CN100496681C - External direct current field self-assembly manufactured adjustable equal dimension triangular hole inorganic films - Google Patents
External direct current field self-assembly manufactured adjustable equal dimension triangular hole inorganic films Download PDFInfo
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- CN100496681C CN100496681C CNB2003101065804A CN200310106580A CN100496681C CN 100496681 C CN100496681 C CN 100496681C CN B2003101065804 A CNB2003101065804 A CN B2003101065804A CN 200310106580 A CN200310106580 A CN 200310106580A CN 100496681 C CN100496681 C CN 100496681C
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- China
- Prior art keywords
- direct current
- delthyrium
- preparation
- electric field
- microballoon
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- 238000001338 self-assembly Methods 0.000 title claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- 239000004005 microsphere Substances 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 230000000694 effects Effects 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 5
- 230000005684 electric field Effects 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 230000000737 periodic effect Effects 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 15
- 230000005611 electricity Effects 0.000 abstract 4
- 239000003292 glue Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 17
- 239000011521 glass Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011806 microball Substances 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention is a manufacturing method for self assembly of electricity field control glue particle and triangle hole inorganic film: it adjusts the pH value of the silicon dioxide equal-radius micro-sphere suspension to 4-12, the invention adds a direct current outer electricity field to the micro-sphere suspension, the electricity density is 0.1-1000V/cm, makes the charge deposited at the board through the effect of the outer electricity field, thus forms the template. The efficiency of the invention is high, and the quality of the product is high.
Description
One, technical field
The present invention relates to a kind ofly prepare inoranic membrane by applying the self assembly of direct current external electric field, especially by applying the method that the direct current external electric field is controlled the colloidal particle self assembly and prepared adjustable delthyrium inoranic membrane, promptly the isometrical microballoon of silica is carried out self assembly by applying the direct current external electric field, prepare the inoranic membrane of adjustable delthyrium size.
Two, background technology
To the research of adjustable port size inoranic membrane, not only have important scientific research value, and have important practical value.Adjustable delthyrium inoranic membrane is not only in fields such as film separation, catalysis, and has extremely wide application prospect equally in photoelectron (photonic crystal) field.
To preparation of inorganic, prior art is sneaked into combustibility usually or discharged gas at high temperature in matrix material (as aluminium oxide etc.) pore former material (as carbon dust, calcium carbonate) etc. is prepared required shape by the technology for preparing pottery, and then passes through sintered specimen.In sintering process, pore former volatilizees by burning or decomposes, and at the inner porous channel that forms of sample, finally prepares inorganic porous membrane.
Yet this method has significant limitation, and it is adjustable that prepared inoranic membrane is difficult to obtain the aperture size homogeneous.
Three, summary of the invention
The present invention is by applying the method for direct current external electric field, and the microballoon self assembly that relies on the effect of electric field force will have certain specific charge goes out adjustable delthyrium inoranic membrane.One of advantage of this method is the microballoon very little to particle diameter, also available this method preparation.This is because if microspherulite diameter is less, when the active force of itself equates with the active force of Brownian movement in the suspension, can by improve the voltage of direct current external electric field that applies or shorten two distance between electrodes, thereby raising electric-field intensity, make the electric field force that acts on the microballoon active force greater than the microballoon Brownian movement, thereby might make the orientated deposition under the effect of electric field force of the little microballoon of particle diameter, form the delthyrium inoranic membrane of quality three-dimensional periodic arrangement preferably long range ordered structure.
The objective of the invention is: the effect of direct current external electric field that utilization adds makes the silicon dioxide microsphere that has negative electrical charge be self-assembled into the equidimension delthyrium inoranic membrane of periodic arrangement on flat boards such as dull and stereotyped electro-conductive glass.The size of inoranic membrane delthyrium can accurately be controlled by the diameter of regulating colloid micro ball.Sedimentation time is shorter, has higher efficient, guarantees to prepare high-quality periodic arrangement equidimension delthyrium inoranic membrane.
The object of the present invention is achieved like this: the present invention adopts a kind of simple and feasible method, at first the isometrical microsphere suspension liquid of the silica of preparation is regulated pH value 4-12, then by in microsphere suspension liquid, applying the direct current external electric field, electric-field intensity is 0.1-1000V/cm, make with the microballoon of certain specific charge outside under the effect of electric field, orientated deposition on flat boards such as dull and stereotyped electro-conductive glass, thereby the equidimension delthyrium inoranic membrane of formation periodic arrangement.
It is the 8-10 scope that the isometrical microsphere suspension liquid of silica of preparation is regulated pH value, makes that the Zeta-potential of microballoon reaches less and even minimum of a value in the suspension, carries out applied voltage again and deposits.
Characteristics of the present invention are: from the silicon dioxide microsphere the suspension being applied the effect of direct current external electric field, can prepare equidimension delthyrium inoranic membrane.The sedimentation time of the inventive method is short, efficient height, the equidimension delthyrium inoranic membrane quality height of preparation.
The invention will be further described below in conjunction with accompanying drawing and by embodiment;
The apparatus structure schematic diagram of Fig. 1 the inventive method is promptly by applying the device schematic diagram of direct current external electric field.
The graph of a relation of Fig. 2 silicon dioxide microsphere Zeta-potential and pH value
Graph of a relation between Fig. 3 ethyl orthosilicate addition and the silicon dioxide microsphere diameter
The SEM photo of Fig. 4 equidimension delthyrium inoranic membrane, Fig. 4 A, B, C represent the photo of different multiplying.
Device shown in Figure 1,1, the suspension of metal plate, 2, ITO (Indium Tin Oxide) conductive glass plate, 3, silicon dioxide microsphere.
The enforcement illustration of method is seen Fig. 1.
(top electrode connects negative electric-field intensity: 0.1-1000V/cm, and bottom electrode just connects, and this determines connection according to the Zeta-potential of microballoon in the suspension positive and negative.If the Zeta-potential of microballoon is for negative in the suspension, then top electrode connects negatively, and bottom electrode just connects; If the Zeta-potential of microballoon is for just in the suspension, then top electrode just connects, and bottom electrode connects negative).Electric-field intensity commonly used is 10-200V/cm, can guarantee that preparation efficiency is higher, can guarantee the voltage of safety again.Backing material: ITO (Indium Tin Oxide) conductive glass plate or metal plate all can.
The isometrical microsphere suspension liquid control method of silica: with ethyl orthosilicate (tetraethylorthosilicate, TEOS) progressively join in the ethanolic solution that contains ammoniacal liquor, under stationary temperature (testing used temperature range is 40-65 ℃), electromagnetic agitation 24 hours obtains isometrical silicon dioxide microsphere.The size of regulating isometrical silicon dioxide microsphere by the concentration of control TEOS and ammoniacal liquor.Regulate the pH value by the amount that ammoniacal liquor drips.(with the wet chemistry method preparation, diameter generally commonly used is about 150nm～1000nm).The microballoon that obtains in the suspension is isometrical silicon dioxide microsphere.
According to device shown in Figure 1, under the condition that applies the direct current external electric field, can prepare the template that the three-dimensional periodic long-range order is arranged.
Arrange in the process of long range ordered structure template at the preparation three-dimensional periodic, at first studied the influence (see figure 2) of different pH values silicon dioxide microsphere Zeta-potential in the suspension.Under the condition of pH value=8-9.0, find in the pH value to be at 9.0 o'clock, the silicon dioxide microsphere Zeta-potential has smaller value in the suspension.With this pH value as the optimal pH that adds the direct current external electric field.
Relation between the addition of ethyl orthosilicate and the diameter of silicon dioxide microsphere as shown in Figure 3, the addition of ethyl orthosilicate is many more, the diameter of silicon dioxide microsphere is big more.
Then, under the condition of pH value=9.0, silicon dioxide microsphere suspension is applied DC electric field, the power-on and power-off anode-cathode distance is 1cm, and applied voltage 100V treats in the silica suspension after the solvent evaporates, can prepare film shape sample, this sample is carried out sem observation, and (Scanned Electronic Microscopy, SEM), wherein the SEM photo of specimen surface is seen Fig. 4 A, B, C.As can be seen from Figure 4, silicon dioxide microsphere is arranged in long-range order equidimension delthyrium structure.
Claims (4)
1, a kind of equidimension delthyrium preparation of inorganic method, at first the isometrical microsphere suspension liquid of the silica of preparation being regulated the pH value is 4-12, it is characterized in that adopting the method for extra electric field control colloidal particle self assembly, by being to apply the direct current external electric field in the isometrical microsphere suspension liquid of described silica of 150nm～1000nm at diameter, if the Zeta-potential of microballoon is for negative in the suspension, then top electrode connects negatively, and bottom electrode just connects; If the Zeta-potential of microballoon is for just in the suspension, then top electrode just connects, and bottom electrode connects negative, electric-field intensity is 0.1-1000V/cm, make charged microballoon outside under the effect of electric field, orientated deposition on conducting plate, thus form the template that three-dimensional periodic is arranged long range ordered structure.
2, by the described equidimension delthyrium of claim 1 preparation of inorganic method: it is characterized in that the size of regulating the isometrical microballoon of silica by the concentration of control ethyl orthosilicate and ammoniacal liquor.
3, by the described equidimension delthyrium of claim 1 preparation of inorganic method: it is characterized in that the isometrical microsphere suspension liquid pH of silica value is 8-9.0.
4, by the described equidimension delthyrium of claim 1 preparation of inorganic method: the electric-field intensity that it is characterized in that applying the direct current external electric field is 10-200V/cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101065804A CN100496681C (en) | 2003-12-09 | 2003-12-09 | External direct current field self-assembly manufactured adjustable equal dimension triangular hole inorganic films |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101065804A CN100496681C (en) | 2003-12-09 | 2003-12-09 | External direct current field self-assembly manufactured adjustable equal dimension triangular hole inorganic films |
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|---|---|
| CN1546213A CN1546213A (en) | 2004-11-17 |
| CN100496681C true CN100496681C (en) | 2009-06-10 |
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| CNB2003101065804A Expired - Fee Related CN100496681C (en) | 2003-12-09 | 2003-12-09 | External direct current field self-assembly manufactured adjustable equal dimension triangular hole inorganic films |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050955B (en) * | 2009-10-28 | 2012-07-18 | 北京化工大学 | Preparation method of polystyrene-based mesoporous silica film |
| CN104928759B (en) * | 2015-07-14 | 2018-03-30 | 哈尔滨工业大学 | A kind of method using the quick assembling colloidal crystal of absorption layer by layer |
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Granted publication date: 20090610 Termination date: 20111209 |