CN104962234A - Titania-doped diamond composite abrasive particle and preparation method and application thereof - Google Patents
Titania-doped diamond composite abrasive particle and preparation method and application thereof Download PDFInfo
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- CN104962234A CN104962234A CN201510241996.XA CN201510241996A CN104962234A CN 104962234 A CN104962234 A CN 104962234A CN 201510241996 A CN201510241996 A CN 201510241996A CN 104962234 A CN104962234 A CN 104962234A
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- titania
- doped diamond
- abrasive particles
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Abstract
The present invention discloses a titania-doped diamond composite abrasive particle and a preparation method and application thereof, the titania-doped diamond composite abrasive particle includes a diamond core with the particle diameter of 50nm-10mum and a titania shell, the titania shell is prepared by constant temperature hydrolysis reaction, titanyl sulfate is used as a precursor, the titania shell is co-doped with Fe<3 +> and N, and the N / Ti mole ratio is 1% to 13%. The titania-doped diamond composite abrasive particle can be widely used for preparing consolidated and semi-consolidated and free polishing tools, semi-consolidated flexible polishing tools prepared from the titania-doped diamond composite abrasive particle not only can significantly improve the SiC wafer processing efficiency, but also can obtain smooth and nondestructive surface quality.
Description
Technical field
The invention belongs to Ultraprecision Machining field, be specifically related to a kind of titania-doped diamond Compostie abrasive particles and its preparation method and application.
Background technology
SiC, as one of the core of third generation semiconductor material, because it has the excellent physicochemical property such as large energy gap, high heat conductance, high disruptive field intensity, is widely used in the field such as High performance IC and LED illumination.Along with the fast development of information technology and photoelectric technology, SiC wafer not only demand sharply increases, and it is also proposed the higher requirement such as ultra-smooth, not damaged to its processing quality.
Because SiC hardness is high, fragility large, mechanical polishing is difficult to obtain smooth harmless surface, and therefore CMP remains the topmost processing mode of current SiC wafer.Traditional CMP (Chemical Mechanical Polishing) process adopts free gold hard rock abrasive machining, there is diamond abrasive grain waste serious, the problem that working (machining) efficiency is lower.And the erosion resistance of SiC is very good, not only chemical reaction effect is not obvious, and polishing fluid is serious environment pollution also.The domestic and international Ultra-precision Turning to sic wafer also has the mode adopting novel consolidation and semi-consolidated super hard abrasive at present, but the lifting of working (machining) efficiency is limited, and easily causes physical abuse.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of titania-doped diamond Compostie abrasive particles is provided.
Another object of the present invention is to the preparation method that above-mentioned titania-doped diamond Compostie abrasive particles is provided.
Another object of the present invention is the application providing above-mentioned titania-doped diamond Compostie abrasive particles.
Concrete technical scheme of the present invention is as follows:
A kind of titania-doped diamond Compostie abrasive particles, comprise diamond core and the titanium dioxide shell of particle diameter 50nm ~ 10 μm, this titanium dioxide shell is prepared by constant temperature hydrolysis reaction and presoma is titanyl sulfate, and on this titanium dioxide shell, codoped has Fe simultaneously
3+with N, N/Ti mol ratio is 1% ~ 13%.
In a preferred embodiment of the invention, described N/Ti mol ratio is 1% ~ 10%.
A preparation method for above-mentioned titania-doped diamond Compostie abrasive particles, comprises the steps:
(1) added to by diamond abrasive grain in distilled water and carry out shearing and ultrasonic disperse, form uniform and stable suspension, the particle diameter of this diamond abrasive grain is 50nm ~ 10 μm;
(2) by titanyl sulfate heating for dissolving rear and Fe in water
3+solution mixes, then joins the NH dissolved
4in Cl solution, form mixing solutions, Fe in this mixing solutions
3+massfraction be 0.1% ~ 0.7%, N/Ti mol ratio be 1% ~ 13%;
(3) mixing solutions prepared by suspension step (1) prepared and step (2) mixes, carry out constant temperature hydrolysis reaction while stirring, temperature of reaction is 40 ~ 55 DEG C, and the reaction times is 10 ~ 27 hours, and stirring velocity is 50 ~ 75rmp;
(4) material obtained after step (3) being reacted carries out centrifugation, and washing is dry, obtains described titania-doped diamond Compostie abrasive particles.
In a preferred embodiment of the invention, the particle diameter of described diamond abrasive grain is 50nm, 100nm, 250nm, 500nm, at least one in 1 μm, 3 μm, 5 μm and 10 μm.
In a preferred embodiment of the invention, described step (2) is: by titanyl sulfate heating for dissolving rear and Fe in water
3+solution mixes, then joins the NH dissolved
4in Cl solution, form mixing solutions, Fe in this mixing solutions
3+massfraction be 0.1% ~ 0.5%, N/Ti mol ratio be 1% ~ 10%.
In a preferred embodiment of the invention, described step (3) is: mixing solutions prepared by the suspension prepare step (1) and step (2) mixes, carry out constant temperature hydrolysis reaction while stirring, temperature of reaction is 40 ~ 50 DEG C, reaction times is 12 ~ 24 hours, and stirring velocity is 60rmp.
The application of above-mentioned titania-doped diamond Compostie abrasive particles in consolidation, semi-consolidated and free polishing tool processing SiC wafer.
The invention has the beneficial effects as follows:
1, titania-doped diamond Compostie abrasive particles of the present invention comprises diamond core and the titanium dioxide shell of particle diameter 50nm ~ 10 μm, this titanium dioxide shell is prepared by constant temperature hydrolysis reaction and presoma is titanyl sulfate, and on this titanium dioxide shell, codoped has Fe simultaneously
3+and N, N/Ti mol ratio is 1% ~ 13%, can be widely used in the preparation of consolidation, semi-consolidated and free polishing tool, the semi-consolidated flexible polishing instrument utilizing this Compostie abrasive particles to prepare, the working (machining) efficiency of SiC wafer can not only be significantly improved, and smooth harmless surface quality can also be obtained;
2, preparation method's technique of titania-doped diamond Compostie abrasive particles of the present invention is simple, with low cost, is beneficial to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure of titania-doped diamond Compostie abrasive particles prepared by the embodiment of the present invention 1;
Fig. 2 is transmission electron microscope (TEM) figure of titania-doped diamond Compostie abrasive particles prepared by the embodiment of the present invention 2.
Embodiment
By reference to the accompanying drawings below by way of embodiment technical scheme of the present invention is further detailed and is described.
Embodiment 1
First 3 of 500mg μm of diamond abrasive grains are placed in 50ml distilled water, successively carry out shearing and ultrasonic disperse, obtain suspension; Secondly by 7.838g coating presoma titanyl sulfate heating for dissolving together with appropriate nine water iron nitrates are in 150ml distilled water, then by NH
4cl joins in the solution dissolved, and obtains mixing solutions.Then above-mentioned suspension and mixing solutions are mixed that (wherein the concentration of titanyl sulfate is 0.2mol/L, Fe in mixed solution
3+massfraction be 0.2%, N/Ti mol ratio be 5%), and pour into heating in water bath in flask, temperature controls at 40 DEG C, stirring reaction 18 hours under the stirring velocity of 60rpm.After having reacted, clean on whizzer with distilled water, in 45 DEG C of dry about 12h in loft drier, just obtain described titania-doped diamond Compostie abrasive particles (as shown in Figure 1).
Utilize the titania-doped diamond Compostie abrasive particles prepared in above-described embodiment, and diamond abrasive grain is prepared into sodium alginate polished film respectively, utilizes AUTOPOL-1000S automatic grinding and polishing device, under identical experiment condition, carry out polishing experiments contrast.Machined parameters is as follows: lap speed 90rpm, sample tray rotating speed 80rpm, polish pressure 3kg, polishing duration 60min.Concrete polish results sees the following form 1.
Table 13 μm of diamonds post-treatment wafer effect comparison before modified
Embodiment 2
First the diamond abrasive grain of the 250nm of 200mg is placed in 50ml distilled water, successively carries out shearing and ultrasonic disperse, obtain suspension; Secondly by 7.838g coating presoma titanyl sulfate heating for dissolving together with appropriate nine water iron nitrates are in 150ml distilled water, then by NH
4cl joins in the solution dissolved, and obtains mixing solutions.Then above-mentioned suspension and mixing solutions are mixed that (wherein the concentration of titanyl sulfate is 0.2mol/L, Fe in mixed solution
3+massfraction be 0.1%, N/Ti mol ratio be 1%), and pour into heating in water bath in flask, temperature controls at 50 DEG C, stirring reaction 15 hours under the stirring velocity of 60rpm.After having reacted, clean on whizzer with distilled water, in 45 DEG C of dry about 12h in loft drier, just obtain described titania-doped diamond Compostie abrasive particles (as shown in Figure 2).
Utilize the titania-doped diamond Compostie abrasive particles prepared in above-described embodiment, and diamond abrasive grain is prepared into sodium alginate polished film respectively, utilizes AUTOPOL-1000S automatic grinding and polishing device, under identical experiment condition, carry out polishing experiments contrast.Machined parameters is as follows: lap speed 120rpm, sample tray rotating speed 80rpm, polish pressure 2.5kg, polishing duration 90min.Concrete polish results sees the following form 2.
Table 2 250n diamond post-treatment wafer effect comparison before modified
As can be seen from table 1 and table 2 comparing result, polishing tool prepared by titania-doped diamond Compostie abrasive particles of the present invention can improve working (machining) efficiency and the processing quality of SiC wafer.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (7)
1. a titania-doped diamond Compostie abrasive particles, it is characterized in that: the diamond core and the titanium dioxide shell that comprise particle diameter 50nm ~ 10 μm, this titanium dioxide shell is prepared by constant temperature hydrolysis reaction and presoma is titanyl sulfate, and on this titanium dioxide shell, codoped has Fe simultaneously
3+with N, N/Ti mol ratio is 1% ~ 13%.
2. a kind of titania-doped diamond Compostie abrasive particles as claimed in claim 1, is characterized in that: described N/Ti mol ratio is 1% ~ 10%.
3. a preparation method for titania-doped diamond Compostie abrasive particles, is characterized in that: comprise the steps:
(1) added to by diamond abrasive grain in distilled water and carry out shearing and ultrasonic disperse, form uniform and stable suspension, the particle diameter of this diamond abrasive grain is 50nm ~ 10 μm;
(2) by titanyl sulfate heating for dissolving rear and Fe in water
3+solution mixes, then joins the NH dissolved
4in Cl solution, form mixing solutions, Fe in this mixing solutions
3+massfraction be 0.1% ~ 0.7%, N/Ti mol ratio be 1% ~ 13%;
(3) mixing solutions prepared by suspension step (1) prepared and step (2) mixes, carry out constant temperature hydrolysis reaction while stirring, temperature of reaction is 40 ~ 55 DEG C, and the reaction times is 10 ~ 27 hours, and stirring velocity is 50 ~ 75rmp;
(4) material obtained after step (3) being reacted carries out centrifugation, and washing is dry, obtains described titania-doped diamond Compostie abrasive particles.
4. the preparation method of a kind of titania-doped diamond Compostie abrasive particles as claimed in claim 3, is characterized in that: the particle diameter of described diamond abrasive grain is 50nm, 100nm, 250nm, 500nm, at least one in 1 μm, 3 μm, 5 μm and 10 μm.
5. the preparation method of a kind of titania-doped diamond Compostie abrasive particles as claimed in claim 3, is characterized in that: described step (2) is: by titanyl sulfate heating for dissolving rear and Fe in water
3+solution mixes, then joins the NH dissolved
4in Cl solution, form mixing solutions, Fe in this mixing solutions
3+massfraction be 0.1% ~ 0.5%, N/Ti mol ratio be 1% ~ 10%.
6. the preparation method of a kind of titania-doped diamond Compostie abrasive particles as claimed in claim 3, it is characterized in that: described step (3) is: mixing solutions prepared by the suspension prepare step (1) and step (2) mixes, carry out constant temperature hydrolysis reaction while stirring, temperature of reaction is 40 ~ 50 DEG C, reaction times is 12 ~ 24 hours, and stirring velocity is 60rmp.
7. the application of the titania-doped diamond Compostie abrasive particles described in claim 1 or 2 in consolidation, semi-consolidated and free polishing tool processing SiC wafer.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105856087A (en) * | 2016-04-22 | 2016-08-17 | 柳州凯通新材料科技有限公司 | Preparing method for superhard diamond abrasive materials for high-precision cutting grinding wheel |
| CN113480974A (en) * | 2021-08-04 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Grinding composition and application thereof |
| WO2022199193A1 (en) * | 2021-03-25 | 2022-09-29 | 华侨大学 | Method for detecting interfacial frictional chemical reaction between abrasive grains and diamond wafer substrate |
| US11982650B2 (en) | 2021-03-25 | 2024-05-14 | Huaqiao University | Method for testing interfacial tribochemical reaction between abrasive and diamond wafer |
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| US20050086870A1 (en) * | 2003-10-28 | 2005-04-28 | Nihon Microcoating Co., Ltd. | Diamond polishing particles and method of producing same |
| US20080237535A1 (en) * | 2007-03-19 | 2008-10-02 | Speedfam Co., Ltd. | Composition for polishing semiconductor wafer, and method of producing the same |
| CN102719220A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive grain in grain/alumina core-shell structure and preparation method and application of composite abrasive grain |
| CN102719219A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive particle with abrasive particle/nickel oxide core-shell structure, and preparation method and application thereof |
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2015
- 2015-05-13 CN CN201510241996.XA patent/CN104962234B/en active Active
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| US20050086870A1 (en) * | 2003-10-28 | 2005-04-28 | Nihon Microcoating Co., Ltd. | Diamond polishing particles and method of producing same |
| US20080237535A1 (en) * | 2007-03-19 | 2008-10-02 | Speedfam Co., Ltd. | Composition for polishing semiconductor wafer, and method of producing the same |
| CN102719220A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive grain in grain/alumina core-shell structure and preparation method and application of composite abrasive grain |
| CN102719219A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive particle with abrasive particle/nickel oxide core-shell structure, and preparation method and application thereof |
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| K.HANADA,ET AL.: "Development of self-lubricating titania/diamond nanoparticle composite", 《MATERIALS SCIENCE AND TECHNOLOGY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105856087A (en) * | 2016-04-22 | 2016-08-17 | 柳州凯通新材料科技有限公司 | Preparing method for superhard diamond abrasive materials for high-precision cutting grinding wheel |
| WO2022199193A1 (en) * | 2021-03-25 | 2022-09-29 | 华侨大学 | Method for detecting interfacial frictional chemical reaction between abrasive grains and diamond wafer substrate |
| US11982650B2 (en) | 2021-03-25 | 2024-05-14 | Huaqiao University | Method for testing interfacial tribochemical reaction between abrasive and diamond wafer |
| CN113480974A (en) * | 2021-08-04 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Grinding composition and application thereof |
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| CN104962234B (en) | 2017-05-03 |
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Effective date of registration: 20200817 Address after: Room 310, 3 / F, building 11, Yichuang Science Park, 50 Weixin Road, Suzhou Industrial Park, Suzhou, Jiangsu Province Patentee after: Suzhou Celte New Material Co., Ltd Address before: Fengze District of Quanzhou city east of Fujian province 362000 Patentee before: HUAQIAO University |