GB2421031A - Production of nano-sized powders using flame pyrolysis - Google Patents
Production of nano-sized powders using flame pyrolysis Download PDFInfo
- Publication number
- GB2421031A GB2421031A GB0427057A GB0427057A GB2421031A GB 2421031 A GB2421031 A GB 2421031A GB 0427057 A GB0427057 A GB 0427057A GB 0427057 A GB0427057 A GB 0427057A GB 2421031 A GB2421031 A GB 2421031A
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- United Kingdom
- Prior art keywords
- fine powders
- ultra fine
- nano
- powders
- metals
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Links
- 239000000843 powder Substances 0.000 title claims abstract description 68
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 39
- 239000002184 metal Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000000446 fuel Substances 0.000 claims abstract description 22
- 150000002739 metals Chemical class 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000009257 reactivity Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 3
- 229910000497 Amalgam Inorganic materials 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical class CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 29
- 235000019441 ethanol Nutrition 0.000 abstract description 29
- 239000007788 liquid Substances 0.000 abstract description 6
- 150000004706 metal oxides Chemical class 0.000 abstract description 4
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 3
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 150000001299 aldehydes Chemical class 0.000 abstract description 2
- 150000002148 esters Chemical class 0.000 abstract description 2
- 150000002170 ethers Chemical class 0.000 abstract description 2
- 150000002576 ketones Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 21
- 150000003839 salts Chemical class 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000001354 calcination Methods 0.000 description 9
- 239000007921 spray Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000013459 approach Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000003345 natural gas Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 159000000013 aluminium salts Chemical class 0.000 description 3
- 239000007900 aqueous suspension Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011882 ultra-fine particle Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- YWGBSAFMEBIEFL-UHFFFAOYSA-N copper dioxido(oxo)manganese Chemical compound [Cu+2].[O-][Mn]([O-])=O YWGBSAFMEBIEFL-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical group O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000012717 electrostatic precipitator Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000005200 wet scrubbing Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000001164 aluminium sulphate Substances 0.000 description 1
- 235000011128 aluminium sulphate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000012505 colouration Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005367 electrostatic precipitation Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 229940008718 metallic mercury Drugs 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000011009 synthetic ruby Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- B22F1/0018—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/34—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of sprayed or atomised solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
- C01G9/03—Processes of production using dry methods, e.g. vapour phase processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/02—Amorphous compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Nanotechnology (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
Ultra fine powders of metals, metal oxides, complex metal oxides and mixtures of metals and oxides produced by a development of the flame pyrolysis technique, involving the use of a water miscible secondary fuel. Such powders are in the particle diameter range 1 to 50 nano metres and have improved physical, catalytic and chemical reactivity properties. Such powders can be compressed and calcined to produce shaped components. The secondary fuel is preferably a combustible liquid such as alcohols, aldehydes, ketones, esters and ethers, most probably being methylated ethyl alcohol.
Description
IMPROVED ULTRA FI IE POWDERS The present invention relates to a system for
the manufacture of improved ultra fine powders.
This invention covers powders comprised of metals either alone or in combination with oxygen. This definition includes mixtures and compounds of metals with or without the corresponding or different oxides.
Ultra fine powders are herein defined as solid materials in which the individual grain size is below one micron in diameter, that is below one millionth of one metre in diameter.
Many of the uses of such ultra fine powders depend on the reactivity of the materials involved and it is known that their reactivity increases with decreasing particle diameter.
This is to say that finer particles are more reactive.
This patent covers improvements to ultra fine powders which means making them even finer, that is smaller in particle diameter than can be obtained by the current form of the conventional manufacturing processes.
The present invention describes a modification to the current form of the conventional manufacturing process which produces improved ultra fine powders close to I nano metre in diameter, that is approaching one thousanth of one millionth of one metre in diameter. 2.
Most of the conventional industrial manufacturing processes for the production of ultra fine powders involves the spraying of liquid droplets into a flame or plasma.
In the most usual form of these conventional industrial processes a metal salt dissolved in an aqueous solution is sprayed into a natural gas fuelled flame. In this form the process is known as Flame Pyrolysis.
Flame pyrolysis has been used on an industrial scale to produce such products as ultra fine metal oxides, metal silicates, metal phosphates, mixed oxides, sub oxides, interstitial oxides and some metals.
These products of conventional flame pyrolysis are sufficiently fine for existing applications such as pigments and catalysts, that is to say that they are sub micron in particle diameter.
However it has recently been recognised that there are many further potential applications for flame pyrolysis products provided still finer powders can be produced.
To be sufficiently fine for these new applications the process of flame pyrolysis needs to be developed further so that it can produce improved ultra fine powders with grain diameters approaching nano particulate sizes, that is to say approaching one thousanth of one millionth of one metre.
Specifically, there are significant markets for improved ultra fine powders with grain diameters between I and 50 nano metres. The current form of conventional flame pyrolysis can not be used economically to produce powders with grain diameter below nano metres. However, variations in the current form of production have been attempted. 4.
It has been the aim of my research to further develop the flame pyrolysis techniques so that it can be used for the economic manufacture of industrial tonnage quantities of 1 to nano metre diameter particulate solid oxides and metals.
It has now been discovered according to the present invention that a modified approach to flame pyrolysis can economically produce tonnage quantities of nano sized particulate solid oxides and metals, with particle diameters in the range I to 50 nano metres.
More over it has been found that the reactivity of these I to 50 nano metre sized products produced is greatly improved over all previously known materials produced by conventional flame pyrolysis. This increased reactivity makes these improved ultra fine powders ideal for a range of new applications.
The invention described herein, namely improved ultra fine powders, provides for the economic manufacture of novel highly reactive forms of many oxides and some metals.
The basis of the present invention is the addition of a secondary fuel to the flame pyrolysis feed. That is to say that the conventional process known as flame pyrolysis is modified so that the aqueous salt solution feed to the spray head contains a secondary fuel.
In every other respect the fuelling of the flame pyrolysis rig is exactly the same as in conventional flame pyrolysis, ie the primary natural gas fuel is still used.
Many combustible liquids can be used as this secondary fuel but it has been found that the most effective are liquid fuels which are miscible with water. These include for example alcohols, aldehydes, ketones, esters and ethers. 3.
Attempts to produce such nano particulate powders will now be reviewed.
It is known that the use of sprays that produce ultra fine droplets of salt solutions have been tried in the feed system of flame pyrolysis rigs. Such modified sprays do produce finer pyrolysed powders. However, particles with diameter below 250 nano metres have proved to be uneconomic or impossible to make by this modification of the conventional flame pyrolysis technique Another known approach to producing finer powders by flame pyrolysis is to feed the flame with more dilute solutions of metal salts. Again this does produce finer pyrolysed powders but not usually finer than 250 nano metres in diameter. Moreover such an approach reduces production rates and increases fuel consumption and is therefore only of relevance to laboratory scale production rather than industrial ie tonnage manufacture.
The combination of finer sprays and dilute feed solution has also been tried. The results are very fine powders with diameters down to 150 nano metres but still not nano sized powders in the desired range of 1 to 50 nano metres. As would be expected such combined approaches to making nano sized particles by diluting the feed and spraying finer droplets, are uneconomic.
Not with standing the above mentioned attempts to develop the flame pyrolysis process there remains a major commercial opportunity for the economic manufacture of tonnage quantities of nano sized oxides and metals. However, these new opportunities require particle diameters in the range I to 50 nano metres. 5.
The preferred secondary fuel is industrial alcohol ie methylated ethyl alcohol.
The effect produced by adding this secondary fuel to a flame pyrolysis feed is that the droplets produced by the spray head explode when they enter the flame. This explosive effect shatters the embryonic grains as they form thereby comminuting the powder produced.
This exploding droplet effect is a novel feature of the improved version of the flame pyrolysis process described herein. This exploding droplet effect cannot be achieved via conventional flame pyrolysis using gas as a single fuel.
The results of using water miscible secondary fuels is that this modified form of flame pyrolysis is able to produce I to 50 nano metre sized ultra fine particles. Moreover it has been found that these nano sized ultra fine particles are almost completely devoid of crystal structure. This is to say that they are amorphous.
Such amorphous I to 50 nano metre sized ultra fine oxide and or metal powders have been shown to be far more reactive than any previous flame pyrolysis powders. Many have physical and chemical properties dissimilar to the equivalent conventionally sized powders.
The individual grain sizes of these amorphous nano sized ultra fine oxide and or metal powders have been measured to be in ranges between I and 50 nanometres in particle diameter. Individual product types can now be manufactured with closely specified grain diameter sizes within the nano particle range, of 1 to 50 nano metres. 6.
The improved form of flame pyrolysis described herein can be used for the industrial scale production of a wide range of physically different and chemically diverse products.
It should be noted that the use of the secondary fuel does not significantly increase the fuels costs involved in flame pyrolysis. This is because the secondary fuel substitutes, in part, for the primary fuel namely natural gas.
Moreover it has been found that the use of the secondary fuel enables flame pyrolysis rigs to be operated at a higher flame temperature than is possible using natural gas alone.
Also it has been noticed that the flame produced when the secondary fuel is used transfers a higher proportion of thermal energy to the embryonic particles generated in the reaction.
Overall, it has been found that the use of the secondary fuel drives the flame reactions further towards completion than is the case in conventional flame pyrolysis.
The result of using this modified form of flame pyrolysis is that a range of improved ultra fine powders that are novel physico chemical compositions of matter can be produced.
These improved powders are not only finer but also of purer form and having greater chemical reactivity than is possible via conventional flame pyrolysis.
Taken together this improved form of flame pyrolysis provides a manufacturing route to a wide range of industrially important nano sized powders.
The phrases nano sized particles and nano sized particulates are used herein to differentiate between the products described in this invention as compared with conventional ultra fine powders which are referred to herein as sub micron particles. 7.
Examples of specific nano particulate powders which have been manufactured on an industrial scale via this process will now be described.
Simple oxides, for example aluminium oxides ie alumina, can be produced via this modified form of flame pyrolysis. This is produced from a feed of an alcohol water solution of aluminium sulphate, or other thermally decomposable aluminium salt. The product is a nano sized highly reactive alumina powder of use in the manufacture of advanced ceramic components via isostatic pressing.
Another example of a simple oxide is zinc oxide. This is produced from a feed of an alcohol water solution of zinc nitrate, or other thermally decomposable zinc salt. The product is a nano sized zinc oxide powder of use as an ultra violet light scatterer in sun screens.
A further example of a simple oxide is titanium dioxide. This is produced from a feed of an alcohol water solution of titanium tetra chloride, or other thermally decomposable titanium salt. The product is a nano sized titanium oxide powder of use as a white pigment with improved covering power.
A still further example of a simple oxide is chromium sesqui oxide. This is produced from a feed of an alcohol water solution of chromic acid anhydride, or other thermally decomposable chromium salt, made up immediately prior to flame spraying. The product is a nano sized chromium sequi oxide of use in ultra fine tribology applications.
Similar approaches have been used to manufacture simple oxides of silicon, gallium, germanium, tin, lead, vanadium, manganese, iron, cobalt, nickel, copper and zirconium.
The above mentioned simple oxides are only examples, many other simple oxides can also be produced as described herein. 8.
More complicated oxides can also be manufactured on an industrial scale via this modified form of flame pyrolysis.
Mixed oxides, for example chromium oxide doped alumina, can be produced. The feed in this case is an alcohol water solution of an aluminium salt and a chrome salt. The product is a nano sized synthetic ruby powder of use in advanced abrasive applications, bearings and the jeweller'y industries.
Complex oxides, for example glass or glaze powders, can be produced. The feed in this case is an alcohol water solution of mixed salts of for example lead, silica, alkali metal and colouring metals. The product is a nano sized glaze powder with high strength and colour of use in ceramic colouration, and, chemical reactor lining.
Mixed oxide catalysts, for example copper manganite, can be produced. The feed in this case is an alcohol water solution of a thermally decomposable copper salt and a manganese salt. The product is a nano sized copper manganite powder with high catalytic surface effect.
Various synthetic minerals have to be produced. The feed in this case is an alcohol water solution of mixed salts of for example aluminium, silicon, magnesium and an alkali metal.
The product is a nano sized synthetic mineral with a structural formula conferred by the ratio of the oxides derived from the feed solution.
Interstitial oxides, for example, titanium nickel yellow, can be produced. The feed in this case is an alcohol water solution of thermally decomposable titanium and nickel salts. The product is a nano sized yellow pigment with unusual brightness.
Many synthetic mineral of commercial importance can be produced for example speciality cementitious products. 9.
Ref ractories can be produced. The feed in this case is an alcohol water suspension of for example sub micron ceramic powders such as alumina together with thermally decomposable salts of for example aluminium, magnesium, chromium and zirconium.
The initial product is a submicron agglomerate based on alumina, physically associated with nano sized particles of secondary phase oxides.
Glass ceramics can be produced. The feed in this case is an alcohol water solution of for example thermally decomposable salts of silica, alumina and zinc. The initial product is a nano sized mixed oxide powder. Upon subsequent slow calcination of pressed shapes made from this powder, crystals grow within the glassy phase and ultra hard wearing glass ceramic components can be manufactured.
Phosphates both simple and complex can also be produced using appropriate combinations of thermally decomposable salts plus phosphoric acid in alcohol water solutions. In this way controlled release anti corrosive products can be manufactured.
Silicates both simple and complex can also be produced using appropriate combinations of thermally decomposable salts of for example aluminium plus alkali metal silicates in alcohol water solutions. In this way synthetic minerals such as zeolites can be manufactured.
Aluminates both simple and complex can also be produced using appropriate combinations of thermally decomposable aluminium salts in alcohol water solutions.
Our research is containing and from recent work we believe that various sub oxides can also be produced as described herein.
All the above mentioned complicated oxides, phosphates, silicates and aluminates are only examples, many other complex oxides can also be produced as described herein. i a
Some nano sized metal containing particles can also be manufactured on an industrial scale via this modified form of flame pyrolysis.
Mercury can be recovered from waste organo mercurial compounds. The feed in this case is an alcohol water solution or suspension of an organo mercurial compound. The product is liquid metallic mercury, with very low emission of unburned organics.
Amalgams and alloys can be produced. The feed in these cases are alcohol water solutions of thermally decomposable salts of dissimilar metals, which yield the metals rather than oxides.
Noble metals and some metals of the platinum group can be produced. The feed in this case is an alcohol water solution of a thermally decomposable metal salt which pyrolyses to the metal. The product is a nano sized amorphous metal powder of high chemical purity and catalytic reactivity. Nobel, platonic and other metals deposited in the form of nano sized particulates and or coatings can be produced. The feed in these cases are alcohol water solutions of the thermally decomposable salts plus slurried sub micron mineral or oxide eg alumina or silica feeds.
Cermets can be produced. The feed in this case is an alcohol water solution of thermally decomposable salts that yield an oxide and a metal. The product is a nano sized cermet powder of interest in high technology applications.
Metal metal composite powders can be produced. The feed in this case is an alcohol water suspension of an sub micron metal powder together with a thermally decomposable salt that yields a dissimilar metal. The result is a sub micron agglomerate with a metal core in a nano sized dissimilar metal coating. 11.
Glassy cermets can be produced. The feed in this case is an alcohol water solution of two or more thermally decomposable salts that yield a glaze incorporating metal atoms.
These experimental materials are of interest in high technology.
Metal metal oxide powders can be produced. The feed in this case is an alcohol water suspension of an sub micron metal powder together with thermally decomposable salts of the same or a dissimilar metal. The result is a sub micron agglomerate with a metal core and a nano sized oxide coating.
The above mentioned metal containing products are only examples, many other metal and metal containing compositions of matter can also be produced as described herein.
The overall manufacturing process by which all the products exemplified herein can be made, will now be described.
A conventional flame pyrolysis rig comprises a feed head, a calcination tube, a dry separation zone and a wet scrubbing zone.
The feed head is a plate that fits over one end of the calcination tube. Mounted centrally on this plate and pointing into the centre of the calcination tube is a compressed air driven fine liquid droplet generating spray. The thermally decomposable salts held in an alcohol water solution or slurried suspension are fed into the calcination tube via the feed head.
The calcination tube is fed with natural gas via rows of gas air inlets. A pilot flame nozzle and flame failure device are fitted to the calcination tube.
The fine droplets of feed are flame pyrolised in the calcination tube. The result is a smoke of ultra fine particulates plus exhaust gases. 12.
Beyond the calcination tube are linked conventional dry powder separation facilities, such as elutriation columns and or electro static precipitators. This dry separation zone yields the various fractions of nano particulates. Dry separation is vital if cementitious products are to be manufactured. Finally the exhaust gases pass into a water scrubber where the last traces of the product together with absorbed gases are removed from the exhaust stream.
In the modified form of flame pyrolsis used in producing the improved ultra fine particles described herein certain minor modifications need to be made to the conventional flame pyrolsis rig as described above.
In particular, because the powders produced are finer the dry powder separation facilities, such as air elutriation columns and or electro static precipitators need to be improved in effectiveness. These efficiency improvement may conventionally be achieved by reducing the exhaust air speeds. This is effected by using larger diameter elutriation and electostatic precipitation tubes. Further improvements in the recovery rates of ultra fine powders can be made by using pulsed air injection at the elutriation and or electrostatic precipitation stages.
Finally, more effiecient wet scrubbing can be achieved, even in the case of nano sized particulates, by diffusing the exhaust stream through filled packed columns.
In addition to the above minor modifications in the design of flame pyrolsis rigs the only significant alteration to the conventional process, to produce nano sized particulates, is the physical addition of alcohol to the feed head spray. This is a purely formulatory change that does not require additional equipment. 13.
Industrial alcohol, that is methylated ethyl alcohol is the preferred secondary fuel. This may be added in place of water, in the spray head feed, at a rate between 1 O% and 100%. Our preferred replacement rate is 50% ie the feed solutes are composed of 50% alcohol secondary fuel and 50% water.
All of the features disclosed in this specification and all of the steps in the manufacturing process described, may be combined in any combination, except combinations which are mutually exclusive.
Each feature disclosed in this specification may be replaced by alternative features serving the same purpose. Thus each feature disclosed is one example of a generic series of equivalent or similar features.
The invention is not restricted to the details of the foregoing embodiments. The invention extends to any novel one, or any novel combinations, of the features disclosed in this specification and or any novel combination of the steps of the manufacturing process so disclosed. 14.
Claims (12)
1. Improved ultra fine powders with particle diameters in the 1 to 50 nano metre range.
2. Improved ultra fine powders according to claim 1, wherein the particles produced are more chemically reactive than conventional ultra fine powders.
3. Improved ultra fine powders according to claim 1 wherein the particles produced have amorphous rather than crystalline structures..
4. Improved ultra fine powders according to claim I wherein the particles produced have greater pigmentary properties than conventional fine powders.
5. Improved ultra fine powders according to claim I wherein the particles produced have stronger physical bonding properties, when compressed, than conventional fine powders.
6. Improved ultra fine powders according to claim I wherein the particles produced have greater catalytic and or chemical reactivity than conventional fine powders.
7. Improved ultra fine powders according to claim I wherein the particles are metals, or mixtures or amalgams or alloys of metals.
8. Improved ultra fine powders according to claim 1 wherein the particles produced are oxides of metals.
9. Improved ultra fine powders according to claim I wherein the particles produced are complex oxides.
10. Improved ultra fine powders according to claim I wherein the particles produced are mixtures of metals and oxides.
11. A process for the manufacture of such improved ultra fine powders, based on flame pyrolysis but utilising a water miscible secondary fuel.
12. A method for the industrial scale manufacture of nano sized solid particles substantially as described herein.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2399867A1 (en) * | 2010-06-25 | 2011-12-28 | Evonik Degussa GmbH | Method for producing mixed oxides containing lithium |
| ES2941332A1 (en) * | 2021-11-18 | 2023-05-19 | Univ Jaume I | Procedure for obtaining in situ a ground ceramic pigment (Machine-translation by Google Translate, not legally binding) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5358695A (en) * | 1993-01-21 | 1994-10-25 | Physical Sciences, Inc. | Process for producing nanoscale ceramic powders |
| US5958361A (en) * | 1993-03-19 | 1999-09-28 | Regents Of The University Of Michigan | Ultrafine metal oxide powders by flame spray pyrolysis |
| EP1134302A1 (en) * | 2000-03-17 | 2001-09-19 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | New process for the production of nanostructured solid powders and nano-particles films by compartimentalised solution thermal spraying (CSTS) |
| US6656588B1 (en) * | 1998-12-01 | 2003-12-02 | The Regents Of The University Of Michigan | Ultrafine powders and their use as lasing media |
| US20040050207A1 (en) * | 2002-07-17 | 2004-03-18 | Wooldridge Margaret S. | Gas phase synthesis of nanoparticles in a multi-element diffusion flame burner |
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| DE102004041747A1 (en) * | 2004-08-28 | 2006-03-02 | Degussa Ag | Indium-tin mixed oxide powder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5358695A (en) * | 1993-01-21 | 1994-10-25 | Physical Sciences, Inc. | Process for producing nanoscale ceramic powders |
| US5958361A (en) * | 1993-03-19 | 1999-09-28 | Regents Of The University Of Michigan | Ultrafine metal oxide powders by flame spray pyrolysis |
| US6656588B1 (en) * | 1998-12-01 | 2003-12-02 | The Regents Of The University Of Michigan | Ultrafine powders and their use as lasing media |
| EP1134302A1 (en) * | 2000-03-17 | 2001-09-19 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | New process for the production of nanostructured solid powders and nano-particles films by compartimentalised solution thermal spraying (CSTS) |
| US20040050207A1 (en) * | 2002-07-17 | 2004-03-18 | Wooldridge Margaret S. | Gas phase synthesis of nanoparticles in a multi-element diffusion flame burner |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2399867A1 (en) * | 2010-06-25 | 2011-12-28 | Evonik Degussa GmbH | Method for producing mixed oxides containing lithium |
| WO2011160940A1 (en) * | 2010-06-25 | 2011-12-29 | Evonik Degussa Gmbh | Method for producing mixed oxides comprising lithium |
| CN102906023A (en) * | 2010-06-25 | 2013-01-30 | 赢创德固赛有限公司 | Method for producing mixed oxides comprising lithium |
| CN102906023B (en) * | 2010-06-25 | 2015-04-01 | 赢创德固赛有限公司 | Method for producing mixed oxides comprising lithium |
| ES2941332A1 (en) * | 2021-11-18 | 2023-05-19 | Univ Jaume I | Procedure for obtaining in situ a ground ceramic pigment (Machine-translation by Google Translate, not legally binding) |
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| GB0427057D0 (en) | 2005-01-12 |
| GB2421031B (en) | 2008-03-26 |
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