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WO1999035665A1 - Ruban metallique pour processeur a faisceau d'electrons - Google Patents

Ruban metallique pour processeur a faisceau d'electrons Download PDF

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Publication number
WO1999035665A1
WO1999035665A1 PCT/US1999/000233 US9900233W WO9935665A1 WO 1999035665 A1 WO1999035665 A1 WO 1999035665A1 US 9900233 W US9900233 W US 9900233W WO 9935665 A1 WO9935665 A1 WO 9935665A1
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WO
WIPO (PCT)
Prior art keywords
foil
electron beam
titanium alloy
window
cold
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1999/000233
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English (en)
Inventor
Joseph E. Kotwis
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
EIDP Inc
Original Assignee
EI Du Pont de Nemours and Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Publication of WO1999035665A1 publication Critical patent/WO1999035665A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J33/00—Discharge tubes with provision for emergence of electrons or ions from the vessel; Lenard tubes
    • H01J33/02—Details
    • H01J33/04—Windows

Definitions

  • This invention relates to a novel window foil comprising a titanium alloy exhibiting excellent cold reliability, as well as a combination of excellent oxidation resistance and improved mechanical properties at high temperatures, for use in electron beam processors.
  • EBP electron beam processor
  • the electron beam processor is used in various applications including crosslinking and grafting of polymeric materials, curing of coatings and inks, pasteurization of foodstuff, sterilization of medical products, etc. and so on, wherein the electrons pass through a thin window foil to reach the product treatment area.
  • An electron beam processor typically comprises: a) a power supply, b) an electron emitter, c) an accelerator for shaping the emitted particles into a beam and for directing and accelerating the energized particle beam toward an irradiation window, d) an irradiation window comprising a metal foil, e) a window support structure which provides mounting and cooling for the window foil, and f) a vacuum chamber from which air molecules are removed so air cannot interfere with the generation of the particle beam.
  • Electron beam energy is expressed by the acceleration voltage, which is typically in the range of 100 kV to 10,000 kV.
  • the difference between the pressure on the inside of the window foil and the outside is typically 1 atm, and can be as high as 10 atms or more in some applications.
  • the window foil in an EBP is typically made of a low atomic number material to minimize the absorption of electrons.
  • the foil must be vacuum-tight and capable of withstanding the pressure differentials in the system. In order to achieve optimum efficiency, the foil should be very thin. Additionally, the foil should be capable of withstanding high temperatures of 600°F or more.
  • Titanium is chemically active at elevated temperatures and will oxidize in air, resulting in the formation of a scale. Hence, the foil undergoes severe corrosion damage by reaction with the atmosphere or special gas outside of the chamber. Ti and its alloys have the tendency to creep at elevated temperatures.
  • ⁇ Creep (Met.) a time-dependent plastic deformation of metals under steady load, which leads to eventual rupture of the metals).
  • the window foil is subject to relatively high stresses and deformed by the pressure differential between the chamber and the product treatment area.
  • the thin foil is heated by the thermions generated during the passage of the electron beams, raising the foil temperature up to 400°F or more.
  • the stress created by a combination of the pressure differential and the high temperature causes the foil to rupture after a short period of time.
  • U.S. Patent No. 5,486,703 relates to an electron beam window with improved cooling design, employing a window foil of pure titanium or an alpha titanium alloy similar to a grade 9 (3%A1 and 1% V).
  • U.S. Patent No. 4,362,965 discloses an improved support configuration for the window and evaluates various materials for window foils.
  • the window is a complex foil composite comprising: a) a polyester film and b) a low Z metal film laminated with polyester or vapor deposited on the polyester film, with Z referring to atomic number.
  • a polyethylene crosslinking application typically runs at high energy level with a voltage of 150 to 500kV and a current level between 0.4 and 1.5 Ampere, and an elevated foil temperature of 400°F or more.
  • a very thin window foil having a thickness of .005" or less is often used to allow effective electron beam penetration.
  • the thin window foil routinely fails after a short period of time in service due to creep fatigue and corrosion. The foil failure requires excessive downtime to remove the old window foil and replace it with a new one.
  • the present invention relates to method of constructing a window foil for use with electron beam processors.
  • the invention resides in the discovery that an alpha-beta or essentially beta titanium alloy with inherent good formability and rollability characteristics, after being rolled to a desired thickness to be used as a window foil in an electron beam processor, then subject to heat treatment, develops significantly improved strength and creep resistance at elevated foil temperatures above 400°F, and prolongs the service life of the window considerably over that of a window foil in the prior art.
  • the present invention also provides an electron beam processor and the like which generates an electron beam, and a window foil for use with the electron beam processor.
  • the foil comprises a titanium alloy having inherent good formability and rollability characteristics, heat treated to provide improved strength and creep resistance at elevated foil temperatures above 400°F and prolong the service life of the foil.
  • the foil comprises a titanium alloy having inherent good formability and rollability characteristics, rolled to a thickness of 0.005" or less, and heat treated to provide a window foil with excellent electron penetration, a prolonged service life, as well as improved strength and creep resistance characteristics at elevated foil temperatures above 400°F.
  • a window foil for use with electron beam processors comprising a foil exhibiting significantly improved strength and creep resistance characteristics, and a significantly longer service life than that of a foil constructed from pure titanium and alpha titanium alloys of the prior art.
  • the window foil is made from a titanium alloy with inherent good oxidation resistance, good formability and rollability characteristics, consisting essentially of, in weight percent, molybdenum 14 to 16, niobium 2.5 to 3.5, silicon 0.15 to 0.25, aluminum 2.5 to 3.5, and oxygen 0.12 to 0.16, and balance titanium and incidental impurities.
  • the window foil is conventionally formulated and rolled into sheet stock. The sheet stock is then formed to produce a thin foil suitable for electron beam processors. Subsequent heat treatments provide a window foil with surprisingly improved strength and creep resistance characteristics at high temperatures.
  • Another aspect of the invention is a method of cross-linking polymer materials by electron irradiating, wherein the electron beam irradiator employs a window foil made from a non-alpha titanium alloy having good formability and rollability characteristics, being subject to heat treatment before or after being formed to a desired thickness to develop improved strength and creep resistance characteristics at least twice that of alpha titanium alloys at elevated foil temperatures above 400°F, thus prolonging the service life of the window foil.
  • Figure 1 is a diagram of an embodiment of an electron beam processor.
  • Figures 2A and 2B are perspective views showing various embodiments of a window support structure.
  • Figure 3 is a graph showing the temperature distribution profile in a typical window foil during the irradiation process.
  • Figure 4 is a graph showing the tensile properties of the preferred titanium alloy used in the window foil of the present invention as a function of temperature.
  • Figure 5 is a graph showing the creep properties of the preferred titanium alloy used in the window foil of the present invention as a function of temperature and time under plastic deformation.
  • an EBP includes a housing which provides an enclosure defining a vacuum chamber 1.
  • the interior of a chamber 1 is maintained under vacuum conditions by a vacuum pump 2.
  • electron beam is emitted from an electron generating source 3, which consists of an energized filament made of metal such as tungsten and heated by a power source.
  • the electrons 9 that are generated by this heating are accelerated by an electron accelerating means 20.
  • This electron accelerating means 20 consists of a cathode 4 and anode 5.
  • the electrons are accelerated by the electric field created by high voltage that is applied to cathode 4 and anode 5.
  • the electrons 9 pass out of the chamber through an electron beam permeable window foil 7 and strike the product 8 to be irradiated.
  • Figures 2A and 2B show a perspective view of various embodiments of the window foil 7 and its window supporting frame 6.
  • the typical material of construction for the support structure is copper or beryllium copper, designed to remove heat from the window foil 7.
  • pipes 10 are used to cool the support structure and the window foil 7 with a coolant such as pressurized nitrogen.
  • Other cooling methods may be employed in conjunction with and/or separate from the cooling pipes such as the use of fins or slots between the pipes to increase the heat removal.
  • Figure 2B shows another embodiment of a window, with the window supporting frame 6 being a perforated water-cooled support structure to cool the window foil 7 with water-cooled pipes.
  • other window support structures and cooling methods well known in the art may also be employed as well.
  • FIG. 3 is a profile showing the local axi-symmetric temperature distribution in a window foil during the irradiation process, from the center of the window foil at a temperature of up to 950°F (510°C) to the edge of the window foil adjacent to the window frame at about 400°F (200°C).
  • the thermal profile analysis was done using a computer model of the operation of an electron beam processor. In this computer model, a vacuum load is first applied to a window foil of 0.0006" thick supported by a copper window frame with counter-flow cooling water at 25°C to remove heat from the support frame, then the foil is heated in an irradiation process.
  • a window foil as employed in an electron beam processor as described and modeled above is widely employed in various industrial applications, such as polymerization of materials.
  • electrons are directed toward the surface of a polymeric material, such as a film, and causing chemically reactive species such as free radicals or ions to form.
  • the free radicals are capable of undergoing or participating in a host of secondary reactions such as cross- linking of the polymer, degradation of the polymer, recombination reactions and grafting co-polymerization or polymerization.
  • Titanium has two elemental crystal structures, one is a closed-packed hexagonal (commonly known as alpha), the other a body-centered cubic (commonly known as beta).
  • alpha a closed-packed hexagonal
  • beta a body-centered cubic
  • the beta structure is found only at high temperatures (above the beta transus temperature or also known as the alpha / beta processing temperature), unless the titanium is alloyed to maintain a beta structure at lower temperatures.
  • the addition of other alloying elements to a titanium base will favor either the alpha or beta forms.
  • titanium and alloy compositions there is a range of titanium and alloy compositions, some of which tend to embody the characteristics of alpha and others which are more similar to beta.
  • the window foils in the prior art employ pure titaniums ASTM grades 1 and 2, an alpha rich alloy ASTM grade 9 and variations thereof. Pure titaniums are known for their excellent corrosion characteristics. Alpha rich titanium alloys generally exhibit excellent creep strength characteristics.
  • Titaniums with a mixture of alpha and beta phases ⁇ alpha-beta titaniums, and beta titanium alloys or essentially beta titanium alloys that are heat-treatable are of interest to this invention. These alloys lend themselves to improvement for a window foil application through microstructure tailoring.
  • the microstructure is produced by heat treatment for about over ' ⁇ hour at a temperature below the beta transus temperature to impart the titanium alloy with higher strength, ductility, and resistance to fatigue crack initiation. When the alloys undergo this type of heat treatment and upon cooling from this temperature, they develop a microstructure consisting of fine, equiaxed regions of alpha grains interspersed and bonded with the thin films of beta in the alloys.
  • Suitable alpha-beta titanium alloys include:
  • Ti- 17 Ti-5Al-2Sn-2Zr-4Mo-4Cr with excellent creep resistance properties, known as Ti- 17;
  • Ti-6Al-2Sn-4Zr-6Mo with short-term strength as well as long-term creep strength also known as Ti-6246
  • Ti-4.5Al-3V-2Mo-2Fe is hardenable with superior superplastic formability properties, also known as SP-700;
  • Ti-5Al-5Sn-2Zr-2Mo-0.25Si offers good tensile, stress rupture, and creep resistance properties in high temperature applications of 800 to 1000°F, known as TI-5522-S;
  • Beta and essentially beta alloys contemplated for use according to the invention include the following:
  • Ti-11.5Mo-6Zr-4.5Sn with excellent cold formability and strength potential known as Beta III
  • Ti-15V-3Al-3Cr-3Sn known and readily available as Ti-15-3, with good workability and creep resistance and thermal stability after heat treatments; Ti-8Mo-8V-2Fe-3Al with good formability and age hardening characteristics, known as Ti-8823;
  • a preferred titanium alloy for reasons of operability, commercial availability, and economics is disclosed in U.S. Patent No. 4,980,127 to Titanium Metals Corporation of America ("Timer").
  • Commercial products which incorporate the titanium alloy disclosed in this patent are sold by Timet of 400 Rouser Road, Pittsburgh, PA 15230, under the trademark Timetal® 2 IS.
  • Timet® 21 S, or Ti-15Mo-3Al-2.7Nb-0.25 Si possesses inherent excellent oxidation resistance, creep resistance, and fabricability, as well as surprisingly improved mechanical properties and thermal stability after heat treatments.
  • Timet® 21 S has a nominal composition comprising 15 percent molybdenum, 3 percent aluminum, 3 percent niobium or columbium, and 0.2 percent silicon, with a beta transus temperature about 1485°F or 807°C.
  • the alloy has the following composition in weight percent:
  • molybdenum 14.0 to 16.0;
  • niobium or columbium 2.4 to 3.2;
  • the material may be surface-conditioned by pickling, grinding, trimming and etching in- between the rolling steps as required.
  • the material is then shipped as coils of strips in gages between 0.012" to 0.1" thick.
  • the material is typically provided in the beta solution-treated condition, which precipitates ⁇ to provide strengthening on aging.
  • the thickness of the solution-treated coils is preferably further reduced by either hot or cold forming to the desired thickness for a window foil.
  • the foil should preferably be rolled to the ultimate window thickness in the range of 0.0004" to .005".
  • a thick foil prolongs service life at the expense of energy consumption.
  • Thin window foils maximize electron penetration and lower energy usage at the expense of shortened life.
  • a hot process on a hand-mill using cover sheets to form packs for heat retention is the other viable option.
  • the pack process offers the opportunity to cross-roll to minimize texture, it is labor- intensive and inherently a lower-yield process.
  • a duplex annealing treatment may be employed. The treatment begins with a solution annealing at a temperature about 50 to 100°F below the beta transus temperature of the alloy. Additionally, exposure of solution heat-treated material to temperatures of 500-800°F should be kept to less than one hour to avoid the possibility of embrittlement. If forming temperature exceeds the beta transus temperature (about 1485°F for the preferred Ti alloy Ti- 15Mo-3Al-2.7Nb-0.25Si), time at such temperature should be minimized to avoid excessive grain growth. Therefore, cold forming is most preferred.
  • the material is then annealed at a temperature below the beta transus temperature, on the order of 1450°F or less, and run through a multi-stand rolling mill.
  • the cold rolling and annealing is repeated until a sheet of the desired thickness is achieved.
  • the cold rolling process may incorporate intermediate vacuum or inert gas annealing.
  • the coil is not received from the manufacturer in a solution-treated condition, then the foil is first solution annealed before being cooled in a vacuum tower at a relatively rapid pace.
  • additional annealing treatments such as single or duplex aging treatments are imposed on the foil to achieve improved mechanical properties.
  • the additional aging is done after the foil is rolled to the desired thickness.
  • the heat treatments can be done prior to final thickness with the only expense being the loss of some ductility and thus it is more difficult to roll the foil to the final desired thickness in the downstream process.
  • the titanium foil is preferably wrapped or rolled around a hollow mandrel with a large diameter, forming a roll.
  • the foil should be loosely wrapped around the mandrel and forming a roll having a thickness of V" or so in foil, so as to allow heat penetration to all layers of the roll for an even and uniform aging.
  • the roll is then aged in a vacuum oven or inert gas oven kept at a temperature on the order of about 800°F to about 1300°F, and heated at such a rate that the titanium roll reaches the aging temperature in the absolute minimum amount of time.
  • the window foil of the desired thickness be single-aged at temperatures on the order of about 800°F to about 1300°F for over '/_ hour, preferably for a period ranging from 2 to 16 hours, and most preferably on the order of 8 hours. It is most preferred that the aging should be at 1150°F for 7 hours, then at a reduced temperature of 1100°F for another hour. Aging over 60 hours may provide higher strength, but will decrease ductility and fracture toughness.
  • the titanium roll After aging, the titanium roll should be cooled to room temperature at a preferred cooling rate of about 200°F per hour.
  • a duplex age is recommended.
  • the window foil is initially aged at 800°F to about 1300°F for a period over Vi hour as in the single-aged process described above, then followed by another aging at about 800°F to about 1200°F for at least another Vi hour ("duplex aging").
  • duplex aging is recommended to retain ductility.
  • the high temperature "weakens" the grains relative to the grain boundaries, and the second aging stage stabilizes the grains against embrittlement.
  • the foil be aged for electron beam irradiation applications at temperatures above 400°F to improve mechanical properties of the titanium alloy, and thus the window foil. If the foil is not aged, potential exists for embrittlement in the foil by the precipitation of omega phase or very fine alpha. It is also critical that care be taken during aging to avoid heating too slowly, because this can result in very high strength with concomitant low ductility. Additionally, temperature controls with an upper cutoff be employed to prevent temperature from exceeding beta transus if solution-treated titanium coils are used as the starting materials.
  • the material can be stress relieved without adversely affecting its strength or ductility. Stress relieving treatments decrease undesirable stresses that may result from cold forming or thermal stresses from the heat treatment process. During stress relief, care should be taken to prevent overaging to lower strength. This includes cooling from stress relief temperature to about 900°F at a preferred rate of less than 100°F per hour. Below this temperature, cooling is optional. Oil or water quenching is not recommended since this can induce residual stresses. Vacuum or inert gas furnaces of the electrical resistance type are most preferable for aging the material. Temperature control equipment should be accurate to ⁇ and controllable to within +_15°F. Aging results in a window foil with significantly improved mechanical properties.
  • Ultimate tensile strength of the resulting titanium alloy is on the order of 150-180 Ksi, and ranging upward as high as 210Ksi with ductility still above 2%.
  • Figure 4 serves to demonstrate the tensile strength properties over a wide range of temperatures up to 1100°F (600°C) of the preferred titanium alloy, Ti- 15Mo-3Al-2.7Nb-0.25Si, used in the window foil of the present invention after strip aging at 1100°F for 8 hours.
  • Table 1 is a compilation of data comparing and contrasting the room temperature properties of prior art materials, pure titanium ASTM grades 1, 2, and 3, and alpha titanium alloy ASTM grade 9, with the preferred titanium alloy of the invention before and after heat treatment at various aging temperatures. It should be noted that the higher the aging temperature, the lower the improved yield strength and tensile strength, and the higher the ductility.
  • Figure 5 is a plot that shows the creep results over a wide temperature range for the preferred alloy Ti-15Mo-3Al-2.7Nb-0.25Si, after strip aging at 1100°F for 8 hours.
  • "creep” is shown as a time-dependent plastic deformation of metals under steady load.
  • a window foil employing the preferred titanium alloy, Ti-15Mo-3Al-2.7Nb-0.25Si retains the inherent excellent oxidation resistance properties relative to pure titaniums exhibited by imaged Ti alloys even at high temperatures as shown in Table 4 below: Table 4 - Oxidation resistance at various test temperatures
  • a titanium alloy is formulated having a nominal composition of 15 percent molybdenum, 3 percent aluminum, 3 percent niobium or columbium, and 0.2 percent silicon. The balance is titanium with the trace elements being maintained below the maximum level set forth in the preferred composition above.
  • the material is forged, rolled and surfaced conditioned into a sheet of .05" thick and rolled into a 50 lb. coil.
  • a first specimen is cut from the sheet and cold-rolled to a foil of 0.0005" thick and appropriate width covering the electron beam window size, rolled into a coil about 500 feet long.
  • a most preferable range of .0005" to .0009" provides an optimum thickness that allows for maximum electron penetration, low energy consumption, as well as a window life at least 5 times that of the prior art under similar conditions.
  • the specimen is aged at 1150°F for 7 hours, then 1100°F for 1 hour, and then air-cooled.
  • the specimen has an ultimate yield strength of about 140 Ksi at an elevated temperature of 800°F.
  • a sheet of foil appropriate size covering the window frame is cut from the coil and tautly extended over a window frame. Thereafter, the window foil is subject to operation in accordance with the procedures of an electron beam processor.
  • the window employs the preferred titanium alloy is expected to have a service life extended in proportion with the improvement in strength and creep resistance property as compared with the pure titanium alloys and the alpha titanium alloys of the prior art under the same operating conditions.
  • a sheet is cut from the coil, and cold-rolled into a coil with an ultimate thickness of 0.0005".
  • the foil is then duplex-aged, first aging at 1275°F for 8 hours, then duplex aging at about 1200°F for another 8 hrs.
  • a sheet of foil of the appropriate size covering a window frame is cut from the coil and tautly extended over a window frame. The duplex aging gives the foil the prerequisite maximum long-term thermal stability for elevated temperature operations up to 1200°F.
  • the window employs the preferred titanium alloy is metallurgically stable for at least 1000 hrs. at a temperature up to 1 HOT.

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Abstract

L'invention concerne un ruban métallique pour processeur à faisceau d'électrons qui comprend un alliage en titane apte au traitement thermique, offrant une excellente capacité de formage à froid, une meilleure limite d'élasticité et une résistance au fluage importante sous températures élevées. Cette amélioration de la résistance au fluage sous températures élevées prolonge la durée de vie du ruban métallique. En particulier, l'invention concerne des titanes alpha-bêta et des titanes bêta (alliages) qui sont aptes au traitement thermique.
PCT/US1999/000233 1998-01-08 1999-01-07 Ruban metallique pour processeur a faisceau d'electrons Ceased WO1999035665A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US7078098P 1998-01-08 1998-01-08
US60/070,780 1998-01-08

Publications (1)

Publication Number Publication Date
WO1999035665A1 true WO1999035665A1 (fr) 1999-07-15

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PCT/US1999/000233 Ceased WO1999035665A1 (fr) 1998-01-08 1999-01-07 Ruban metallique pour processeur a faisceau d'electrons

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001035438A1 (fr) * 1999-11-05 2001-05-17 Energy Sciences, Inc. Appareil a faisceau de particules
EP1775752A3 (fr) * 2005-10-15 2007-06-13 Burth, Dirk, Dr. Procédé de fabrication d'une fenêtre de sortie d'électrons par érodage
CN106409637A (zh) * 2010-12-02 2017-02-15 利乐拉瓦尔集团及财务有限公司 电子出射窗箔

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4980127A (en) * 1989-05-01 1990-12-25 Titanium Metals Corporation Of America (Timet) Oxidation resistant titanium-base alloy
US5486703A (en) * 1992-10-01 1996-01-23 W. R. Grace & Co.-Conn. Hydronic cooling of particle accelerator window

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4980127A (en) * 1989-05-01 1990-12-25 Titanium Metals Corporation Of America (Timet) Oxidation resistant titanium-base alloy
US5486703A (en) * 1992-10-01 1996-01-23 W. R. Grace & Co.-Conn. Hydronic cooling of particle accelerator window

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001035438A1 (fr) * 1999-11-05 2001-05-17 Energy Sciences, Inc. Appareil a faisceau de particules
US6426507B1 (en) 1999-11-05 2002-07-30 Energy Sciences, Inc. Particle beam processing apparatus
US6610376B1 (en) 1999-11-05 2003-08-26 Energy Sciences, Inc. Particle beam processing apparatus
EP1775752A3 (fr) * 2005-10-15 2007-06-13 Burth, Dirk, Dr. Procédé de fabrication d'une fenêtre de sortie d'électrons par érodage
CN106409637A (zh) * 2010-12-02 2017-02-15 利乐拉瓦尔集团及财务有限公司 电子出射窗箔

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