CN107032358A - A kind of method that silica particles coat alundum (Al2O3) - Google Patents
A kind of method that silica particles coat alundum (Al2O3) Download PDFInfo
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- CN107032358A CN107032358A CN201710223466.1A CN201710223466A CN107032358A CN 107032358 A CN107032358 A CN 107032358A CN 201710223466 A CN201710223466 A CN 201710223466A CN 107032358 A CN107032358 A CN 107032358A
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- CN
- China
- Prior art keywords
- al2o3
- alundum
- silica particles
- coat
- powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
Abstract
The invention discloses a kind of method that silica particles coat alundum (Al2O3), using wet chemistry method in ethylenediamine tetra-acetic acid and dibutyl amine solution, under heating and stirring condition, add tert-butoxy aluminium, the organic ion solution containing aluminium element is obtained, then SiO 2 powder is added in the organic ion solution, heating stirring is dried to obtain gel, gel is put into Muffle kiln roasting afterwards, you can coat one layer of alundum (Al2O3) layer in silica particles.Composite of the present invention is in granular form, and particle size is determined by the granular size of Primary silica, and alundum (Al2O3) coating thickness can be adjusted according to demand.The alundum (Al2O3) coated silica composite of the present invention is especially suitable for preparing the silicon dioxide structure material of high tridymite phase and high cristobalite phase content, and preparation is simple, process is easy to control, is especially suitable for large-scale production.
Description
Technical field
The present invention relates to composite, more particularly to a kind of side that alundum (Al2O3) is coated in silica particles
Method.
Background technology
Silica is also known as silica, chemical formula SiO2, there is two kinds of amorphous silica and crystalline silica to there is shape
Formula.The representative of amorphous silica is glass.Crystalline silica is different because of crystal structure, is divided into quartz, tridymite and side
Three kinds of quartz.
Pure quartz is clear crystal, and the quartz of big and transparent prism-shaped is crystal.If the crystal containing trace impurity is carried
Different colours, there is amethyst, yellow quartz etc..Common sand is tiny quartz crystal, has yellow ground (more iron tramp) and white
Sand (impurity is few, purer).
Tridymite (Tridymite) is SiO2Stable phase between 870~1470 DEG C.It is changed into ashlar when temperature is higher
English；It is changed into quartz during lower temperature, but it is very slow (transformation of reconstruction formula).There is alkali metal oxide (such as Al2O3) or halogenation
Transformation can be accelerated in the presence of the mineralizers such as thing.
Cristobalite (Cristobalite) is SiO2In 1500 DEG C or so of stable phase, cristobalite include low temperature cristobalite and
High temperature cristobalite.High temperature cristobalite generally there are in acidic lava, and low temperature cristobalite is in white or milky, glassy lustre.Ashlar
English phase SiO2Good thermal shock, be the important materials of heat shock resistance refractory ceramics mould.
Preparing the crystalline silica (SiO of various different crystal structures2) when, it is necessary to by alundum (Al2O3) (Al2O3)
It is used as sintering adjuvant.Traditional handicraft directly mixes the powder particle of silica and alundum (Al2O3), two kinds of powder particles
Between contact it is uneven, silica into mutually more difficult.
The content of the invention
The purpose of the present invention is exactly to provide one kind in silica to overcome deficiencies of the prior art
The method of grain Surface coating alundum (Al2O3).
The present invention is achieved by the following technical solutions：
A kind of method that silica particles coat alundum (Al2O3), comprises the following steps：
(1) ethylenediamine tetra-acetic acid is dissolved in solvent, heats and keeping temperature is 70-120 DEG C, in dropwise addition under stirring
Dibutyl amine simultaneously continues stirring 3-8 hours, adds tert-butoxy aluminium and continues stirring 3-8 hours, fully obtains having containing aluminium after reaction
Machine solion, wherein the ratio of the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy aluminium is 1:0.5~2:0.5~2；
(2) SiO 2 powder is added in the solution of organic ion containing aluminium, in stirring at 70-120 DEG C until volatilization
Drying forms gel, and gel is transferred in Muffle furnace and is calcined 4-10 hours at 500-700 DEG C, obtains alundum (Al2O3) cladding
SiO 2 powder.
Optionally, the particle diameter of the SiO 2 powder is 20 μm -100 μm.
Optionally, the mass ratio of the SiO 2 powder and the organic ion containing aluminium solution is 1:1.5-1:9.
Optionally, the alundum (Al2O3) is in forming clad, the thickness of the clad outside the SiO 2 powder
For 100nm-500nm.
Optionally, the solvent is absolute ethyl alcohol.
Optionally, in step (1), the ratio of the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy aluminium is 1:1:1.
Optionally, in step (1), the reaction temperature is 90-100 DEG C.
Optionally, in step (2), the sintering temperature is 550-650 DEG C, and the time is 5-8 hours.
The present invention is to be based on following reaction：
Wherein, ethylenediamine tetra-acetic acid (EDTA) is trilon；EDTA is a polyacid, in the solution with H4Y,
The forms such as H3Y-, HY3-, Y4- are present, and wherein Y4- can directly coordinate the stable complex of generation with many kinds of metal ions, coordinate
Than for 1：1, cooperatively form solion with aluminium ion.Tert-butoxy aluminium (Aluminum tert-butoxide) is used as Al sources,
Aluminium ion is provided.Dibutyl amine (Dibutylamine) is used to suppress ionic crystal.By above-mentioned reaction, the complex for forming aluminium is molten
Liquid, adds after silica dioxide granule and dries and be calcined, you can the SiO 2 powder with alundum (Al2O3) clad is made,
Particle size is determined that its coating thickness can be adjusted according to demand by Primary silica granular size.
The preparation method of the present invention is simple and easy to apply, mild condition, and controllability is strong, is especially suitable for large-scale industrial production.System
The alundum (Al2O3) coated silica composite obtained can improve the contact area between two kinds of materials, and it is mutually difficult to reduce into
Degree, is especially suitable for preparing the silicon dioxide structure material of high tridymite phase and high cristobalite phase content.
Brief description of the drawings
Fig. 1 is the structural representation of the SiO 2 powder for the alundum (Al2O3) cladding that the present invention is prepared.
Embodiment
The present invention is described in further detail with reference to embodiment and accompanying drawing, but the present invention is not limited thereto.
Embodiment 1
2.21g ethylenediamine tetra-acetic acids are dissolved in 20g absolute ethyl alcohols, in heating on heating stirrer, simultaneously keeping temperature is
100 DEG C, in 1.18g dibutyl amine is added dropwise under stirring and continues to stir 4 hours, said temperature is kept, the tertiary fourths of 1.87g are added
Epoxide aluminium simultaneously continues to stir 4 hours, fully obtains the solution of organic ion containing aluminium after reaction.By the silica that particle diameter is 50 μm
Powder is added in the solution of organic ion containing aluminium, and stirring, will up to volatile dry formation honey shape gel at a temperature of 100 DEG C
Gel, which is transferred in crucible, to be used in Muffle furnace in 5 hours of 600 DEG C of roasting temperatures, obtained the titanium dioxide of alundum (Al2O3) cladding
Si powder.
The structure of the SiO 2 powder of obtained alundum (Al2O3) cladding is as shown in figure 1, wherein alundum (Al2O3) is coated
Layer 2 is coated on the surface of silica dioxide granule 1, and the thickness of alundum (Al2O3) clad 2 is 100nm.
Embodiment 2
4.42g ethylenediamine tetra-acetic acids are dissolved in 20g absolute ethyl alcohols, in heating on heating stirrer, simultaneously keeping temperature is
100 DEG C, in 2.36g dibutyl amine is added dropwise under stirring and continues to stir 4 hours, said temperature is kept, the tertiary fourths of 3.74g are added
Epoxide aluminium simultaneously continues to stir 4 hours, fully obtains the solution of organic ion containing aluminium after reaction.By the silica that particle diameter is 50 μm
Powder is added in the solution of organic ion containing aluminium, and stirring, will up to volatile dry formation honey shape gel at a temperature of 100 DEG C
Gel, which is transferred in crucible, to be used in Muffle furnace in 5 hours of 600 DEG C of roasting temperatures, obtained the titanium dioxide of alundum (Al2O3) cladding
Si powder.
The structure of the SiO 2 powder of obtained alundum (Al2O3) cladding is as shown in figure 1, wherein alundum (Al2O3) is coated
Layer 2 is coated on the surface of silica dioxide granule 1, and the thickness of alundum (Al2O3) clad is 200nm.
Those of ordinary skill in the art understand, when design parameter of the invention changes in following ranges, remain to access
Technique effect same as the previously described embodiments or close：
A kind of method that silica particles coat alundum (Al2O3), comprises the following steps：
(1) ethylenediamine tetra-acetic acid is dissolved in solvent, heats and keeping temperature is 70-120 DEG C, in dropwise addition under stirring
Dibutyl amine simultaneously continues stirring 3-8 hours, adds tert-butoxy aluminium and continues stirring 3-8 hours, fully obtains having containing aluminium after reaction
Machine solion, wherein the ratio of the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy aluminium is 1:0.5~2:0.5~2；It is excellent
Choosing, the solvent is absolute ethyl alcohol, and reaction temperature is 90-100 DEG C, the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy
The ratio of aluminium is 1:1:1；
(2) SiO 2 powder is added in the solution of organic ion containing aluminium, in stirring at 70-120 DEG C until volatilization
Drying forms gel, and gel is transferred in Muffle furnace and is calcined 4-10 hours at 500-700 DEG C, obtains alundum (Al2O3) cladding
SiO 2 powder；It is preferred that, the particle diameter of the SiO 2 powder is 20 μm -100 μm, the SiO 2 powder and institute
The mass ratio for stating the solution of organic ion containing aluminium is 1:1.5-1:9, the sintering temperature is 550-650 DEG C, and the time is 5-8 hours.
The alundum (Al2O3) is in forming clad outside the SiO 2 powder, the thickness of the clad is 100nm-500nm.
Above-described embodiment is only used for further illustrating a kind of silica particles cladding alundum (Al2O3) of the present invention
Method, but the invention is not limited in embodiment, what every technical spirit according to the present invention was made to above example appoints
What simple modification, equivalent variations and modification, each falls within the protection domain of technical solution of the present invention.
Claims (8)
1. a kind of method that silica particles coat alundum (Al2O3), it is characterised in that comprise the following steps：
(1) ethylenediamine tetra-acetic acid is dissolved in solvent, heats and keeping temperature is 70-120 DEG C, in two fourths are added dropwise under stirring
Amine simultaneously continue stirring 3-8 hour, add tert-butoxy aluminium simultaneously continue stirring 3-8 hour, fully react after obtain contain aluminium it is organic from
Sub- solution, wherein the ratio of the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy aluminium is 1:0.5~2:0.5~2；
(2) SiO 2 powder is added in the solution of organic ion containing aluminium, in stirring at 70-120 DEG C until volatile dry
Gel is formed, gel is transferred in Muffle furnace and is calcined 4-10 hours at 500-700 DEG C, the two of alundum (Al2O3) cladding are obtained
Silicon oxide powder.
2. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：It is described
The particle diameter of SiO 2 powder is 20 μm -100 μm.
3. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：It is described
The mass ratio of SiO 2 powder and the organic ion containing aluminium solution is 1:1.5-1:9.
4. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：It is described
Alundum (Al2O3) is in forming clad outside the SiO 2 powder, the thickness of the clad is 100nm-500nm.
5. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：It is described
Solvent is absolute ethyl alcohol.
6. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：Step
(1) in, the ratio of the ethylenediamine tetra-acetic acid, dibutyl amine and tert-butoxy aluminium is 1:1:1.
7. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：Step
(1) in, the reaction temperature is 90-100 DEG C.
8. the method that silica particles according to claim 1 coat alundum (Al2O3), it is characterised in that：Step
(2) in, the sintering temperature is 550-650 DEG C, and the time is 5-8 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219362A (en) * | 2018-02-07 | 2018-06-29 | 廊坊暖康管业有限公司 | Nano-silicon composite insulation boards |
| CN108314873A (en) * | 2018-02-07 | 2018-07-24 | 廊坊暖康管业有限公司 | Nano-silicon polymerize thermal insulation board |
| CN108862292A (en) * | 2018-09-10 | 2018-11-23 | 江西师范大学 | A method of regulation silicon dioxide microsphere partial size |
| CN111768891A (en) * | 2020-07-09 | 2020-10-13 | 江苏国瓷泓源光电科技有限公司 | Aluminum paste for PERC solar cell |
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| CN1547553A (en) * | 2000-11-21 | 2004-11-17 | ���ʿ����о�����˾ | A new aluminum trihydroxide phase and catalysts made therefrom |
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| CN1812007A (en) * | 2006-01-18 | 2006-08-02 | 南京大学 | High-stability Fc/Al203 composite nano particles with nuclear/shell structure and producing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108219362A (en) * | 2018-02-07 | 2018-06-29 | 廊坊暖康管业有限公司 | Nano-silicon composite insulation boards |
| CN108314873A (en) * | 2018-02-07 | 2018-07-24 | 廊坊暖康管业有限公司 | Nano-silicon polymerize thermal insulation board |
| CN108862292A (en) * | 2018-09-10 | 2018-11-23 | 江西师范大学 | A method of regulation silicon dioxide microsphere partial size |
| CN111768891A (en) * | 2020-07-09 | 2020-10-13 | 江苏国瓷泓源光电科技有限公司 | Aluminum paste for PERC solar cell |
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Application publication date: 20170811 |