CN1830775A - Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method - Google Patents
Method of preparing spherical nanometer SiO2 using powder quartz by chemical precipitation method Download PDFInfo
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Abstract
A process for preparing non-crystalline spherical SiO2 nanoparticles from quartz mineral by chemical deposition method features use of disperser (absolute alcohol or pholyethanel-6000), spherical catalyst (ammonia water) and precipitant (sulfuric acid). The product used as the filler of LSI package has high purity (99.996-99.999%) and 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 chemical precipitation law technology to prepare ball shaped nano SiO
2The processing method of material belongs to the mineral material field.The ball shaped nano SiO of the present invention's preparation
2Material 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)].
Ball shaped nano SiO
2Material 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.Along with the fast development in computer market, network information technology market, the CPU integrated level is increasing, and arithmetic speed is more and more faster, broadband large vol transmission network, and extensive, super large-scale integration market scale constantly enlarges ball shaped nano SiO
2Material 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.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, 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, and prolonged the work-ing life of mould greatly.[Zhang Jun, 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 the chemical precipitation law technology to prepare ball shaped nano SiO
2The patent application of the technology of material or bibliographical information.The objective of the invention is, provide that a kind of to adopt cheap natural high-quality powder quartz ore raw material be basic raw material, adopt the chemical precipitation method preparation to have the SiO of good characteristics such as sphere, nanometer
2The processing method of powder body material.
Three, summary of the invention
The present invention is a basic raw material with cheap natural high-quality konilite, adopts the chemical precipitation law technology, is that dispersion agent, ammoniacal liquor are that spherical catalyst and sulfuric acid are precipitation agent with dehydrated alcohol, polyoxyethylene glycol-6000, preparation electronic package material ball shaped nano SiO
2Material.
The present invention is basic raw material with the natural powdery quartz, adopts the chemical precipitation law technology to prepare ball shaped nano SiO
2The technology of material 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, the control glass melting temperature is 950 ± 5 ℃ and is incubated half an hour, prepares 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 water glass solution.
(4) by the preparation base fluid of ammonia volume 1.0～1.2mol/L, dehydrated alcohol consumption 10～20%, polyoxyethylene glycol-6000 consumption 0.8～1.2g/L.
(5) under temperature is 30～50 ℃ condition, will be set by step the concentration of (3) preparation be that 0.1～0.3mol/L water glass solution slowly is added drop-wise to set by step in the base fluid of (4) preparation, stirred formation water glass mixed system 10～20 minutes.
(6) control speed dropping sulfuric acid concentration is the sulphuric acid soln of 0.5～1.5mol/L in the water glass mixed system of (5) preparation set by step, drops to till 8～4 until the pH of precipitation solution value, stops to add acid, forms H
4SiO
4White precipitate.
(7) on the basis of step (6), insulation ageing 1～1.5 hour, filter dehydration, the distilled water wash precursor adds a spot of dehydrated alcohol and disperseed 1.5～2 hours in precursor.
(8) will be set by step the precursor of (7) preparation under 110～150 ℃ of conditions, dry the back and grinds, calcine also for 400～700 ℃ and be incubated 1～2 hour, the white powder of gained is ball shaped nano SiO
2
With above-mentioned steps, the product that makes is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope
2Phase, ball shaped nano SiO
2Particle diameter is 60nm～100nm, and particle distribution is even, the dispersity height, and the nodularization rate reaches more than 85～95%, does not produce crystallization in calcining below 700 ℃.
The ball shaped nano SiO of the present invention's preparation
2Material product be raw material with tetraethoxy or service water glass usually at present, adopt the ultra tiny SiO of chemical precipitation law technology preparation
2Compare, have following obvious advantage and unusual effect:
1. the preparation ball shaped nano SiO that adopts of the present invention
2The basic raw material of material is cheap, resourceful natural powdery quartz raw mineral materials.
2. the ball shaped nano SiO of the present invention preparation
2Material particle size is thin.Its particle diameter is 60nm～100nm, and particle distribution is even, the dispersity height, and agglomeration is not obvious.
3. the ball shaped nano SiO of the present invention preparation
2Impurities of materials content is low.Fe
2O
3Content only is 0.001～0.004wt%, impurity F e
3+Content is only for utilizing the ultra tiny SiO of tetraethoxy or service water glass preparation
2About 1/10.
4. the ball shaped nano SiO of the present invention preparation
2Material nodularization rate height.Its nodularization rate reaches 85～95%.
5. the ball shaped nano SiO of the present invention preparation
2The stability of material height.It does not produce crystallization in calcining below 700 ℃.
The ball shaped nano SiO of the present invention's preparation
2Material can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Four, embodiment
Following examples further specify the present invention, but do not limit the present invention.
Embodiment 1:
A kind of natural powdery quartz that utilizes of the present invention prepares ball shaped nano SiO
2Processing method, this processing method is a basic raw material with natural high-quality konilite, adopts the chemical precipitation law technology, prepares high ball shaped nano SiO
2Material.Its technological process is: utilize concentration for the hydrochloric acid of 1.0mol/L the natural powdery quartz removal of impurities to be handled, 1: 3 in molar ratio ratio uniform mixing of konilite after the removal of impurities and yellow soda ash is to carry out frit reaction under 950 ± 5 ℃ of conditions in temperature, the preparation sodium silicate solid.The sodium silicate solid that reacts completely is slowly cooled to room temperature and adds distilled water, under boiled condition, dissolve, filter then and obtain clarifying water glass solution.Be under 50 ℃ the condition in temperature, with concentration is that the 0.3mol/L water glass solution slowly is added drop-wise in the base fluid of preparing by the processing condition of ammonia volume 1.2mol/L, dehydrated alcohol consumption 20%, polyoxyethylene glycol-6000 consumption 1.0g/L, forms the water glass mixed system.Control speed dropping sulfuric acid concentration is the sulphuric acid soln of 1.2mol/L in the water glass mixed system, drops to till 8 until the pH of precipitation solution value, stops to add acid, forms H
4SiO
4White precipitate.Insulation ageing 1 hour, filter dehydration, the distilled water wash precursor adds a spot of dehydrated alcohol and disperseed 1.5 hours in precursor.Pulverize the oven dry back under 120 ℃ of conditions, and 700 ± 5 ℃ of calcinings also are incubated 1 hour, and the white powder of gained is ball shaped nano SiO
2
With above-mentioned steps, the ball shaped nano SiO that makes
2Material is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope
2Phase, ball shaped nano SiO
2Particle diameter is about 90nm, and particle distribution is even, the dispersity height, and the nodularization rate reaches more than 90%, does not produce crystallization in calcining below 700 ℃.
This ball shaped nano SiO
2Material can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Embodiment 2:
A kind of natural powdery quartz that utilizes of the present invention prepares ball shaped nano SiO
2Processing method, this processing method is a basic raw material with natural high-quality konilite, adopts the chemical precipitation law technology, prepares high ball shaped nano SiO
2Material.The raw material that it adopted, water glass solution preparation technology, dispersion agent, spherical catalyst and precipitation agent kind are similar to Example 1.But be under 45 ℃ the condition in temperature, with concentration is that the 0.1mol/L water glass solution slowly is added drop-wise in the base fluid of preparing by the processing condition of ammonia concn 1.0mol/L, dehydrated alcohol consumption 15%, polyoxyethylene glycol-6000 consumption 0.8g/L, forms the water glass mixed system.Control speed dropping concentration is the sulphuric acid soln of 0.5mol/L in the water glass mixed system, drops to till 6 until the pH of precipitation solution value, stops to add acid, forms H
4SiO
4White precipitate.Insulation ageing 1.5 hours, filter dehydration, the distilled water wash precursor adds a spot of dehydrated alcohol and disperseed 2 hours in precursor.Pulverize the oven dry back under 120 ℃ of conditions, and 700 ℃ of calcinings also are incubated 1.5 hours, and the white powder of gained is ball shaped nano SiO
2
With above-mentioned steps, the ball shaped nano SiO that makes
2Material is accredited as pure amorphous structure SiO through X-ray diffraction and scanning electronic microscope
2Phase, ball shaped nano SiO
2Particle diameter is about 70nm, and particle distribution is even, the dispersity height, and the nodularization rate reaches more than 90%, does not produce crystallization in calcining below 700 ℃.
This ball shaped nano SiO
2Material can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
Claims (5)
1. one kind is utilized konilite to prepare ball shaped nano SiO with chemical precipitation method
2Method, it is characterized in that this material is is basic raw material with cheap natural high-quality konilite mineral, adopt the chemical precipitation law technology to be prepared from.The ball shaped nano SiO of the present invention's preparation
2Material can be used as on a large scale, the high-quality filler of super large-scale integration encapsulation.
2 one kinds are utilized natural powdery quartz to be basic raw material, adopt the chemical precipitation law technology to prepare ball shaped nano SiO
2The method of material, 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, the control glass melting temperature is 950 ± 5 ℃ and is incubated half an hour, prepares 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 water glass solution.
(4) by the preparation base fluid of ammonia volume 1.0～1.2mol/L, dehydrated alcohol consumption 10～20%, polyoxyethylene glycol-6000 consumption 0.8～1.2g/L.
(5) under temperature is 30～50 ℃ condition, will be set by step the concentration of (3) preparation be that 0.1～0.3mol/L water glass solution slowly is added drop-wise to set by step in the base fluid of (4) preparation, stirred formation water glass mixed system 10～20 minutes.
(6) control speed dropping sulfuric acid concentration is the sulphuric acid soln of 0.5～1.5mol/L in the water glass mixed system of (5) preparation set by step, drops to till 8～4 until the pH of precipitation solution value, stops to add acid, forms H
4SiO
4White precipitate.
(7) on the basis of step (6), insulation ageing 1～1.5 hour, filter dehydration, the distilled water wash precursor adds a spot of dehydrated alcohol and disperseed 1.5～2 hours in precursor.
(8) will be set by step the precursor of (7) preparation under 110～150 ℃ of conditions, dry the back and grinds, calcine also for 400～700 ℃ and be incubated 1～2 hour, the white powder of gained is ball shaped nano SiO
2
3. ball shaped nano SiO according to claim 1
2The described ball shaped nano SiO of preparation methods and claim 2
2The preparation technology of material is characterized in that the particle diameter of this material is 60nm～100nm, and particle distribution is even, the dispersity height, and the nodularization rate reaches more than 85～95%.
4. ball shaped nano SiO according to claim 1
2The described ball shaped nano SiO of preparation methods and claim 2
2The preparation technology of material is characterized in that the foreign matter content of this material is low.Fe
2O
3Content only is 0.001～0.004wt%, impurity F e
3+Content only for utilize tetraethoxy or service water glass preparation nano silicon micronization about 1/10.
5. ball shaped nano SiO according to claim 1
2The described ball shaped nano SiO of preparation methods and claim 2
2The preparation technology of material is characterized in that prepared ball shaped nano SiO
2Material is non-crystalline state, and the thermostability height does not produce crystallization in calcining below 700 ℃.
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Cited By (8)
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| CN100413782C (en) * | 2007-02-13 | 2008-08-27 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN102618926A (en) * | 2011-01-31 | 2012-08-01 | 姜兴盛 | Traditional Chinese medicine for treating tonsillitis and pharyngitis |
| CN104058417A (en) * | 2014-07-04 | 2014-09-24 | 新沂功勋矿业有限公司 | Method for preparing monodisperse spherical nanosilicon dioxide through natural powder quartz |
| CN104475013A (en) * | 2014-12-18 | 2015-04-01 | 广西大学 | Preparation method of adsorbing agent for pressure swing adsorption purification of shale gas |
| CN106499145A (en) * | 2016-09-13 | 2017-03-15 | 内蒙古博大新型墙体材料研究所 | A kind of complex heat-preservation fire resisting energy-saving decorated sheet and preparation method thereof |
| CN106957059A (en) * | 2017-03-15 | 2017-07-18 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN110817933A (en) * | 2019-09-30 | 2020-02-21 | 成都理工大学 | Montmorillonite-loaded nano ZnO composite uvioresistant agent and preparation technology thereof |
| 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 |
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| CN1046921C (en) * | 1996-07-26 | 1999-12-01 | 中国科学院固体物理研究所 | Prepn. for controllable grain size non-crystal nm silicon dioxide |
| CN1186253C (en) * | 2003-08-12 | 2005-01-26 | 上海交通大学 | Prepn of mesoporous spherical nano Sio2 particle |
| CN1273381C (en) * | 2004-03-18 | 2006-09-06 | 武汉大学 | Method for preparing submicro and nano silicon dioxide in spherical shape |
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| CN100413782C (en) * | 2007-02-13 | 2008-08-27 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN102618926A (en) * | 2011-01-31 | 2012-08-01 | 姜兴盛 | Traditional Chinese medicine for treating tonsillitis and pharyngitis |
| CN102618926B (en) * | 2011-01-31 | 2015-04-15 | 姜兴茂 | Method for preparing spherical nanomonocrystalline particle |
| CN104058417A (en) * | 2014-07-04 | 2014-09-24 | 新沂功勋矿业有限公司 | Method for preparing monodisperse spherical nanosilicon dioxide through natural powder quartz |
| CN104475013A (en) * | 2014-12-18 | 2015-04-01 | 广西大学 | Preparation method of adsorbing agent for pressure swing adsorption purification of shale gas |
| CN106499145A (en) * | 2016-09-13 | 2017-03-15 | 内蒙古博大新型墙体材料研究所 | A kind of complex heat-preservation fire resisting energy-saving decorated sheet and preparation method thereof |
| CN106957059A (en) * | 2017-03-15 | 2017-07-18 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN106957059B (en) * | 2017-03-15 | 2019-03-19 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN110817933A (en) * | 2019-09-30 | 2020-02-21 | 成都理工大学 | Montmorillonite-loaded nano ZnO composite uvioresistant agent and preparation technology thereof |
| 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 |
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