US3795601A - Electrodiffused protective coating system - Google Patents

Electrodiffused protective coating system Download PDF

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US3795601A
US3795601A US00212644A US3795601DA US3795601A US 3795601 A US3795601 A US 3795601A US 00212644 A US00212644 A US 00212644A US 3795601D A US3795601D A US 3795601DA US 3795601 A US3795601 A US 3795601A
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alloy
aluminum
coating
former
bath
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W Rentz
G Brewer
R Swider
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Ford Motor Co
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Ford Motor Co
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/02—Electrophoretic coating characterised by the process with inorganic material

Definitions

  • a process for producing articles resistant to high temperature corrosion which comprises the combination of (a) controlled electrodeposition of particulate metal, particularly aluminum, aluminum alloy, a mixture of aluminum and at least one other metal or metal oxide or a mixture of aluminum and at least one alloy, and a heatfugitive, chemically ionizable organic film-former upon the surface of a substrate selected from nickel alloys, cobalt alloys, and iron alloys, and (b) controlled heat treatment of the thus coated substrate in an ambient essentially inert to the particles deposited to remove the organic film-former and to ditfuse the metal or metals of the deposit into a surface of the alloy substrate.
  • Metallic articles having high temperature corrosion resistance find a variety of uses in industry.
  • turbine engine components e.g., turbine wheels, nozzles, shrouds and thermocouple probes, which are subjected to corrosive conditions at temperatures up to 2000 F. or higher.
  • metallic articles requiring high temperature corrosion resistance have as their major component, i.e., 40 to 80 weight percent or higher, nickel, cobalt or iron.
  • turbine components such as those above mentioned, are commonly formed from nickel alloys and cobalt alloys, particularly the so-called super alloys.
  • An improved process for surface modification of metallic articles to improve their corrosion resistance at high temperatures comprises the combination of (a) controlled electrodeposition of a particulate metal-rich coating of aluminum particles and a heat-fugitive, chemically ionizable organic film-former upon the substrate selected from nickel alloys, cobalt alloys, and iron alloys, and (b) controlled heat treatment of the thus coated substrate in an ambient essentially inert to the particles deposited to remove the film-former and to diffuse the metal or metals of the deposit into a surface of the alloy substrate.
  • the metallic substrate upon which the particulate metal is deposited is a substrate which after being processed in accordance with this invention exhibits corrosion resistance at high temperatures. Obviously, various uses of metal parts subjected to high temperatures require varying degrees of high temperature corrosion resistance.
  • Iron alloys which are surface modified in accordance with this invention include those which contain very small amounts of alloying components, e.g., carbon steel, as well as those alloys wherein the alloying component or components constitute a substantial percentage of the alloy.
  • the iron alloys contain a minimum of weight percent iron and commonly much more, e.g., about to about 99 weight percent iron.
  • a broad spectrum of iron base materials are suitable for this process including carbon steels, stainless steels and nodular irons.
  • Both cast and wrought alloys of these types can be processed provided heat treatment in a non-oxidizing atmosphere at 1300 F. or above is permissable, i.e., provided that the temperature selected in this range is compatible with recognized metallurgical practices for such alloy.
  • Typical examples of such iron alloys include the following:
  • the nickel and cobalt base materials used herein typically contain about 5 to about 25 weight percent chromium for oxidation resistance, although nickel and cobalt alloys Without chromium exist and can be surface modified by this process.
  • Various amounts of refractory elements such as tungsten, tantalum, columbium, molybdenum, zirconium and hafnium are commonly added as solid solution strengtheners and/or carbide formers to improve high temperature strength.
  • Aluminum and/ or titanium are added to certain of the nickel base materials to produce age hardening response for additional high temperature strength. In such alloys, the total aluminum plus titanium contents may be as high as 10 weight percent in some alloys. Typical examples of such nickel and cobalt base wt. percent Y) alloy.
  • While a single electrodeposition prosubstrate compositions include the following: vidrng a coating containing all of the particulate metal to TABLE II Components, wt. percent of- Alloy Ni Co Fe Cr Al Ti M W Ta Cb Si Zr B C Other (F) Medium Cr level wrought Ni-base 7.2 15. 8 20 04 .50 Mn (G) High Cr level wrought Ni-base 1 5 18. 2 22. 0 9.0 0. 6 .50 10 50 Mn (H) Wrought age-hardenable Ni-base 18.5 15.0 4.3 3.5 5.2 .03 .08 (1) Cast age-hardenable Ni-base 6. 0 6. 0 4.0 4. 0 8. 0 2.
  • the nickel alloys contain about 40 of this invention to carry out successive electrodepositions weight percent nickel, commonly about 50 to about 80 of diiferent particulate metals. weight percent. Even when the nickel content of the Atypical composition of the aluminum powder or flake alloy is between 40 and 50 weight percent, it is the largest used is as follows: single component of the alloy. correspondingly, the cobalt Weight percent alloys contain above 40 weight percent cobalt, commonly Aluminum 97.0 min. about 50 to about 80 weight percent. Similarly, when the A1 0 2.0 max. cobalt content of the alloy is between 40 and 50 weight Fe 0.25 max. percent, it is the largest single component of the alloy. SOih n h max. t er meta ics, eac max. (B) PRETREATMENT OF SUBSTRATE Other metallics, total 0.15 max.
  • the areas to be coated are preferably grit blasted with suitable particulate abrasive, e.g., aluminum oxide par-
  • suitable particulate abrasive e.g., aluminum oxide par-
  • the welght ratio of alummum to other metal or metals in the particulate metal in those embodiments wherein at procedure is performed not longer than minutes prior 30 pgrtlculate 1n t e f IILl of pagticulate alloy is in to immersion of the part into the coating bath.
  • t 6 range 0 3 out 200'1 to a out Areas not requiring coating may be left uncoated by (D) THE HEAT-FUGITIVE, CHEMICALLY- leaving these portions out of the coating bath during elec- IONIZABLE ORGANIC FILM-FORMER trodeposition whenever this is feasible. In the alternative, these portions may be masked to prevent coating although immersed. Any suitable masking material may be used. For such a process, a suitable masking material is one that will remain in place during the electrodeposition process, will prevent surface contact of the masked area by the bath during the processing and which will not 40 significantly interfere with the chemical composition of the bath. Examples of a suitable insulative masking material are rubber, wax, plastic, a removable sleeve of The electrodeposition may be either anodic or cathodic.
  • the film-former is acidic, is intimately dispersed (at least partially neutralized) in the bath with a water-soluble base, e.g., ammonia, water-soluble amine, or an inorganic base such as sodium hydroxide, potassium hydroxide, lithium hydroxide, etc., and when so dispersed has, afiinity for the anode of an electrodeposition cell.
  • a water-soluble base e.g., ammonia, water-soluble amine, or an inorganic base such as sodium hydroxide, potassium hydroxide, lithium hydroxide, etc.
  • the film-former is basic and is intimately dispersed (at least partially neumetal, etc. tralized) in the bath with a water soluble acid, e.g., water- (C) PARTICULATE METAL DEPOSITED soluble organic acids such as acetic acid or mineral acid AND DIFFUSED such as phosphoric acid, etc.
  • Acidic film-forming materials include but not by way The articulate metal to be electrode osit d d bseqeuntfi, diffused into the Substratg g i i of limitation, any of the polycarboxylic acid resins used the electrodeposition of paint from an aqueous bath. average particle diameter 111 the range of about 0.05 to m about 20 prefarably about 4 to about 9 microns in the They include coupled 011s such as sunflower, safilower,
  • the median particle size Penna hempseed walnut Seed dehydrated Castor Tape- 50 seed, tomato seed, menhaden, corn, tung, soya, oiticia, or range greater than 50 Percent 18 the like the olefinic double bonds in the oil bein conless than) 6 to 30 microns 1n the case of aluminum.
  • the coupling agent even g ii deposlts adlnsable. that.
  • 0 being an acyclic odefinic acid or anhydride, preferably ff if figf f g i 2 2 22 g: p i i paitlclebslze maleic anhydride, but also crotonic acid, citraconic acid 44 microns However ⁇ , ggg g if; g or anhydride, fumaric acid, or an acyclic olefim'c alde- 1 q o es y hyde or ester of an acyclic olefinic ester such as acrolein, i as lfnay f i i Y fi gravlta vinyl acetate methyl maleate, etc or even a polybasic iona se mg rom e eectro eposition at
  • the particulate metal used in this process is om that acid such as phthahc or succinic, particularly coupled l C 'd when
  • the preferred metallic particles are aluminum particles, resms the estenficauon Products of a polyol with polybasic acid particularly glyceride drying oil-extended 3222; gfi fi g gli f g g 'p fgfii g gg alkyd resins; acidic hydrocarbon drying oil polymers such i as those made from maleinized copolymers of butadiene 23x3: fi z i fi gi g 2& fig ii i zgi gg z 2 and diisobutylene; diphenolic acid and the
  • the acidic material is an organic acid containing at least about 12 carbon atoms, e.g., lauric acid (dodecanoic acid), stearic acid (octodecanoic aid), etc. These are preferably used in conjunction with a minor amount of neutral or essentially neutral filmforming polymers, e.g., polyesters, hydrocarbon resins, polyacrylates, polymethacrylates, etc., but may be used alone or with the aforementioned carboxylic acid resins.
  • lauric acid diodecanoic acid
  • stearic acid octodecanoic aid
  • the cationic film-forming material may be either a monomer or polymer having one or more primary, secondary or tertiary amine groups in its molecular structure.
  • the basic material contains at least 12 carbon atoms, e.g., lauryl amine, stearyl amine, etc. Obviously, when the basic material is polymeric, it will be of substantially greater molecular weight. These are preferably used in conjunction with a minor amount of neutral film-forming polymers but may be used alone. It is also within the scope of this invention to employ with the carrier resin nonionic or essentially nonionic organic dispersal assistants and/or thickeners. An example of such a material is hydroxy propyl methyl cellulose.
  • the principal carrier resin i.e., the major (above 50 weight percent) proportion of the organic film-former
  • the principal carrier resin i.e., the major (above 50 weight percent) proportion of the organic film-former
  • it is a carboxylic acid which is at least partially neutralized in the electroddeposition bath with a suitable water-soluble base.
  • the preferred water-soluble base is a water-soluble amine.
  • ammonia or an inorganic base such as sodium hydroxide or potassium hydroxide may also be used.
  • the neutralizing agent may be a water-soluble, low molecular weight organic acid or suitable mineral acid.
  • the principal film-forming organic material is chemically ionized in the bath, behaves as electrolyte in the bath, and moves toward the electrode upon which it is deposited because of its macro ionic nature and not simply as a colloidal particle.
  • the heat-fugitive, chemically-ionizable film-former and any other organics electrodeposited with the particulate metal are essentially removed from the coating, at least primarily by vaporization, during the firing step.
  • the organics deposited must be materials which vaporize at or below the temperature used in firing. Thus, there materials will ordinarily vaporize below 1300 F., commonly below 1000 F.
  • the coating bath consists of an aqueous suspension of particulate metal, solubilizer or otherwise dispersed chemically-ionizable, fihn-former with optional employment of a nonionic organic dispersal assistant or thickener.
  • the total weight of non-volatile solids i.e., particulate metal (powder or flake) and organic additives, should comprise between about 3 and about 35 Weight percent of the bath.
  • the weight ratio of metal powder to electrodepositable organic non-volatiles should be above 4:1 although ratios in excess of 3:1 can be used. In certain embodiments, this will range from a ratio in excess of 5:1 to as high as 15-2021.
  • the concentration of filmformer in the bath is advantageously in the range of about 0.2 to about 2 parts by weight per 100 parts by weight of bath. However, fairly good results are obtained in the range of about 0.2 to about 7 parts by weight of bath.
  • the concentration of hydroxy propyl methyl cellulose or similar material, if used, should be about 1 to about 6 grams per liter of bath.
  • a weighed amount of the carrier resin is solubilized or otherwise dispersed by blending with an aqueous solution of the base, e.g., 1 normal solution of NaOH.
  • sodium hydroxide solution is advantageously added slowly to the resin and mixed thoroughly to produce a homogeneous dispersion. For each gram of resin non-volatiles, about 0.75 ml. of the sodium hydroxide solution is added. Deionized water (maximum conductivity of 40 micro IIlhOs) is then added to produce the desired bath volume. Finally, weighed amounts of particulate metal and hydroxy propyl methyl cellulose or other thickener, if used, are added to the aqueous resin dispersion. Continued mechanical agitation of the bath is advantageously maintained from this point until after electrodeposition is complete to minimize settling and gas evolution.
  • (F) COATING BY ELECTRODEPOSITION The pretreated part to be coated is immersed in the coating bath while maintaining a positive D.C. potential, in the range of 10 to 450, advisedly in the range of 10 to 200, and preferably in the range of 10 to 50 volts for a time in the range of 0.5 to 5 minutes to obtain a coating having average depth in the range of about 2 to about 10, commonly about 3 to about 7, mils, depending on the density of the film which is a function of the coarseness and shape of the metal particles, the volume ratio of metal particles to organic film-former in the deposited film, the impressed potential of electrodeposition, the time of deposition, and the composition of the substrate.
  • a positive D.C. potential in the range of 10 to 450, advisedly in the range of 10 to 200, and preferably in the range of 10 to 50 volts for a time in the range of 0.5 to 5 minutes to obtain a coating having average depth in the range of about 2 to about 10, commonly about 3 to about 7, mils,
  • the heat diffusion step is carried out in a vacuum of about 10 mm. Hg or greater, i.e., a lower pressure, preferably at a pressure not in excess of 5 10- mm. Hg.
  • the heat diffuser is carried out in a hydrogen atmosphere having dew point below about 75 F.
  • the coated article In firing, the coated article is supported on a support that does not undergo chemical reaction in the firing process, e.g., aluminum oxide.
  • the following procedure can be used.
  • the coated part is charged to the heating zone.
  • the vacuum is established and the heating zone is heated to 1000-1200 F. and held at that temperature until the initial vacuum is restored and the organic portion of the coating has decomposed and the vapors therefrom are removed from the heating zone before heating the part to diffusion temperature.
  • Diffusion is carried out by heating the article to a temperature above the melting point of the deposited particlate metal layer.
  • the diffusion temperature will ordinarily be in the range of about 1300 to about 2200 F., commonly between about 1600 and about 1900 F. for nickel alloys and cobalt alloys for a time in the range of about 2 to about 8, preferably about 4 to about 8, hours or until the desired diffusion of metal from the deposit into the alloy substrate is achieved.
  • the iron alloys are commonly heated to a temperature above about 1400 F. for a similar period of time.
  • Diffused coating thickness can be determined on parts by microscopic inspection of cross sectional test samples.
  • the average depth will ordinarily be in the range of about 2 to about 5, preferably about 3 to about 4, mils.
  • the actual dimensional change per side of a coated part due to coating application would normally be 50% :25 of the dilfused coating thickness.
  • Electrodeposition A coating bath of the dispersion of (D) above is placed in an electrodeposition cell and in contact with the anode thereof.
  • a nickel alloy substrate is grit blasted at 80 p.s.i., immersed in this bath, and electrically connected as the cathode of this cell.
  • the composition of the cathode is as follows:
  • a potential of 100 volts is applied for 1 minute and a 2 mil thick deposit is formed.
  • This procedure is repeated except that the coating time is 2 minutes, and a deposit of about 3 mils thickness is formed.
  • the coated substrates are rinsed with water and oven dried at 180 F. for 30 minutes. They are then separately charged to the heating zone, a vacuum of about 5x10" mm. Hg is established, and the heating zone is heated to 1200 F. and held at that temperature until the initial vacuum is restored and the organic portion of the coating has decomposed and the vapors therefrom are removed from the heating zone before heating the part to a difiusion temperature of 1900" F. Such vacuum and such temperature are maintained for 8 hours and the substrate is cooled in vacuum.
  • an inert gas such as nitrogen or helium.
  • hydrogen is introduced and the part is heated to 1000 F. and held for 15 minutes to purge the decomposition products of the organic portion of the coating from the retort.
  • the part is subsequently heated to 1900 F. and held for 8 hours. Cooling is carried out in the vacuum.
  • Example 2 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a carbon steel alloy, alloy A described in detail in Table I and the temperature of diffusion is about 1400 F.
  • Example 3 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is an austenitic stainless steel, alloy B described in detail in Table I, and the temperature of diffusion is about 1500 F.
  • Example 4 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is martensitic stainless steel, alloy C described in detail in Table I, and the temperature of diffusion is about 1400 F.
  • Example 5 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a ferritic stainless steel alloy, alloy D described in detail in Table I, and the temperature of diffusion about 1400 F.
  • Example 6 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a ductile nodular iron alloy, alloy E described in detail in Table I, and the temperature of diffusion is about 1400 F.
  • Example 7 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a wrought cobalt-base alloy, alloy I described in detail in Table II, and the temperature of diffusion is about 1920 F.
  • EXAMPLE 8 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a cast cobalt-base alloy, alloy L described in detail in Table II, and the temperature of diffusion is about 1875 F. This procedure is repeated except for the difference that the diffusion temperature is about 2100 F.
  • Example 9 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a wrought age-hardenable Ni-base alloy, alloy H described in detail in Table II, and the temperature of diffusion is about 1950 F. This procedures is repeated except for the difference that the tem perature of diffusion is about 1600 F.
  • Example 10 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a high chromium level, wrought nickel-base alloy, alloy G described in detail in Tzbble II, and the temperature of diffusion is about 18 0 F.
  • Example 11 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a medium chromium level, wrought nickel-base alloy, alloy F described in detail in Table II, and the temperature of diffusion is about 1950 F.
  • Example 12 The procedures of Example 1 are repeated except for the differences that the nickel-base alloy cathode is replaced with a cathode that is a wrought cobalt-base alloy, alloy K described in detail in Table II, and the temperature of diffusion is about 1600 F. This procedure is repeated except that the temperature of diffusion is about 1925 F.
  • Electrodeposition This bath is placed in an electrodeposition cell and in contact with the cathode thereof.
  • the first substrate described in detail in Example 1 is electrically connected with this cell as anode and immersed in the bath after first being sand blasted at 80 p.s.i.
  • An impressed DC potential of 50 volts is applied for 30 seconds and a coating averaging about 4-5 mils thickness is obtained upon the anode substrate. Two such anodes are thus prepared.
  • An impressed DC potential of 100 volts is applied for 30 seconds and a coating averaging about 6-7 mils thickness is obtained on a duplicate anode. Two such coated are thus prepared.
  • the coatings are rinsed in water and oven dried as in Example 1. Finally, the first set of coatings are heat diffused in vacuum employed in Example 1 and the second set of coatings are heat diffused in hydrogen as described in Example 1.
  • EXAMPLE 14 The procedures of Example 13 are repeated except for the difference that the sodium hydroxide in the electrodeposition bath is replaced with 2.9 grams of diethylamine.
  • Methacrylic acid 2 2-ethyl hexyl acrylate 630
  • Styrene 1034 Hydroxy ethyl methacrylate 210
  • Azobisisobutyronitrile 21 (e)
  • the temperature of 140 C. is held for 0.5 hour and the resin recovered.
  • the resin has an acid value of about 71 and an XY Gardener-Holdt viscosity at 50% solids in butyl Cellosolve.
  • EXAMPLE 16 The procedures of Example 1 and 13 are repeated except for the difference that the particulate metal electrodeposited and diffused is a mixture of 62 weight percent aluminum powder and 38 weight percent platinum powder.
  • EXAMPLE 17 The procedures of Examples 1 and 13 are repeated except for the difference that the particulate metal electrodeposited and diffused is a mixture of weight percent aluminum powder and 25 weight percent chromium powder.
  • EXAMPLE 18 The procedures of Examples 1 and 13 are repeated except for the difference that the particulate metal electrodeposited and diffused is a mixture of 60 weight percent aluminum powder and 40 weight percent palladium powder.
  • EXAMPLE 22 The procedure of Examples 1 and 13 are repeated except that the temperature of heat diffusion is about 1350 F.
  • the weight ratio of metal particles to film-former'in the coating deposited is in excess of 3:1 and preferably in excess of 4: 1.
  • the coated substrate Prior to diffusion of the metal of the coating into the surface of the substrate, the coated substrate is heated in a heating zone in an ambient essentially inert to the metal particle in the coating to a decomposition temperature above the temperature required to decompose the organic film-former in the coating and below the diffusion temperature.
  • a decomposition temperature above the temperature required to decompose the organic film-former in the coating and below the diffusion temperature. This will ordinarily be between about 800 F. and about 1215 F., more commonly in the range of about 1000 F. and about 1200 F.
  • This decomposition temperature is maintained until the organic film-former in the coating is essentially decomposed and gaseous products of such film-former are formed in the heating zone. These gaseous products are then essentially evacuated from the heating zone.
  • the ambient is maintained and the temperature of the heating zone is raised to the diffusion temperature. For practical results, this will be at least about 50 F. above the melting point of aluminum.
  • the diffusion temperature is maintained for a time in excess of
  • a process for modifying the surface of a metal substrate of which the major component by weight is selected from cobalt, nickel and iron and constitutes at least 40 weight percent of said substrate comprising electrocodepositing upon said metal substrate a coating of (I) metal particles having average diameter in the range of 0.5 to 20 microns selected from (A) aluminum comprising particles wherein the weight ratio of aluminum to other metal is in the range of 200:1 to 1:3 and which are selected from (1) aluminum alloy particles,
  • said substrate constitutes one of two electrodes in contact with said coating bath, and wherein (A) the weight ratio of metal particles in said bath to film-former in said bath is maintained above 3:1,
  • the concentration of film-former in said bath is maintained in the range of about 0.2 to about 7 weight percent
  • a process in accordance with claim 1 wherein said concentration of film-former in said bath is maintained in the range of about 0.2 to about 2 weight percent.
  • a process for modifying the surface of a metal substrate of which the major component by weight is selected from cobalt, nickel and iron and constitutes at least 40 weight percent of said substrate comprising electrocodepositing upon said metal substrate a 3 to 7 mil coating of (I) aluminum particles having average diameter in the range of 0.5 to 20 microns, and
  • said substrate constitutes one of two electrodes in contact with said coating bath, and wherein (A) the weight ratio of aluminum particles in said bath to film-former in said bath is maintained above 3:1,
  • the concentration of film-former in said bath is maintained in the range of about 0.2 to about 7 weight percent
  • a process in accordance with claim 9 wherein said diffusion temperature is in the range of about 1550 F. to about 1950 F. and is maintained for a time in the range of 2 to 8 hours.
  • a process in accordance with claim 9 wherein said ambient is a hydrogen atmosphere having dew point below about F.
  • a process in accordance with claim 9 wherein said decomposition temperature is in the range of about 800 F. to about 1215 F.
  • a process in accordance with claim 9 wherein said decomposition temperature is in the range of about 1000 F. to about 1200 F.

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US20060205855A1 (en) * 2004-11-12 2006-09-14 Zhiyong Xia Polyester polymer and copolymer compositions containing metallic titanium particles
US20060222795A1 (en) * 2005-03-31 2006-10-05 Howell Earl E Jr Polyester polymer and copolymer compositions containing particles of one or more transition metal compounds
US20060287472A1 (en) * 2005-06-16 2006-12-21 Jernigan Mary T High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
US20070066719A1 (en) * 2005-09-16 2007-03-22 Zhiyong Xia Polyester polymer and copolymer compositions containing particles of titanium nitride and carbon-coated iron
US20070066714A1 (en) * 2005-09-16 2007-03-22 Zhiyong Xia Polyester polymer and copolymer compositions containing carbon-coated iron particles
US20070260002A1 (en) * 2006-05-04 2007-11-08 Zhiyong Xia Titanium nitride particles, methods of making them, and their use in polyester compositions
US20080058495A1 (en) * 2006-09-05 2008-03-06 Donna Rice Quillen Polyester polymer and copolymer compositions containing titanium and yellow colorants
US7655746B2 (en) 2005-09-16 2010-02-02 Eastman Chemical Company Phosphorus containing compounds for reducing acetaldehyde in polyesters polymers
US20110300405A1 (en) * 2010-06-03 2011-12-08 General Electric Company Oxidation resistant components and related methods
US20130243036A1 (en) * 2010-03-31 2013-09-19 Cambridge Enterprise Limited Thermocouple apparatus and method

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US3823093A (en) * 1972-06-30 1974-07-09 Du Pont Silver capacitor metallizations containing copper polynary oxides
FR2644361B1 (fr) * 1989-03-14 1991-05-24 Pechiney Rech Gie Procede de fabrication d'une membrane semi-permeable sur un support conducteur poreux par electrophorese
FR2655275B2 (fr) * 1989-03-14 1992-02-21 Pechiney Recherche Perfectionnement au procede de fabrication d'un tube poreux revetu interieurement d'une membrane semi-permeable par electrophorese.
FR2682401B1 (fr) * 1991-10-09 1993-11-26 Sochata Procede de depot electrophoretique de poudre metallique pour rechargement de pieces par brasage-diffusion et bain utilise.
US6755613B1 (en) * 1999-05-14 2004-06-29 Siemens Aktiengesellschaft Component and method for producing a protective coating on a component
JP5857794B2 (ja) * 2012-02-27 2016-02-10 株式会社Ihi 拡散層付き金属材料ならびにその製造方法
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US20060052504A1 (en) * 2004-09-03 2006-03-09 Zhiyong Xia Polyester polymer and copolymer compositions containing metallic nickel particles
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US20060106146A1 (en) * 2004-11-12 2006-05-18 Zhiyong Xia Polyester polymer and copolymer compositions containing titanium nitride particles
US8039577B2 (en) * 2004-11-12 2011-10-18 Grupo Petrotemex, S.A. De C.V. Polyester polymer and copolymer compositions containing titanium nitride particles
US20060205855A1 (en) * 2004-11-12 2006-09-14 Zhiyong Xia Polyester polymer and copolymer compositions containing metallic titanium particles
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US20080153962A1 (en) * 2004-11-12 2008-06-26 Eastman Chemical Co. Polyester polymer and copolymer compositions containing titanium nitride particles
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US20060287472A1 (en) * 2005-06-16 2006-12-21 Jernigan Mary T High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
US8557950B2 (en) 2005-06-16 2013-10-15 Grupo Petrotemex, S.A. De C.V. High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
US8987408B2 (en) 2005-06-16 2015-03-24 Grupo Petrotemex, S.A. De C.V. High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
US7776942B2 (en) 2005-09-16 2010-08-17 Eastman Chemical Company Polyester polymer and copolymer compositions containing particles of titanium nitride and carbon-coated iron
US20070066714A1 (en) * 2005-09-16 2007-03-22 Zhiyong Xia Polyester polymer and copolymer compositions containing carbon-coated iron particles
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US20070066719A1 (en) * 2005-09-16 2007-03-22 Zhiyong Xia Polyester polymer and copolymer compositions containing particles of titanium nitride and carbon-coated iron
US20070260002A1 (en) * 2006-05-04 2007-11-08 Zhiyong Xia Titanium nitride particles, methods of making them, and their use in polyester compositions
US20080058495A1 (en) * 2006-09-05 2008-03-06 Donna Rice Quillen Polyester polymer and copolymer compositions containing titanium and yellow colorants
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Also Published As

Publication number Publication date
DE2263520B2 (de) 1979-07-19
FR2166050A1 (enrdf_load_stackoverflow) 1973-08-10
IT973655B (it) 1974-06-10
DE2263520C3 (de) 1980-03-20
FR2166050B1 (enrdf_load_stackoverflow) 1975-06-20
JPS5526705B2 (enrdf_load_stackoverflow) 1980-07-15
DE2263520A1 (de) 1973-07-12
JPS4873342A (enrdf_load_stackoverflow) 1973-10-03
GB1418655A (en) 1975-12-24
CA984332A (en) 1976-02-24

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