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US6329017B1 Expired / Lapsed US ⏱️ 0.0 years remaining

Mesoporous silica film from a solution containing a surfactant and methods of making same

Assignee: Battelle Memorial Institute Inc
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Filing: 1999-10-04
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Granted: 2001-12-11
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Expires: 2019-10-04
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Abstract

Abstract The present invention is a mesoporous silica film having a low dielectric constant and method of making having the steps of combining a surfactant in a silica precursor solution, spin-coating a film from this solution mixture, forming a partially hydroxylated mesoporous film, and dehydroxylating the hydroxylated film to obtain the mesoporous film. It is advantageous that the small polyoxyethylene ether surfactants used in spin-coated films as described in the present invention will result in fine pores smaller on average than about 20 nm. The resulting mesoporous film has a dielectric constant less than 3, which is stable in moist air with a specific humidity. The present invention provides a method for superior control of film thickness and thickness uniformity over a coated wafer, and films with low dielectric constant.

Inventors

  • 👤 Jun Liu
  • 👤 Karel Domansky
  • 👤 Xiaohong Li
  • 👤 Glen E. Fryxell
  • 👤 Suresh Baskaran
  • 👤 Nathan J. Kohler
  • 👤 Suntharampillai Thevuthasan
  • 👤 Christopher A. Coyle
  • 👤 Jerome C. Birnbaum

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 15:48
CPC Classifications
H; H10; H10P; H10P14/00; H10P14/60; H10P14/66; H10P14/665; C; C01; C01B; C01B37/00; C01B37/02; H10P14/65; H10P14/6516; H10P14/6529; H10P14/668; H10P14/6681; H10P14/6687; H10P14/6689; H10P14/69; H10P14/692; H10P14/6921; H10P14/69215; H10P14/63; H10P14/6326; H10P14/6342; H10P14/6684; H10P14/6686; H10P14/6922; Y; Y10; Y10T; Y10T428/00; Y10T428/249921; Y10T428/249953; Y10T428/249967; Y10T428/249969; Y10T428/249971; Y10T428/249972

Claims Analysis

Total Claims: 79
Claim 1
Independent Claim 100 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film, said mesoporous film having a porosity that is disordered, said disorder being characterized by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 2
Independent Claim 100 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film, said mesoporous film having a porosity that is disordered, said disorder being characterized by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 3
Dependent Claim 16 words
The method as recited in claim 1 , wherein said surfactant is a polyoxyethylene ether surfactant.
Claim 4
Dependent Claim 127 words
The method as recited in claim 2 , wherein said polyoxyethylene ether surfactant is C 12 H 25 (CH 2 CH 2 O) 10 OH also known as C 12 EO 10 or 10 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 10 OH also known as C 16 EO 10 or 10 cetyl ether; C 18 H 37 (CH 2 CH 2 O) 10 OH also known as C 18 EO 10 or 10 stearyl ether, C 12 H 25 (CH 2 CH 2 O) 4 OH also known as C 12 EO 4 or 4 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 2 OH also known as C 16 EO 2 or 2 cetyl ether or combinations thereof.
Claim 5
Dependent Claim 47 words
The method as recited in claim 1 , wherein said surfactant is in combination with organic co-solvents and with a chemical agent selected from the group consisting of a second surfactant, smaller hydrophilic molecular compounds characterized by molecular weights of less than or equal to approximately 1150.
Claim 6
Dependent Claim 30 words
The method as recited in claim 4 , wherein said second surfactant is selected from the group consisting of non-ionic surfactant, catonic surfactant, anionic surfactant, amphoteric surfactant and combinations thereof.
Claim 7
Dependent Claim 16 words
The method as recited in claim 5 , wherein said cationic surfactant is an ammonium-based surfactant.
Claim 8
Dependent Claim 27 words
The method as recited in claim 4 , wherein said smaller hydrophilic molecular compounds are selected from the group consisting of glycerol, propylene glycol, and ethylene glycol.
Claim 9
Dependent Claim 24 words
The method as recited in claim 4 , wherein said organic co-solvents are selected from the group consisting of mesitylene, octane and combinations thereof.
Claim 10
Dependent Claim 38 words
The method as recited in claim 1 , wherein said silica precursor is selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), methyl triethoxysilane, phenyl triethoxy silane, dimethyl dimethoxy silane, ethyl triethyoxysilane, and combinations thereof.
Claim 11
Dependent Claim 16 words
The method as recited in claim 1 , wherein said aqueous solvent comprises ethanol and water.
Claim 12
Dependent Claim 25 words
The method as recited in claim 1 , wherein said catalyst is selected from the group consisting of inorganic acid, organic acid and combinations thereof.
Claim 13
Dependent Claim 18 words
The method as recited in claim 1 , wherein said precursor solution includes at least one other surfactant.
Claim 14
Dependent Claim 33 words
The method as recited in claim 12 , wherein said at least one other surfactant is selected from the group consisting of non-ionic surfactant, cationic surfactant, anionic surfactant, amphoteric surfactant and combinations thereof.
Claim 15
Dependent Claim 23 words
The method as recited in claim 1 , wherein dehydroxylating occurs in the presence of a silicon-based organic compound in the vapor phase.
Claim 16
Dependent Claim 16 words
The method as recited in claim 14 , wherein the silicon-based organic compound is a silane.
Claim 17
Dependent Claim 36 words
The method as recited in claim 15 , wherein the silane is selected from the group consisting of trimethyl iodosilane, trimethyl chlorosilane, dimethyl dimethoxy silane, demethyl dichloro silane, hexaphenyl disilazane, diphenyl tetramethyl silazane and hexamethyl disilazane.
Claim 18
Independent Claim 97 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution, wherein said precursor solution includes at least one smaller hydrophilic molecular compound characterized by a molecular weight that is less than that of said surfactant; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film and forming a hydroxylated film with disordered porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film.
Claim 19
Independent Claim 97 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution, wherein said precursor solution includes at least one smaller hydrophilic molecular compound characterized by a molecular weight that is less than that of said surfactant; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film and forming a hydroxylated film with disordered porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film.
Claim 20
Dependent Claim 32 words
The method as recited in claim 17 , wherein said at least one smaller hydrophilic molecular compound is selected from the group consisting of glycerol, propylene glycol, ethylene glycol and combinations thereof.
Claim 21
Independent Claim 82 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution, wherein said precursor solution includes at least one organic co-solvent; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant from said templated film and forming a hydroxylated film with disordered porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film.
Claim 22
Independent Claim 82 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution, wherein said precursor solution includes at least one organic co-solvent; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant from said templated film and forming a hydroxylated film with disordered porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film.
Claim 23
Dependent Claim 27 words
The method as recited in claim 19 , wherein said at least one organic co-solvent is selected from the group consisting of mesitylene, octane and combinations thereof.
Claim 24
Independent Claim 106 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant to form a hydroxylated mesoporous film characterized by a porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film.
Claim 25
Independent Claim 106 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant to form a hydroxylated mesoporous film characterized by a porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film.
Claim 26
Dependent Claim 127 words
The method as recited in claim 21 , wherein said polyoxyethylene ether surfactant is C 12 H 25 (CH 2 CH 2 O) 10 OH also known as C 12 EO 10 or 10 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 10 OH also known as C 16 EO 10 or 10 cetyl ether; C 18 H 37 (CH 2 CH 2 O) 10 OH also known as C 18 EO 10 or 10 stearyl etler; C 12 H 25 (CH 2 CH 2 O) 4 OH also known as C 12 EO 4 or 4 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 2 OH also known as C 16 EO 2 or 2 cetyl ether or combinations thereof.
Claim 27
Dependent Claim 18 words
The method as recited in claim 21 , wherein said precursor solution includes at least one other surfactant.
Claim 28
Dependent Claim 48 words
The method as recited in claim 21 , wherein said precursor solution includes an agent selected from the group consisting of a second surfactant, a smaller hydrophilic molecular compound characterized by a molecular weight of less than or equal to approximately 1150, an organic co-solvent and combinations thereof.
Claim 29
Dependent Claim 33 words
The method as recited in claim 23 , wherein said at least one other surfactant is selected from the group consisting of non-ionic surfactant, cationic surfactant, anionic surfactant, amphoteric surfactant and combinations thereof.
Claim 30
Dependent Claim 30 words
The method as recited in claim 24 , wherein said second surfactant is selected from the group consisting of non-ionic surfactant, cationic surfactant, anionic surfactant, amphoteric surfactant and combinations thereof.
Claim 31
Dependent Claim 29 words
The method as recited in claim 24 , wherein said smaller hydrophilic molecular compound is selected from the group consisting of glycerol, propylene glycol, ethylene glycol and combinations thereof.
Claim 32
Dependent Claim 24 words
The method as recited in claim 24 , wherein said organic co-solvent is selected from the group consisting of mesitylene, octane and combinations thereof.
Claim 33
Dependent Claim 34 words
The method as recited in claim 21 wherein said silica precursor is selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate, methyl triethoxysilane, phenyl triethoxy silane, dimethyl dimethoxy silane and combinations thereof.
Claim 34
Dependent Claim 13 words
The method as recited in claim 21 wherein said aqueous solvent includes ethanol.
Claim 35
Dependent Claim 25 words
The method as recited in claim 21 , wherein said catalyst is selected from the group consisting of inorganic acid, organic acid and combinations thereof.
Claim 36
Dependent Claim 23 words
The method as recited in claim 21 , wherein dehydroxylating occurs in the presence of a silicon-based organic compound in the vapor phase.
Claim 37
Dependent Claim 16 words
The method as recited in claim 32 , wherein the silicon-based organic compound is a silane.
Claim 38
Dependent Claim 33 words
The method as recited in claim 33 , wherein the silane is selected from the group consisting of trimethyl iodosilane, trimethyl chlorosilane, dimethyl dichloro silane, hexaphenyl disilazane, diphenyl tetramethyl silazane and hexamethyl disilazane.
Claim 39
Independent Claim 104 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 40
Independent Claim 104 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 41
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor wit) an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered, lacking a regular geometric arrangement of pores, and the pore structure is characterized by a major x-ray diffraction peak between about 0.75 and about 2 degrees 2-theta.
Claim 42
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor wit) an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered, lacking a regular geometric arrangement of pores, and the pore structure is characterized by a major x-ray diffraction peak between about 0.75 and about 2 degrees 2-theta.
Claim 43
Independent Claim 104 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said precursor solution includes at least one smaller hydrophilic molecular compound characterized by a molecular weight that is less than that of said surfactant.
Claim 44
Independent Claim 104 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said precursor solution includes at least one smaller hydrophilic molecular compound characterized by a molecular weight that is less than that of said surfactant.
Claim 45
Dependent Claim 32 words
The method as recited in claim 37 , wherein said at least one smaller hydrophilic molecular compound is selected from the group consisting of glycerol, propylene glycol, ethylene glycol and combinations thereof.
Claim 46
Independent Claim 89 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said precursor solution includes at least one organic co-solvent.
Claim 47
Independent Claim 89 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said precursor solution includes at least one organic co-solvent.
Claim 48
Dependent Claim 27 words
The method as recited in claim 39 , wherein said at least one organic co-solvent is selected from the group consisting of mesitylene, octane and combinations thereof.
Claim 49
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said catalyst is a carboxylic acid selected from the group consisting of methanoic acid (formic acid), ethanoic acid (acetic acid), ethandioic acid (oxalic acid), butanoic acid (butyric acid), and combinations thereof.
Claim 50
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant that is a polyoxethylene ether surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant forming a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said catalyst is a carboxylic acid selected from the group consisting of methanoic acid (formic acid), ethanoic acid (acetic acid), ethandioic acid (oxalic acid), butanoic acid (butyric acid), and combinations thereof.
Claim 51
Independent Claim 93 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, an acid and a polyoxethylene other surfactant into a precursor solution; (b) spincoating said precursor solution into a templated film; (c) removing said aqueous solvent, said acid and said surfactant to form a hydroxylated film characterized by a porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film.
Claim 52
Independent Claim 93 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, an acid and a polyoxethylene other surfactant into a precursor solution; (b) spincoating said precursor solution into a templated film; (c) removing said aqueous solvent, said acid and said surfactant to form a hydroxylated film characterized by a porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film to obtain said mesoporous film.
Claim 53
Dependent Claim 127 words
The method as recited in claim 42 , wherein said polyoxyethylene ether surfactant is C 12 H 25 (CH 2 CH 2 O) 10 OH also known as C 12 EO 10 or 10 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 10 OH also known as C 16 EO 10 or 10 cetyl ether; C 18 H 37 (CH 2 CH 2 O) 10 OH also known as C 18 EO 10 or 10 stearyl ether, C 12 H 25 (CH 2 CH 2 O) 4 OH also known as C 12 EO 4 or 4 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 2 OH also known as C 16 EO 2 or 2 cetyl ether or combinations thereof.
Claim 54
Dependent Claim 16 words
The method as recited in claim 42 , wherein said silica precursor is tetraethyl orthosilicate (TEOS).
Claim 55
Dependent Claim 16 words
The method as recited in claim 42 , wherein said aqueous solvent comprises ethanol and water.
Claim 56
Dependent Claim 14 words
The method as recited in claim 42 , wherein said acid is hydrochloric acid.
Claim 57
Independent Claim 227 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, an acid and a polyoxethylene ether surfactant into a precursor solution; (b) spin-coating said precursor solution into a templated film; (c) removing said aqueous solvent, said acid and said surfactant forming a hydroxylated film; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said polyoxyethylene ether surfactant is C 12 H 25 (CH 2 CH 2 O) 10 OH also known as C 12 EO 10 or 10 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 10 OH also known as C 16 EO 10 or 10 cetyl ether; C 18 H 37 (CH 2 CH 2 O) 10 OH also known as C 18 EO 10 or 10 stearyl ether; C 12 H 25 (CH 2 CH 2 O) 4 OH also known as C 12 EO 4 or 4 lauryl ether; C 16 CH 33 (CH 2 CH 2 O) 2 OH also known as C 16 EO 2 or 2 cetyl ether or combinations thereof and wherein said polyoxyethylene ether surfactant is in combination with at least one other surfactant at least one hydrophilic molecular compound characterized by a molecular weight that is less than that of said polyoxyethylene ether surfactant, and with at least one organic solvent.
Claim 58
Independent Claim 227 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, an acid and a polyoxethylene ether surfactant into a precursor solution; (b) spin-coating said precursor solution into a templated film; (c) removing said aqueous solvent, said acid and said surfactant forming a hydroxylated film; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said polyoxyethylene ether surfactant is C 12 H 25 (CH 2 CH 2 O) 10 OH also known as C 12 EO 10 or 10 lauryl ether; C 16 H 33 (CH 2 CH 2 O) 10 OH also known as C 16 EO 10 or 10 cetyl ether; C 18 H 37 (CH 2 CH 2 O) 10 OH also known as C 18 EO 10 or 10 stearyl ether; C 12 H 25 (CH 2 CH 2 O) 4 OH also known as C 12 EO 4 or 4 lauryl ether; C 16 CH 33 (CH 2 CH 2 O) 2 OH also known as C 16 EO 2 or 2 cetyl ether or combinations thereof and wherein said polyoxyethylene ether surfactant is in combination with at least one other surfactant at least one hydrophilic molecular compound characterized by a molecular weight that is less than that of said polyoxyethylene ether surfactant, and with at least one organic solvent.
Claim 59
Dependent Claim 15 words
The method as recited in claim 47 , wherein said small surfactants are ammonium-based surfactants.
Claim 60
Dependent Claim 17 words
The method as recited in claim 48 , wherein said ammonium-based surfactants are cetyl trimethyl ammonium chloride.
Claim 61
Dependent Claim 26 words
The method as recited in claim 47 , wherein said smaller hydrophilic molecules are selected from the group consisting of glycerol, propylene glycol, and ethylene glycol.
Claim 62
Dependent Claim 22 words
The method as recited in claim 47 , wherein said organic co-solvents are selected from the group consisting of mesitylene and octane.
Claim 63
Independent Claim 101 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film characterized by porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film with a gaseous silicon-based organic compound to obtain said mesoporous film.
Claim 64
Independent Claim 101 words
A method of making a mesoporous film comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) spin coating said precursor solution into a templated film; (c) removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film characterized by porosity that is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta; and (d) dehydroxylating said hydroxylated film with a gaseous silicon-based organic compound to obtain said mesoporous film.
Claim 65
Dependent Claim 14 words
The method of claim 52 , wherein the silicon-based organic compound is a silane.
Claim 66
Dependent Claim 34 words
The method of claim 52 , wherein said silane is selected from the group consisting of trimethyl iodosilane, trimethyl chlorosilane, dimethyl dimethoxy silane, dimethyl dichloro silane, hexaphenyl disilazane, diphenyl tetramethyl silazane and hexamethyl disilazane.
Claim 67
Independent Claim 96 words
A method of making a mesoporous film comprising the steps of: (e) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (f) spin coating said precursor solution into a templated film; (g) removing said aqueous solvent, said catalyst and said surfactant from said templated film and forming a hydroxylated film; and (h) dehydroxylating said hydroxylated film with a gaseous silicon-based organic compound and obtaining said mesoporous film, wherein said dehydroxylation of said film occurs in alternating exposures of said film to a vacuum and to the gaseous silane.
Claim 68
Independent Claim 96 words
A method of making a mesoporous film comprising the steps of: (e) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (f) spin coating said precursor solution into a templated film; (g) removing said aqueous solvent, said catalyst and said surfactant from said templated film and forming a hydroxylated film; and (h) dehydroxylating said hydroxylated film with a gaseous silicon-based organic compound and obtaining said mesoporous film, wherein said dehydroxylation of said film occurs in alternating exposures of said film to a vacuum and to the gaseous silane.
Claim 69
Independent Claim 107 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto said substrate to form a templated film; (c) substantially removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 70
Independent Claim 107 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto said substrate to form a templated film; (c) substantially removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 71
Dependent Claim 12 words
The method of claim 56 , wherein said dispensing involves spin coating.
Claim 72
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto a substrate for form a templated film; (c) substantially removing said aqueous solvent, said catalyst and said surfactant to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, said film being characterized by disordered porosity and said film having a thickness of between approximately 0.1 micron and approximately 1.5 microns, said thickness having a standard deviation of less than approximately +/−5%.
Claim 73
Independent Claim 111 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto a substrate for form a templated film; (c) substantially removing said aqueous solvent, said catalyst and said surfactant to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, said film being characterized by disordered porosity and said film having a thickness of between approximately 0.1 micron and approximately 1.5 microns, said thickness having a standard deviation of less than approximately +/−5%.
Claim 74
Dependent Claim 12 words
The method of claim 58 , wherein said dispensing involves spin coating.
Claim 75
Independent Claim 116 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto a substrate to form a templated film; (c) heating said templated film, said dispensing and said heating collectively substantially removing said aqueous solvent, said catalyst and said surfactant from said templated firm to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, said film being characterized by disordered porosity and said film being of substantially uniform thickness having a standard deviation of less than approximately +/−5%.
Claim 76
Independent Claim 116 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto a substrate to form a templated film; (c) heating said templated film, said dispensing and said heating collectively substantially removing said aqueous solvent, said catalyst and said surfactant from said templated firm to form a hydroxylated film having porosity; and (d) dehydroxylating said hydroxylated film and obtaining said mesoporous film, said film being characterized by disordered porosity and said film being of substantially uniform thickness having a standard deviation of less than approximately +/−5%.
Claim 77
Dependent Claim 12 words
The method of claim 60 , wherein said dispensing involves spin coating.
Claim 78
Independent Claim 97 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto said substrate to form a templated film; and (c) substantially removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a mesoporous film having porosity; wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.
Claim 79
Independent Claim 97 words
A method of making a mesoporous film with a surfactant containing solution, the method comprising the steps of: (a) combining a silica precursor with an aqueous solvent, a catalyst and a surfactant into a precursor solution; (b) dispensing said precursor solution onto said substrate to form a templated film; and (c) substantially removing said aqueous solvent, said catalyst and said surfactant from said templated film to form a mesoporous film having porosity; wherein said porosity is disordered as indicated by an absence of a major x-ray diffraction peak in the range of 2 to 6 degrees 2-theta.

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