US2447789A - Evaporating crucible for coating apparatus - Google Patents

Evaporating crucible for coating apparatus Download PDF

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US2447789A
US2447789A US584450A US58445045A US2447789A US 2447789 A US2447789 A US 2447789A US 584450 A US584450 A US 584450A US 58445045 A US58445045 A US 58445045A US 2447789 A US2447789 A US 2447789A
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crucible
plate
coating
heat
evaporation
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Edgar E Barr
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Polaroid Corp
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Polaroid Corp
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/243Crucibles for source material

Description

Aug. 24, 1948. BARR 2,447,789

EVAPORATING CRUCIBLE FOR COATING APPARATUS Filed March 23, 1945 INVENTOR.

5 54. BY Z V Patented Aug. 24, 1948 LUNFI TED :srarzas PATENT rrircE :EVABORATING CRUCIBLE FOR COATING APPARATUS --Edgar E. Barr; North Woburn, Mass, as'signor to Polaroid Corporation, Cambridge, Mass a :corporation of Delaware Application March 23, 1945, Serial No. 584,450

. ,1 This invention relates toa'new and'iniproved crucibleparticula-rlyadapted for use in the production of 'optical' elements by the evaporation and deposition of light-transmitting materials in a-vacuum.

-'Ithas recently been discovered that optically homogeneous and useful, light-transmitting films *canbeproduced by the evaporation of a variety 'of" classes of'organic compounds and the deposition of said evaporated compounds on asuitable support-in a vacuum. It appears that in carry- -ingoutthis work it is desirable that the entire charge of material to be evaporated ice-heated to theevaporation point'before any evaporation be- "gins. -Otherwise-there is a tendency for the vat charge-within the crucible and for preventing the -escape therefromof particles greater than a predetermined-size.

A further object is to provide a crucible having *the above'advantages and comprising ablock -'of "heat-conducting metal or other material provided with at least one and preferably a= mul-tiplicity of cavities therein for holding the charge to be evaporated, and provided also with screen or baflie means for preventing the escape from said crucible of particles appreciably greater than molecular size.

Other objects and advantages will in part appear and in part be pointed out in the following description of one or more embodiments of the invention which are given as nonlimiting examples in connection with the accompanying drawings, in which:

Figure 1 is a view in vertical section of a crucible embodying a form of the invention; and

Figure 2 is a plan view, partly broken away, of the crucible shown in Fig. 1.

In the drawings, body member ill comprises a block of steel or any other suitable heat-conducting metal or other material, and is shown as cylindrical but may be of an other desired shape. Annular flange I2 projects upwardly from the outer rim of body member Ill and may be secured thereto in any suitable way but is most conveniently formed integrally therewith as by 2 Claims. (Cl.-'219--19) member .I 0.

boring outthe upper portion of an initially-solid block. Cavitiesorcells il within body'member til are designed to-hold the charge of material tabs-evaporated. Cells Htmaybe of any'desired shape but are most'conveniently made circular-in cross section "by drillinginto the -body There are preferably provided as many'of cells as can conveniently bearranged in honeycomb fashion in body member to, and

'theyshould extend well into-butnot through said body, member.

For example, ii the depth of body member it: is of the orderof one inch, cells *l l 'may-be-one-half inch in depth and a-ccnvcnient 'diameter'is approximately one-eighth of aninch.

."It'is desirable "to provide the-crucible oi the zinventi'onwith suitablescreening -means forpreventing the escape during evaporation of parti- 'cles tappreciably greater than molecular :size.

"This may'be done by-means o'f any-suitable fine meshrscreenbut preferred results a have been ob- 'tained with the use of asolid plate Iii of steel-or other suitable rigid material. As shownin the :drawings, "the 'radius of plate I5 is preferably just suflicientl smaller than the inner radi-us oi "flange 12 'to leave an annular space 46 '(Fig. 2) therebetween. the orderof 0.10 inch in width.

1 *rality-of short studs 20 adapted to support plate l5. Studs 20 ma for example be of the order of one-sixteenth of an inch in height, and this arrangement has the advantage that plate I5 is readily removable to permit access to cells I4 for charging or cleaning the crucible. It is also desirable to provide body member In with some non-heat-conducting mounting means such, for example, as legs 22 of porcelain or similar material.

In use, it is desirable that heat may be applied relatively rapidly to the crucible of the invention and a suitable arrangement for this purpose is shown in Fig. 1. It will be understood that said crucible is intended for use with conventional evacuation apparatus comprising any suitable bell jar means, not shown, and base plate 24. Elements 25 and 25 represent heating filaments of any suitable metal and shape, a convenient shape being spiral as indicated at 25 in Fig. 2. The desirability of bringing the entire charge to the evaporation temperature before appreciable vaporization begins has already been noted. It is greatly facilitated by the crucible of the inven- 3 tion. The honeycomb construction acts to conduct heat uniformly throughout the charge, and this in turn makes it possible to apply heat rapidly with minimum danger of uneven heating or overheating any portion of the charge before the balance has reached the evaporation point. One advantage of these features is a substantial reduction in the time necessary for the evaporation and deposition of a film of any given thickness,

and makes practical the use of the two filaments shown in Fig. 1. On the other hand, any insumciently heated particles which might tend to rise into vapor are effectively prevented from doing so by contact with plate I5, since it is necessary for the vapor to travel first sidewise through space l8 and then upwards through space 16 before leaving the crucible. Plate 15 has the further advantage of shielding the deposited film from any efiects of sputtering within the crucible.

It will be apparent that the above-described construction is subject to considerable variation without departing from the scope of the invention. For example, it has been pointed out that screening means other than plate l5 may be used and that the mounting for said screening means may be varied in many ways. The size of annular space I6 may readily be altered by changing the size or shape of plate 15 to limit the passage from the crucible of particles greater than any predetermined size. It will also be noted that the shape of the crucible or of the cavities for the charge may be altered at will, but the circular configurations are shown because of the ease with which they may be reproduced as Well as their general efiiciency. Many other variations which do not alter the principles of the invention will doubtless be apparent to those skilled in the art, and it is accordingly intended that all matter contained in the foregoing description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense.

It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described, and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.

What is claimed is:

1. In an evaporation apparatus, the combination comprising a crucible comprising, in combination, a substantially cylindrical body member comprising readily heat-conducting material, means providing a multiplicity of cavities extending into but not through said body member from the upper surface thereof, screen means positioned adjacent said cells and preventing the escape therefrom of particles greater than a predetermined size, and means providing a plurality of filament elements positioned closely adjacent said crucible and adapted to emit radiant heat, one of said filaments being positioned above said body member and another being positioned below said body member.

2. [in an evaporation apparatus, the combination comprising a crucible comprising, in combination, a substantially cylindrical body member comprising a readily heat-conducting metal, mounting means for said body member comprising substantially non-heat-conducting material, means providing a multiplicity of substantially tubular cells extending substantially perpendicularly into but not through said body member from the top thereof, an annular flange member extending upwardly from the outer rim of said body member, a substantially rigid, circular plate member having a radius slightly smaller than the inner radius of said flange member whereby when said plate is positioned within said flange member an annular space remains therebetween, stud means for removably mounting said plate within said flange and in spaced relation with the tops thereof and of said cells, and means providing a plurality of filament elements positioned closely adjacent said crucible and adapted to emit radiant heat, one of said filaments being positioned above said body member and another being positioned below said body member.

EDGAR E. BARR.

REFERENCES CITED Siebertz July 4, 1939 OTHER REFERENCES Strong: Procedures in Experimental Physics, pages 173 and 182. Prentice-Hall, Inc., New York (1946).

US584450A 1945-03-23 1945-03-23 Evaporating crucible for coating apparatus Expired - Lifetime US2447789A (en)

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Cited By (61)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2610606A (en) * 1946-09-26 1952-09-16 Polytechnic Inst Brooklyn Apparatus for the formation of metallic films by thermal evaporation
US2902574A (en) * 1958-02-03 1959-09-01 Hughes Aircraft Co Source for vapor deposition
US3117210A (en) * 1959-07-13 1964-01-07 Wisconsin Alumni Res Found Apparatus for evaporating materials
US3405251A (en) * 1966-05-31 1968-10-08 Trw Inc Vacuum evaporation source
US3427432A (en) * 1966-06-10 1969-02-11 Granville Phillips Co Sublimation device
US3640762A (en) * 1970-05-26 1972-02-08 Republic Steel Corp Method for vaporizing molten metal
US3740043A (en) * 1970-05-26 1973-06-19 Republic Steel Corp Apparatus for vaporizing molten metal
US5239611A (en) * 1991-02-14 1993-08-24 Hilmar Weinert Series evaporator
US6237529B1 (en) 2000-03-03 2001-05-29 Eastman Kodak Company Source for thermal physical vapor deposition of organic electroluminescent layers
US20030111014A1 (en) * 2001-12-18 2003-06-19 Donatucci Matthew B. Vaporizer/delivery vessel for volatile/thermally sensitive solid and liquid compounds
US20030232138A1 (en) * 2002-06-17 2003-12-18 Marko Tuominen System for controlling the sublimation of reactants
US20040014314A1 (en) * 2002-04-24 2004-01-22 Brooks Joseph F. Evaporative deposition with enhanced film uniformity and stoichiometry
US6837939B1 (en) * 2003-07-22 2005-01-04 Eastman Kodak Company Thermal physical vapor deposition source using pellets of organic material for making OLED displays
US20050186340A1 (en) * 2004-02-23 2005-08-25 Eastman Kodak Company Device and method for vaporizing temperature sensitive materials
US20050208216A1 (en) * 2004-03-22 2005-09-22 Michael Long High thickness uniformity vaporization source
US20050208220A1 (en) * 2004-03-22 2005-09-22 Eastman Kodak Company Vaporizing fluidized organic materials
US20050244580A1 (en) * 2004-04-30 2005-11-03 Eastman Kodak Company Deposition apparatus for temperature sensitive materials
US20050241585A1 (en) * 2004-04-30 2005-11-03 Eastman Kodak Company System for vaporizing materials onto a substrate surface
US20050281948A1 (en) * 2004-06-17 2005-12-22 Eastman Kodak Company Vaporizing temperature sensitive materials
US20060062915A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering particulate material to a vaporization zone
US20060062920A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering particulate material to a vaporization zone
US20060062918A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering organic powder to a vaporization zone
US20060062919A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering organic powder to a vaporization zone
US20060099345A1 (en) * 2004-11-09 2006-05-11 Eastman Kodak Company Controlling the application of vaporized organic material
US20060099344A1 (en) * 2004-11-09 2006-05-11 Eastman Kodak Company Controlling the vaporization of organic material
US20060150915A1 (en) * 2005-01-11 2006-07-13 Eastman Kodak Company Vaporization source with baffle
US20060177578A1 (en) * 2005-02-04 2006-08-10 Eastman Kodak Company Feeding particulate material to a heated surface
US20060177576A1 (en) * 2005-02-04 2006-08-10 Eastman Kodak Company Controllably feeding organic material in making OLEDs
US20060174509A1 (en) * 2005-02-04 2006-08-10 Eastman Kodak Company Feeding organic material to a heated surface
US20060251810A1 (en) * 2005-05-03 2006-11-09 Eastman Kodak Company Metering material to promote rapid vaporization
US20060251811A1 (en) * 2005-05-03 2006-11-09 Eastman Kodak Company Controllably feeding powdered or granular material
US20060275542A1 (en) * 2005-06-02 2006-12-07 Eastman Kodak Company Deposition of uniform layer of desired material
US20060273713A1 (en) * 2005-06-02 2006-12-07 Eastman Kodak Company Process for making an organic light-emitting device
US20070026146A1 (en) * 2005-07-27 2007-02-01 Eastman Kodak Company Vaporizing material at a uniform rate
US20070074899A1 (en) * 2005-08-23 2007-04-05 Nitto Denko Corporation Production method of suspension board with circuit
US20070098891A1 (en) * 2005-10-31 2007-05-03 Eastman Kodak Company Vapor deposition apparatus and method
US20070104864A1 (en) * 2005-11-10 2007-05-10 Eastman Kodak Company Deposition system using sealed replenishment container
US20070104890A1 (en) * 2005-11-10 2007-05-10 Eastman Kodak Company Purifying organic materials for physical vapor deposition
US20070231490A1 (en) * 2006-03-29 2007-10-04 Eastman Kodak Company Uniformly vaporizing metals and organic materials
US20070248753A1 (en) * 2006-04-20 2007-10-25 Eastman Kodak Company Vapor deposition of a layer
US20080041310A1 (en) * 2002-07-23 2008-02-21 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US20090136668A1 (en) * 2002-07-23 2009-05-28 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US20100009080A1 (en) * 2008-07-10 2010-01-14 Asm International N.V. Fluidized bed evaporator
US20100122659A1 (en) * 2008-11-14 2010-05-20 Michael Long Metering and vaporizing particulate material
US20100122656A1 (en) * 2008-11-14 2010-05-20 Michael Long Particulate material metering and vaporization
US20100122658A1 (en) * 2008-11-14 2010-05-20 Michael Long Metering of particulate material and vaporization thereof
WO2010096340A1 (en) 2009-02-17 2010-08-26 Global Oled Technology Llc Simplified powder feeding and vaporization apparatus
US20100255198A1 (en) * 2006-08-31 2010-10-07 Advanced Technology Materials, Inc. Solid precursor-based delivery of fluid utilizing controlled solids morphology
US20110023862A1 (en) * 2008-04-11 2011-02-03 Toshiba Mitsubishi-Electric Indus. Sys.Corp. Heat equalizer
US20110033973A1 (en) * 2007-09-20 2011-02-10 Global Oled Technology Llc Deposition apparatus for temperature sensitive materials
US7993459B2 (en) 2005-10-24 2011-08-09 Global Oled Technology Llc Delivering particulate material to a vaporization zone
US8027574B2 (en) 2007-08-06 2011-09-27 Global Oled Technology Llc Vaporization of thermally sensitive materials
US20130224380A1 (en) * 2012-02-28 2013-08-29 Massachusetts Institute Of Technology Single-Unit Reactor Design for Combined Oxidative, Initiated, and Plasma-Enhanced Chemical Vapor Deposition
US20140335271A1 (en) * 2012-01-10 2014-11-13 Hzo, Inc. Boats configured to optimize vaporization of precursor materials by material deposition apparatuses
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US20160025329A1 (en) * 2013-04-17 2016-01-28 Venkata Sundereswar Rao VEMPATI Energy efficient pressure less steam generator
WO2016179325A1 (en) 2015-05-04 2016-11-10 Global Oled Technology Llc Entwined manifolds for vapor deposition and fluid mixing
US20180148836A1 (en) * 2014-07-01 2018-05-31 Aixtron Se Apparatus and method for generating a vapor for a cvd or pvd device
US10385452B2 (en) 2012-05-31 2019-08-20 Entegris, Inc. Source reagent-based delivery of fluid with high material flux for batch deposition
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2100045A (en) * 1935-10-12 1937-11-23 Alexander Paul Deposition of metallic films from metal vaporized in vacuo
US2164595A (en) * 1936-12-07 1939-07-04 Siemens Ag Method of coating electrodes

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2100045A (en) * 1935-10-12 1937-11-23 Alexander Paul Deposition of metallic films from metal vaporized in vacuo
US2164595A (en) * 1936-12-07 1939-07-04 Siemens Ag Method of coating electrodes

Cited By (122)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2610606A (en) * 1946-09-26 1952-09-16 Polytechnic Inst Brooklyn Apparatus for the formation of metallic films by thermal evaporation
US2902574A (en) * 1958-02-03 1959-09-01 Hughes Aircraft Co Source for vapor deposition
US3117210A (en) * 1959-07-13 1964-01-07 Wisconsin Alumni Res Found Apparatus for evaporating materials
US3405251A (en) * 1966-05-31 1968-10-08 Trw Inc Vacuum evaporation source
US3427432A (en) * 1966-06-10 1969-02-11 Granville Phillips Co Sublimation device
US3640762A (en) * 1970-05-26 1972-02-08 Republic Steel Corp Method for vaporizing molten metal
US3740043A (en) * 1970-05-26 1973-06-19 Republic Steel Corp Apparatus for vaporizing molten metal
US5239611A (en) * 1991-02-14 1993-08-24 Hilmar Weinert Series evaporator
US6237529B1 (en) 2000-03-03 2001-05-29 Eastman Kodak Company Source for thermal physical vapor deposition of organic electroluminescent layers
EP1130129A1 (en) 2000-03-03 2001-09-05 Eastman Kodak Company Source for thermal physical vapor deposition of organic electroluminescent layers
US20030111014A1 (en) * 2001-12-18 2003-06-19 Donatucci Matthew B. Vaporizer/delivery vessel for volatile/thermally sensitive solid and liquid compounds
WO2003052160A1 (en) * 2001-12-18 2003-06-26 Advanced Technology Materials, Inc. Vaporiser/delivery vessel for volatile/thermally sensitive solid and liquid compounds
EP1466030A4 (en) * 2001-12-18 2008-07-23 Advanced Tech Materials Vaporiser/delivery vessel for volatile/thermally sensitive solid and liquid compounds
EP1466030A1 (en) * 2001-12-18 2004-10-13 Advanced Technology Materials, Inc. Vaporiser/delivery vessel for volatile/thermally sensitive solid and liquid compounds
US20040014314A1 (en) * 2002-04-24 2004-01-22 Brooks Joseph F. Evaporative deposition with enhanced film uniformity and stoichiometry
US20050268855A1 (en) * 2002-04-24 2005-12-08 Brooks Joseph F Evaporative deposition with enhanced film uniformity and stoichiometry
US20110076402A1 (en) * 2002-06-17 2011-03-31 Asm International N.V. System for controlling the sublimation of reactants
US20030232138A1 (en) * 2002-06-17 2003-12-18 Marko Tuominen System for controlling the sublimation of reactants
US7601225B2 (en) 2002-06-17 2009-10-13 Asm International N.V. System for controlling the sublimation of reactants
US7851019B2 (en) * 2002-06-17 2010-12-14 Asm International N.V. Method for controlling the sublimation of reactants
US8309173B2 (en) 2002-06-17 2012-11-13 Asm International N.V. System for controlling the sublimation of reactants
US20060024439A2 (en) * 2002-06-17 2006-02-02 Asm International N.V. System for controlling the sublimation of reactants
US20080274276A1 (en) * 2002-06-17 2008-11-06 Asm International N.V. System for controlling the sublimation of reactants
US9469898B2 (en) 2002-07-23 2016-10-18 Entegris, Inc. Method and apparatus to help promote contact of gas with vaporized material
US8444120B2 (en) 2002-07-23 2013-05-21 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US7556244B2 (en) 2002-07-23 2009-07-07 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US20090136668A1 (en) * 2002-07-23 2009-05-28 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US8128073B2 (en) 2002-07-23 2012-03-06 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US20080041310A1 (en) * 2002-07-23 2008-02-21 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US7828274B2 (en) 2002-07-23 2010-11-09 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US10465286B2 (en) 2002-07-23 2019-11-05 Entegris, Inc. Method and apparatus to help promote contact of gas with vaporized material
US20110052482A1 (en) * 2002-07-23 2011-03-03 Advanced Technology Materials, Inc. Method and apparatus to help promote contact of gas with vaporized material
US9004462B2 (en) 2002-07-23 2015-04-14 Entegris, Inc. Method and apparatus to help promote contact of gas with vaporized material
US6837939B1 (en) * 2003-07-22 2005-01-04 Eastman Kodak Company Thermal physical vapor deposition source using pellets of organic material for making OLED displays
US20050016461A1 (en) * 2003-07-22 2005-01-27 Eastman Kodak Company Thermal physical vapor deposition source using pellets of organic material for making oled displays
US7704554B2 (en) 2004-02-23 2010-04-27 Global Oled Technology Llc Device and method for vaporizing temperature sensitive materials
US20050186340A1 (en) * 2004-02-23 2005-08-25 Eastman Kodak Company Device and method for vaporizing temperature sensitive materials
US20070207261A1 (en) * 2004-02-23 2007-09-06 Michael Long Device and method for vaporizing temperature sensitive materials
US7232588B2 (en) 2004-02-23 2007-06-19 Eastman Kodak Company Device and method for vaporizing temperature sensitive materials
US7364772B2 (en) 2004-03-22 2008-04-29 Eastman Kodak Company Method for coating an organic layer onto a substrate in a vacuum chamber
US20050208216A1 (en) * 2004-03-22 2005-09-22 Michael Long High thickness uniformity vaporization source
US20050208220A1 (en) * 2004-03-22 2005-09-22 Eastman Kodak Company Vaporizing fluidized organic materials
US7238389B2 (en) 2004-03-22 2007-07-03 Eastman Kodak Company Vaporizing fluidized organic materials
US20050241585A1 (en) * 2004-04-30 2005-11-03 Eastman Kodak Company System for vaporizing materials onto a substrate surface
US20050244580A1 (en) * 2004-04-30 2005-11-03 Eastman Kodak Company Deposition apparatus for temperature sensitive materials
US20050281948A1 (en) * 2004-06-17 2005-12-22 Eastman Kodak Company Vaporizing temperature sensitive materials
US7501151B2 (en) 2004-09-21 2009-03-10 Eastman Kodak Company Delivering particulate material to a vaporization zone
US20060062915A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering particulate material to a vaporization zone
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US20060062920A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering particulate material to a vaporization zone
US7288285B2 (en) 2004-09-21 2007-10-30 Eastman Kodak Company Delivering organic powder to a vaporization zone
US20060062919A1 (en) * 2004-09-21 2006-03-23 Eastman Kodak Company Delivering organic powder to a vaporization zone
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US7288286B2 (en) 2004-09-21 2007-10-30 Eastman Kodak Company Delivering organic powder to a vaporization zone
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US20060099345A1 (en) * 2004-11-09 2006-05-11 Eastman Kodak Company Controlling the application of vaporized organic material
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