CN102931149A - Nano-silicon dioxide and nano-silicon nitride composite material and preparation method thereof - Google Patents
Nano-silicon dioxide and nano-silicon nitride composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a nano-silicon dioxide and nano-silicon nitride composite material. The nano-silicon dioxide and nano-silicon nitride composite material comprises a plurality of microparticles formed by coating nano-silicon dioxide on the surface of nano-silicon nitride, wherein the mass ratio of the nano-silicon dioxide to the nano-silicon nitride is (1:10)-(10:1). The nano-silicon nitride and the nano-silicon dioxide are compounded according to the mass ratio of (1:10)-(10:1), so that the composite material is favorable in stability and lower in dielectric constant and can be widely applied to the fields of package of super-large-scale integrated circuits and electronics and the like. The invention further provides a manufacturing method of the nano-silicon dioxide and nano-silicon nitride composite material.
Description
Technical field
The present invention relates to the preparations of nanomaterials technical field, particularly relate to a kind of nano silicon clad nano silicon nitride composite material and preparation method thereof.
Background technology
Nano-silicon nitride is a kind of important structural material, and it is a kind of superhard material, and itself has lubrification, and wear-resistant; Except hydrofluoric acid, it not with other inorganic acid reaction, resistance to corrosion is strong, and is anti-oxidant during high temperature.And it can also resist thermal shock, is heated in air more than 1000 ℃, and sharply more sharply heating of cooling can be not cracked yet.Specific to the physical property aspect, silicon nitride material has the characteristics such as hardness is high, wear-resistant, modulus of elasticity is large, intensity is high, high temperature resistant, thermal coefficient of expansion is little, conductive coefficient is large, good thermal shock, density is low, skin-friction coefficient is little, electrical insulation capability is good; And the chemical property aspect, it is the advantage such as corrosion-resistant, anti-oxidant in addition.In Electronic Packaging, the Double-protection that silicone adds silicon nitride film can significantly improve the water resistance of electronic module.Silicon nitride is widely used in semiconductor device and semiconductor integrated circuit as a kind of passivation and insulating film material.But itself dielectric constant is higher, has hindered its application at the encapsulation field insulating material.
Particle diameter is very little because having for nano silicon, specific area large, adsorption power reaches by force the characteristics such as surface energy is large and has the performances such as small-size effect, quantum effect, skin effect and interfacial effect.Nowadays, along with the development that nanometer technology is advanced by leaps and bounds, the synthetic and application of different types of nanometer titanium dioxide silicon materials has also risen to a new height.But compare with silicon nitride, the thermal stability of nano silicon and chemical stability than nano-silicon nitride a little less than.
Although nano-silicon nitride and nano silicon respectively have advantage, its limitation is not satisfy the high performance requirements of hyundai electronics encapsulation field.
Summary of the invention
Based on this, be necessary to provide a kind of good stability, nano silicon that dielectric constant is lower-nano silicon nitride composited material.
Further, provide a kind of nano silicon-nano silicon nitride composited material preparation method.
A kind of nano silicon-nano silicon nitride composited material comprises a plurality ofly being coated on the particulate that the nano silicon nitride silicon face forms by nano silicon that wherein, the mass ratio of described nano-silicon nitride and described nano silicon is 1:1 ~ 10:1.
Among embodiment, the particle diameter of described particulate is 20 nanometers ~ 100 nanometers therein.
Among embodiment, comprise the steps: therein
Under stirring condition, will obtain mixture in dispersant and the nano-silicon nitride adding solvent, in described mixture, drip acid solution, obtain the nano-silicon nitride dispersion liquid, wherein, the solid-to-liquid ratio of described dispersant, nano-silicon nitride and solvent is 0.1 ~ 10g:5 ~ 100g:10 ~ 200mL;
Stir described nano-silicon nitride dispersion liquid, and the pH value of regulating described nano-silicon nitride dispersion liquid is 9 ~ 12, then drip the solution that contains tetraethoxysilane to described nano-silicon nitride dispersion liquid, at room temperature reacted 36 hours ~ 84 hours, obtain suspension, wherein, the mass ratio of described tetraethoxysilane and described nano-silicon nitride is 10 ~ 200:5 ~ 100;
Described suspension is carried out the centrifugal thing that is precipitated, wash described sediment and drying and obtain nano silicon-nano silicon nitride composited material.
Therein among embodiment, described dispersant is selected from least a in silane coupler KH-560 and the silane resin acceptor kh-550.
Therein among embodiment, described solvent is selected from least a in ethanol, acetone and the butanone.
Therein among embodiment, the described step that obtains the nano-silicon nitride dispersion liquid is specially under stirring and hyperacoustic effect, will dispersant and nano-silicon nitride add in the solvent and obtain mixture, drip the pH value in the described mixture and be 3.5 ~ 6 oxalic acid solution and obtain the nano-silicon nitride dispersion liquid.
Among embodiment, stir the step of described nano-silicon nitride dispersion liquid under 500 rev/mins ~ 1300 rev/mins rotating speed, stirring 5 minutes ~ 20 minutes therein.
Among embodiment, the described solution that contains tetraethoxysilane is for to be dissolved in tetraethoxysilane in the ethanol, and ultrasonic being uniformly dispersed obtains therein.
Therein among embodiment, the step of described washing is specially: under ul-trasonic irradiation, with described sediment with at least a washing the in ethanol, acetone or the butanone, then carry out centrifugal, repeat described washing and centrifugal each obtain pure sediment 5 times.
Therein among embodiment, the step of described drying be specially in 80 ℃ lower dry 10 hours, then the heating rate with 10 ℃/min is warming up to 400 ℃, and is lower dry 10 hours at 400 ℃.
Above-mentioned nano silicon-nano silicon nitride composited material comprises and a plurality ofly is coated on the particulate that the nano silicon nitride silicon face forms by nano silicon, nano-silicon nitride is as internal layer, can bring into play preferably advantage of nano-silicon nitride thermal stability and chemical stability, nano silicon is outer as coating, so that this composite material can be brought into play the lower advantage of nano silicon dielectric constant, nano silicon and nano-silicon nitride in mass ratio 1.546:1 carry out compound, so that the good stability of this composite material, dielectric constant is lower, can be widely used in the fields such as very lagre scale integrated circuit (VLSIC) Electronic Packaging.
Description of drawings
Fig. 1 is the nano silicon-nano silicon nitride composited material preparation method flow diagram of an execution mode;
Fig. 2 is the scanning electron microscope (SEM) photograph of the nano silicon-nano silicon nitride composited material of embodiment 1 preparation;
Fig. 3 is the scanning electron microscope (SEM) photograph of the nano silicon-nano silicon nitride composited material of embodiment 4 preparation.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement much to be different from alternate manner described here, and those skilled in the art can be in the situation that do similar improvement without prejudice to intension of the present invention, so the present invention is not subjected to the restriction of following public implementation.
The nano silicon of one execution mode-nano silicon nitride composited material comprises a plurality ofly being coated on the particulate that the nano silicon nitride silicon face forms by nano silicon.
Wherein, the mass ratio of nano-silicon nitride and nano silicon is 1:1 ~ 10:1.
The particle diameter of particulate is preferably 20 nanometers ~ 100 nanometers.
Nano-silicon nitride nanometer and silicon dioxide in mass ratio 1:1 ~ 10:1 carry out compoundly, and nano-silicon nitride can be brought into play nano-silicon nitride in the advantage of physics and chemistry aspect of performance as internal layer, and is better such as thermal stability and chemical stability; Nano silicon is outer as coating, the particle diameter of nano silicon is very little so that this composite material has, specific area large, adsorption power reaches by force the characteristics such as surface energy is large, the lower advantage of the dielectric constant of nano silicon particularly, thereby so that this nano silicon-nano silicon nitride composited material combines the advantage of two nano silicons and nano-silicon nitride, good and bad complementary, have advantages of that good stability, dielectric constant are lower, can be widely used in the fields such as very lagre scale integrated circuit (VLSIC) Electronic Packaging.
See also Fig. 1, the nano silicon of an execution mode-nano silicon nitride composited material preparation method comprises the steps:
Step S110: under stirring condition, with obtaining mixture in dispersant and the nano-silicon nitride adding solvent, in mixture, drip acid solution, obtain the nano-silicon nitride dispersion liquid.
Dispersant is used for making the nano-silicon nitride Uniform Dispersion, to obtain stable nano-silicon nitride dispersion liquid.
Dispersant is at least a in silane coupler KH-560 and silane resin acceptor kh-550 preferably.
It is the nano-silicon nitride of 15nm ~ 80nm that nano-silicon nitride preferably adopts particle diameter.
Solvent is selected from least a in ethanol, acetone and the butanone.
In order to improve the dispersion effect of nano-silicon nitride, in the process of preparation of nano silicon nitride dispersion liquid under stirring and hyperacoustic double action, to obtain mixture in dispersant and the nano-silicon nitride adding solvent, then drip the pH value in the mixture and be 3.5 ~ 6 acid solution, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness.
Acid solution can for oxalic acid solution, salpeter solution, hydrochloric acid solution etc., be preferably oxalic acid solution.
The purpose that adds acid solution is that nano-silicon nitride more stably is scattered in the solvent.The addition of acid solution be observe nano-silicon nitride and be dispersed in the solvent till.
Wherein, the solid-to-liquid ratio of dispersant, nano-silicon nitride and solvent is 0.1 ~ 10g:5 ~ 100g:10 ~ 200mL, so that nano-silicon nitride is scattered in the solvent equably.
Step S120: stir the nano-silicon nitride dispersion liquid, and the pH value of regulating the nano-silicon nitride dispersion liquid is 9 ~ 12, then contains the solution of tetraethoxysilane to the dropping of nano-silicon nitride dispersion liquid, at room temperature reacted 36 hours ~ 84 hours, obtain suspension.
The nano-silicon nitride dispersion liquid was stirred 5 minutes ~ 20 minutes under 500 rev/mins ~ 1300 rev/mins rotating speed, then the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid is 9 ~ 12, drip lentamente again the solution that contains tetraethoxysilane, at room temperature reacted at last 36 hours ~ 84 hours, and obtained the suspension of white.
Can stir with the agitating device of routine, such as mechanical stirring device, magnetic stirring apparatus etc., lower to equipment requirement.Present embodiment adopts the magnetic stirring apparatus of German instrument section (IKA).
Wherein, contain the solution of tetraethoxysilane for tetraethoxysilane is dissolved in the ethanol, and ultrasonic being uniformly dispersed obtains.Tetraethoxysilane is soluble in the ethanol, tetraethoxysilane is dissolved in the modest viscosity that makes tetraethoxysilane in the ethanol, and is easy to operate, can accurately control the addition of tetraethoxysilane.And, be beneficial to the nano silicon that the tetraethoxysilane reaction generates the pattern rule having of ethanol.
Contain in the solution of tetraethoxysilane, the solid-to-liquid ratio of tetraethoxysilane and ethanol is 1.5 ~ 30:10.
Before reacting, nano-silicon nitride was stirred 5 minutes ~ 20 minutes under 500 rev/mins ~ 1300 rev/mins rotating speed, be conducive to further prevent the nano-silicon nitride reunion, be coated on the particulate that the nano silicon nitride silicon face forms to prepare the uniform nano silicon of particle size distribution.
The mass ratio of tetraethoxysilane and nano-silicon nitride is 10 ~ 200:5 ~ 100.
Big or small nano-silicon nitride Uniform Dispersion by suitable technology controlling and process appropriate particle size, adopting the mass ratio of tetraethoxysilane and nano-silicon nitride is 10 ~ 200:5 ~ 100, and in conjunction with concrete reaction condition, control the thickness of nano silicon coating layer, be coated on the particle size of the particulate of nano silicon nitride silicon face formation with the control nano silicon.
Reaction is at room temperature carried out, and reaction condition is gentle, and energy consumption is low, and preparation cost is low.
Step S130: suspension is carried out the centrifugal thing that is precipitated, and washing precipitate and drying obtain nano silicon-nano silicon nitride composited material.
Suspension is carried out the centrifugal thing that is precipitated, under ul-trasonic irradiation, with sediment with at least a washing the in ethanol, acetone or the butanone, then carry out centrifugal, repeated washing and centrifugal each obtain pure sediment 5 times.
Pure sediment is positioned in the muffle furnace, and drying is 10 hours under 80 ℃, and then the heating rate with 10 ℃/min is warming up to 400 ℃, and drying is 10 hours under 400 ℃, obtains nano silicon-nano silicon nitride composited material.
The nano silicon for preparing-nano silicon nitride composited material comprises and a plurality ofly is coated on the particulate that the nano silicon nitride silicon face forms by nano silicon.The particle size of particulate is 20 nanometers ~ 100 nanometers, and wherein, the mass ratio of nano-silicon nitride and nano silicon is 1:1 ~ 10:1.
Above-mentioned nano silicon-nano silicon nitride composited material preparation method, technique is simple, and reaction condition is gentle, and is low for equipment requirements, and raw material are cheap, the comprehensive production cost of material is low, are easy to realize large-scale industrial production.
The method is by adopting suitable technological parameter, prepares that particle size distribution range is little, the nano silicon of favorable dispersibility-nano silicon nitride composited material.The method controllability is good, in nano silicon-nano silicon nitride composited material, the thickness of nano silicon coating layer and nanometer titanium dioxide silicone content are easy to control, thereby can implement change production technology, the different different composite materials of performance that obtain of production nanometer titanium dioxide silicone content particle diameters different, particulate according to different purposes, to enlarge the range of application of nano silicon-nano silicon nitride composited material.
And it is higher that this method prepares nano silicon-nano silicon nitride composited material purity, up to 99.8%.
It below is specific embodiment.
Embodiment 1
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the nano-silicon nitride that takes by weighing Silane coupling agent KH550, the 5g of 0.1g adds 10mL and is mixed with mixture in the acetone, then be 4 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 1000rpm rotating speed behind the stirring 10min is 9, then the solution that contains tetraethoxysilane that slowly to drip the ultrasonic tetraethoxysilane meltage that mixes be 15g, at room temperature react 64h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with acetone, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 20 ~ 40nm, and average grain diameter is that 25nm(is referring to Fig. 2).
Through the component content analysis, the mass percent of nano silicon is 45.2%, and the mass percent of nano-silicon nitride is 54.0%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.2%(nano silicon and nano-silicon nitride).
Embodiment 2
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the nano-silicon nitride that takes by weighing Silane coupling agent KH550, the 10g of 0.2g adds in the 20mL ethanol and is mixed with mixture, then be 5 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 1300rpm rotating speed behind the stirring 15min is 10, then the solution that contains tetraethoxysilane that slowly to drip the ultrasonic tetraethoxysilane meltage that mixes be 30g, at room temperature react 50h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with ethanol, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 50 ~ 100nm, and average grain diameter is 100nm.
Through the component content analysis, the mass percent of nano silicon is 45.6%, and the mass percent of nano-silicon nitride is 54.2%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.1%(nano silicon and nano-silicon nitride).
Embodiment 3
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the nano-silicon nitride that takes by weighing silane coupler KH560, the 5g of 0.1g adds in the 10mL ethanol and is mixed with mixture, then be 3.8 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 1000rpm rotating speed behind the stirring 10min is 11, then the solution that contains tetraethoxysilane that slowly to drip the ultrasonic tetraethoxysilane meltage that mixes be 10g, at room temperature react 70h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with ethanol, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 60 ~ 100nm, and average grain diameter is 90nm.
Through the component content analysis, the mass percent of nano silicon is 18.6%, and the mass percent of nano-silicon nitride is 80.8%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.4%(nano silicon and nano-silicon nitride).
Embodiment 4
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the nano-silicon nitride that takes by weighing silane coupler KH560, the 10g of 0.2g adds 10mL and is mixed with mixture in the acetone, then be 4 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 900rpm rotating speed behind the stirring 10min is 10, then the solution that contains tetraethoxysilane that slowly to drip the ultrasonic tetraethoxysilane meltage that mixes be 25g, at room temperature react 72h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with acetone, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 40 ~ 45nm, and average grain diameter is that 50nm(is referring to Fig. 3).
Through the component content analysis, the mass percent of nano silicon is 41.2%, and the mass percent of nano-silicon nitride is 57.9%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.8%(nano silicon and nano-silicon nitride).
Embodiment 5
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the Silane coupling agent KH550,10 the nano-silicon nitride that take by weighing 0.2g add in the 10mL butanone and are mixed with mixture, then be 4.5 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 1100rpm rotating speed behind the stirring 20min is 10, then the solution that contains tetraethoxysilane that slowly to drip the ultrasonic tetraethoxysilane meltage that mixes be 28g, at room temperature react 70h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with ethanol, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 40 ~ 80nm, and average grain diameter is 60nm.
Through the component content analysis, the mass percent of nano silicon is 43.9%, and the mass percent of nano-silicon nitride is 55.6%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.5%(nano silicon and nano-silicon nitride).
Embodiment 6
Preparation nano silicon-nano silicon nitride composited material
(1) under stirring and hyperacoustic effect, the nano-silicon nitride that takes by weighing 5g silane coupler KH560,5g Silane coupling agent KH550,50g adds in the mixed liquor of 50mL butanone and 50mL acetone and is mixed with mixture, then be 3.5 oxalic acid solution to wherein slowly dripping pH, obtain preferably nano-silicon nitride dispersion liquid of dispersiveness;
(2) the nano-silicon nitride dispersion liquid being placed the pH value that drips ammoniacal liquor adjusting nano-silicon nitride dispersion liquid under the 1300rpm rotating speed behind the stirring 20min is 10, then slowly dripping the ultrasonic tetraethoxysilane meltage that mixes is the teos solution of 100g, at room temperature react 84h, obtain the suspension of white, suspension is filtered be precipitated thing;
(3) above-mentioned sediment is carried out supersound washing with ethanol, then centrifugal, washing and centrifugally respectively repeat 5 times and obtain pure sediment, the sediment that this is pure places muffle furnace, in 80 ℃ of lower dry 10h, then the heating rate with 10 ℃/min is warming up to 400 ℃, namely obtains white nano silicon-nano silicon nitride composited material at 400 ℃ of lower dry 10h.
Through sem test, the grain diameter scope of gained nano silicon-nano silicon nitride composited material is 30 ~ 90nm, and average grain diameter is 55nm.
Through the component content analysis, the mass percent of nano silicon is 35.6%, and the mass percent of nano-silicon nitride is 63.7%.The purity of nano silicon-nano silicon nitride composited material is the mass percentage content sum of 99.3%(nano silicon and nano-silicon nitride).
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (10)
1. nano silicon-nano silicon nitride composited material is characterized in that, comprises a plurality ofly being coated on the particulate that the nano silicon nitride silicon face forms by nano silicon, and wherein, the mass ratio of described nano-silicon nitride and described nano silicon is 1:1 ~ 10:1.
2. nano silicon according to claim 1-nano silicon nitride composited material is characterized in that, the particle diameter of described particulate is 20 nanometers ~ 100 nanometers.
3. nano silicon-nano silicon nitride composited material preparation method is characterized in that, comprises the steps:
Under stirring condition, will obtain mixture in dispersant and the nano-silicon nitride adding solvent, in described mixture, drip acid solution, obtain the nano-silicon nitride dispersion liquid, wherein, the solid-to-liquid ratio of described dispersant, nano-silicon nitride and solvent is 0.1 ~ 10g:5 ~ 100g:10 ~ 200mL;
Stir described nano-silicon nitride dispersion liquid, and the pH value of regulating described nano-silicon nitride dispersion liquid is 9 ~ 12, then drip the solution that contains tetraethoxysilane to described nano-silicon nitride dispersion liquid, at room temperature reacted 36 hours ~ 84 hours, obtain suspension, wherein, the mass ratio of described tetraethoxysilane and described nano-silicon nitride is 10 ~ 200:5 ~ 100;
Described suspension is carried out the centrifugal thing that is precipitated, wash described sediment and drying and obtain nano silicon-nano silicon nitride composited material.
4. nano silicon according to claim 3-nano silicon nitride composited material preparation method is characterized in that, described dispersant is selected from least a in silane coupler KH-560 and the silane resin acceptor kh-550.
5. nano silicon according to claim 3-nano silicon nitride composited material preparation method is characterized in that, described solvent is selected from least a in ethanol, acetone and the butanone.
6. nano silicon according to claim 3-nano silicon nitride composited material preparation method, it is characterized in that, the described step that obtains the nano-silicon nitride dispersion liquid is specially under stirring and hyperacoustic effect, will dispersant and nano-silicon nitride add in the solvent and obtain mixture, drip the pH value in the described mixture and be 3.5 ~ 6 oxalic acid solution and obtain the nano-silicon nitride dispersion liquid.
7. nano silicon according to claim 3-nano silicon nitride composited material preparation method is characterized in that, stirs the step of described nano-silicon nitride dispersion liquid for stirring 5 minutes ~ 20 minutes under 500 rev/mins ~ 1300 rev/mins rotating speed.
8. nano silicon according to claim 3-nano silicon nitride composited material preparation method is characterized in that, the described solution that contains tetraethoxysilane is for to be dissolved in tetraethoxysilane in the ethanol, and ultrasonic being uniformly dispersed obtains.
9. nano silicon according to claim 3-nano silicon nitride composited material preparation method, it is characterized in that, the step of described washing is specially: under ul-trasonic irradiation, with described sediment with at least a washing the in ethanol, acetone or the butanone, then carry out centrifugal, repeat described washing and centrifugal each obtain pure sediment 5 times.
10. nano silicon according to claim 3-nano silicon nitride composited material preparation method, it is characterized in that, the step of described drying be specially in 80 ℃ lower dry 10 hours, then the heating rate with 10 ℃/min is warming up to 400 ℃, and is lower dry 10 hours at 400 ℃.
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| CN105068188A (en) * | 2015-09-17 | 2015-11-18 | 苏州鼎旺科技有限公司 | Optical fiber filter structure for optical communication |
| CN108129752A (en) * | 2018-01-23 | 2018-06-08 | 苏州聚康新材料科技有限公司 | The preparation method of suspension polymerisation nanometer silicon dioxide composite material |
| CN109749583A (en) * | 2019-01-29 | 2019-05-14 | 占军 | Anticorrosion abrasion-resistant coating material and preparation method thereof |
| CN109749583B (en) * | 2019-01-29 | 2021-09-28 | 浙江汇智实业股份有限公司 | Anti-corrosion wear-resistant coating material and preparation method thereof |
| CN115873559A (en) * | 2022-12-28 | 2023-03-31 | 河南创研新材料科技有限公司 | Silicon dioxide-silicon carbide gel composite microsphere and preparation method thereof |
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