * | 2021-01-04 | 2021-04-16 | 上海晖研材料科技有限公司 | Surface-modified cerium oxide particles and polishing solution containing same |
| CN112778972A (en) * | 2021-03-10 | 2021-05-11 | 安徽禾臣新材料有限公司 | Polishing powder for fine polishing of electronic display screen and production method thereof |
| CN112778911A (en) * | 2021-01-04 | 2021-05-11 | 上海晖研材料科技有限公司 | Application of surface-modified cerium oxide particles as polishing solution abrasive particles |
| CN115093795A (en) * | 2022-07-04 | 2022-09-23 | 深圳市永霖科技有限公司 | Magnetorheological polishing solution for ultra-precise polishing of semiconductor wafer |
| CN115319649A (en) * | 2022-09-03 | 2022-11-11 | 深圳市永霖科技有限公司 | PU (polyurethane) polishing abrasive paper for glass polishing and preparation method thereof |
| CN116285895A (en) * | 2023-03-09 | 2023-06-23 | 上海大学 | Ethylenediamine tetraacetic acid grafted cerium oxide composite abrasive particles, preparation method and application thereof |
-
2009
- 2009-09-22 CN CN200910196102A patent/CN101659850A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775958A (en) * | 2012-08-16 | 2012-11-14 | 上海华明高纳稀土新材料有限公司 | Cerium oxide polishing material for stone grinding tool and preparation method thereof |
| CN106867411A (en) * | 2015-10-15 | 2017-06-20 | 三星电子株式会社 | For the paste compound, its preparation method, polishing method, the method for manufacture semiconductor devices and the polissoir that chemically-mechanicapolish polish |
| CN106590442A (en) * | 2017-01-22 | 2017-04-26 | 海城海美抛光材料制造有限公司 | Preparation method of cerium dioxide polishing powder liquid |
| CN107827141A (en) * | 2017-11-03 | 2018-03-23 | 上海映智研磨材料有限公司 | Nano ceric oxide and preparation method thereof |
| CN107827141B (en) * | 2017-11-03 | 2019-10-22 | 上海映智研磨材料有限公司 | Nano ceric oxide and preparation method thereof |
| CN109486240A (en) * | 2018-12-26 | 2019-03-19 | 江南大学 | A kind of preparation method of surface amine groups oxide nano rare earth |
| CN110713820A (en) * | 2019-10-29 | 2020-01-21 | 河南联合精密材料股份有限公司 | Preparation method of hydrophobic modified diamond abrasive |
| CN111471217A (en) * | 2020-05-12 | 2020-07-31 | 上海应用技术大学 | Modified nano cerium oxide and preparation method thereof, and modified nano cerium oxide flame-retardant polyformaldehyde and preparation method thereof |
| CN112094493A (en) * | 2020-08-14 | 2020-12-18 | 沈阳化工大学 | Nano-modified thermoplastic polyurethane elastomer polishing material and preparation method thereof |
| CN112662202A (en) * | 2021-01-04 | 2021-04-16 | 上海晖研材料科技有限公司 | Surface-modified cerium oxide particles and polishing solution containing same |
| CN112778911A (en) * | 2021-01-04 | 2021-05-11 | 上海晖研材料科技有限公司 | Application of surface-modified cerium oxide particles as polishing solution abrasive particles |
| CN112662202B (en) * | 2021-01-04 | 2022-05-10 | 上海晖研材料科技有限公司 | Surface-modified cerium oxide particles and polishing solution containing same |
| CN112778911B (en) * | 2021-01-04 | 2022-08-23 | 上海晖研材料科技有限公司 | Application of surface-modified cerium oxide particles as polishing solution abrasive particles |
| CN112778972A (en) * | 2021-03-10 | 2021-05-11 | 安徽禾臣新材料有限公司 | Polishing powder for fine polishing of electronic display screen and production method thereof |
| CN115093795A (en) * | 2022-07-04 | 2022-09-23 | 深圳市永霖科技有限公司 | Magnetorheological polishing solution for ultra-precise polishing of semiconductor wafer |
| CN115093795B (en) * | 2022-07-04 | 2023-09-01 | 深圳市永霖科技有限公司 | Magnetorheological polishing solution for ultra-precise polishing of semiconductor wafer |
| CN115319649A (en) * | 2022-09-03 | 2022-11-11 | 深圳市永霖科技有限公司 | PU (polyurethane) polishing abrasive paper for glass polishing and preparation method thereof |
| CN115319649B (en) * | 2022-09-03 | 2023-08-04 | 深圳市永霖科技有限公司 | PU polishing sand paper for glass polishing and preparation method thereof |
| CN116285895A (en) * | 2023-03-09 | 2023-06-23 | 上海大学 | Ethylenediamine tetraacetic acid grafted cerium oxide composite abrasive particles, preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101659850A (en) | Modified nanometer cerium oxide and preparation and application thereof | |
| Zhang et al. | Surface modification of ceria nanoparticles and their chemical mechanical polishing behavior on glass substrate | |
| Zhao et al. | Synthesis, characterization of CeO2@ SiO2 nanoparticles and their oxide CMP behavior | |
| CN103571333B (en) | CMP (Chemical-Mechanical Polishing) polishing liquid with mixed grinding materials for alkaline sapphire substrate and preparation method thereof | |
| CN106044786B (en) | Big partial size silica solution of polydispersion and preparation method thereof | |
| CN101475791B (en) | Preparation and use of cerium oxide / silicon oxide compound abrasive | |
| CN100337925C (en) | Crytalline ceric oxide sol and making method thereof | |
| CN102408871A (en) | Porous nano composite abrasive particle containing polishing active elements, polishing solution composition and preparation method thereof | |
| CN102343547A (en) | Thermochemistry mechanical polishing method of sapphire substrate material and polishing solution | |
| CN101671538B (en) | Method for preparing silica/ceria composite abrasive grains | |
| WO2009021364A1 (en) | The method of controlling scratching of the polished surface of silicon wafer | |
| CN104357012A (en) | Abrasive compound, preparation method thereof and application thereof to chemico-mechanical polishing | |
| CN113621346B (en) | Suspension auxiliary agent applied to large-size silicon wafer grinding, preparation method and application thereof | |
| CN106281043B (en) | A kind of magnetorheological chemical mechanical polishing liquid and its application method for SiC single crystal piece | |
| CN104312441A (en) | Silicon-cerium polishing liquid and preparation method thereof | |
| Chen et al. | Synergetic effect of organic cores and inorganic shells for core/shell structured composite abrasives for chemical mechanical planarization | |
| CN108034363B (en) | Combined polishing solution | |
| Xie et al. | Chemical mechanical polishing of silicon wafers using developed uniformly dispersed colloidal silica in slurry | |
| CN102372273A (en) | Silica sol with double grain diameters and preparation method thereof | |
| CN106010297A (en) | Preparation method of aluminum oxide polishing solution | |
| CN108161584B (en) | Ultra-precise polishing method for metal workpiece | |
| CN104531067B (en) | A kind of hydridization abrasive material and preparation method and the purposes in Ultraprecise polished | |
| CN108034362A (en) | A kind of composite polishing liquid and preparation method thereof | |
| Han et al. | Research progress on the application of ceria nanoparticles as abrasives in dielectric layer CMP and post cleaning: Structure, morphology, doping, and mechanism | |
| CN108864947A (en) | A kind of nano diamond polishing liquid and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANGHAI XIN ANNA ELECTRONIC TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: SHANGHAI INST. OF MICROSYSTEM +. INFORMATION TECHN, CHINESE ACADEMY OF SCIENCES Effective date: 20120427 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 200050 CHANGNING, SHANGHAI TO: 201506 JINSHAN, SHANGHAI |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20120427 Address after: 201506, 285, Lane 2, Tiangong Road, Jinshan Industrial Zone, Shanghai, Shanghai Applicant after: Shanghai Xin'anna Electronic Technology Co., Ltd. Address before: 200050 Changning Road, Shanghai, No. 865, No. Applicant before: Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100303 |