CN102730705A - Preparation method for array hole low dielectric material - Google Patents
Preparation method for array hole low dielectric material Download PDFInfo
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- CN102730705A CN102730705A CN2012102373642A CN201210237364A CN102730705A CN 102730705 A CN102730705 A CN 102730705A CN 2012102373642 A CN2012102373642 A CN 2012102373642A CN 201210237364 A CN201210237364 A CN 201210237364A CN 102730705 A CN102730705 A CN 102730705A
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Abstract
The invention discloses a preparation method for the array hole low dielectric material. Micro-nano bobbles are introduced into a low dielectric material body, so that the micro-nano bobbles have a certain arrangement rule after being subjected to a self-assembling process, and then the bobbles are removed to obtain regularly-arranged arrangement holes in the material body. The size and the distribution of a single-layer bobble template prepared with a self-assembling method which is provided by the invention are even and controllable, the film has the advantages of higher forming intensity and even performance, and the defects of poor mechanical strength, big possibility of locally collapsing and different performances between each area of the common porous material are overcome.
Description
Technical field
The invention belongs to thin-film material processing technology of preparing field, especially a kind of preparation method of array dielectric materials.
Background technology
Along with the unicircuit integrated level increases, device size micro-nanoization, the density of electronic devices and components improve makes line capacitance, layer capacitance and metal connecting line resistance become big, thereby causes problems such as signal lag, noise, power loss more outstanding.For addressing these problems, use dielectric materials to do the inexorable trend that dielectric insulation layer is the unicircuit development.At present research is more has inorganic low-k materials (decolorizing carbon nitrogen film, polycrystalline boron nitrogen film, fluorine silex glass etc.), organic low-k materials (polyimide, Vilaterm-aryl compound, ppe, Vestolen PP 7052 etc.) and hybrid inorganic-organic low-k materials (being mixed with the organic siloxane polymer).Because the specific inductivity of air approaches vacuum, thinks that generally speaking its relative permittivity is 1.Therefore, material internal is filled certain air, and promptly the material porous is a kind of effective ways that reduce material dielectric constant.The insulating material SiO lower like the k value
2The middle hole of injecting forms aerosol (porosity can reach 98%, and specific inductivity is low to reach 1.05) or xerogel (porosity is generally at 50-90%, and specific inductivity is generally between 1.3 to 2.5).
Though porous material can reduce the specific inductivity of material, the porous characteristic has also influenced the physical strength of film, and is complicated more to the Wiring technique requirement of copper conductor.In addition, in the existing technology, the porous of preparation is often brought negative impact because of skewness to the surface property of material, such as making material surface specific inductivity everywhere inconsistent etc.
Therefore be necessary to propose a kind of array hole dielectric materials preparation technology that can improve the distribution situation of material hole, to solve the problem in the existing technology.
Summary of the invention
In view of this, the present invention provides a kind of hole to be distributed with rule, the adjustable array hole dielectric materials of pore size preparation method, thus improve the physical strength and the surface arrangement characteristic of material.
The preparation method of a kind of array hole dielectric materials that proposes according to the object of the invention comprises step:
Clean substrate;
In said substrate, apply the solution contain polymer globules, the solution of this coating is carried out solvent evaporates and self-assembly processing, this polymer globules rule is arranged in the substrate;
Prepare silicate sol with acidic hydrolysis and basic polycondensation two-step approach, this silicate solutions is spin-coated on substrate surface forms wet gel, the thickness of this wet gel is less than the diameter of polymer globules;
To this wet gel wear out, drying and thermal treatment obtains xerogel;
Remove the polymer globules in the said xerogel, obtain having the dielectric materials of array hole.
Preferably, the step of said cleaning substrate is distinguished ultrasonic cleaning 2 times, each 10 minutes successively for adopting acetone, ethanol and deionized water.
Preferably, the said solution that contains polymer globules is that PS is received ball solution, and it is 100nm-500nm that this PS is received the diameter of ball, and the solid content of this solution is 1%-10%, and the coating of this solution is adopted and dripped a mode that is coated with and carry out.
Preferably, before the said PS of coating is received ball solution, comprise also hydrophilic treatment carried out in substrate that this hydrophilic treatment employing concentration is 98% H
2SO
4With concentration be 30% H
2O
2The mixed solution that forms by the mixed of 3:1 cleans substrate.
Preferably, said solvent evaporates and self-assembly are handled to be specially and vinylbenzene is reunited in said coating are received substrate after the ball solution and be placed on and leave standstill 24 hours in the atmosphere, make solvent evaporates and make PS receive ball to accomplish self-assembly.
Preferably, the said solution that contains polymer globules is the toluene solution of PS-b-PMMA, and the coating of this solution adopts the mode of spin coating to carry out.
Preferably; Said solvent evaporates and self-assembly are handled to be specially the substrate that has applied the PS-b-PMMA toluene solution were heated 24 hours under 180 ℃ of environment, immerse in 80 ℃ of acetate the completion self assembling process again 20 minutes; Use washed with de-ionized water at last, and use nitrogen drying.
Preferably, the acidic hydrolysis of said silicate sol is meant stirring after tetraethoxy, ethanol, water and the mixed in hydrochloric acid, and to form standardized solution, wherein the ratio of hydrochloric acid and churning time are looked hydrolysis rate and the degree of tetraethoxy and decided.
Preferably, the basic polycondensation of described silicate sol is meant in said standardized solution and adds ammoniacal liquor and ethanol, makes the tetraethoxy after the hydrolysis begin polycondensation, and forming polymerisate is silicate sol.
Preferably; The said concrete steps that obtain xerogel are: earlier with wet gel in alcohol atmosphere, carry out burin-in process, the colloid after will wearing out carries out drying treatment, at last the sample after the drying treatment is warming up to 200 ℃-500 ℃ with the speed of 1 ℃/min under 60 ℃ temperature again; Kept 2 hours, and cool off with the speed of 2 ℃/min.
Preferably, the polymer globules in the said xerogel of said removal is specially: earlier xerogel is immersed in to dissolve in the organic solvent and removes polymer globules, dry down at 60 ℃ then and remove all solvents, finally obtain having the dielectric materials of array hole.
Compared with prior art; The advantage of array hole dielectric materials of the present invention is: the ball casement plate that does not still have individual layer at present can be used for the preparation of nano-porous film; When the thickness of film during less than the diameter of bead, the cavity of film is run through from bottom to up, helps to improve radiating effect; The size of the support frame of film can help to improve the physical strength of film through reducing the distribution density regulation and control of bead; Reticulated structure is periodically extension, can guarantee that the performance difference at each position of film is less.Provided by the present invention, utilize the individual layer bead template of self-assembly method preparation, size be evenly distributed and controlled, the shaping strength of film is higher, the performance homogeneous has overcome general porous material bad mechanical strength, local collapse easily, the shortcoming that each region performance is totally different.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the preparing method's of an array hole dielectric materials of the present invention schematic flow sheet.
Fig. 2 is the corresponding structural representation of aforesaid method.
Fig. 3 is the side signal comparison diagram of the embodiment one and the sample of embodiment two preparations.
Embodiment
In the technology of existing preparation porous low dielectric material, the array hole of the implementation rule of having no idea is arranged and to the adjusting of hole density, is caused the physical strength of existing porous low dielectric material and surface property in use to have many deficiencies.
The present invention is directed to deficiency of the prior art; A kind of dielectric materials preparation method that can realize having the array hole that rule arranges has been proposed; Through in the dielectric materials main body, introducing the micro-nano bead; Make these micro-nano beads have certain arranging rule, remove bead then, thereby obtain the array hole that rule is arranged in body of material through behind the self assembling process.The array hole dielectric materials that makes through this method; Not only the performance of material surface has good consistence; And owing to can control the arranging density of micro-nano bead and the thickness of body of material; So can be good at solving the problem of mechanical strength, thereby realize the making of high quality dielectric materials.
Please in the lump referring to Fig. 1 and Fig. 2, Fig. 1 is the preparing method's of an array hole dielectric materials of the present invention schematic flow sheet.Fig. 2 is the corresponding structural representation of aforesaid method.As shown in the figure, preparation method of the present invention comprises step:
S1: clean substrate;
S2: in said substrate, apply the solution contain polymer globules, the solution of this coating is carried out solvent evaporates and self-assembly processing, this polymer globules rule is arranged in the substrate;
S3: prepare silicate sol with acidic hydrolysis and basic polycondensation two-step approach, this silicate solutions is spin-coated on substrate surface forms wet gel, the thickness of this wet gel is less than the diameter of polymer globules;
S4: to this wet gel wear out, drying and thermal treatment obtains xerogel;
S5: remove the polymer globules in the said xerogel, obtain having the dielectric materials of array hole.
Step S1 is specially and adopts acetone, ethanol and deionized water to distinguish ultrasonic cleaning 2 times successively; Each 10, minute; To guarantee the clean level of substrate surface, the scavenging solution that adopts when cleaning simultaneously also can be wetting with substrate surface, for follow-up coating work is got ready.For some and the lower coating solution of substrate caking ability, also need do hydrophilic treatment, to increase the tack of coating solution in the subsequent process at substrate surface.
The diameter of the polymer globules of selecting for use among the step S2 should look required dielectric materials body thickness and design pore size and decide, can run through unitary piece of material in order to guarantee polymer globules, the minimum material thickness that is greater than of its diameter.In addition, the polymer globules of selecting for use should be a kind of organic solution that is soluble in, and is higher than under 500 ℃ the environment existence that can be stable in temperature.
In the present invention, this polymer globules solution is preferably PS and receives ball solution or polystyrene-poly TEB 3K di-block copolymer (hereinafter to be referred as toluene solution PS-b-PMMA).
Especially, when polymer globules solution is PS when receiving ball solution, it is 100nm-500nm that this PS is received the diameter of ball; The solid content of this solution is 1%-10%, through the solid content of regulator solution, promptly regulates PS and receives the quantity of ball; It is densely covered to realize regulating bead arranging after covering; Regulate array hole density thereby reach, the size of the support frame of body of material film is enlarged, improve the purpose of the physical strength of film.
The coating of this solution adopts a mode that is coated with to carry out.Drip be coated with before, preferably hydrophilic treatment is carried out in substrate, make drip when being coated with PS receive ball solution can be preferably attached to substrate surface.This hydrophilic treatment employing concentration is 98% H
2SO
4With concentration be 30% H
2O
2The mixed solution that forms by the mixed of 3:1 cleans substrate.
After applying completion; The solvent evaporates that PS is received in the ball solution is fallen; And make PS receive the ball self-assembly to be arranged in lattice array; The self-assembly here is meant that receiving ball with PS is base unit, receives the interaction of non covalent bond between the ball by PS, makes PS receive the spontaneous tissue of ball or gathering and is one and stablizes, have certain regular geometric structure arranged.Said solvent evaporates and self-assembly are handled to be specially and vinylbenzene is reunited in said coating are received substrate after the ball solution and be placed on and leave standstill 24 hours in the atmosphere, make solvent evaporates and make PS receive ball to accomplish self-assembly.
And when the said solution that contains polymer globules was the toluene solution of PS-b-PMMA, the coating of this solution adopted the mode of spin coating to carry out.After applying completion, equally need be with the solvent evaporates in the PS-b-PMMA toluene solution, so that the PS ball carries out self-assembly.Be specially the substrate that will apply the PS-b-PMMA toluene solution and under 180 ℃ of environment, heated 24 hours, immersed again in 80 ℃ of acetate 20 minutes, accomplish self assembling process, use washed with de-ionized water at last, and use nitrogen drying.
The concrete steps of preparation silicate sol are among the step S3: acidic hydrolysis: with stirring after tetraethoxy (hereinafter to be referred as TEOS), ethanol, water and the mixed in hydrochloric acid; To form standardized solution; Wherein the ratio of hydrochloric acid and churning time are looked hydrolysis rate and the degree of TEOS and are decided; When being 1:3:1 such as the mol ratio when TEOS, second alcohol and water, then the molar ratio of hydrochloric acid is 1.4 * 10
-3About.Churning time then need make the abundant hydrolysis of TEOS greater than 1 hour.Basic polycondensation: in said worth standardized solution, add ammoniacal liquor and ethanol, stir simultaneously, make the TEOS after the hydrolysis begin polycondensation, forming polymerisate is silicate sol.Churning time makes the viscosity of silicate sol and decides, and needs usually to stir about 2 hours, obtains viscous modulus in the 8-14cP silicate sol.
The mode of silicate sol under this viscosity with spin coating covered in the substrate, form wet gel, require the thickness of this wet gel to be lower than the diameter of above-mentioned polymer globules, so, polymer globules can realize to the running through of above-mentioned wet gel, referring to Fig. 3.
Among the step S4 above-mentioned wet gel is prepared into xerogel; Detailed process for earlier with wet gel in alcohol atmosphere, carry out burin-in process, the colloid after will wearing out carries out drying treatment, at last the sample after the drying treatment is warming up to 200 ℃-500 ℃ with the speed of 1 ℃/min under 60 ℃ temperature again; Kept 2 hours; And cool off with the speed of 2 ℃/min, until normal temperature.
Among the final step S5, the xerogel that obtains is immersed in the organic solvent removes polymer globules with dissolving, then 60 ℃ down oven dry remove all solvents, obtain having the dielectric materials of array hole after final and the substrate disengaging.
To carry out clear, intactly description to technical scheme of the present invention through embodiment below.Obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
Embodiment one:
Step 1: use acetone, ethanol and deionized water to Si substrate ultrasonic cleaning 10 minutes respectively, use dense H again
2SO
4(98%): H
2O
2The mixing solutions of=3:1 carries out wetting ability to be handled.
Step 2: choose solid content and be 3% 500nm ordinary polystyrene and receive the aqueous solution of ball, drip at the Si substrate surface and be coated with, solvent is volatilization naturally in air, and places more than 24 hours, treats that it carries out self-assembly, obtains the nanometer bead of regular distribution.
Step 3: (mol ratio 1:3:1:1.4 * 10-3) be hybridly prepared into standardized solution at room temperature stirred 90 minutes with tetraethoxy (TEOS), ethanol, water and hydrochloric acid earlier; Get ten milliliters standardized solution again, the ammonia soln of the 0.05M/L of adding 2ml and 14 milliliters ethanol stirred 110 minutes, treated its viscous modulus when 8-14cP, in the big saturation steam of ethanol, carried out spin coating, 2000 rev/mins of speed, 18 seconds time; Still early wear out and 60 ℃ of following dryings under this atmosphere and the room temperature then; Last under 300 ℃, heat-treating obtains the thick xerogel of 400nm.
Step 4: immerse sample in the toluene solvant, ultrasonic cleaning, drying is enough down at 60 ℃ to take out the back, obtains exsiccant array hole dielectric materials.
Embodiment two:
Step 1: use acetone, ethanol and deionized water to Si substrate ultrasonic cleaning 10 minutes respectively, use dense H again
2SO
4(98%): H
2O
2The mixing solutions of=3:1 carries out wetting ability to be handled.
Step 2: choose solid content and be 1% 500nm ordinary polystyrene and receive the aqueous solution of ball, drip at the Si substrate surface and be coated with, solvent is volatilization naturally in air, and places more than 24 hours, treats that it carries out self-assembly, obtains the nanometer bead of regular distribution.
Step 3: (mol ratio 1:3:1:1.4 * 10-3) be hybridly prepared into standardized solution at room temperature stirred 90 minutes with tetraethyl silicate (TEOS), ethanol, water and hydrochloric acid earlier; Get ten milliliters standardized solution again, the ammonia soln of the 0.05M/L of adding 2ml and 14 milliliters ethanol stirred 110 minutes, treated its viscous modulus when 8-14cP, in the ethanol atmosphere, carried out spin coating, 2000 rev/mins of speed, 18 seconds time; Still early wear out and 60 ℃ of following dryings under this atmosphere and the room temperature then; Last under 300 ℃, heat-treating obtains the thick xerogel of 400nm.
Step 4: immerse sample in the toluene solvant, ultrasonic cleaning, drying is enough down at 60 ℃ to take out the back, obtains exsiccant array hole dielectric materials.
Embodiment three:
Step 1: use acetone, ethanol and deionized water respectively to Si substrate ultrasonic cleaning 10 minutes.
Step 2: after the toluene solution of PS-b-PMMA (poly (styrene-co-methyl-methacrylate)) is spin-coated on the Si substrate surface; 180 ℃ were heated 24 hours; Immersed again in 80 ℃ of acetate 20 minutes, and accomplished self assembling process, use washed with de-ionized water at last; And use nitrogen drying, obtain the nanometer bead of regular distribution.
Step 3: (mol ratio 1:3:1:1.4 * 10-3) be hybridly prepared into standardized solution at room temperature stirred 90 minutes with tetraethyl silicate (TEOS), ethanol, water and hydrochloric acid earlier; Get ten milliliters standardized solution again, the ammonia soln of the 0.05M/L of adding 2ml and 14 milliliters ethanol stirred 110 minutes, treated its viscous modulus when 8-14cP, in the ethanol atmosphere, carried out spin coating, 2000 rev/mins of speed, 18 seconds time; Still under this atmosphere and room temperature, wear out then and 60 ℃ of following dryings; Last under 300 ℃, heat-treating obtains the thick xerogel of 400nm.
Step 4: immerse sample in the toluene solvant, ultrasonic cleaning, drying is enough down at 60 ℃ to take out the back, obtains exsiccant array hole dielectric materials.
With the array hole dielectric materials, carry out the test of porosity and dielectric properties.Through test, the porosity of this sample surpasses 60%, and relative permittivity can reduce to 2.Please continue referring to Fig. 3, it is the side signal comparison diagram of the embodiment one and the sample of embodiment two preparations, and the density of reflection solution is to the influence of the distribution density of bead.The distribution density of polymer globules obviously influences the porosity of film, thereby changes the relative permittivity of material.
In sum; The present invention proposes a kind of preparation method of array hole dielectric materials; Through in the dielectric materials main body, introducing the micro-nano bead; Make these micro-nano beads have certain arranging rule, remove bead then, thereby obtain the array hole that rule is arranged in body of material through behind the self assembling process.The prior art of comparing, provided by the present invention, utilize the individual layer bead template of self-assembly method preparation; Size be evenly distributed and controlled, the shaping strength of film is higher, the performance homogeneous; Overcome general porous material bad mechanical strength, easy local collapse, the shortcoming that each region performance is totally different.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (11)
1. the preparation method of an array hole dielectric materials is characterized in that, comprises step:
Clean substrate;
In said substrate, apply the solution contain polymer globules, the solution of this coating is carried out solvent evaporates and self-assembly processing, this polymer globules rule is arranged in the substrate;
Prepare silicate sol with acidic hydrolysis and basic polycondensation two-step approach, this silicate solutions is spin-coated on substrate surface forms wet gel, the thickness of this wet gel is less than the diameter of polymer globules;
To this wet gel wear out, drying and thermal treatment obtains xerogel;
Remove the polymer globules in the said xerogel, obtain having the dielectric materials of array hole.
2. array hole dielectric materials preparation method as claimed in claim 1 is characterized in that: the step of said cleaning substrate is specially and adopts acetone, ethanol and deionized water to distinguish ultrasonic cleaning 2 times, each 10 minutes successively.
3. array hole dielectric materials preparation method as claimed in claim 1; It is characterized in that: the said solution that contains polymer globules is that PS is received ball solution; It is 100nm-500nm that this PS is received the diameter of ball; The solid content of this solution is 1%-10%, and the coating of this solution adopts a mode that is coated with to carry out.
4. array hole dielectric materials preparation method as claimed in claim 3 is characterized in that: before the said PS of coating is received ball solution, comprise also hydrophilic treatment is carried out in substrate that this hydrophilic treatment employing concentration is 98% H
2SO
4With concentration be 30% H
2O
2The mixed solution that forms by the mixed of 3:1 cleans substrate.
5. array hole dielectric materials preparation method as claimed in claim 3; It is characterized in that: said solvent evaporates and self-assembly are handled to be specially and vinylbenzene is reunited in said coating are received substrate after the ball solution and be placed on and leave standstill 24 hours in the atmosphere, make solvent evaporates and make PS receive ball to accomplish self-assembly.
6. array hole dielectric materials preparation method as claimed in claim 1 is characterized in that: the said solution that contains polymer globules is the toluene solution of PS-b-PMMA, and the coating of this solution adopts the mode of spin coating to carry out.
7. array hole dielectric materials preparation method as claimed in claim 6; It is characterized in that: said solvent evaporates and self-assembly are handled to be specially the substrate that has applied the PS-b-PMMA toluene solution were heated 24 hours under 180 ℃ of environment; Immersed again in 80 ℃ of acetate 20 minutes; Accomplish self assembling process, use washed with de-ionized water at last, and use nitrogen drying.
8. array hole dielectric materials preparation method as claimed in claim 1; It is characterized in that: the acidic hydrolysis of said silicate sol is meant stirring after tetraethoxy, ethanol, water and the mixed in hydrochloric acid; To form standardized solution, wherein the ratio of hydrochloric acid and churning time are looked hydrolysis rate and the degree of tetraethoxy and are decided.
9. array hole dielectric materials preparation method as claimed in claim 8; It is characterized in that: the basic polycondensation of described silicate sol is meant and in said standardized solution, adds ammoniacal liquor and ethanol; Make the tetraethoxy after the hydrolysis begin polycondensation, forming polymerisate is silicate sol.
10. array hole dielectric materials preparation method as claimed in claim 1; It is characterized in that: the said concrete steps that obtain xerogel are: earlier with wet gel in alcohol atmosphere, carry out burin-in process, the colloid after will wearing out carries out drying treatment, at last the sample after the drying treatment is warming up to 200 ℃-500 ℃ with the speed of 1 ℃/min under 60 ℃ temperature again; Kept 2 hours, and cool off with the speed of 2 ℃/min.
11. array hole dielectric materials preparation method as claimed in claim 1; It is characterized in that: the polymer globules in the said xerogel of said removal is specially: earlier xerogel is immersed in to dissolve in the organic solvent and removes polymer globules; Dry down at 60 ℃ then and remove all solvents, finally obtain having the dielectric materials of array hole.
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| CN201210237364.2A CN102730705B (en) | 2012-07-10 | 2012-07-10 | Preparation method for array hole low dielectric material |
| PCT/CN2012/086635 WO2014008744A1 (en) | 2012-07-10 | 2012-12-14 | Preparation method of low dielectric material with array holes |
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|---|---|---|---|---|
| WO2014008744A1 (en) * | 2012-07-10 | 2014-01-16 | 苏州大学 | Preparation method of low dielectric material with array holes |
| CN106278371A (en) * | 2016-09-30 | 2017-01-04 | 温州生物材料与工程研究所 | A kind of functional hierarchical three-dimensional porous silica-base film preparation method and biologic applications thereof |
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| CN1544324A (en) * | 2003-11-20 | 2004-11-10 | 中国科学院上海技术物理研究所 | Silica dioxide aerogel membrane material preparation method |
| CN101582331A (en) * | 2009-05-27 | 2009-11-18 | 彩虹集团公司 | Method for preparing platinum counter electrode of dye-sensitized solar battery with large surface area |
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| CN1817786A (en) * | 2006-01-18 | 2006-08-16 | 南京大学 | Two-dimensional fractional standing point array with ordered Fe/SiO2 composite nanometer particle and production thereof |
| CN102183561A (en) * | 2011-02-21 | 2011-09-14 | 常熟理工学院 | Spherical-cavity microelectrode array biosensor and preparation method thereof |
| CN102691102A (en) * | 2012-06-04 | 2012-09-26 | 中国科学院半导体研究所 | Method for manufacturing substrate of sapphire nanometer bowl array pattern |
| CN102694088A (en) * | 2012-06-06 | 2012-09-26 | 中国科学院半导体研究所 | Roughening method for indium tin oxide (ITO) nanobowl array of GaN-based light-emitting diode (LED) |
| CN102730705B (en) * | 2012-07-10 | 2014-11-05 | 苏州大学 | Preparation method for array hole low dielectric material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544324A (en) * | 2003-11-20 | 2004-11-10 | 中国科学院上海技术物理研究所 | Silica dioxide aerogel membrane material preparation method |
| CN101582331A (en) * | 2009-05-27 | 2009-11-18 | 彩虹集团公司 | Method for preparing platinum counter electrode of dye-sensitized solar battery with large surface area |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014008744A1 (en) * | 2012-07-10 | 2014-01-16 | 苏州大学 | Preparation method of low dielectric material with array holes |
| CN106278371A (en) * | 2016-09-30 | 2017-01-04 | 温州生物材料与工程研究所 | A kind of functional hierarchical three-dimensional porous silica-base film preparation method and biologic applications thereof |
| CN106278371B (en) * | 2016-09-30 | 2019-05-14 | 温州生物材料与工程研究所 | A kind of three-dimensional porous silica-base film preparation method of functionality hierarchical and its biologic applications |
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