CN104109405A - Surface-modified c-Si as well as preparation method and application thereof - Google Patents
Surface-modified c-Si as well as preparation method and application thereof Download PDFInfo
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- CN104109405A CN104109405A CN201410364653.8A CN201410364653A CN104109405A CN 104109405 A CN104109405 A CN 104109405A CN 201410364653 A CN201410364653 A CN 201410364653A CN 104109405 A CN104109405 A CN 104109405A
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Abstract
The invention discloses surface-modified c-Si as well as a preparation method and application thereof. The method for preparing the surface-modified c-Si comprises the following steps: performing acid liquor treatment on the surfaces of c-Si nanoparticles, dispersing the c-Si nanoparticles subjected to acid liquor treatment, and reacting the c-Si nanoparticles subjected to acid liquor treatment with a silane coupling agent at the temperature of 70-90 DEG C. According to the method for preparing the surface-modified c-Si, the surfaces of the c-Si nanoparticles are modified by adopting the silane coupling agent, so that the prepared surface-modified c-Si has excellent dispersing performance, limitation of instruments is avoided, and the production cost is reduced.
Description
Technical field
The invention belongs to nano particle surface modifying technical field, particularly c-Si of a kind of surface modification and preparation method thereof and application.
Background technology
High refractive index optical material has good development prospect in glasses lens, optical filter, photoelectric device, high reflection and antireflection coatings field, and therefore high-index material is one of optical material of people's primary study always.Conventional inorganic materials has very high specific refractory power (ranges of indices of refraction is adjustable from 2.0～5.0), but inorganic materials density is large, poor toughness, be difficult for processing, especially preparing in antireflection coatings, because the specific refractory power of inorganic materials is difficult adjustable continuously, this has just increased the cost of the course of processing.
Be compared to inorganic materials, organic materials is more easily processed, and organic materials has better resistance to impact shock simultaneously.But the specific refractory power of organic materials can only regulate by the change of group (1.3～1.7) in a relatively little scope, cannot meet the high refractive index demand of people for material.
The high refractive index composite material concurrent of developing easy processing and the high impact strength of organic materials, and the feature of inorganic materials high refractive index high stability, therefore becomes the focus of people's research gradually.But how to avoid inorganic materials to be separated with organic materials in matrix material, the gathering of avoiding inorganic materials is the problem that people can not ignore in the time preparing matrix material.
Particularly, as the high refractive index matrix material that contains crystalline silicon (c-Si).C-Si has up to 4.30 specific refractory power and 0.073 low optical absorption coefficient under 500nm wavelength, and therefore people are attempting utilizing diverse ways to prepare the high refractive index film layer material of c-Si doping always.But because c-Si is difficult for processing, surface can high easily be assembled simultaneously, and therefore people's present stage is also confined to plasma etching method, chemical Vapor deposition process and high-energy mechanical ball milling method etc. to the working method of c-Si.But these methods are all subject to the restriction of the processing means such as instrument.Therefore, how c-Si is carried out to modification, to improve its dispersing property, can be uniform and stable be dispersed in organic materials, reduce or even avoid its clustering phenomena be we endeavour always solve problem.
Summary of the invention
The above-mentioned deficiency that the object of the invention is to overcome prior art, provides c-Si of a kind of surface modification and preparation method thereof, to solve in existing c-Si and organic composite material due to c-Si bad dispersibility, the technical problem of clustering phenomena easily occurs.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of c-Si surface modifying method, comprises the steps:
Obtain c-Si nanoparticle, and acid solution processing is carried out in its surface;
To carry out acid solution described c-Si nanoparticle after treatment and be scattered in organic solvent, form dispersion system;
Described dispersion system is heated to, after 70～90 DEG C, add silane coupling agent, and the temperature that keeps described dispersion system is 70～90 DEG C and reacts; After question response finishes, carry out solid-liquid separation, washing, drying treatment, obtain the c-Si nanoparticle of surface modification.
And, a kind of c-Si of surface modification, it is to be prepared by above-mentioned c-Si surface modifying method.
And the c-Si of above-mentioned surface modification is at display device, the application in optical mirror slip and photoelectric material.
Compared with prior art, above-mentioned c-Si surface modifying method adopts silane coupling agent to carry out modifying and decorating to c-Si nanoparticle surface, make the c-Si of the surface modification preparing there is excellent dispersing property, thereby overcome the existing deficiency that c-Si working method is existed as plasma etching method, chemical Vapor deposition process and high-energy mechanical ball milling method, avoid being subject to the restriction of instrument, reduced production cost.
In addition, the c-Si of the surface modification preparing by above-mentioned c-Si surface modifying method is owing to having excellent dispersing property, thereby give the uniform specific refractory power of matrix material that itself and organism form, and specific refractory power is high, easily processing, there is high impact strength, avoided occurring in matrix material c-Si clustering phenomena.Just, because the c-Si of above-mentioned surface modification has this excellent dispersing property, it can be at display device, is used widely, and improves the optical property of related products in optical mirror slip and photoelectric material.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of c-Si surface modifying method.The method comprises the steps:
S01: obtain c-Si nanoparticle, and acid solution processing is carried out in its surface;
S02: will carry out acid solution described c-Si nanoparticle after treatment and be scattered in organic solvent, and form dispersion system;
S03: described dispersion system is heated to, after 70～90 DEG C, add silane coupling agent, and the temperature that keeps described dispersion system is 70～90 DEG C and reacts; After question response finishes, carry out solid-liquid separation, washing, drying treatment, obtain the c-Si nanoparticle of surface modification.
Particularly, the c-Si nanoparticle in above-mentioned steps S01 is selected the c-Si nanoparticle of this area commercialization.
The method of in one embodiment, in step S01, this c-Si nanoparticle surface being carried out to acid solution processing is as follows:
C-Si nanoparticle is dipped in to H
2sO
4/ HNO
3with H
2o
2mixing solutions in boil to without micro-bubble produce after, carry out solid-liquid separation, cleaning, drying treatment.
At dry c-Si nanoparticle at H
2sO
4/ HNO
3with H
2o
2mixing solutions in the process of boiling, this c-Si nanoparticle surface oxide treatment, makes this c-Si nanoparticle surface generate SiO
2layer.The oxidizing reaction occurring in this oxidation processes has: Si+H
2o
2→ H
2o+SiO
2.
Wherein, H
2sO
4/ HNO
3with H
2o
2volume ratio be 1:9-9:1.H
2sO
4/ HNO
3with H
2o
2mixing solutions can be by dense H
2sO
4/ HNO
3the H that (mass concentration is 98%) and mass concentration are 30%
2o
2according to H
2sO
4/ HNO
3with H
2o
2volume ratio be 1:9-9:1, the ratio that is specially 7:3 is carried out combination treatment and is obtained.This H
2sO
4/ HNO
3refer to H
2sO
4or HNO
3or H
2sO
4with HNO
3mixed solution.
Until c-Si nanoparticle, after acid solution is processed, the object of reaction system being carried out to solid-liquid separation is from reaction system, to separate through acid solution c-Si nanoparticle after treatment, as adopted centrifugation to separate solid-liquid.The method of washing can be successively with centrifugal after deionized water and ethanol supersound washing nanoparticle, to remove residual reaction solution.Be dried and can adopt vacuum-drying.
In above-mentioned steps S02, in dispersion system, be preferably (0.01～3) g:(50～200 through the solid-to-liquid ratio of acid solution c-Si nanoparticle after treatment and organic solvent) ml.This dispersion concentration can effectively ensure through acid solution c-Si nanoparticle after treatment dispersed.Wherein, organic solvent is preferably at least one in dehydrated alcohol, propyl alcohol, butanols, Virahol, dimethyl formamide or DMAA.This preferred organic solvent has certain polarity, can make to process c-Si nanoparticle dispersion effect through acid solution better, forms stable dispersion system.
The mode being scattered in organic solvent through acid solution c-Si nanoparticle after treatment can adopt ultrasonic dispersion.Certainly, as long as can be by the dispersed middle organic solvent of acid solution c-Si nanoparticle after treatment, all within embodiment of the present invention scope of disclosure.
In above-mentioned steps S03, the c-Si nanoparticle in dispersion system and silane coupling agent carry out in reaction process, the SiO that silane coupling agent and c-Si nanoparticle surface generate
2react, make the alkoxyl group hydrolysis of silane coupling agent be grafted to SiO
2surface, modifies c-Si nanoparticle surface to realize.
In order to make c-Si nanoparticle surface be able to abundant modifying and decorating, the relative c-Si nanoparticle of this silane coupling agent is excessive, and in one embodiment, this silane coupling agent add-on is 5～15% of c-Si nanoparticle quality.
In another embodiment, this silane coupling agent is selected at least one in 3-aminopropyl triethoxysilane (KH-550), 3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560), 3-(methacryloxypropyl) propyl trimethoxy silicane (KH-570), 3-(trimethoxysilyl)-1-propylmercaptan (KH-590).Select the more effective modification c-Si nanoparticle surface of silane coupling agent energy of this kind, significantly improve the dispersing property of the c-Si nanoparticle of product surface modification.
It is sufficient reaction that silane coupling agent reacts at 70～90 DEG C of temperature with c-Si nanoparticle, until reaction finishes.Contriver finds under study for action, and at this temperature, the reaction times is controlled at 24～48 hours, substantially can ensure both complete reactions, thereby save the unnecessary reaction times, has improved production efficiency.
In order to improve reaction efficiency and this silane coupling agent to be modified c-Si nano particle surface modifying more uniformly, then when adding silane coupling agent, reaction system is attended by the operation of stirring.
Therefore, above-mentioned c-Si surface modifying method adopts silane coupling agent to carry out modifying and decorating to c-Si nanoparticle surface, makes the c-Si of the surface modification preparing have excellent dispersing property.And avoid the restriction of instrument, reduced production cost.
Correspondingly, on the basis based on above-mentioned c-Si surface modifying method, the embodiment of the present invention also provides a kind of c-Si of surface modification, and this is directly prepared by above-mentioned c-Si surface modifying method.Have excellent dispersing property just because of the c-Si of this surface modification, it can be prepared into together with organism to high refractive index matrix material, and give this matrix material uniform specific refractory power, and specific refractory power is high, easily processing, has high impact strength.Therefore, the c-Si of this surface modification with and be prepared into high refractive index matrix material together with organism all can be at display device, in optical mirror slip and photoelectric material, be used widely, and improve the optical property of related products.
Now, taking c-Si of surface modification and preparation method thereof as example, the present invention is further elaborated.
Embodiment 1
C-Si of a kind of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification comprises the steps:
S11: the c-Si nanoparticle of 5g is dipped in to the dense H of 200ml
2sO
4/ 30%H
2o
2mixing solutions in the (H of massfraction 98%
2sO
4h with massfraction 30%
2o
2, both volume ratio 7:3) boil to producing without micro-bubble; Be cooled to room temperature by nanoparticle centrifugation after boiling, then use successively after deionized water and ethanol supersound washing nanoparticle centrifugally again, vacuum is drained stand-by;
S12: the nanoparticle of the processing in 3g step S11 is dispersed in 200ml anhydrous isopropyl alcohol, dispersion system is heated to 75 DEG C, in agitation condition downhill reaction system, adds 0.2g silane coupling agent 3-aminopropyl triethoxysilane (KH-550); 75 DEG C of reactions of maintenance system 48 hours, are cooled to room temperature, by nanoparticle and Virahol centrifugation, clean nanoparticle final vacuum successively drain with acetone and ethanol, have just obtained the c-Si nanoparticle of surface modification.
Dispersivity test: the c-Si nanoparticle of surface modification prepared by the present embodiment 1 adopts the way of ultrasonic dispersion to be dispersed in Virahol with the concentration of 10mg/ml, its dispersion soln can be stablized and deposits more than 1 month.
Embodiment 2
C-Si of a kind of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification comprises the steps:
S21: the c-Si nanoparticle of 3g is dipped in to the dense H of 100ml
2sO
4/ 30%H
2o
2mixing solutions in the (H of massfraction 98%
2sO
4h with massfraction 30%
2o
2, both volume ratio 7:3) boil to producing without micro-bubble; Be cooled to room temperature by nanoparticle centrifugation after boiling, then use successively after deionized water and ethanol supersound washing nanoparticle centrifugally again, vacuum is drained stand-by;
S22: the nanoparticle that 2g said process was processed is dispersed in 150ml dimethyl formamide, dispersion system is heated to 60 DEG C, in agitation condition downhill reaction system, adds 0.3g silane coupling agent 3-(trimethoxysilyl)-1-propylmercaptan; 60 DEG C of reactions of maintenance system 36 hours, are cooled to room temperature, by nanoparticle and dimethyl formamide centrifugation, clean nanoparticle final vacuum successively drain with acetone and ethanol, have just obtained the c-Si nanoparticle of surface modification.
Dispersivity test: the c-Si nanoparticle of surface modification prepared by the present embodiment 2 adopts the way of ultrasonic dispersion to be dispersed in polyvinyl alcohol with the concentration of 10mg/ml, its dispersion soln can be stablized and deposits more than 1 month.
Embodiment 3
C-Si of a kind of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification comprises the steps:
S31: the c-Si nanoparticle of 3g is dipped in to the dense H of 100ml
2sO
4/ 30%H
2o
2mixing solutions in the (H of massfraction 98%
2sO
4h with massfraction 30%
2o
2, both volume ratio 7:3) boil to producing without micro-bubble.Be cooled to room temperature by nanoparticle centrifugation after boiling, then use successively after deionized water and ethanol supersound washing nanoparticle centrifugally again, vacuum is drained stand-by.
S32: the nanoparticle that 2g said process was processed is dispersed in 150ml dimethyl formamide, dispersion system is heated to 90 DEG C, in agitation condition downhill reaction system, adds 0.3g silane coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560).90 DEG C of reactions of maintenance system 24 hours, are cooled to room temperature, by nanoparticle and dimethyl formamide centrifugation, clean nanoparticle final vacuum successively drain with acetone and ethanol, have just obtained the c-Si nanoparticle of surface modification.
Dispersivity test: the c-Si nanoparticle of surface modification prepared by the present embodiment 3 adopts the way of ultrasonic dispersion to be dispersed in DMAA with the concentration of 10mg/ml, its dispersion soln can be stablized and deposits more than 1 month.
Embodiment 4
C-Si of a kind of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification comprises the steps:
S41: the c-Si nanoparticle of 3g is dipped in to the dense HNO of 200ml
3/ 30%H
2o
2mixing solutions in (dense HNO
3h with massfraction 30%
2o
2, both volume ratio 1:9) boil to producing without micro-bubble.Be cooled to room temperature by nanoparticle centrifugation after boiling, then use successively after deionized water and ethanol supersound washing nanoparticle centrifugally again, vacuum is drained stand-by.
S42: the nanoparticle that 2g said process was processed is dispersed in 150ml butanols, dispersion system is heated to 80 DEG C, in agitation condition downhill reaction system, adds 0.3g silane coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560).90 DEG C of reactions of maintenance system 24 hours, are cooled to room temperature, by nanoparticle and butanols centrifugation, clean nanoparticle final vacuum successively drain with acetone and ethanol, have just obtained the c-Si nanoparticle of surface modification.
Dispersivity test: the c-Si nanoparticle of surface modification prepared by the present embodiment 3 adopts the way of ultrasonic dispersion to be dispersed in DMAA with the concentration of 10mg/ml, its dispersion soln can be stablized and deposits more than 1 month.
Embodiment 5
C-Si of a kind of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification comprises the steps:
S51: the HNO that the c-Si nanoparticle of 3g is dipped in to the dense volume ratio 1:1 of 50ml
3with H
2sO
4mixing acid/30%H
2o
2mixing solutions in (dense HNO
3h with massfraction 30%
2o
2, both volume ratio 1:9) boil to producing without micro-bubble.Be cooled to room temperature by nanoparticle centrifugation after boiling, then use successively after deionized water and ethanol supersound washing nanoparticle centrifugally again, vacuum is drained stand-by.
S52: the nanoparticle that 2g said process was processed is dispersed in 50ml Virahol, dispersion system is heated to 80 DEG C, in agitation condition downhill reaction system, adds 0.3g silane coupling agent 3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560).90 DEG C of reactions of maintenance system 24 hours, are cooled to room temperature, by nanoparticle and Virahol centrifugation, clean nanoparticle final vacuum successively drain with acetone and ethanol, have just obtained the c-Si nanoparticle of surface modification.
Dispersivity test: the c-Si nanoparticle of surface modification prepared by the present embodiment 3 adopts the way of ultrasonic dispersion to be dispersed in Virahol with the concentration of 10mg/ml, its dispersion soln can be stablized and deposits more than 1 month.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a c-Si surface modifying method, comprises the steps:
Obtain c-Si nanoparticle, and acid solution processing is carried out in its surface;
To carry out acid solution described c-Si nanoparticle after treatment and be scattered in organic solvent, form dispersion system;
Described dispersion system is heated to, after 70～90 DEG C, add silane coupling agent, and the temperature that keeps described dispersion system is 70～90 DEG C and reacts; After question response finishes, carry out solid-liquid separation, washing, drying treatment, obtain the c-Si nanoparticle of surface modification.
2. c-Si surface modifying method according to claim 1, is characterized in that: described silane coupling agent add-on is 5～15% of described c-Si nanoparticle quality.
3. c-Si surface modifying method according to claim 1 and 2, is characterized in that: described silane coupling agent is selected at least one in 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl trimethoxy silicane, 3-(methacryloxypropyl) propyl trimethoxy silicane, 3-(trimethoxysilyl)-1-propylmercaptan.
4. c-Si surface modifying method according to claim 1 and 2, is characterized in that: the temperature that keeps described dispersion system is that 60～90 DEG C of times of reacting are 24～48 hours.
5. c-Si surface modifying method according to claim 1, it is characterized in that: being scattered in the step of organic solvent carrying out acid solution described c-Si nanoparticle after treatment, the solid-to-liquid ratio of described c-Si nanoparticle and organic solvent is (0.01～3) g:(50～200) ml.
6. according to the c-Si surface modifying method described in claim 1,2 or 5, it is characterized in that: being scattered in the step of organic solvent carrying out acid solution described c-Si nanoparticle after treatment, described organic solvent is selected at least one in dehydrated alcohol, propyl alcohol, butanols, Virahol, dimethyl formamide or DMAA.
7. c-Si surface modifying method according to claim 1, is characterized in that: the method that described c-Si nanoparticle surface is carried out to acid solution processing is as follows:
Described c-Si nanoparticle is dipped in to H
2sO
4/ HNO
3with H
2o
2mixing solutions in boil to without micro-bubble produce after, carry out solid-liquid separation, cleaning, drying treatment; Wherein, H
2sO
4/ HNO
3with H
2o
2volume ratio be 1:9-9:1.
8. c-Si surface modifying method according to claim 7, is characterized in that: described c-Si nanoparticle and H
2sO
4/ HNO
3with H
2o
2the solid-to-liquid ratio of mixing solutions be g (0.01～5) g:(100～200) ml.
9. a c-Si for surface modification, is characterized in that: the c-Si of described surface modification is prepared by the arbitrary described c-Si surface modifying method of claim 1-8.
10. if the c-Si of the surface modification in claim 9 is at display device, the application in optical mirror slip and photoelectric material.
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2014
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| CN1232833A (en) * | 1998-04-10 | 1999-10-27 | 协和化学工业株式会社 | Process for production of coupling agent-treated inorganic particles and use thereof |
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Address after: 518000 31 / F, block B, building 7, Wanke Yuncheng phase 3, Nanshan District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Water New Material Co.,Ltd. Address before: 518000 Guangdong city of Shenzhen province Nanshan District Nantou two road crossing forward hot electrons strategic emerging industrial park 10 Patentee before: Shenzhen Water New Material Co.,Ltd. |
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Denomination of invention: Surface modified c-Si and its preparation method and application Effective date of registration: 20230525 Granted publication date: 20160824 Pledgee: Shenzhen small and medium sized small loan Co.,Ltd. Pledgor: Shenzhen Water New Material Co.,Ltd. Registration number: Y2023980041875 |