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Title: Methods for synthesizing microporous crystals and microporous crystal membranes

Abstract

A method of making a microporous crystal material, comprising: a. forming a mixture comprising NaOH, water, and one or more of an aluminum source, a silicon source, and a phosphate source, whereupon the mixture forms a gel; b. heating the gel for a first time period, whereupon a first volume of water is removed from the gel and micoroporous crystal nuclei form, the nuclei having a framework; and c.(if a membrane is to be formed) applying the gel to a solid support seeded with microporous crystals having a framework that is the same as the framework of the nuclei; d. heating the gel for a second time period. during which a second volume of water is added to the gel; wherein the rate of addition of the second volume of water is between about 0.5 and about 2.0 fold the rate of removal of the first volume of water.

Inventors:
; ;
Publication Date:
Research Org.:
Ohio State Innovation Foundation, Columbus, OH (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1343308
Patent Number(s):
9,561,477
Application Number:
14/194,199
Assignee:
Ohio State Innovation Foundation NETL
DOE Contract Number:
FE0007632
Resource Type:
Patent
Resource Relation:
Patent File Date: 2014 Feb 28
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Dutta, Prabir, Severance, Michael, and Sun, Chenhu. Methods for synthesizing microporous crystals and microporous crystal membranes. United States: N. p., 2017. Web.
Dutta, Prabir, Severance, Michael, & Sun, Chenhu. Methods for synthesizing microporous crystals and microporous crystal membranes. United States.
Dutta, Prabir, Severance, Michael, and Sun, Chenhu. Tue . "Methods for synthesizing microporous crystals and microporous crystal membranes". United States. doi:. https://www.osti.gov/servlets/purl/1343308.
@article{osti_1343308,
title = {Methods for synthesizing microporous crystals and microporous crystal membranes},
author = {Dutta, Prabir and Severance, Michael and Sun, Chenhu},
abstractNote = {A method of making a microporous crystal material, comprising: a. forming a mixture comprising NaOH, water, and one or more of an aluminum source, a silicon source, and a phosphate source, whereupon the mixture forms a gel; b. heating the gel for a first time period, whereupon a first volume of water is removed from the gel and micoroporous crystal nuclei form, the nuclei having a framework; and c.(if a membrane is to be formed) applying the gel to a solid support seeded with microporous crystals having a framework that is the same as the framework of the nuclei; d. heating the gel for a second time period. during which a second volume of water is added to the gel; wherein the rate of addition of the second volume of water is between about 0.5 and about 2.0 fold the rate of removal of the first volume of water.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Tue Feb 07 00:00:00 EST 2017},
month = {Tue Feb 07 00:00:00 EST 2017}
}

Patent:

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  • Microporous metallic membrsnes with pores less than 0.05 mu can be produced by forming an alloy of the desired metal and a metal distinctly more unstable than the desired metal. The unstable metal is then removed by subjecting its ions to an extraction potential by either a purely chemical (selective attack) process or by an electrolytic process. (D.C.W.)
  • A method for synthesizing I-III-VI.sub.2 compounds, including: melting a Group III element; adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound; and adding a Group VI element to the single phase I-III compound under heat, with mixing, and/or via vapor transport. The Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C. Preferably, the Group I element consists of a neutron absorber and the group III element consistsmore » of In or Ga. The Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C. Preferably, the Group VI element consists of S, Se, or Te. Optionally, the method also includes doping with a Group IV element activator.« less
  • New alloys of Cu/sub x/Ag/sub (1-x)/InSe/sub 2/ (where x ranges between 0 and 1 and preferably has a value of about 0.75) and CuIn/sub y/Ga/sub (1-y)/Se/sub 2/ (where y ranges between 0 and 1 and preferably has a value of about 0.90) in the form of single crystals with enhanced structure perfection, which crystals are substantially free of fissures, are disclosed. Processes are disclosed for preparing the new alloys of Cu/sub x/Ag/sub (1-x)/InSe/sub 2/. The process includes placing stoichiometric quantities of a Cu, Ag, In, and Se reaction mixture or stoichiometric quantities of a Cu, In, Ga, and Se reactionmore » mixture in a refractory crucible in such a manner that the reaction mixture is surrounded by B/sub 2/O/sub 3/, placing the thus loaded crucible in a chamber under a high pressure atmosphere of inert gas to confine the volatile Se to the crucible, and heating the reaction mixture to its melting point. The melt can then be cooled slowly to form, by direct solidification, a single crystal with enhanced structure perfection, which crystal is substantially free of fissures.« less
  • New alloys of Cu.sub.x Ag.sub.(1-x) InSe.sub.2 (where x ranges between 0 and 1 and preferably has a value of about 0.75) and CuIn.sub.y Ga.sub.(1-y) Se.sub.2 (where y ranges between 0 and 1 and preferably has a value of about 0.90) in the form of single crystals with enhanced structure perfection, which crystals are substantially free of fissures are disclosed. Processes are disclosed for preparing the new alloys of Cu.sub.x Ag.sub.(1-x) InSe.sub.2. The process includes placing stoichiometric quantities of a Cu, Ag, In, and Se reaction mixture or stoichiometric quantities of a Cu, In, Ga, and Se reaction mixture in amore » refractory crucible in such a manner that the reaction mixture is surrounded by B.sub.2 O.sub.3, placing the thus loaded crucible in a chamber under a high pressure atmosphere of inert gas to confine the volatile Se to the crucible, and heating the reaction mixture to its melting point. The melt can then be cooled slowly to form, by direct solidification, a single crystal with enhanced structure perfection, which crystal is substantially free of fissures.« less
  • This patent describes Quaternary IB-IIIA-Se/sub 2/ alloys of high-quality, single crystal chalcopyrite structure having large single crystal grains greater than about 5mm and free of cracks and voids of the size which interfere with good optical absorption coefficients and high band-gap energies. The alloy structure are selected from the group consisting of Cu/sub chi/Ag/sub (l-chi)/InSe/sub 2/ and CuIn/sub y/Ga/sub (l-y)/Se/sub 2/, where chi is in the range of about 0.65 to 0.8, and where y is in the range of about 0.85 to .095, produced by the process comprising the steps of: placing in a refractory container a reaction mixturemore » of Cu, Ag, In, and Se, or a reaction mixture of Cu, In, Ga, and Se, where such reaction mixture is calculated by atomic percent to produce and desired alloy; placing B/sub 2/O/sub 3/ in the container in a quantity sufficient for the B/sub 2/O/sub 3/ to completely cover and encapsulate the reaction mixture when the B/sub 2/O/sub 3/ is melted; placing the container and its the reaction mixture and B/sub 2/O/sub 3/ contents in an enclosed chamber; creating an environment of pressurized inert or nonreactive gas in the enclosed chamber and over the container and its contents; while containing the environment of pressurized gas, heating the container and its the contents to a temperature to at least completely melt the contents of the container, and holding such temperature for a sufficient period of time to equilibrate the melt and synthesize and alloy; and then lowering the temperature of the melt in a controlled manner to solidify it as a quaternary IB-IIIA-Se/sub 2/ alloy of high-quality, single-crystal chalcopyrite structure.« less