CN1830774A - Method of preparing high purity spherical nanometer noncrystalline silicon micropowder using natural powder quartz - Google Patents
Method of preparing high purity spherical nanometer noncrystalline silicon micropowder using natural powder quartz Download PDFInfo
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- CN1830774A CN1830774A CN 200510021670 CN200510021670A CN1830774A CN 1830774 A CN1830774 A CN 1830774A CN 200510021670 CN200510021670 CN 200510021670 CN 200510021670 A CN200510021670 A CN 200510021670A CN 1830774 A CN1830774 A CN 1830774A
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- amorphous silicon
- purity spherical
- spherical nano
- nano amorphous
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Abstract
A process for preparing the high-purity spherical nanoparticles of non-crystalline Si from natural quartz powder by sol-gel technique features use of disperser and spherical catalyst. The product contains SiO2 (99.89-99.95 Wt%), and impurities including Al ions, Fe2O3, Na ions, Cl ions and SO4 ions, and has high stability.
Description
One, technical field
The present invention relates to adopt the natural high-quality konilite mineral with cheap is basic raw material, adopts the method for sol-gel technology preparing high-purity spherical nano amorphous silicon micro mist, belongs to the mineral material field.The high-purity spherical nano amorphous silicon micro mist of the present invention's preparation can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Two, technical background
Powder quartz ore is a kind of flint mineral deposit of natural output, a kind of novel silicon raw material that forms by microlitic quartzite weathering [Yu Zhiwei coats with lacquer little roc, Hu Xiaoping etc. western powder quartz ore development and use researchs [J]. and Chinese non-metallic mineral industry is led, 2002, (3)].China's powder quartz ore aboundresources, according to incompletely statistics, only ground powder quartz ore prospective reservess such as Jiangxi, Hunan and Guizhou just reach 1.5 hundred million tons of [Mu Guodong, Shi Nicheng, the horse Zhe is living etc. the reactive behavior research [J] of konilite under different curing conditions. and silicate circular, 2002, (1)].Konilite has a series of good physicochemical property, at many industrial circles wide application prospect is arranged.The konilite structural formula is SiO
2, be white in color, canescence or yellowish white, the general 2～10um of granularity, 50～75 ° of whiteness are neutral, and Mohs' hardness is 7, density 2.55～2.65g/cm
3, unit weight 1.96g/ml, pH are 6.3,1730 ℃ of refractoriness [Yu Zhiwei, Deng Huiyu. a kind of infant industry raw mineral materials-konilite [J]. Chinese non-metallic mineral industry periodical, 1999, (1)].Its chemical ingredients is slightly variant according to the place of production, general SiO
2All more than 98%, impurity has Fe to content
2O
3, Al
2O
3, CaO, MgO, K
2O, Na
2O, TiO
2Deng, do not contain Mn, Cu etc. and cause aging element and poisonous elements such as Pb, As, Hg, other micronutrient levels all is near or below detection limit, do not contain crystal water [Yu Zhiwei. the application [J] of konilite filler in the vulcanite goods. nonmetalliferous ore, 2001,24 (2)].
High-purity spherical nano amorphous silicon micro mist is as a kind of novel mineral material in short supply, because it has high-performances such as high dielectric, high heat-resisting, high moisture-proof, high filler loading capacity, low bulk, low-stress, low impurity, low-friction coefficient, is the high-quality functional stuffing of a kind of ideal electronics, electrical equipment, Chemicals.Fast development along with computer market, network information technology market, the CPU integrated level is increasing, arithmetic speed is more and more faster, broadband large vol transmission network, on a large scale, the super large-scale integration market scale constantly enlarges, the high-purity spherical nano silicon powder also demonstrates vast potential for future development as the packing material of unicircuit epoxy plastic cement thereupon.Now also more and more higher to the requirement of the packing material of unicircuit encapsulating compound, not only require high-purityly, ultra-fine, but also unicircuit encapsulating compound particles of packing material shape has been proposed the requirement of spheroidization.As the high-quality filler of electronic seal material, for the thermal expansivity that guarantees plastic cement is little, thermal conductivity is low, and near the thermal expansivity of silicon single crystal, this just requires the high purifying of silicon powder.Super-refinement, spheroidization mean that the silicon powder filling ratio increases, loading level can be up to 80～90%, and filling ratio is high more just more near the thermal expansivity of silicon single crystal, and the use properties of the electronic component of Sheng Chaning is also just good more thus, the plastic cement stress concentration minimum of making, intensity is the highest, and is little to the wearing and tearing of mould, makes to prolong [Zhang Jun greatly in work-ing life of mould, Song Shouzhi, Gai Guosheng. high pure and ultra-fine electron grade spherical silica powder research [J]. electronic component and material, 2004,23 (1)].
Prepare nanometer SiO at present
2Method mechanical shaping method, gas-phase decomposition method, arc process, chemical precipitation method and sol-gel method are arranged.The mechanical shaping method combines with grinding with pulverizing and realizes the super-refinement of material powder, suitably controls the condition of mechanical shaping method, can obtain ultrafine particle crystalloid SiO
2The gas-phase decomposition method is to be basic raw material with the silicon tetrachloride, adopts the hydrolysis under hydroxide sulphur high temperature of silicon tetrachloride gas to make the nanometer SiO of smoke-like
2Chemical precipitation method is identical with the raw material that sol-gel method adopts, and the basic raw material that adopts is tetraethoxy or service water glass usually.To be silicate obtain nanometer SiO loose, finely divided, that be precipitated out with flocculent structure by acidifying to chemical precipitation method
2Sol-gel method is to add acid basicity is reduced in silicon alkoxide, thereby bring out the polyreaction of silicate, the poly-attitude silicate ion particle diameter of the height that exists with the colloidal particle form in the system is constantly increased, form silicon sol, along with the further reduction of system pH, SiO
2The micelle cohesion forms the silicon gel, anhydrates and promptly gets nanometer SiO
2[Zhang Milin, fourth is founded a state, Jing Xiaoyan, etc. the preparation of nano silicon, modification and application [J]. chemical engineer, 2003,99 (6)].
In the technology of the present invention and the common document [Yin Mingzhi, Yao Xi, Wu Xiaoqing etc. sol-gel processing prepares nano silicon dioxide sol and porous silica film [J]. silicate journal, 2002, (6) 30; Zhang Milin, fourth is founded a state, Jing Xiaoyan, etc. the preparation of nano silicon, modification and application [J]. chemical engineer, 2003,99 (6); Zheng Dianmo, Su Xuejun. chemical precipitation method prepares nanometer SiO
2Research. University Of Nanchang's journal, 2003,25 (6); Li Maoqiong, Xiang Jinzhong, Hu Yongmao etc. nanometer SiO
2Preparation and performance study. Yunnan University's journal (natural science edition), 2002,24 (6)] in said preparation nanometer SiO
2So the key distinction be basic raw material with the natural powdery quartz, rather than be basic raw material with tetraethoxy or service water glass.By retrieval, do not find to utilize natural powdery quartz to be basic raw material, adopt colloidal sol-gel technique to prepare the patent application or the bibliographical information of the method for high-purity spherical nano amorphous silicon micro mist.The objective of the invention is, a kind of processing method that adopts the silicon powder material of good characteristics such as cheap natural high-quality powder quartz ore raw material to be that basic raw material preparation has high-purity, spherical, ultra-fine, non-crystalline state is provided.
Three, summary of the invention
The present invention is a basic raw material with natural high-quality konilite, adopts colloidal sol-gel technique, is dispersion agent with dehydrated alcohol and polyoxyethylene glycol-6000, and ammoniacal liquor is spherical catalyst, preparation electronic package material high-purity spherical nano amorphous silicon micro mist.
The present invention is basic raw material with the natural powdery quartz, adopts colloidal sol-gel technique to prepare the preparation method of high-purity spherical nano amorphous silicon micropowder material, and following processing step is arranged:
(1) natural powdery quartz being carried out removal of impurities handles.Get a certain amount of konilite, add the hydrochloric acid of 0.8～1.2mol/L, konilite is immersed in the acid fully, stirred 10～20 minutes, add distilled water wash, be washed till and use AgNO
3Detection does not have chlorion, after the filtration filter cake is dried.
(2) will be set by step konilite raw material and the ratio uniform mixing of yellow soda ash 1: 3 in molar ratio～3.5 of (1) preparation, put and carry out frit reaction in the smelting furnace, control glass melting temperature and be 950 ± 5 ℃ and be incubated half an hour, obtain sodium silicate solid.
(3) will slowly cool to room temperature and add distilled water through the sodium silicate solid that step (2) high-temperature fusion reacts completely, under boiled condition, dissolve, filter and obtain clarifying sodium silicate solution.
(4) prepare base fluid by ammonia volume 1.0～2.0mol/L, dehydrated alcohol consumption 10～20%, polyoxyethylene glycol-6000 consumption 0.3～1.0g/L, keep base fluid pH value in 10.6～11.2 scopes.
(5) with concentration be the sulphuric acid soln of 1.6～2.0mol/L and set by step (3) preparation concentration be 1.1～1.7g/L sodium silicate solution slowly be added drop-wise to set by step together (4) preparation base fluid in, and the rate of titration of regulating sulfuric acid and water glass, make the pH value maintain 8～10 scopes, powerful simultaneously the stirring.
(6) set by step reacted 20～30 minutes after sodium silicate solution drips (5), drips sulfuric acid fast, makes the pH value of system be reduced to 4～6 fast, and reduce stirring velocity, progressively forms silicon gel particles suspension.
(7) the silicon gel particles suspension ageing that step (6) is prepared is 2～3 hours.
(8) the silicon gel that step (7) is prepared is washed with distilled water to BaCl
2Detection does not have sulfate radical, and suction filtration becomes filter cake, adds a spot of dehydrated alcohol as dispersion agent in filter cake, mixes 100～110 ℃ of oven dry.
(9) sample with step (8) preparation grinds, and places smelting furnace, is heated to 600 ± 5 ℃ and be incubated 30 minutes, and the white powder of gained is a high-purity spherical nano amorphous silicon micro mist.
With above-mentioned steps, the product that makes is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope and transmission electron microscope
2Phase, the silicon powder material particle size is 50nm～100nm, particle distribution is even, the dispersity height, the nodularization rate reaches 85～95%, is not producing crystallization after the calcining below 1000 ℃.Chemical ingredients is: 99.89～99.95wt%SiO
20.008～0.012wt%Al
3+0.001～0.004wt%Fe
2O
32.0～4.0ppm Na
+≤ 1ppm Cl
-≤ 1ppm SO
4 2-
The high-purity spherical nano silicon powder goods of the present invention preparation be raw material with tetraethoxy or service water glass usually at present, adopt the nano silicon micronization of colloidal sol-gel technique preparation to compare, have following obvious advantage and unusual effect:
1. the basic raw material of the preparation high-purity spherical nano amorphous silicon micropowder material of the present invention's employing is cheap natural high-quality powder quartz ore raw material.
2. the high-purity spherical nano amorphous silicon micro mist purity height of the present invention preparation.SiO
2Weight percent reaches 99.89～99.95%.Foreign matter content is: 0.008～0.012wt%Al
3+0.001～0.004wt%Fe
2O
32.0～4.0ppm Na
+≤ 1ppm Cl
-≤ 1ppm SO
4 2-Impurity F e
3+Content only for utilize tetraethoxy or service water glass preparation nano silicon micronization 1/10.
3. the high-purity spherical nano amorphous silicon micro mist fine size of the present invention preparation.Its particle diameter is 50nm～100nm, and particle distribution is even, the dispersity height, and agglomeration is not obvious.
4. the high-purity spherical nano amorphous silicon micro mist sphere of powder rate height of the present invention preparation.Its nodularization rate reaches 85～95%.
5. the high-purity spherical nano amorphous silicon micro mist stability of the present invention's preparation is high, does not produce crystallization in calcining below 1000 ℃.
Four, embodiment
Following examples further specify the present invention, but do not limit the present invention.
Embodiment 1:
The present invention is a kind of method of utilizing natural powdery quartz to prepare high-purity spherical nano amorphous silicon micro mist, and this method is to be basic raw material with natural high-quality konilite, adopts colloidal sol-gel technique, preparation high-purity spherical nano amorphous silicon micro mist.Its technological process is: utilize concentration to handle for the hydrochloric acid of 1.2mol/L carries out removal of impurities to natural powdery quartz, 1: 3.5 in molar ratio ratio uniform mixing of konilite after the removal of impurities and yellow soda ash, put and carry out frit reaction in the smelting furnace, the control glass melting temperature is 950 ± 5 ℃ and is incubated half an hour, the preparation sodium silicate solid.Sodium silicate solid is slowly cooled to room temperature and adds distilled water, under boiled condition, dissolve, filter then and obtain clarifying sodium silicate solution.With concentration is that the sulphuric acid soln of 1.8mol/L and concentration are that slowly to be added drop-wise to pH value by ammonia volume 1.0mol/L, dehydrated alcohol consumption 20%, polyoxyethylene glycol-6000 consumption 1.0g/L preparation together be in 11 the base fluid to the 1.7g/L sodium silicate solution, and the rate of titration of regulating sulfuric acid and water glass, make the pH value reduce to 9, the powerful stirring when dripping.After sodium silicate solution drips, reacted 25 minutes, drip sulfuric acid fast, make the pH value of system be reduced to 6 fast, and reduce stirring velocity, make the ageing of silicon gel particles suspension after 2.5 hours, washing is to using BaCl
2Detection does not have sulfate radical, and suction filtration becomes filter cake, adds a spot of dehydrated alcohol as dispersion agent in filter cake, and oven dry grinds then, places smelting furnace to be heated to 600 ± 5 ℃ and be incubated 30 minutes, and the white powder of gained is the high-purity spherical nano silicon powder.
With above-mentioned steps, the product that makes is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope and transmission electron microscope
2Phase, the silicon powder material particle size is 50nm～90nm, particle distribution is even, the dispersity height, the nodularization rate reaches more than 90%, does not produce crystallization in calcining below 1000 ℃.Its SiO
2Weight percent reaches 99.89wt%, and foreign matter content is: 0.009wt%Al
3+0.001wt%Fe
2O
33.5ppm Na
+≤ 1ppm Cl
-≤ 1ppm SO
4 2-
This high-purity spherical nano amorphous silicon micro mist can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Embodiment 2:
The present invention is a kind of method of utilizing natural powdery quartz to prepare high-purity spherical nano amorphous silicon micro mist, and this method is to be basic raw material with natural high-quality konilite, adopts colloidal sol-gel technique, preparation high-purity spherical nano amorphous silicon micro mist.The raw material that it adopted, sodium silicate solution preparation technology, dispersion agent, spherical catalyst kind are similar to Example 1.But with concentration is that the sulphuric acid soln of 1.6mol/L and concentration are that slowly to be added drop-wise to pH value by ammonia volume 1.8mol/L, dehydrated alcohol consumption 18%, polyoxyethylene glycol-6000 consumption 0.3g/L preparation together be in 10.8 the base fluid to the 1.4g/L sodium silicate solution, and the rate of titration of regulating sulfuric acid and water glass, make the pH value reduce to 8.5, the stirring of brute force when dripping.After sodium silicate solution drips, reacted 20 minutes, drip sulfuric acid fast, make the pH value of system be reduced to 5.5 fast, and reduce stirring velocity, make the ageing of silicon gel particles suspension after 2 hours, the washing suction filtration becomes filter cake, adds a spot of dehydrated alcohol as dispersion agent in filter cake, and oven dry grinds then, place smelting furnace to be heated to 600 ± 5 ℃ and be incubated 30 minutes, the white powder of gained is the high-purity spherical nano silicon powder.
With above-mentioned steps, the product that makes is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope and transmission electron microscope
2Phase, the silicon powder material particle size is 60nm～80nm, particle distribution is even, the dispersity height, the nodularization rate reaches more than 90%, does not produce crystallization in calcining below 1000 ℃.Its SiO
2Weight percent reaches 99.90wt%, and foreign matter content is: 0.011wt%Al
3+0.002wt%Fe
2O
33.2ppm Na
+≤ 1ppm Cl
-≤ 1ppm SO
4 2-
This high-purity spherical nano amorphous silicon micro mist can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Claims (7)
1. one kind is basic raw material with cheap natural high-quality konilite mineral, adopt colloidal sol-gel technique to prepare the method for high-purity spherical nano amorphous silicon micro mist, the high-purity spherical nano amorphous silicon micro mist of preparation can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
2 one kinds of methods of utilizing cheap natural high-quality konilite mineral to prepare high-purity spherical nano amorphous silicon micro mist, its feature has following processing step:
(1) natural powdery quartz being carried out removal of impurities handles.Get a certain amount of konilite, add the hydrochloric acid of 0.8～1.2mol/L, konilite is immersed in the acid fully, stirred 10～20 minutes, add distilled water wash, be washed till and use AgNO
3Detection does not have chlorion, after the filtration filter cake is dried.
(2) will be set by step konilite raw material and the ratio uniform mixing of yellow soda ash 1: 3 in molar ratio～3.5 of (1) preparation, put and carry out frit reaction in the smelting furnace, control glass melting temperature and be 950 ± 5 ℃ and be incubated half an hour, obtain sodium silicate solid.
(3) will slowly cool to room temperature and add distilled water through the sodium silicate solid that step (2) high-temperature fusion reacts completely, under boiled condition, dissolve, filter and obtain clarifying sodium silicate solution.
(4) prepare base fluid by ammonia volume 1.0～2.0mol/L, dehydrated alcohol consumption 10～20%, polyoxyethylene glycol-6000 consumption 0.3～1.0g/L, keep base fluid pH value in 10.6～11.2 scopes.
(5) with concentration be the sulphuric acid soln of 1.6～2.0mol/L and set by step (3) preparation concentration be 1.1～1.7g/L sodium silicate solution slowly be added drop-wise to set by step together (4) preparation base fluid in, and the rate of titration of regulating sulfuric acid and water glass, make the pH value maintain 8～10 scopes, powerful simultaneously the stirring.
(6) set by step reacted 20～30 minutes after sodium silicate solution drips (5), drips sulfuric acid fast, makes the pH value of system be reduced to 4～6 fast, and reduce stirring velocity, progressively forms silicon gel particles suspension.
(7) the silicon gel particles suspension ageing that step (6) is prepared is 2～3 hours.
(8) the silicon gel that step (7) is prepared is washed with distilled water to BaCl
2Detection does not have sulfate radical, and suction filtration becomes filter cake, adds a spot of dehydrated alcohol as dispersion agent in filter cake, mixes 100～110 ℃ of oven dry.
(9) sample with step (8) preparation grinds, and places smelting furnace, is heated to 600 ± 5 ℃ and be incubated 30 minutes, and the white powder of gained is a high-purity spherical nano amorphous silicon micro mist.
3. the preparation technology of claim 1 described high-purity spherical nano amorphous silicon micropowder preparing process and the described high-purity spherical nano amorphous silicon of claim 2 micro mist is characterized in that this material is that employing is a basic raw material with cheap natural high-quality konilite mineral.
4. the preparation technology of claim 1 described high-purity spherical nano amorphous silicon micropowder preparing process and the described high-purity spherical nano amorphous silicon of claim 2 micro mist is characterized in that the SiO of this material
2Weight percent reaches 99.89～99.95%.
5. the preparation technology of claim 1 described high-purity spherical nano amorphous silicon micropowder preparing process and the described high-purity spherical nano amorphous silicon of claim 2 micro mist is characterized in that this material has 0.008～0.012wt%Al
3+0.001～0.004wt%Fe
2O
32.0～4.0ppm Na
+≤ 1ppm Cl
-≤ 1ppm SO
4 2-Low impurity content.
6. the preparation technology of high-purity spherical nano amorphous silicon micropowder preparing process according to claim 1 and the described high-purity spherical nano amorphous silicon of claim 2 micro mist, the particle diameter that it is characterized in that this material is 50nm～100nm, particle distribution is even, dispersity height, nodularization rate are 85～95%.
7. the preparation technology of high-purity spherical nano amorphous silicon micropowder preparing process according to claim 1 and the described high-purity spherical nano amorphous silicon of claim 2 micro mist, it is characterized in that this material is non-crystalline state, the thermostability height does not produce crystallization in calcining below 1000 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008098470A1 (en) * | 2007-02-13 | 2008-08-21 | Maohao Yuan | A method for preparing high purity and ultrafine spherical silica micropowder |
| CN102659124A (en) * | 2012-04-12 | 2012-09-12 | 南昌大学 | Method for preparing nanometer silicon powder by sol-microemulsion-hydro-thermal system |
| CN103043668A (en) * | 2011-10-13 | 2013-04-17 | 沈阳黎明航空发动机(集团)有限责任公司 | Preparation method of core additive |
| CN111747422A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN114436267A (en) * | 2022-02-14 | 2022-05-06 | 连云港淼晶硅材料有限公司 | Preparation method of high-purity superfine silicon powder |
-
2005
- 2005-09-15 CN CN 200510021670 patent/CN1830774A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008098470A1 (en) * | 2007-02-13 | 2008-08-21 | Maohao Yuan | A method for preparing high purity and ultrafine spherical silica micropowder |
| CN100413782C (en) * | 2007-02-13 | 2008-08-27 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN103043668A (en) * | 2011-10-13 | 2013-04-17 | 沈阳黎明航空发动机(集团)有限责任公司 | Preparation method of core additive |
| CN103043668B (en) * | 2011-10-13 | 2014-11-19 | 沈阳黎明航空发动机(集团)有限责任公司 | Preparation method of core additive |
| CN102659124A (en) * | 2012-04-12 | 2012-09-12 | 南昌大学 | Method for preparing nanometer silicon powder by sol-microemulsion-hydro-thermal system |
| CN111747422A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN111747422B (en) * | 2020-06-22 | 2023-07-28 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN114436267A (en) * | 2022-02-14 | 2022-05-06 | 连云港淼晶硅材料有限公司 | Preparation method of high-purity superfine silicon powder |
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