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US3930085A Expired / Lapsed US ⏱️ 0.0 years remaining

Preparation of thermal barriers

Assignee: United States Department of the Army
•
Filing: 1975-02-13
•
Granted: 1975-12-30
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Expires: 1995-02-13
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Abstract

Abstract Method is disclosed for preparation of a thermal barrier for a polyimide substrate. The thermal barrier meets the requirements of withstanding a front surface exposure temperature of 3,000*F for 90 seconds without permitting a rear surface temperature of above 700*F. The thermal barrier structure has a honeycomb core or a foamed ceramic core that is coated with a zircon-silica composition which fills or coats the core. From one to four laminating layers of facing sheets of quartz fabric that is impregnated with a zircon-silica composition is employed to produce a reflective front facesheet. The rear surface of the thermal barrier is comprised of a layer of a glass-polyimide laminate which is attached using a polyimide or ceramic adhesive to form a back facesheet.

Inventors

  • 👤 Walter T Pasiuk

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 22:51
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/01; C04B35/48; C04B35/481; B; B32; B32B; B32B3/00; B32B3/10; B32B3/12; B32B9/00; B32B9/04; B32B9/047; B64; B64G; B64G1/00; B64G1/22; B64G1/52; B64G1/58; C04B35/622; C04B35/626; C04B35/62605; C04B35/62625; C04B35/6263; C04B35/6264; C04B35/62645; C04B35/62655; C04B35/6269; C04B35/71; C04B35/78; C04B35/80; C04B35/82; C04B37/00; C04B37/003; C04B37/005; B32B2260/00; B32B2260/02; B32B2260/021; B32B2307/00; B32B2307/30; B32B2307/306; B32B2307/40; B32B2307/416; C04B2235/00; C04B2235/02; C04B2235/30; C04B2235/32; C04B2235/3201; C04B2235/34; C04B2235/3418; C04B2235/3427; C04B2235/50; C04B2235/52; C04B2235/5208; C04B2235/5216; C04B2235/522; C04B2235/5228; C04B2235/5264; C04B2235/65; C04B2235/656; C04B2235/6567; C04B2235/658; C04B2235/6581; C04B2235/70; C04B2235/80; C04B2237/00; C04B2237/02; C04B2237/04; C04B2237/06; C04B2237/062; C04B2237/09; C04B2237/30; C04B2237/32; C04B2237/34; C04B2237/341; C04B2237/345; C04B2237/348; C04B2237/36; C04B2237/363; C04B2237/38; Y; Y10; Y10T; Y10T428/00; Y10T428/24; Y10T428/24149; Y10T428/249921; Y10T428/249953; Y10T428/249967; Y10T428/249969; Y10T428/24997; Y10T428/249986; Y10T428/249987; Y10T428/24999; Y10T428/249991; Y10T428/26; Y10T428/261

Claims Analysis

Total Claims: 6
Claim 1
Independent Claim 769 words
A METHOD FOR PREPARATION OF THERMAL BATTERIES THAT EMPLOY EITHER A HONEYCOMB CORE HAVING A PREDETERMINED CELL SIZE WITH THE HONEYCOMB CORE BEING CONSTRUCTED OF A REINFORCED PLASTIC SELECTED FROM GLASS-PHENOLIC, GLASS-POLYIMIDE, AND NYLONPHENOLIC; OR A FIBER REINFORCED CERAMIC FOAM BLOCK CORE, SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE FORMED BY MOLDING AND CURING A CERAMIC SLURRY FORMULATION COMPOSED OF 50 PERCENT BY WEIGHT OF A LAMINATE CERAMIC POWDER CONTAINING 77.3 PERCENT BY WEIGHT ZIRCON AND 22.7 PERCENT BY WEIGHT SILICA, 42 PERCENT BY WEIGHT OF SODIUM SILICATE LIQUID, AND 8 PERCENT BY WEIGHT OF ALUMINA-SILICA CERAMIC REINFORCING FIBERS, SAID ALUMINA-SILICA CERAMIC REINFORCING FIBERS HAVING A DIAMETER OF ABOUT 2.8 MICRONS AND HAVING RANDOWM LENGTHS THAT ARE RETAINED ON 30 MEXH SIZE SCREEN, SAID FIBERS BEING PREPARED USE BY MIXING FOR ABOUT 3 HOURS WITH A WATER/TOLUENE SOLUTION CONTAINING 9 PARTS WATER AND 1 PART TOLUENE, FOLLOWED BY DECANTING THE SOLUTION, AND DRYING THE FIBERS IN AIR CIRCULATING OVEN AT 400*F UNTIL DRY, SAID CURING OF CERAMIC SLURRY FORMULATION BEING ACCOMPLISHED BY AIR CURING 16 HOURS AT ROOM TEMPERATURE, 3 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, 2 HOURS AT 400*F, SAID METHOD FOR PREPARATION OF THERMAL BARRIERS COMPRISING: I. PROVIDING SAID HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE AND PREPARING THE SURFACE THEREOF BY CLEANING AND ETCHING WHICH IS ACCOMPLISHED BY CLEANING AND ETCHING IN HOT 5 PERCENT SODIUM HYDROXIDE SOLUTION OF ABOUT 200*F AND FOLLOWED BY WASHING WITH DISTILLED OR DEIONIZED WATER; II. DIPPING SAID HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A CERAMIC MIX SLURRY COMPOSED OF 80 PARTS BY WEIGHT OF CASTING MIXED OXIDE CERAMIC CONTAINING 90 PERCENT ZIRCON AND 10 SILICA, 15 PARTS BY WEIGHT OF SODIUM SILICATE LIQUID, AND SUFFICIENT QUANTITY OF WATER IN AMOUNT OF 5 PARTS OR MORE TO ADJUST VISCOSITY OF CERAMIC MIX TO ENABLE A THIN UNIFORM COATING TO BE APPLIED DURING SAID DIPPING, REPEAT SAID DIPPING WHILE SAID HONEYCOMB CORE OR SAID FILM REINFORCED CERAMIC FOAM BLOCK CORE IS TURNED OVER 180* TO ACHIEVE COMPLETE COVERAGE, AND THEN WHILE HOLDING SAID HONEYCOMB CORE OR SAID REINFORCED CERAMIC FOAM BLOCK CORE IN A HORIZONTAL POSITION, TAPPING SAID CORE TO REMOVE ANY EXCESS CERAMIC MIX; III. PLACING SAID COATED HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A HORIZONTAL POSITION OR A RIGID DRYING RACK AND TURN 180* EVERY FEW MINUTES UNTIL SAID CERAMIC MIX HARDENS AND NO MORE FLOW IS EVIDENT AND THEN AIR DRYING AT ROOM TEMPERATURE FOR A MINIMUM OF 16 HOURS; IV. CLAMPING SAID AIR DRIED, COATED HONEYCOMB CORE OR SAID AIR DRIED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE TO DRYING FORMS AFTER FIRST APPLYING HIGH HEAT OF 400*-500*F WITH HOT AIR GUN RAPIDLY TO ANY AREA TO BE SHAPED, AND THEN PLACING SAID DRYING FORM WITH SAID CLAMPED, AIR DRIED, COATED HONEYCOMB CORE OR SAID CLAMPED, AIR DRIED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A HOT AIR CIRCULATING OVEN AND CURING FOR 2 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, AND 4 HOURS AT 400*F, AND ALLOWING TO COOL TO ROOM TEMPERATURE; V. COMPLETING A LAMINATING PROCEDURE FOR THE TOP SURFACE TO FORM A FRONT FACESHEET FOR SAID CURED, COATED HONEYCOMB CORE OR SAID CURED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE BY FIRST WETTING THE TOP SURFACE WITH SAID CERAMIC MIX SLURRY, SANDTHEN APPLYING SAID CERAMIC MIXSLURRY TO EACH SURFACE OF A QUARTZ FABRIC AND RUBBING THE SLURRY INTO SAID QUARTZ FABRIC TO IMPREGNATE SAID QUARTZ FABRIC WITH SAID SLURRY AND THEN WIPING THE EXCESS SLURRY OFF, AND SUBSEQUENTLY, LAYING A FIRST PLY OF THE IMPREGNATED QUARTZ FABRIC ON THE TOP SURFACE OF SAID CURED, COATED, HONEYCOMB CORE OR SAID CURED, COATED, FIBER REINFORCED CERAMIC FOAM BLOCK CORE, AND REPEATING SAID LAMINATING PROCEDURE UNTIL AT LEAST FOUR PILES OF IMPREGNATED QUARTZ FABRIC ARE LAID ONTO FORM AN UNCURED FRONT FACESHEET ON THE THERMAL BARRIER ASSEMBLY; VI. PREPARING SAID THERMAL BARRIER ASSEMBLY FOR VACUUM BAG MOLDING AND CURING SAID THERMAL BARRIER ASSEMBLY UNDER VACUUM FOR 16 HOURS AT ROOM TEMPERATURE, THEN IN A HOT AIR CIRCULATING OVEN FOR 3 HOURS AT 3 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, 2 HOURS AT 400*F, AND THEN ALLOWING SAID THERMAL BARRIER ASSEMBLY TO COOL TO ROOM TEMPERATURE AND THEN REMOVING THE THERMAL BARRIER ASSEMBLY; AND THEREAFTER, VII. PROVIDING A BACK FACESHEET FOR THE REAR SURFACE OF SAID THERMAL BARRIER ASSEMBLY WHICH COMPRISES ATTACHING A GLASS-POLYIMIDE LAMINATE TO SAID REAR SURFACE WITH AN ADHESIVE SELECTED FROM A POLYIMIDE-FILM ADHESIVE AND AN CERAMIC ADHESIVE.
Claim 2
Independent Claim 769 words
A METHOD FOR PREPARATION OF THERMAL BATTERIES THAT EMPLOY EITHER A HONEYCOMB CORE HAVING A PREDETERMINED CELL SIZE WITH THE HONEYCOMB CORE BEING CONSTRUCTED OF A REINFORCED PLASTIC SELECTED FROM GLASS-PHENOLIC, GLASS-POLYIMIDE, AND NYLONPHENOLIC; OR A FIBER REINFORCED CERAMIC FOAM BLOCK CORE, SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE FORMED BY MOLDING AND CURING A CERAMIC SLURRY FORMULATION COMPOSED OF 50 PERCENT BY WEIGHT OF A LAMINATE CERAMIC POWDER CONTAINING 77.3 PERCENT BY WEIGHT ZIRCON AND 22.7 PERCENT BY WEIGHT SILICA, 42 PERCENT BY WEIGHT OF SODIUM SILICATE LIQUID, AND 8 PERCENT BY WEIGHT OF ALUMINA-SILICA CERAMIC REINFORCING FIBERS, SAID ALUMINA-SILICA CERAMIC REINFORCING FIBERS HAVING A DIAMETER OF ABOUT 2.8 MICRONS AND HAVING RANDOWM LENGTHS THAT ARE RETAINED ON 30 MEXH SIZE SCREEN, SAID FIBERS BEING PREPARED USE BY MIXING FOR ABOUT 3 HOURS WITH A WATER/TOLUENE SOLUTION CONTAINING 9 PARTS WATER AND 1 PART TOLUENE, FOLLOWED BY DECANTING THE SOLUTION, AND DRYING THE FIBERS IN AIR CIRCULATING OVEN AT 400*F UNTIL DRY, SAID CURING OF CERAMIC SLURRY FORMULATION BEING ACCOMPLISHED BY AIR CURING 16 HOURS AT ROOM TEMPERATURE, 3 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, 2 HOURS AT 400*F, SAID METHOD FOR PREPARATION OF THERMAL BARRIERS COMPRISING: I. PROVIDING SAID HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE AND PREPARING THE SURFACE THEREOF BY CLEANING AND ETCHING WHICH IS ACCOMPLISHED BY CLEANING AND ETCHING IN HOT 5 PERCENT SODIUM HYDROXIDE SOLUTION OF ABOUT 200*F AND FOLLOWED BY WASHING WITH DISTILLED OR DEIONIZED WATER; II. DIPPING SAID HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A CERAMIC MIX SLURRY COMPOSED OF 80 PARTS BY WEIGHT OF CASTING MIXED OXIDE CERAMIC CONTAINING 90 PERCENT ZIRCON AND 10 SILICA, 15 PARTS BY WEIGHT OF SODIUM SILICATE LIQUID, AND SUFFICIENT QUANTITY OF WATER IN AMOUNT OF 5 PARTS OR MORE TO ADJUST VISCOSITY OF CERAMIC MIX TO ENABLE A THIN UNIFORM COATING TO BE APPLIED DURING SAID DIPPING, REPEAT SAID DIPPING WHILE SAID HONEYCOMB CORE OR SAID FILM REINFORCED CERAMIC FOAM BLOCK CORE IS TURNED OVER 180* TO ACHIEVE COMPLETE COVERAGE, AND THEN WHILE HOLDING SAID HONEYCOMB CORE OR SAID REINFORCED CERAMIC FOAM BLOCK CORE IN A HORIZONTAL POSITION, TAPPING SAID CORE TO REMOVE ANY EXCESS CERAMIC MIX; III. PLACING SAID COATED HONEYCOMB CORE OR SAID FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A HORIZONTAL POSITION OR A RIGID DRYING RACK AND TURN 180* EVERY FEW MINUTES UNTIL SAID CERAMIC MIX HARDENS AND NO MORE FLOW IS EVIDENT AND THEN AIR DRYING AT ROOM TEMPERATURE FOR A MINIMUM OF 16 HOURS; IV. CLAMPING SAID AIR DRIED, COATED HONEYCOMB CORE OR SAID AIR DRIED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE TO DRYING FORMS AFTER FIRST APPLYING HIGH HEAT OF 400*-500*F WITH HOT AIR GUN RAPIDLY TO ANY AREA TO BE SHAPED, AND THEN PLACING SAID DRYING FORM WITH SAID CLAMPED, AIR DRIED, COATED HONEYCOMB CORE OR SAID CLAMPED, AIR DRIED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE IN A HOT AIR CIRCULATING OVEN AND CURING FOR 2 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, AND 4 HOURS AT 400*F, AND ALLOWING TO COOL TO ROOM TEMPERATURE; V. COMPLETING A LAMINATING PROCEDURE FOR THE TOP SURFACE TO FORM A FRONT FACESHEET FOR SAID CURED, COATED HONEYCOMB CORE OR SAID CURED, COATED FIBER REINFORCED CERAMIC FOAM BLOCK CORE BY FIRST WETTING THE TOP SURFACE WITH SAID CERAMIC MIX SLURRY, SANDTHEN APPLYING SAID CERAMIC MIXSLURRY TO EACH SURFACE OF A QUARTZ FABRIC AND RUBBING THE SLURRY INTO SAID QUARTZ FABRIC TO IMPREGNATE SAID QUARTZ FABRIC WITH SAID SLURRY AND THEN WIPING THE EXCESS SLURRY OFF, AND SUBSEQUENTLY, LAYING A FIRST PLY OF THE IMPREGNATED QUARTZ FABRIC ON THE TOP SURFACE OF SAID CURED, COATED, HONEYCOMB CORE OR SAID CURED, COATED, FIBER REINFORCED CERAMIC FOAM BLOCK CORE, AND REPEATING SAID LAMINATING PROCEDURE UNTIL AT LEAST FOUR PILES OF IMPREGNATED QUARTZ FABRIC ARE LAID ONTO FORM AN UNCURED FRONT FACESHEET ON THE THERMAL BARRIER ASSEMBLY; VI. PREPARING SAID THERMAL BARRIER ASSEMBLY FOR VACUUM BAG MOLDING AND CURING SAID THERMAL BARRIER ASSEMBLY UNDER VACUUM FOR 16 HOURS AT ROOM TEMPERATURE, THEN IN A HOT AIR CIRCULATING OVEN FOR 3 HOURS AT 3 HOURS AT 150*F, 2 HOURS AT 250*F, 2 HOURS AT 350*F, 2 HOURS AT 400*F, AND THEN ALLOWING SAID THERMAL BARRIER ASSEMBLY TO COOL TO ROOM TEMPERATURE AND THEN REMOVING THE THERMAL BARRIER ASSEMBLY; AND THEREAFTER, VII. PROVIDING A BACK FACESHEET FOR THE REAR SURFACE OF SAID THERMAL BARRIER ASSEMBLY WHICH COMPRISES ATTACHING A GLASS-POLYIMIDE LAMINATE TO SAID REAR SURFACE WITH AN ADHESIVE SELECTED FROM A POLYIMIDE-FILM ADHESIVE AND AN CERAMIC ADHESIVE.
Claim 3
Dependent Claim 87 words
The method of claim 1 wherein said laminating procedure employs four plies of said impregnated quartz fabric in forming said facesheet on the top surface of said cured, coated honeycomb core and wherein said glass-polyimide laminate is comprised of one layer of quartz fabric impregnated with a polyimide resin that is attached to said rear surface with a polyimide-film adhesive, and wherein said honeycomb core has a predetermined cell size of about three-eighths inch and wherein said honeycomb is constructed of a reinforced plastic selected from glass-phenolic.
Claim 4
Dependent Claim 98 words
A thermal barrier prepared in accordance with the method as set forth in claim 2 and wherein said thermal barrier has a thickness from about 0.4 inch to about 0.5 inch with said front facesheet being about 0.06 inch thick and with said back facesheet being about 0.015 inch thick, said thermal barrier characterized by having a weight of about 2.7 to about 2.9 pounds per square foot and having a dielectric constant of about 1.84 at 3 GHz for the honeycomb core and having a dielectric constant of about 4.0 at 3 GHz for the front facesheet.
Claim 5
Dependent Claim 64 words
The method of claim 1 wherein said laminating procedure employs four plies of said impregnated quartz fabric in forming said facesheet on the top surface of said cured, coated fiber reinforced ceramic foam block core and wherein said glass-polyimide laminate is comprised of one layer of quartz fabric impregnated with a polyimide resin that is attached to said rear surface with a polyimide-film adhesive.
Claim 6
Dependent Claim 76 words
A thermal barrier prepared in accordance with the method as set forth in claim 4 and wherein said thermal barrier has a thickness from about 0.4 inch to about 0.5 inch thick with said front facesheet being about 0.06 inch thick and with said back facesheet being about 0.015 inch thick, said thermal barrier characterized by a weight of about 3 pounds per square foot and having a dielectric constant of about 2.7 at 3 GHz.

References Cited (Backward Citations)

US3235441A Cited
US3513051A Cited
US3703422A Cited
US3553054A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-12-29 1979-06-30 1979-12-30 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-12-29 1983-06-30 1983-12-30 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-12-29 1987-06-30 1987-12-30 $7700.00 Window Closed / Lapsed

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