US5460701A — Method of making nanostructured materials

Claim 1

Independent Claim 253 words

A method of synthesizing nanocrystalline material, comprising the steps of: providing a chamber for holding means for generating a nanocrystalline aerosol selected from the group consisting of a metal, a semiconductor and a ceramic; further providing a nonconsumable cathode having a longitudinal axis and shielded against chemical reaction by a working gas flow which also creates an elongated ionized arc, said working gas flow consisting essentially of a non-oxidizing gas including at least one of hydrogen gas and nitrogen gas and further including an inert gas; further providing in the chamber a consumable anode inclined at an angle relative to the longitudinal axis of said cathode for providing material vaporizable from said anode by said elongated ionized arc; providing first means for injecting a gas into the chamber; using said first means to inject at least one of a quench and a reaction gas within the boundaries of said elongated ionized arc and causing truncation of said arc at a point of injection, thereby establishing an arc truncation point; maintaining said arc between said cathode and anode by injecting the working gas and at least one of the quench and reaction gas into the chamber, and forming the nanocrystalline aerosol containing nanocrystals; providing second means for injecting a gas into the chamber; using said second means to inject a cooling gas stream into the nanocrystalline aerosol at a point downstream beyond said arc truncation point to prevent further substantial agglomeration of the nanocrystals; and cooling the nanocrystalline aerosol to form the nanocrystalline material.

Claim 2

Independent Claim 253 words

A method of synthesizing nanocrystalline material, comprising the steps of: providing a chamber for holding means for generating a nanocrystalline aerosol selected from the group consisting of a metal, a semiconductor and a ceramic; further providing a nonconsumable cathode having a longitudinal axis and shielded against chemical reaction by a working gas flow which also creates an elongated ionized arc, said working gas flow consisting essentially of a non-oxidizing gas including at least one of hydrogen gas and nitrogen gas and further including an inert gas; further providing in the chamber a consumable anode inclined at an angle relative to the longitudinal axis of said cathode for providing material vaporizable from said anode by said elongated ionized arc; providing first means for injecting a gas into the chamber; using said first means to inject at least one of a quench and a reaction gas within the boundaries of said elongated ionized arc and causing truncation of said arc at a point of injection, thereby establishing an arc truncation point; maintaining said arc between said cathode and anode by injecting the working gas and at least one of the quench and reaction gas into the chamber, and forming the nanocrystalline aerosol containing nanocrystals; providing second means for injecting a gas into the chamber; using said second means to inject a cooling gas stream into the nanocrystalline aerosol at a point downstream beyond said arc truncation point to prevent further substantial agglomeration of the nanocrystals; and cooling the nanocrystalline aerosol to form the nanocrystalline material.

Claim 3

Dependent Claim 63 words

The method as defined in claim 1 wherein said consumable anode is selected from the group consisting of chromium, aluminum, zirconium, yttrium, silicon, titanium and iron, and the nanocrystalline material resulting from the method is selected from the group consisting of stoichiometric silicon compounds of said reaction gas, stoichiometric titanium compounds of said reaction gas, and stoichiometric iron compounds of said reaction gas.

Claim 4

Dependent Claim 16 words

The method as defined in claim 2 wherein said reaction gas comprises art oxygen containing gas.

Claim 5

Dependent Claim 16 words

The method as defined in claim 2 wherein said reaction gas comprises a nitrogen containing gas.

Claim 6

Dependent Claim 89 words

The method as defined in claim 1 wherein a reaction zone having a first characteristic reaction zone color is formed near the intersection of the longitudinal axes of said anode and cathode with a first ionized arc disposed adjacent said cathode having a second characteristic color and said arc near said anode having a third characteristic color, said method of synthesizing nanocrystalline material being optimized for rate of production by generating a maximum color separation among the first, second and third characteristic colors formed during performance of the method.

Claim 7

Dependent Claim 49 words

The method as defined in claim 5 wherein the nanocrystalline material being formed consists essentially of an iron oxide and said reaction zone has a characteristic yellow color, said are near said cathode has a characteristic red color, and said are near said anode has a characteristic green color.

Claim 8

Dependent Claim 36 words

The method as defined in claim 1 wherein the nanocrystalline material has a grain size distribution of average size of about 8 nanometers and 18 nanometers for ZrO 2 and Al 2 O 3 , respectively.

Claim 9

Dependent Claim 76 words

The method as defined in claim 1 further including the step of forming consolidated material from the nanocrystalline material and wherein the consolidated material includes pores disposed between solid nanocrystalline grains and the pores have a characteristic pore size distribution associated with the consolidated material with said pore size distribution having an average diameter less than about 20 nanometers and the nanocrystalline grains having a size distribution with an average diameter less than about 50 nanometers.

Claim 10

Dependent Claim 55 words

The method as defined in claim 1 wherein at least one of flow rate of said working gas is controlled, flow rate of said quench and/or reaction gas is controlled and the location relative to the anode of the point of quench/reaction gas injection is controlled to vary the particle diameter of said nanocrystalline material.

Claim 11

Dependent Claim 63 words

The method as defined in claim 1 further including the steps of: providing a cyclone for turbulent mixing to prevent agglomeration of said nanocrystalline aerosol produced in said reaction zone; expanding the cyclonically mixed nanocrystalline material into a large volume chamber to cool the nanocrystalline material; and passing the cooled nanocrystalline material through filter media to separate the nanocrystalline material from the gas.

Claim 12

Independent Claim 28 words

The method as defined in claim I wherein said working gas flow comprises an inert gas selected from the group consisting of He, Ar, Ne, Kr and Xe.

Claim 13

Dependent Claim 28 words

The method as defined in claim 11 wherein said working gas flow further includes a dissociable gas selected from the group consisting of nitrogen, hydrogen and mixtures thereof,

Claim 14

Dependent Claim 25 words

The method as defined in claim 12 wherein the dissociable gas consists essentially of 5-50% by volume hydrogen gas added to the working gas flow.

Claim 15

Dependent Claim 36 words

The method as defined in claim 1 wherein said at least one of the quench and the reaction gas is injected using a concentric gas injection geometry to allow homogeneous injection into said elongated ionized arc.

Claim 16

Dependent Claim 25 words

The method as defined in claim 1 wherein said quench and/or reaction gas comprises at least one of oxygen, nitrogen, helium, air and mixtures thereof.

Claim 17

Dependent Claim 28 words

The method as defined in claim 1 wherein the nanocrystalline material produced is further dispersed into an aqueous solution, the nanocrystalline material having aggregate sizes of 1-50 nm.

Claim 18

Dependent Claim 30 words

The method as defined in claim 1 wherein the synthesizing steps produce the nanocrystalline material with an efficiency of at least 35 kilowatt hours per kilogram of the nanocrystalline material.

Claim 19

Dependent Claim 45 words

The method as defined in claim 1 wherein said reaction gas comprises oxygen and said nanocrystalline material is selected from the group consisting of TiO 2 , ZrO 2 , SiO 2 , Si 3 N 4 , SiC, and Y 2 O 3 .

Claim 20

Dependent Claim 27 words

The method as defined in claim 1 wherein said reaction gas comprises oxygen gas and said nanocrystalline material consists essentially of stoichiometric Al 2 O 3 .

Claim 21

Dependent Claim 26 words

The method as defined in claim 1 wherein said reaction gas comprises oxygen gas and said nanocrystalline material consists essentially of Fe 2 O 3 .

Claim 22

Independent Claim 282 words

A method of synthesizing a controlled particle size range of a nanocrystalline material, comprising the steps of: providing a chamber for holding means for generating a nanocrystalline aerosol selected from the group consisting of a metal, a semiconductor and a ceramic; further providing a nonconsumable cathode having a longitudinal axis and shielded against chemical reaction by a working gas flow which also creates an elongated ionized arc, said working gas flow consisting essentially of a non-oxidizing gas including at least one of hydrogen gas and nitrogen gas and further including an inert gas; further providing in the Chamber a consumable anode inclined at an angle relative to the longitudinal axis of said cathode for providing material vaporizable from said anode by said elongated ionized arc; providing first means for injecting into the chamber at least one of a quench gas and a reaction gas within the boundaries of said elongated ionized arc and using said first means to inject at least one of the quench gas and the reaction gas into said arc at a point, thereby causing truncation of said arc at the point of injection into the arc; using said first means for controlling gas flow rate to change the flow rate of at least one of said quench gas and said reaction gas to control and change the particle size range of the nanocrystalline material to be synthesized; maintaining said arc between said cathode and anode by injecting the working gas and the at least one of quench and reaction gas with a controlled gas flow rate into the chamber to form the nanocrystalline aerosol; and cooling the nanocrystalline aerosol to form the controlled particle size range nanocrystalline material.

Claim 23

Independent Claim 282 words

A method of synthesizing a controlled particle size range of a nanocrystalline material, comprising the steps of: providing a chamber for holding means for generating a nanocrystalline aerosol selected from the group consisting of a metal, a semiconductor and a ceramic; further providing a nonconsumable cathode having a longitudinal axis and shielded against chemical reaction by a working gas flow which also creates an elongated ionized arc, said working gas flow consisting essentially of a non-oxidizing gas including at least one of hydrogen gas and nitrogen gas and further including an inert gas; further providing in the Chamber a consumable anode inclined at an angle relative to the longitudinal axis of said cathode for providing material vaporizable from said anode by said elongated ionized arc; providing first means for injecting into the chamber at least one of a quench gas and a reaction gas within the boundaries of said elongated ionized arc and using said first means to inject at least one of the quench gas and the reaction gas into said arc at a point, thereby causing truncation of said arc at the point of injection into the arc; using said first means for controlling gas flow rate to change the flow rate of at least one of said quench gas and said reaction gas to control and change the particle size range of the nanocrystalline material to be synthesized; maintaining said arc between said cathode and anode by injecting the working gas and the at least one of quench and reaction gas with a controlled gas flow rate into the chamber to form the nanocrystalline aerosol; and cooling the nanocrystalline aerosol to form the controlled particle size range nanocrystalline material.

Claim 24

Dependent Claim 35 words

The method as defined in claim 21 further including the step of controlling particle size by injecting a cooling gas stream into the nanocrystalline aerosol at a point downstream beyond the truncation of said arc.

Claim 25

Dependent Claim 16 words

The method as defined in claim 21 wherein said reaction gas comprises an oxygen containing gas.

Claim 26

Dependent Claim 32 words

The method as defined in claim 21 wherein said working gas flow and said quench and reaction gas are introduced into said chamber as part of an open loop gas flow system.

Claim 27

Dependent Claim 57 words

The method as defined in claim 21 wherein said reaction gas comprises an oxygen containing gas and said nanocrystalline material is selected from the group consisting of TiO 2 , ZrO 2 , Si 3 N 4 , SiC, SiO 2 , Y 2 O 3 , Al 2 O 3 and Fe 2 O 3 .

Claim 28

Dependent Claim 25 words

The method as defined in claim 21 further including the step of dispersing the nanocrystalline material in a liquid solution to form a colloidal suspension.

Claim 29

Dependent Claim 89 words

The method as defined in claim 21 wherein a reaction zone having a first characteristic reaction zone color is formed near the intersection of the longitudinal axes of said anode and cathode with a first ionized arc disposed adjacent said cathode having a second characteristic color and said arc near said anode having a third characteristic color, said method of synthesizing nanocrystalline material being optimized for rate of production by generating a maximum color separation among the first, second and third characteristic colors formed during performance of the method.

Claim 30

Dependent Claim 76 words

The method as defined in claim 21 further including the step of forming consolidated material from the nanocrystalline material and wherein the consolidated material includes pores disposed between solid nanocrystalline grains and the pores have a characteristic pore size distribution associated with the consolidated material with said pore size distribution having an average diameter less than about 20 nanometers and the nanocrystalline grains having a size distribution with an average diameter less than about 50 nanometers.

Claim 31

Dependent Claim 63 words

The method as defined in claim 21 further including the steps of: providing a cyclone for turbulent mixing to prevent agglomeration of said nanocrystalline aerosol produced in said reaction zone; expanding the cyclonically mixed nanocrystalline material into a large volume chamber to cool the nanocrystalline material; and passing the cooled nanocrystalline material through filter media to separate the nanocrystalline material from the gas.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1998-10-23	1999-04-24	1999-10-24	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	2002-10-23	2003-04-24	2003-10-24	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2006-10-23	2007-04-24	2007-10-24	$7700.00	Window Closed / Lapsed

Method of making nanostructured materials

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