CN105153446A - Preparation method and application of periodic organosilica mesoporous (PMO) thin film - Google Patents
Preparation method and application of periodic organosilica mesoporous (PMO) thin film Download PDFInfo
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- CN105153446A CN105153446A CN201510648357.5A CN201510648357A CN105153446A CN 105153446 A CN105153446 A CN 105153446A CN 201510648357 A CN201510648357 A CN 201510648357A CN 105153446 A CN105153446 A CN 105153446A
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- 0 CC(C(CC(C1)C2)(CC1C1)CC21C(NCCC[Si+]*)=O)=O Chemical compound CC(C(CC(C1)C2)(CC1C1)CC21C(NCCC[Si+]*)=O)=O 0.000 description 2
Abstract
The present invention relates to a kind of preparation method and applications of PMO film; Wherein preparation method includes the following steps: that (1) provides chloride compounds;
(2) precursor molecule solution is prepared; The chloride compounds, 3-aminopropyltriethoxysilane and triethylamine are mixed, reacts and precursor molecule solution is made; Chloride compounds: 3-aminopropyltriethoxysilane: the molar ratio of triethylamine is 0.5~1:1~2:1.2~2.4; The structural formula of precursor molecule are as follows:
(3) it prepares coating solution: template, solvent and dilute hydrochloric acid being added into presoma molecular solution, coating solution is made, the additive amount of template is 0~100%; (4) PMO film is prepared; Coating solution is applied to substrate surface, is solidified, PMO film is made. This method reaches the reduction of novel PMO thin-film dielectric constant and the guarantee of mechanical property by increasing molecule pore volume, reducing molecular polarity, the raising degree of cross linking.
Description
Technical field
The present invention relates to a kind of preparation method of order mesoporous organosilicone film, the invention still further relates to the application of the order mesoporous organosilicone film prepared by this preparation method.
Background technology
For reducing the specific inductivity of material, utilize the air introducing pole low-k to enter material hole, making porous dielectric material becomes widely used laboratory facilities.But introduce while hole, also make the stability of material and heat conductivility reduce, thus need to set up theoretically a suitable model and instruct experiment, prediction porosity is on the impact of heat, electrical property.
The preparation of porous low dielectric material usually adopts and comprises sol-gel method, original position grafting and template etc.Wherein, template is due to its template pore-creating agent molecular structure, size adjustable, and pore-creating agent molecular degradation mode (etching, pyrolysis, photodegradation etc.) such as can to design at the flexible and varied property, in the favor of the research field extremely scientists of porous material.The Shen Jun of Tongji University in 2006 teaches with TEOS (tetraethoxy) as silicon source, cats product cetyl trimethylammonium bromide is template, in acid condition, sol-gel method is adopted to prepare mesoporous silicon oxide films, aperture is 4nm, the specific inductivity of film is 2.5, and its mesoporous formation is namely at 300 ~ 400 DEG C, Heating degrades template molecule in nitrogen atmosphere.Refer to prior art " J.Shen, A.Y.Luo, L.F.Yao, X.J.Lin; B.Zhou, G.M.Wu, X.Y.Ni; Lowdielectricconstantsilicafilmswithorderednanoporousstr ucture.Mater.Sci.Eng.C.2007,27,1145-1148. "
The Kang of NUS in 2005 teaches research group and utilizes ultraviolet degradation to gather the segmented copolymer of pentafluorostyrene and polymethylmethacrylate, obtain the fluorine-containing mesoporous polymer film of aperture 30 ~ 50nm, porosity 15 ~ 40%, its specific inductivity can be low to moderate about 1.8.Refer to prior art " G.D.Fu; Z.Yuan; E.T.Kang; K.G.Neoh; D.M.Lai; A.C.H.Huan, NanoporousUltra-Low-Dielectric-ConstantFluoropolymerFilm sviaSelectiveUVDecompositionofPoly (pentafluorostyrene)-block-Poly (methylmethacrylate) CopolymersPreparedUsingAtomTransferRadicalPolymerization .Adv.Funct.Mater.2005,15,315-322. "
Professor Ree of Pohang University of Science and Technology in 2005 using mPCL-6 (six arm poly-epsilon-caprolactones) the star-like dendritic macromole of Trimethoxy silane modification as template pore-creating agent, with polymethylsilsesquioxane (PMSSQ) presoma Homogeneous phase mixing, spin-on techniques is adopted to prepare laminated film, after the content of mPCL-6 is 40% and is degradable at 400 DEG C, the specific inductivity of film can be low to moderate 1.67.Refer to prior art " B.Lee, W.Oh, Y.Hwang; Y.H.Park; J.Yoon, K.S.Jin, K.Heo; J.Kim; K.W.Kim, M.Ree, ImprintingWell-ControlledNanoporesinOrganosilicateDielec tricFilms:Triethoxysilyl-ModifiedSix-ArmedPoly (∈-caprolactone) andItsChemicalHybridizationwithanOrganosilicatePrecursor .Adv.Mater.2005; 17,696-701. "
Although above-mentioned prior art all shows that template achieves certain development preparing in porous low dielectric constant investigation of materials, but in the face of the requirement that integrated circuit industry is more and more higher, also need the specific inductivity constantly reducing material, ensure its mechanical property and thermal property simultaneously.In addition, mostly there is the problems such as rate of moisture absorption is higher, pore size distribution is wider, hole effects of coupling between is obvious, mechanical strength is poor in obtained porous material, also has suitable difficulty for obtaining practical application in super large-scale integration.
Summary of the invention
First technical problem to be solved by this invention is the preparation method providing a kind of PMO film for the state of the art, and the method can ensure mechanical property and the thermal property of PMO film, effectively can reduce again the specific inductivity of PMO film.
Second technical problem to be solved by this invention is to provide the application of a kind of PMO film in super large-scale integration, the PMO film of concrete use has ultralow specific inductivity, thus can solve the problem such as Signal transmissions time delay, noise jamming enhancing, power loss caused because specific inductivity is high.
The present invention solves the technical scheme that above-mentioned first technical problem adopt: a kind of preparation method of PMO film, comprises the steps:
(1) provide such as formula the chloride compounds shown in I;
(2) precursor molecule solution is prepared; Described chloride compounds, APTES and triethylamine are mixed, the obtained precursor molecule solution of reaction; In described precursor molecule solution, chloride compounds: APTES: the mol ratio of triethylamine is 0.5 ~ 1:1 ~ 2:1.2 ~ 2.4; The structural formula of the precursor molecule in described precursor molecule solution is such as formula shown in II:
(3) coating solution is prepared: in described precursor molecule solution, add template, solvent and dilute hydrochloric acid, obtained coating solution, the quality of described template is 0 ~ 100% of precursor molecule quality, in described coating solution, the concentration of described precursor molecule is 0.02 ~ 0.04mol/L, i.e. 0.005 ~ 0.025g/mL;
(4) PMO film is prepared; Described coating solution is applied to substrate surface, solidification, obtained PMO film.
Wherein, in step (1), the preparation process of described chloride compounds is: by 1,3-adamantane acid is added in excessive thionyl chloride, at 60 ~ 90 DEG C, react 8 ~ 12h, obtained reaction mixture, described reaction mixture is dry, obtained described chloride compounds;
Preferably, described reaction mixture uses Rotary Evaporators to be spin-dried for, obtained described chloride compounds.
Wherein, in step (2), chloride compounds: APTES: the mol ratio of triethylamine is 1:2:2.2.
Wherein, in step (2), first described chloride compounds is dissolved in trichloromethane, then the chloroform soln of chloride compounds is added in the mixing solutions of APTES and triethylamine, the obtained described precursor molecule solution of reaction.
Wherein, in step (2), the temperature of reaction preparing described precursor molecule solution is room temperature, and the reaction times is 6 ~ 12h.
Wherein, in step (3), described template is template P123.
Wherein, in step (3), described solvent is ethanol;
Preferably, described dilute hydrochloric acid is 0.5M dilute hydrochloric acid.
Wherein, after step (3), step (3a) is also comprised, substrate pretreatment before step (4); Use ethanol, acetone to carry out supersound washing to described substrate respectively, then described substrate is immersed the cleaning solution process 20 ~ 40min of 80 ~ 100 DEG C, cooling, rinses, obtained pretreated substrate; Described cleaning solution contains hydrogen peroxide and the vitriol oil that massfraction is 30%, and the volume of described hydrogen peroxide and the vitriol oil is 1:2 ~ 5;
Preferably, the volume ratio of described hydrogen peroxide and the vitriol oil is 1:3;
Wherein, described substrate is silicon chip;
Preferably, described substrate is N-type silicon chip;
Preferably, the resistivity of described N-type silicon chip is 0.001 ~ 0.004 Ω m.
Wherein, in step (4), use rotary coating instrument that coating solution is spun on substrate surface;
Preferably, the rotating speed that described rotary coating instrument carries out spin coating is 700 ~ 1000rpm, is preferably 750 ~ 950rpm, more preferably 900rpm;
Preferably, the time that described rotary coating instrument carries out spin coating is 20 ~ 50s, is preferably 25 ~ 45s, more preferably 30s;
Preferably, described solidification refers to first solidification treatment 20 ~ 30h at 50 ~ 80 DEG C, and then at 260 ~ 350 DEG C solidification treatment 2 ~ 8h.
A kind of application of PMO film in super large-scale integration prepared by above-mentioned preparation method.
Compared with prior art, the invention has the advantages that: the present invention, when preparing PMO film, specifically selects diamantane as organic carbon skeleton, because of the stereoeffect of diamantane itself, make precursor molecule have large volume of voids, rigid structure also improves the mechanical strength of material simultaneously.In precursor molecule, 1,3 at diamantane replace, thus connect siloxane groups as silicon source, ensure that the degree of crosslinking of the rear material of solidification.
This preparation method is by increasing molecule volume of voids, reducing molecular polarity, improving degree of crosslinking, to reduce the specific inductivity of PMO film and to ensure its mechanical property.
In addition, after the ordered mesopore structure of PMO film the present invention prepared applies to the inter-level dielectric of super large-scale integration, the problem such as Signal transmissions time delay, noise jamming enhancing, power loss caused because specific inductivity is high can effectively be solved.
Accompanying drawing explanation
Fig. 1 is the high resolution mass spectrum figure of adamantyl presoma prepared by the embodiment of the present invention 1;
Fig. 2 is the infrared spectrum variation diagram of each material in the embodiment of the present invention 1 adamantyl precursor synthesis process;
Fig. 3 be the present invention under frequency 1M, the specific inductivity of PMO film prepared by each embodiment is with the variation diagram of template addition;
Fig. 4 is the variation diagram of specific inductivity with frequency of PMO film prepared by various embodiments of the present invention;
Fig. 5 is the planar cross-sectional SEM figure of PMO film prepared by the embodiment of the present invention 1;
Fig. 6 is the planar cross-sectional SEM figure of PMO film prepared by the embodiment of the present invention 2;
Fig. 7 is the planar cross-sectional SEM figure of PMO film prepared by the embodiment of the present invention 3;
Fig. 8 is the planar cross-sectional SEM figure of PMO film prepared by the embodiment of the present invention 4;
Fig. 9 is the little angle XRD figure of PMO film prepared by various embodiments of the present invention;
Figure 10 is the synthesis schematic diagram of the order mesoporous organosilicon material PMO of the embodiment of the present invention 1.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment is when preparing PMO film, and required raw material is: 1,3-adamantane acid (ADCA), and ladder is uncommon likes reagent, purity 95%, specification 25g; APTES (KH-550), Aladdin reagent, purity 97%, specification 100g; Trichloromethane, traditional Chinese medicines reagent, molecular sieve drying; Ethanol, traditional Chinese medicines reagent, molecular sieve drying; Hydrochloric acid, traditional Chinese medicines reagent; Thionyl chloride, traditional Chinese medicines reagent; Triethylamine, Sigma's reagent, purity 99%, specification 100mL; Poloxamer (P-123), Sigma's reagent, molecular-weight average 5800, specification 250mL.
The preparation method of the PMO film of the present embodiment, comprises the steps:
(1) preparation is such as formula the chloride compounds shown in I;
Concrete preparation process is as follows: to 1; excessive thionyl chloride solution (add excessive dichloride sulfone and refer to that dichloride sulfone and the mol ratio of ADCA are greater than the stoichiometric coefficient ratio in chemical equation) is added in 3-adamantane acid (ADCA); under circulating cooling protection; be heated to 60 ~ 90 DEG C; such as 80 DEG C, reaction 8 ~ 12h.Temperature of reaction herein and the choice criteria in reaction times are that white powder is disappeared, and illustrate that reactant 1,3-adamantane acid (ADCA) reacts completely, product is dissolved in solvent completely, obtained reaction mixture.Use Rotary Evaporators to be spin-dried for reaction mixture, remove unreacted thionyl chloride and excess of solvent, obtain the first chloride compounds.
The reaction formula that this step prepares chloride compounds is as follows:
Wherein, A is ADCA, B is target product chloride compounds.
(2) precursor molecule solution is prepared; APTES (KH-550) and triethylamine is taken, logical drying nitrogen protection in there-necked flask.The first step gained be spin-dried for after product---chloride compounds repeatedly dissolves with a small amount of trichloromethane, the amount of trichloromethane only needs to dissolve chloride compounds, the chloroform soln of chloride compounds is dripped in reaction mixture, under room temperature, react 8h, obtain precursor molecule solution.In precursor molecule solution, chloride compounds: APTES: the mol ratio of triethylamine is 0.5 ~ 1:1 ~ 2:1.2 ~ 2.4, this span can ensure to prepare target product, can ensure again the catalytic performance of triethylamine, namely ensure that yield and speed simultaneously; The mol ratio of the present invention to above-mentioned three kinds of materials does not limit, only need in above-mentioned scope, and the present embodiment is preferably 1:2:2.2.
The reaction that this step mainly occurs is as follows:
Wherein, D is APTES (KH-550), C is precursor molecule ADCS.
(3) prepare coating solution: in presoma molecular solution, add template, before spin coating, add alcohol solvent and 0.5M dilute hydrochloric acid, obtained coating solution, precursor molecule polymerization can be caused.Wherein, in the coating solution of the present embodiment, the content of template is 0%, does not namely add template.
In this step, the effect of alcohol solvent and dilute hydrochloric acid, mainly in order to regulate concentration to the 0.02 ~ 0.04mol/L of precursor molecule in coating solution, is preferably 0.03mol/L; The present invention does not limit the concentration of precursor molecule in coating solution, as long as in above-mentioned scope.
In addition, because the amount of the template of adding in each embodiment is different, and template is added in fluid form, so after different embodiment adds different template, cause liquor capacity inconsistent, so, need the amount regulating alcohol solvent and dilute hydrochloric acid in each embodiment, consistent to ensure the concentration of precursor molecule in each embodiment coating solution.
In addition, the adding proportion of ethanol and dilute hydrochloric acid does not limit, and wherein, the addition of dilute hydrochloric acid will ensure that solution does not occur precipitating (namely precursor molecule premature polymerization becomes particle) before spin coating.
(3a) substrate pretreatment: by substrate---silicon chip (N-type, resistance 0.001 ~ 0.004) is cut into the specification size of 2 × 2cm or 3 × 3cm.Use ethanol, acetone to carry out 20min ultrasonic cleaning to it respectively, then described substrate is immersed in cleaning solution, in 80 ~ 100 DEG C, preferably 90 DEG C, boil silicon chip 20 ~ 40min, preferred 30min, 30% hydrogen peroxide and the vitriol oil mixing solutions of cleaning solution to be ratio be 1:3.
Silicon chip cools, and then uses washed with de-ionized water silicon chip repeatedly, is stored in dehydrated alcohol for subsequent use.
(4) PMO film is prepared; Rotary coating instrument is used to be filmed.3000rpm rotating speed dries at the bottom of silicon wafer-based, again dries, nitrogen hydro-peening silicon chip 10s after propylene glycol monomethyl ether acid esters (PGMEA) solvent washing.Then the coating solution configured is dropped to silicon chip surface, 900rpm30s completes spin coating.Sample is first time solidification treatment 24h at 60 DEG C first, then at 300 DEG C second time solidification treatment 5h.PMO film after solidification, needs to be immersed in dehydrated alcohol and is heated to 70 DEG C, template P123 residual in removing PMO film.Finally, novel PMO film preparation is complete.
Precursor molecule C prepared by this implementation step (2) is adamantyl presoma, and its molecular weight is 630, there will be 653.3623 and belongs to ADCS and add Na (M+23) peak carrying out high resolution mass spectrum test.Viewed from the distribution of the molecular weight peaks obtained from Fig. 1, what do not occur occurring because of-COOH reactive behavior is monosubstituted, takes temperature show to obtain target compound from molecule---adamantyl presoma C.As can see from Figure 2, contrast with the infrared spectrum of two raw materials, can obtain at 3346cm
-1and 2931cm
-1-the NH at place
2peak transfers-NH-peak to and retains in the product, 1716cm
-1-COOH the peak at place, also with amidation generation red shift, describes the generation of reaction, demonstrates product and successfully prepare.
The synthesis schematic diagram of the order mesoporous organosilicon material PMO of the present embodiment as shown in Figure 10.
After the ordered mesopore structure of PMO film prepared by the present embodiment can apply to the inter-level dielectric of super large-scale integration, effectively can solve the problem such as Signal transmissions time delay, noise jamming enhancing, power loss caused because specific inductivity is high.
Embodiment 2
Preparation method's difference from Example 1 of the present embodiment PMO film is: in step (3), and the quality of template is 25% of precursor molecule quality; Meanwhile, by regulating the amount of ethanol, dilute hydrochloric acid, make in coating solution, the concentration of precursor molecule is identical with embodiment 1.
Other steps of the preparation method of the present embodiment PMO film are as embodiment 1.
Embodiment 3
Preparation method's difference from Example 1 of the present embodiment PMO film is: in step (3), and the quality of template is 50% of precursor molecule quality; Meanwhile, by regulating the amount of ethanol, dilute hydrochloric acid, make in coating solution, the concentration of precursor molecule is identical with embodiment 1.
Other steps of the preparation method of the present embodiment PMO film are as embodiment 1.
Embodiment 4
Preparation method's difference from Example 1 of the present embodiment PMO film is: in step (3), and the quality of template is 75% of precursor molecule quality; Meanwhile, by regulating the amount of ethanol, dilute hydrochloric acid, make in coating solution, the concentration of precursor molecule is identical with embodiment 1.
Other steps of the preparation method of the present embodiment PMO film are as embodiment 1.
Embodiment 5
Preparation method's difference from Example 1 of the present embodiment PMO film is: in step (3), and the quality of template is 100% of precursor molecule quality; Meanwhile, by regulating the amount of ethanol, dilute hydrochloric acid, make in coating solution, the concentration of precursor molecule is identical with embodiment 1.
Other steps of the preparation method of the present embodiment PMO film are as embodiment 1.
The specific inductivity of PMO film under frequency 1M of testing example 1 ~ 5 preparation respectively, test result is as shown in Figure 3; The respectively change of PMO film under differing dielectric constant prepared of testing example 1 ~ 5, its specific inductivity with frequency change as shown in Figure 4.As shown in Figure 3 and Figure 4, along with the increase of template, the specific inductivity of thin-film material declines, and when addition is 75%, comparatively stable lowest dielectric constant (~ 1.551MHz) has appearred in material; When addition adds 100% to, specific inductivity has occurred that abnormality increases phenomenon, and possible cause increases with aperture to occur that hole wall disappears, and occurred non-uniform Distribution situation, portion of electrical current punctures and causes specific inductivity to increase.
Fig. 5 ~ 8 are respectively the planar cross-sectional SEM figure of PMO film prepared by embodiment 1 ~ 4, and wherein the right part of flg of Fig. 5 ~ 8 is the section S EM figure of corresponding left hand view; The planar S EM of Fig. 5 ~ 8 can find out that the addition with template increases, the macro morphology of PMO film has had change, and the continuity of film is destroyed, gradually as can be seen from section S EM, there is meso-hole structure in the PMO film inside of embodiment 2,3,4, the distribution in hole is more and more intensive.Embodiment 5 is not put SEM and is illustrated that the progressive failure of its PMO film is serious, occurs macroscopic through hole.
Fig. 9 is the little angle XRD figure of PMO film prepared by embodiment 1 ~ 5; As can be seen from Figure 9, in little angle XRD all there is diffraction peak in example 1 ~ 4, the ordered structure of illustrative material.
Test water contact angle and the mechanical property of PMO film prepared by embodiment 1 ~ 5 respectively, test result is as shown in table 1.
The water contact angle of PMO film prepared by each embodiment of table 1. and mechanical property
| Embodiment | Contact angle/° | Young's modulus/GPa | Hardness/GPa |
| Embodiment 1 | 82.6 | 16.96±0.70 | 0.35±0.02 |
| Embodiment 2 | 74.4 | 14.41±0.55 | 0.27±0.08 |
| Embodiment 3 | 68.9 | 6.32±0.98 | 0.12±0.03 |
| Embodiment 4 | 55.7 | 6.99±0.68 | 0.13±0.02 |
| Embodiment 5 | 55.4 |
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (10)
1. a preparation method for PMO film, is characterized in that, comprises the steps:
(1) provide such as formula the chloride compounds shown in I;
(2) precursor molecule solution is prepared; Described chloride compounds, APTES and triethylamine are mixed, the obtained precursor molecule solution of reaction; In described precursor molecule solution, chloride compounds: APTES: the mol ratio of triethylamine is 0.5 ~ 1:1 ~ 2:1.2 ~ 2.4; The structural formula of the precursor molecule in described precursor molecule solution is such as formula shown in II:
(3) coating solution is prepared: in described precursor molecule solution, add template, solvent and dilute hydrochloric acid, obtained coating solution, the quality of described template is 0 ~ 100% of precursor molecule quality, in described coating solution, the concentration of described precursor molecule is 0.02 ~ 0.04mol/L;
(4) PMO film is prepared; Described coating solution is applied to substrate surface, solidification, obtained PMO film.
2. preparation method according to claim 1, it is characterized in that, in step (1), the preparation process of described chloride compounds is: by 1,3-adamantane acid is added in excessive thionyl chloride, at 60 ~ 90 DEG C, react 8 ~ 12h, obtained reaction mixture, described reaction mixture is dry, obtained described chloride compounds;
Preferably, described reaction mixture uses Rotary Evaporators to be spin-dried for, obtained described chloride compounds.
3. preparation method according to claim 1, is characterized in that: in step (2), chloride compounds: APTES: the mol ratio of triethylamine is 1:2:2.2.
4. preparation method according to claim 1, it is characterized in that: in step (2), first described chloride compounds is dissolved in trichloromethane, again the chloroform soln of chloride compounds is added in the mixing solutions of APTES and triethylamine, the obtained described precursor molecule solution of reaction.
5. the preparation method according to claim 1 or 4, is characterized in that: in step (2), and the temperature of reaction preparing described precursor molecule solution is room temperature, and the reaction times is 6 ~ 12h.
6. preparation method according to claim 1, is characterized in that: in step (3), and described template is template P123.
7. preparation method according to claim 1, is characterized in that: in step (3), and described solvent is ethanol;
Preferably, described dilute hydrochloric acid is 0.5M dilute hydrochloric acid.
8. preparation method according to claim 1, is characterized in that: after step (3), also comprise step (3a), substrate pretreatment before step (4); Use ethanol, acetone to carry out supersound washing to described substrate respectively, then described substrate is immersed the cleaning solution process 20 ~ 40min of 80 ~ 100 DEG C, cooling, rinses, obtained pretreated substrate; Described cleaning solution contains hydrogen peroxide and the vitriol oil that massfraction is 30%, and the volume ratio of described hydrogen peroxide and the vitriol oil is 1:2 ~ 5;
Preferably, the volume ratio of described hydrogen peroxide and the vitriol oil is 1:3;
Preferably, described substrate is silicon chip;
Preferably, described substrate is N-type silicon chip;
Preferably, the resistivity of described N-type silicon chip is 0.001 ~ 0.004 Ω m.
9. preparation method according to claim 1, is characterized in that: in step (4), uses rotary coating instrument that coating solution is spun on substrate surface;
Preferably, the rotating speed that described rotary coating instrument carries out spin coating is 700 ~ 1000rpm, is preferably 750 ~ 950rpm, more preferably 900rpm;
Preferably, the time that described rotary coating instrument carries out spin coating is 20 ~ 50s, is preferably 25 ~ 45s, more preferably 30s;
Preferably, described solidification refers to first solidification treatment 20 ~ 30h at 50 ~ 80 DEG C, and then at 260 ~ 350 DEG C solidification treatment 2 ~ 8h.
10. the application of PMO film in super large-scale integration prepared by the preparation method described in any one of claim 1 ~ 9.
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| WO2021222551A1 (en) * | 2020-04-30 | 2021-11-04 | Tiax Llc | Hydrophobic and omniphobic periodic mesoporous organosilica-based coatings and coating methods |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1335820A (en) * | 1998-12-23 | 2002-02-13 | 贝特勒纪念学院 | Mesoporous silica film from a solution containing a surfactant and methods of making same |
| CN101348385A (en) * | 2008-08-22 | 2009-01-21 | 东华大学 | Preparation of uniform nano-porous SiO2 low dielectric film |
| WO2012151688A1 (en) * | 2011-05-12 | 2012-11-15 | University Of British Columbia | Mesoporous silica and organosilica materials and process for their preparation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335820A (en) * | 1998-12-23 | 2002-02-13 | 贝特勒纪念学院 | Mesoporous silica film from a solution containing a surfactant and methods of making same |
| CN101348385A (en) * | 2008-08-22 | 2009-01-21 | 东华大学 | Preparation of uniform nano-porous SiO2 low dielectric film |
| WO2012151688A1 (en) * | 2011-05-12 | 2012-11-15 | University Of British Columbia | Mesoporous silica and organosilica materials and process for their preparation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021222551A1 (en) * | 2020-04-30 | 2021-11-04 | Tiax Llc | Hydrophobic and omniphobic periodic mesoporous organosilica-based coatings and coating methods |
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