Block copolymer processing for mesostructured inorganic oxide materials
AssigneeThe Regents of the University of California
InventorsGalen D. Stucky, Bradley F. Chmelka, Dongyuan Zhao, Nick Melosh, Qisheng Huo, Jianglin Feng, Peidong Yang, David Pine, David Margolese, Wayne Lukens, Jr., Glenn H. Fredrickson, Patrick Schmidt-Winkel
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Abstract
Mesoscopically ordered, hydrothermally stable metal oxide-block copolymer composite or mesoporous materials are described herein that are formed by using amphiphilic block copolymers which act as structure directing agents for the metal oxide in a self-assembling system.
Claims167
A method of forming a mesoscopically structure material, comprising the steps of:
- combining an amphiphilic block copolymer that functions a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured inorganic-organic composite.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining an amphiphilic block polymer with an inorganic compound of a multivalent metal species under conditions whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized into a mesoscopically structured composite;
- and
- calcining or solvent extracting said mesoscopically structured inorganic oxide-block copolymer composite material to remove the organic species and thereby form the mesoscopically structured inorganic material in the form of fibers with a high surface area.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining an amphiphilic reversed triblock copolymer with an inorganic compound of a multivalent metal species under conditions whereby the reversed triblock copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured composite.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining an amphiphilic star di-block copolymer with an inorganic compound of a multivalent metal species under conditions whereby the star di-block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized into a mesoscopically structured composite.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining an amphiphilic reversed star di-block copolymer with an inorganic compound of a multivalent metal species under conditions whereby the reversed star di-block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized into a mesoscopically structured composite.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining an amphiphilic self-assembling block copolymer that functions as a structure-directing agent with an aqueous soluble metalate precursor species, where the metalate precursor species partition within hydrophilic regions of a self-assembling block copolymer system;
- and
- polymerizing the metalate precursor species under acidic conditions to form a mesoscopically structured inorganic-organic composite.
A method of imparting adsorption and catalytic reaction selectivities to a macroporous multivalent metal oxide material having an ordered mesoporous surface area, comprising functionalizing separately the different mesoscopic and macroscopic pore surfaces of said material of to provide said selectivities.
A method of synthesizing a mesoscopically structured inorganic-organic composite, comprising the step of:
- combining an amphiphilic poly(alkylene oxide) block copolymer having hydrophilic and hydrophobic components that function as structure-directing moieties with an inorganic compound of a multivalent metal species that can form complexes through coordination bonds with alkylene oxide segments of the block copolymer such that the complexes then self-assemble according to mesoscopic ordering directed principally by microphase separation of the block copolymer and polymerize under acidic conditions to form the mesoscopically structured inorganic-organic composite.
A method of forming a three-dimensional meso-macro structured material, comprising the steps of:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation of inorganic compounds and the block copolymer, thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic-block copolymer composite and the aqueous solution of inorganic salt;
- polymerizing the inorganic compounds to form a meso-macro- structured inorganic-organic composite;
- and
- removing the block copolymer from said meso-macro structured inorganic-organic composite to form said meso-macro structured material.
A method of forming a mesoscopically structured material, comprising the steps of:
- combining in a polar solvent an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized under non-aqueous conditions to form a mesoscopically structured inorganic-organic composite.
A mesoscopically ordered porous material comprised of a multivalent metal compound and having a narrow distribution of pore sizes in the mesoscopic size regime that was formed by the following steps:
- combining an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured inorganic-organic composite;
- and
- removing the block copolymer from the mesoscopically structured inorganic-organic composite to form said mesoscopically ordered porous material.
A transparent mesoscopically structured composite in the form of fibers of an amphiphilic block-copolymer and compound of a multivalent metal species.
A thermally stable mesoscopically ordered porous material in the form of fibers comprised of a multivalent metal compound and having a narrow distribution of pore sizes in the mesoscopic size regime.
A macroporous multivalent metal oxide material having ordered mesopores that was formed by the following steps:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with a sol gel containing an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation of inorganic compounds in the sol gel and the block copolymer, thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic-block copolymer composite and the aqueous solution of inorganic salt;
- polymerizing the inorganic compounds to form a meso-macro structured inorganic-organic composite;
- and
- removing the block copolymer and inorganic salt from the meso-macro structured inorganic-organic composite to form said macroporous multivalent metal oxide material with ordered mesopores.
A mesoscopically structured material that was formed by the following steps:
- combining an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured inorganic-organic composite.
A mesoscopically structured material that was formed by the following steps:
- combining an amphiphilic self-assembling block copolymer that functions as a structure-directing agent with an aqueous soluble metalate precursor species, where the metalate precursor species partition within hydrophilic regions of a self-assembling block copolymer system;
- and
- polymerizing the metalate precursor species under acidic conditions to form a mesoscopically structured inorganic-organic composite.
A mesoscopically structured inorganic-organic composite that was formed by the following step:
- combining an amphiphilic poly(alkylene oxide) block copolymer having hydrophilic and hydrophobic components that function as structure-directing moieties with an inorganic compound of a multivalent metal species that can form complexes through coordination bonds with alkylene oxide segments of the block copolymer such that the complexes then self-assemble according to mesoscopic ordering directed principally by microphase separation of the block copolymer and polymerize under acidic conditions to form the mesoscopically structured inorganic-organic composite.
A three-dimensional meso-macro structured inorganic-organic composite that was formed by:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with a sol gel containing an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation inorganic compounds in the sol gel and the block copolymer, thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic compound and the inorganic salt;
- polymerizing the inorganic compounds to form said meso-macro structured inorganic-organic composite;
- and
- removing the block copolymer from said meso-macro structured inorganic-organic composite to form said meso-macro structured material.
A mesoscopically structured material that was formed by combining in a polar solvent an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized under non-aqueous conditions to form a mesoscopically structured inorganic-organic composite.
A method of separating biomolecules from a biological specimen or synthesis mixture, comprising contacting said biological specimen or synthesis mixture with a mesoporous multivalent metal oxide material that was formed by the following steps:
- combining an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured composite;
- and
- removing the block copolymer from the mesoscopically structured composite to form said mesoporous multivalent metal oxide material.
A method of separating biomolecules from a biological specimen or synthesis mixture, comprising contacting said biological specimen or synthesis mixture with a macroporous multivalent metal oxide material having a mesoporous surface area that was formed by the following steps:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with a sol gel containing an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation of inorganic compounds in the sol gel and the block copolymer thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic-block copolymer composite and the aqueous solution of inorganic salt;
- polymerizing the inorganic compounds to form a meso-macro structured composite;
- and
- removing the block copolymer and inorganic salt from the meso-macro structured composite to form said macroporous multivalent metal oxide material that has the mesoporous surface area.
A method of separating organics from a solution, comprising contacting said solution with a mesoporous multivalent metal oxide material that was formed by the following steps:
- combining an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured composite;
- and
- removing the block copolymer from the mesoscopically structured composite to form said mesoporous multivalent metal oxide material.
A method of separating organics from a solution, comprising contacting said solution with a macroporous multivalent metal oxide material having a mesoporous surface area that was formed by the following steps:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with a sol gel containing an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation of inorganic compounds in the sol gel and the block copolymer, thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic-block copolymer phase and the aqueous solution of the inorganic salt;
- polymerizing the inorganic compounds to form a meso-macro structured composite;
- and
- removing the block copolymer and inorganic salt from the meso-macro structured composite to form said macroporous multivalent metal oxide material that has the mesoporous surface.
A method of separating inorganics from a solution, comprising contacting said solution with a mesoporous multivalent metal oxide material that was formed by the following steps:
- combining an amphiphilic block copolymer that functions as a structure-directing agent with an inorganic compound of a multivalent metal species whereby the block copolymer and inorganic compounds are self-assembled and the inorganic compounds are polymerized to form a mesoscopically structured composite;
- and
- removing the block copolymer from the mesoscopically structured composite to form said mesoporous multivalent metal oxide material.
A method of separating inorganics from a solution, comprising contacting said solution with a macroporous multivalent metal oxide material having a mesoporous surface area that was formed by the following steps:
- placing an amphiphilic block copolymer in an aqueous solution of inorganic salt;
- combining the aqueous solution containing the block copolymer with a sol gel containing an inorganic compound of a multivalent metal species to form a multiphase medium that enables microphase separation of inorganic compounds in the sol gel and the block copolymer, thereby forming an inorganic-block copolymer composite wherein the block copolymer functions as a structure-directing agent, and also enables macrophase separation of the inorganic-block copolymer composite and the aqueous solution of inorganic salt;
- polymerizing the inorganic compounds to form a meso-macro structured composite;
- and
- removing the block copolymer and inorganic salt from the meso-macro structured composite to form said macroporous multivalent metal oxide material that has the mesoporous surface area.
Dependencies are inferred from the claim text.