CN104109405B - C-Si of surface modification and preparation method and application - Google Patents
C-Si of surface modification and preparation method and application Download PDFInfo
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- CN104109405B CN104109405B CN201410364653.8A CN201410364653A CN104109405B CN 104109405 B CN104109405 B CN 104109405B CN 201410364653 A CN201410364653 A CN 201410364653A CN 104109405 B CN104109405 B CN 104109405B
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Abstract
The invention discloses c-Si of a kind of surface modification and preparation method and application.The c-Si preparation method of this surface modification include c-Si nanoparticle surface is carried out acid solution process step, by the scattered step of c-Si nano particle processed through acid solution and by the c-Si nano particle that processes through acid solution with silane coupler in 70～90 DEG C of steps reacted.The c-Si preparation method of above-mentioned surface modification uses silane coupler to be modified c-Si nanoparticle surface modifying so that the c-Si of the surface modification prepared has the dispersive property of excellence, it is to avoid is limited by instrument, reduces production cost.
Description
Technical field
The invention belongs to nano particle surface modifying technical field, particularly to a kind of surface modification c-Si and
Its preparation method and application.
Background technology
High index of refraction optical material is coated with in eyeglass, optical filter, photoelectric device, high reflection and antireflective
Layer has good development prospect in field, and therefore high-index material is always the optics of people's primary study
One of material.Conventional inorganic material has the highest refractive index (ranges of indices of refraction is adjustable from 2.0～5.0),
But inorganic material density is big, poor toughness, be difficult to processing, especially in preparing antireflection coatings, due to nothing
The refractive index of machine material is difficult to continuously adjustabe, this adds increased the cost of process.
Being compared to inorganic material, organic material is more easy to processing, and organic material has more preferable shock resistance simultaneously
Intensity.But, the refractive index of organic material can only changing in a relatively small scope by group
(1.3～1.7) regulate, it is impossible to meet people's high index of refraction demand for material.
The high index of refraction composite developed has had easily processing and the high impact strength of organic material concurrently, with
And the feature of inorganic material high index of refraction high stability, therefore it is increasingly becoming the focus of people's research.But how
Inorganic material is avoided to occur to be separated with organic material in the composite, it is to avoid the gathering of inorganic material is people
Problem that can not ignore when preparing composite.
Specifically, such as the high index of refraction composite containing crystalline silicon (c-Si).C-Si is at 500nm wavelength
Under there is the refractive index of up to 4.30 and the low optical absorption coefficient of 0.073, therefore people are attempting always
Utilize different approach to prepare the high refractive index film layer material of c-Si doping.But owing to c-Si is difficult to processing,
Surface can easily be assembled by height simultaneously, and therefore people's present stage is also confined to plasma to the processing method of c-Si
Body etching method, chemical vapour deposition technique and high-energy mechanical ball milling method etc..But these methods are all by instrument etc.
The restriction of manufacturing process.Therefore, how c-Si is modified, to improve its dispersive property so that it is can
Uniform and stable is dispersed in organic material, reduce even avoid its clustering phenomena be we always
The problem endeavouring to solve.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of prior art, it is provided that the c-Si of a kind of surface modification and
Its preparation method, to solve in existing c-Si and organic composite material due to c-Si bad dispersibility, easily occurs poly-
The technical problem of collection phenomenon.
In order to realize foregoing invention purpose, technical scheme is as follows:
A kind of c-Si surface modifying method, comprises the steps:
Obtain c-Si nano particle, and its surface is carried out acid solution process；
Described c-Si nano particle after carrying out acid solution process is scattered in organic solvent, forms dispersion；
After described dispersion is heated to 70～90 DEG C, adds silane coupler, keep described dispersion
Temperature be 70～90 DEG C and react；After question response terminates, carry out separation of solid and liquid, wash, be dried process,
Obtain the c-Si nano particle of surface modification.
And, the c-Si of a kind 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 application in display device, optical mirror slip and photoelectric material.
Compared with prior art, above-mentioned c-Si surface modifying method uses silane coupler to c-Si nano particle
Modifying surface is modified so that the c-Si of the surface modification prepared has the dispersive property of excellence, from
And overcome existing to c-Si processing method such as plasma etching method, chemical vapour deposition technique and high energy mechanical ball
The deficiency that mill method exists, it is to avoid limited by instrument, reduce production cost.
It addition, the c-Si of the surface modification prepared by above-mentioned c-Si surface modifying method is excellent owing to having
Different dispersive property, thus give its uniform refractive index of composite formed with organic matter, and refraction
Rate is high, easily process, have high impact strength, it is to avoid c-Si clustering phenomena occur in composite.Just
Because the c-Si of above-mentioned surface modification has the dispersive property of this excellence, it can be at display device, optical mirror slip
It is used widely with in photoelectric material, and improves the optical property of Related product.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, with
Under in conjunction with the embodiments, the present invention is further elaborated.Should be appreciated that described herein specifically
Embodiment 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 nano particle, and its surface is carried out acid solution process；
S02: the described c-Si nano particle after carrying out acid solution process is scattered in organic solvent, is formed and divides
Prose style free from parallelism system；
S03: after described dispersion is heated to 70～90 DEG C, adds silane coupler, keeps described dispersion
The temperature of system is 70～90 DEG C and reacts；After question response terminates, carry out separation of solid and liquid, wash, be dried
Process, obtain the c-Si nano particle of surface modification.
Specifically, the c-Si nano particle in above-mentioned steps S01 selects the c-Si nano particle that this area is commercial.
In one embodiment, step S01 carries out the method for acid solution process such as to this c-Si nanoparticle surface
Under:
C-Si nano particle is dipped in H2SO4/HNO3With H2O2Mixed solution in boil to without micro-bubble
After generation, carry out separation of solid and liquid, clean, be dried process.
At dry c-Si nano particle at H2SO4/HNO3With H2O2Mixed solution in boil during, should
C-Si nanoparticle surface oxidation processes so that this c-Si nanoparticle surface generates SiO2Layer.At this oxidation
The oxidation reaction occurred during reason has: Si+H2O2→H2O+SiO2。
Wherein, H2SO4/HNO3With H2O2Volume ratio be 1:9-9:1.H2SO4/HNO3With H2O2Mixed
Closing solution can be by dense H2SO4/HNO3(mass concentration is 98%) and mass concentration are the H of 30%2O2
According to H2SO4/HNO3With H2O2The ratio that volume ratio is 1:9-9:1, specially 7:3 carry out mixed processing
Obtain.This H2SO4/HNO3Refer to H2SO4Or HNO3Or H2SO4With HNO3Mixed liquor.
Until c-Si nano particle after acid solution processes, the purpose that reaction system carries out separation of solid and liquid is by through acid
C-Si nano particle after liquid processes is separated from reaction system, as solid in centrifugation can be used to separate
Liquid.The method of washing can be successively with centrifugal, to remove after deionized water and EtOH Sonicate washing nano particle
Go to remain reactant liquor.It is dried and can use vacuum drying.
In above-mentioned steps S02 in dispersion, the c-Si nano particle after acid solution processes and organic solvent
Solid-to-liquid ratio is preferably (0.01～3) g:(50～200) ml.This dispersion concentration can be effectively ensured and process through acid solution
After c-Si nano particle dispersed.Wherein, organic solvent be preferably absolute ethyl alcohol, propyl alcohol, butanol,
At least one in isopropanol, dimethylformamide or DMAA.This preferred organic solvent has
There is certain polarity, can make to process c-Si nano particle dispersion effect through acid solution more preferable, form stable dispersion
System.
The mode that c-Si nano particle after acid solution processes is scattered in organic solvent can use ultrasonic point
Dissipate.Certainly, as long as can by dispersed for the c-Si nano particle after acid solution processes middle organic solvent,
All within embodiment of the present invention scope of disclosure.
In above-mentioned steps S03, the c-Si nano particle in dispersion and silane coupler carry out course of reaction
In, the SiO that silane coupler generates with c-Si nanoparticle surface2React so that silane coupler
Alkoxyl hydrolysis is grafted to SiO2Surface, to realize modifying c-Si nanoparticle surface.
So that c-Si nanoparticle surface is able to abundant modifying and decorating, this silane coupler is received relative to c-Si
Rice corpuscles excess, in one embodiment, this silane coupler addition is c-Si nano particle quality
5～15%.
In another embodiment, this silane coupler select 3-aminopropyl triethoxysilane (KH-550),
3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560), 3-(methacryloxypropyl) propyl group trimethoxy
At least one in base silane (KH-570), 3-(trimethoxysilyl)-1-propanethiol (KH-590).
Select the most modified c-Si nanoparticle surface of silane coupler energy of this kind, significantly improve product table
The dispersive property of the c-Si nano particle that face is modified.
It is sufficiently reaction that silane coupler and c-Si nano particle react at a temperature of 70～90 DEG C, directly
Terminate to reaction.Inventor finds under study for action, and at such a temperature, the reaction time controls at 24～48 hours,
Substantially can guarantee that both reactions completely, thus save the unnecessary reaction time, improve production effect
Rate.
In order to improve reaction efficiency and make this silane coupler more uniform to c-Si nano particle surface modifying
Modify, while adding silane coupler, reaction system is attended by the operation of stirring.
Therefore, above-mentioned c-Si surface modifying method uses silane coupler to change c-Si nanoparticle surface
Sex modification so that the c-Si of the surface modification prepared has the dispersive property of excellence.And avoid instrument
Restriction, reduce production cost.
Correspondingly, on the basis of above-mentioned c-Si surface modifying method, the embodiment of the present invention additionally provides one
Planting the c-Si of surface modification, this is directly prepared by above-mentioned c-Si surface modifying method.Just because of this table
The c-Si of face modification has the dispersive property of excellence, it can be prepared as together with organic matter high index of refraction multiple
Condensation material, and give this composite uniform refractive index, and refractive index is high, easily processes, has high-impact
Hit intensity.Therefore, the c-Si of this surface modification and its be prepared as high index of refraction composite wood together with organic matter
Material all can be used widely in optical mirror slip and photoelectric material at display device, and improve Related product
Optical property.
Now as a example by c-Si of surface modification and preparation method thereof, the present invention is further elaborated.
Embodiment 1
A kind of c-Si of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification include as
Lower step:
S11: the c-Si nano particle of 5g is dipped in the dense H of 200ml2SO4/ 30%H2O2Mixed solution in
(the H of mass fraction 98%2SO4H with mass fraction 30%2O2, both volume ratios 7:3) boil
Produce to without micro-bubble；Boil and be cooled to room temperature afterwards by nano particle centrifugation, spend the most successively
Being centrifuged after ionized water and EtOH Sonicate washing nano particle, vacuum is drained stand-by again；
S12: the nano particle processed in 3g step S11 is dispersed in 200ml anhydrous isopropyl alcohol,
Dispersion is heated to 75 DEG C, in reaction system, adds 0.2g silane coupler 3-under agitation
Aminopropyl triethoxysilane (KH-550)；Holding system 75 DEG C is reacted 48 hours, is cooled to room temperature,
By nano particle and isopropanol centrifugation, drain with acetone and ethanol purge nano particle final vacuum successively,
Just obtain the c-Si nano particle of surface modification.
Dispersivity test: the c-Si nano particle of the surface modification prepared by the present embodiment 1 is with 10mg/ml's
Concentration uses the way of ultrasonic disperse to be dispersed in isopropanol, and its dispersion soln can stably be deposited more than 1 month.
Embodiment 2
A kind of c-Si of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification include as
Lower step:
S21: the c-Si nano particle of 3g is dipped in the dense H of 100ml2SO4/ 30%H2O2Mixed solution in
(the H of mass fraction 98%2SO4H with mass fraction 30%2O2, both volume ratios 7:3) boil
Produce to without micro-bubble；Boil and be cooled to room temperature afterwards by nano particle centrifugation, spend the most successively
Being centrifuged after ionized water and EtOH Sonicate washing nano particle, vacuum is drained stand-by again；
S22: be dispersed in 150ml dimethylformamide by the nano particle that 2g said process processed, will
Dispersion is heated to 60 DEG C, adds 0.3g silane coupler 3-(three under agitation in reaction system
Methoxysilyl)-1-propanethiol；Holding system 60 DEG C is reacted 36 hours, is cooled to room temperature, by nanometer
Particle and dimethylformamide centrifugation, drain with acetone and ethanol purge nano particle final vacuum successively,
Just obtain the c-Si nano particle of surface modification.
Dispersivity test: the c-Si nano particle of the surface modification prepared by the present embodiment 2 is with 10mg/ml's
Concentration use ultrasonic disperse way be dispersed in polyvinyl alcohol, its dispersion soln can stably deposit 1 month with
On.
Embodiment 3
A kind of c-Si of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification include as
Lower step:
S31: the c-Si nano particle of 3g is dipped in the dense H of 100ml2SO4/ 30%H2O2Mixed solution in
(the H of mass fraction 98%2SO4H with mass fraction 30%2O2, both volume ratios 7:3) boil to
Produce without micro-bubble.Boil and be cooled to room temperature afterwards by nano particle centrifugation, spend the most successively from
Being centrifuged after sub-water and EtOH Sonicate washing nano particle, vacuum is drained stand-by again.
S32: be dispersed in 150ml dimethylformamide by the nano particle that 2g said process processed, will
Dispersion is heated to 90 DEG C, adds 0.3g silane coupler 3-under agitation and shrink in reaction system
Glycerin ether oxygen propyl trimethoxy silicane (KH-560).Holding system 90 DEG C is reacted 24 hours, is cooled to
Room temperature, by nano particle and dimethylformamide centrifugation, successively with acetone and ethanol purge nano particle
Final vacuum is drained, and has just obtained the c-Si nano particle of surface modification.
Dispersivity test: the c-Si nano particle of the surface modification prepared by the present embodiment 3 is with 10mg/ml's
Concentration uses the way of ultrasonic disperse to be dispersed in DMAA, and its dispersion soln can stably deposit 1
More than individual month.
Embodiment 4
A kind of c-Si of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification include as
Lower step:
S41: the c-Si nano particle of 3g is dipped in the dense HNO of 200ml3/ 30%H2O2Mixed solution in
(dense HNO3H with mass fraction 30%2O2, both volume ratios 1:9) boil and produce to without micro-bubble
Raw.Boil and be cooled to room temperature afterwards by nano particle centrifugation, surpass with deionized water and ethanol the most successively
Being centrifuged after sound washing nano particle, vacuum is drained stand-by again.
S42: the nano particle that 2g said process processed is dispersed in 150ml butanol, by dispersion
It is heated to 80 DEG C, in reaction system, adds 0.3g silane coupler 3-glycidyl ether oxygen under agitation
Propyl trimethoxy silicane (KH-560).Holding system 90 DEG C is reacted 24 hours, is cooled to room temperature, will
Nano particle and butanol centrifugation, drain with acetone and ethanol purge nano particle final vacuum successively, must
Arrive the c-Si nano particle of surface modification.
Dispersivity test: the c-Si nano particle of the surface modification prepared by the present embodiment 3 is with 10mg/ml's
Concentration uses the way of ultrasonic disperse to be dispersed in DMAA, and its dispersion soln can stably deposit 1
More than individual month.
Embodiment 5
A kind of c-Si of surface modification and preparation method thereof.The preparation method of the c-Si of this surface modification include as
Lower step:
S51: the c-Si nano particle of 3g is dipped in the HNO of dense volume ratio 1:1 of 50ml3With H2SO4Mixing
Acid/30%H2O2Mixed solution in (dense HNO3H with mass fraction 30%2O2, both volume ratios
1:9) boil to without micro-bubble generation.Boil and be cooled to room temperature afterwards by nano particle centrifugation, then
Being centrifuged after washing nano particle with deionized water and EtOH Sonicate successively, vacuum is drained stand-by again.
S52: the nano particle that 2g said process processed is dispersed in 50ml isopropanol, by dispersion
System is heated to 80 DEG C, adds 0.3g silane coupler 3-glycidol ether under agitation in reaction system
Oxygen propyl trimethoxy silicane (KH-560).Holding system 90 DEG C is reacted 24 hours, is cooled to room temperature,
By nano particle and isopropanol centrifugation, drain with acetone and ethanol purge nano particle final vacuum successively,
Just obtain the c-Si nano particle of surface modification.
Dispersivity test: the c-Si nano particle of the surface modification prepared by the present embodiment 3 is with 10mg/ml's
Concentration uses the way of ultrasonic disperse to be dispersed in isopropanol, and its dispersion soln can stably be deposited more than 1 month.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (5)
1. a c-Si surface modifying method, comprises the steps:
Obtain c-Si nano particle, and its surface is carried out acid solution process；
Described c-Si nano particle after carrying out acid solution process is scattered in organic solvent, forms dispersion；
After described dispersion is heated to 70～90 DEG C, adds silane coupler, keep described dispersion
Temperature be 70～90 DEG C and react, the time of reaction is 24～48 hours；After question response terminates, carry out
Separation of solid and liquid, wash, be dried process, obtain the c-Si nano particle of surface modification；
Wherein, described c-Si nano particle is (0.01～3) g:(50～200 with the solid-to-liquid ratio of organic solvent) ml；
Described silane coupler addition is the 5～15% of described c-Si nano particle quality；
The method that described c-Si nanoparticle surface is carried out acid solution process is as follows:
Described c-Si nano particle is dipped in H2SO4/HNO3With H2O2Mixed solution in boil to without small
Bubble produce after, carry out separation of solid and liquid, clean, be dried process；Wherein, H2SO4/HNO3With H2O2's
Volume ratio is 1:9-9:1；
Described c-Si nano particle and H2SO4/HNO3With H2O2The solid-to-liquid ratio of mixed solution be
(0.01～5) g:(100～200) ml.
C-Si surface modifying method the most according to claim 1, it is characterised in that: described silane coupled
3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl trimethoxy silicane, 3-(methyl are selected in agent
Acryloyl-oxy) propyl trimethoxy silicane, at least one in 3-(trimethoxysilyl)-1-propanethiol.
C-Si surface modifying method the most according to claim 1, it is characterised in that: acid solution will carried out
Described c-Si nano particle after process is scattered in the step of organic solvent, and described organic solvent is selected anhydrous
At least one in ethanol, propyl alcohol, butanol, isopropanol, dimethylformamide or DMAA.
4. the c-Si of a surface modification, it is characterised in that: the c-Si of described surface modification is by claim
The arbitrary described c-Si surface modifying method of 1-3 prepares.
5. if the c-Si of the surface modification in claim 4 is in display device, optical mirror slip and photoelectric material
Application.
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