US3559662A - Method and valve apparatus for metering the flow of liquid metal - Google Patents

Method and valve apparatus for metering the flow of liquid metal Download PDF

Info

Publication number
US3559662A
US3559662A US3559662DA US3559662A US 3559662 A US3559662 A US 3559662A US 3559662D A US3559662D A US 3559662DA US 3559662 A US3559662 A US 3559662A
Authority
US
United States
Prior art keywords
liquid
zinc
flow
passage
reservoir
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.)
Expired - Lifetime
Application number
Other languages
English (en)
Inventor
Robert A Iezzi
Laszlo V Sandor
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.)
Republic Steel Corp
Original Assignee
Republic Steel Corp
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 Republic Steel Corp filed Critical Republic Steel Corp
Application granted granted Critical
Publication of US3559662A publication Critical patent/US3559662A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/246—Replenishment of source material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes

Definitions

  • Malleck ABSTRACT A method and means for metering the flow of liquid zinc between a reservoir and a vacuum chamber in a vapor deposition process, comprising a valve body and operator structure composed of graphite which is immersed in the liquid zinc in the reservoir so that the body of zinc acts as an atmosphere-to-vacuum seal, and as a result of the nonwetting of graphite by zinc at the operating temperatures of the deposition process a liquid-to-liquid seal is also achieved within the valve structure.
  • the present invention relates to the fluid flow control art and more particularly to a valve means for controlling the flow of liquid metal to a vacuum chamber in a vapor deposition process.
  • a particularly difficult valving application in this art is controlling the flow of a liquid metal to be used as a coating in a vapor deposition process.
  • a selected substrate which is to be coated is placed in a heated vacuum chamber and the metal for the coating is introduced in liquid form at an inlet.
  • the liquid metal upon exposure to the vacuum evaporates byvirtue of the decreased pressure and increased temperature and subsequently is deposited by condensation on the substrate forming a thin even layer thereon.
  • the process is commonly used for example in coating zinc on steel.
  • the valve controlling the flow of the liquid zinc in the process must necessarily resist the highly corrosive effects of this molten metal and operate at the attendant high temperatures. Moreover, such a valve must provide sealing against the great difference in pressure between the ambient atmosphere and the vacuum in the chamber in which the deposition takes place. If air is permitted to enter the chamber, the zinc tends to oxidize and form undesirable deposits within the chamber environment.
  • the valve of the present invention effectively meters the flow of liquid metals, such as zinc, between a reservoir and a vapor deposition chamber, while maintained at a temperature above the melting point of the metal, and yet remains vacuum tight and leakproof although of comparatively simple and inexpensive construction. In addition, it is of sufficient durability to be comparatively maintenance-free and resists corrosion by or amalgamation with the liquid metal being conducted.
  • liquid metals such as zinc
  • the valve of the invention is constructed of a refractory material, such as graphite, and comprises a valve body, a support frame, and a valve stem or operator having a control handle.
  • the entire valve structure with the exception of the handle, is immersed in the liquid metal which acts to seal the joints against leakage of air into the subatmospheric pressure region at the outflow end of the valve.
  • the nonwetting quality of particular liquid metals with respect to refractory materials, such as graphite at the required operating temperatures, there will be ,no liquid leakage through the various clearances between the valve components.
  • valve of the present invention will be described in conncction with a system for vapor depositing a layer of zinc on a steel substrate. but it will be understood that a number of similar metals. which are capable of use in combination in the vapor deposition process may selected as is known to those skilled in the art.
  • FIG. 1 shows a vapor deposition system of the type in which the improved valve means is to be used.
  • the supply of zinc l, which is to be deposited, is maintained in the liquid state in a reservoir 2.
  • the reservoir 2 may be a large open container such as a commercially available melting pot containing resistive wire 3 as the heating means.
  • the zinc is maintained at a temperature between 788 F its melting point, and up to about 1 to l200 F., at which point it begins to oxidize in the atmosphere.
  • the molten zinc l is delivered through a pipe 4 to a heated, evaporator or vacuum chamber 5.
  • the pressure in the chamber is maintained in the range between l0" and 10- millimeters of mercury.
  • the steel substrate on which the zinc is to be deposited is located in this chamber 5.
  • the liquid zinc upon entering the vacuum chamber 5 evaporates, by virtue of the decreased pressure and increased temperature, and is subsequently deposited by condensation on the substrate forming a thin, even layer thereon.
  • the flow of zinc 1 between the reservoir 2 and the vacuum chamber 5 is controlled by a valve means 6 which is the subject of the present invention.
  • the valve means 6 is shown in more particular detail in FIG. 2 positioned in the reservoir 2.
  • the valve means 6 comprises a valve body 7 and a stem or operator 9, both mounted on a U- shaped frame 8.
  • the stem 9 extends from the valve body 7 and has a crossbar member 10 fastened to its upper end.
  • the crossbar member 10 has a handle 11 mounted on its upper surface by which the stem 9 may be operatively rotated.
  • An arrow 12 is marked at one end of the crossbar l0 and cooperates with an indicator dial 13 mounted on the upper ends of the arms of the frame 8.
  • the indicator dial 13 is calibrated to give an indication of the amount of liquid zinc being metered by the valve 6 for any given amount of stem rotation.
  • the valve outlet accepts a delivery pipe 4 which conducts the zinc to the chamber 5.
  • the pipe 4 which is constructed of chromium carbide treated steel to resist the action of the zinc, extends upwardly through the surface of the zinc l and over the edge of the reservoir 2 for connection to the vacuum chamber 5. Sealing of the entrance port 5a in the vacuum chamber 5 is achieved by welding the supply pipe 4 inthe wall of the chamber 5, or by other suitable vacuum connections.
  • the valve body 7, the stem 9 and the frame 8 are all constructed of a refractory material, preferably graphite. It has been found that under the operating conditions of the deposition process the graphite is not wetted by the liquid zinc. As a result of this phenomenon the valve may be submerged in the liquid zinc without danger of corrosion or other damage at operating temperatures of 788 F. and above, and no zinc will enter the clearances between the cooperating parts. With the valve submerged in the body of zinc, the zinc acts to seal out the air and to seal itself against leakage within the valve thus serving as a structural seal element. No further sealing is necessary so the construction of the valve parts may be simple and uncomplicated, requiring no special structure, materials, or casting.
  • valve body 7 may be in the form of a block with a bore 14 through its center.
  • the delivery pipe 4 is pressfitted in an enlarged end 14a of the bore 14, as shown in FIG. 4, and a tight seal results from the fhermal expansion of the pipe 4 when subjected to the temperature of the liquid zinc 1.
  • Another bore 15 is provided in the valve body 7 perpendicular to the central bore 14 for accommodating the cylindri cal stem or operator 9 which extends through the central bore 14, as best seen in FIG. 3.
  • a cutout portion !6 16 in the lower part of the bore 15 receives an annular flange 17 on the lower end of the stem 9 to prevent longitudinal motion of the stem 9 with respect to the body 7 while permitting rotational motion therein.
  • the frame 8 supports the stem 9 within the valve body 7.
  • the stem 9 is provided with an opening 18 extending transversely therethrough which cooperates with the central bore 14 in the valve body 7 to meter the flow of zinc from inlet 14b to the tube 4 as will be presently described. It has been found that if the valve tolerances are within generally acceptable limits, such as 0.004 inch or less, no leakage will occur in the valve system.
  • the valve body 7 is held on the frame member 8 by two screws, 19, one at either side of the central bore 14.
  • the underside of the frame is appropriately bored at 20 to accept the mounting screws 19 and plug members 21 are fitted in these bores 20 to prevent the liquid zinc from acting directly on the material of the screws.
  • These plug members 21 also act as footings for the frame 8, spacing it from the floor of the reservoir 2.
  • the upper arms of the frame 8 are bored to accept screws 22 which hold the indicator dial 13 thereon. and the upper end of the stem 9 is bored to receive a screw securing the handle thereto.
  • the metering operation of the valve of the present invention is as follows.
  • the valve body 7 is totally immersed in the liquid zinc 1 so that the clearances at the entrance and exit openings of the central bore 14 and the operator bore are all bathed by the zinc l.
  • the supply pipe 4 is fitted in the exit opening 14a before insertion of the valve means 6 into the zinc.
  • the stem 9 is oriented with the axis of its transverse opening 18 perpendicular to the axis of the central bore 14 so as to block or shutoff flow through the valve body 7.
  • the stem 9 When it is desired to supply zinc to the evaporator 5, the stem 9 is rotated by means of the handle 11 thus bringing opening 18 into registration with bore 14.
  • the amount of zinc which is permitted to pass into the tube 4 will be a function of the extent of rotation of the stem 9.
  • the stem 9 is free to rotate in either direction to increase or decrease the degree of registration between bore 14 and stem opening 18 thereby metering the amount of flow.
  • a person operating the valve will have an indication of the amount of flow passing through the valve for a given setting by observing the point on the indicator dial l3 coinciding with the marking 12 on the crossbar member 10. Flow rates in a range from 10 to 75 pounds per minute have been achieved with such a device but almost any flow rate can be obtained depending on the valve dimensions.
  • the system is sealed against the influx of air into the valve means 6 and the delivery pipe 4 by means of the zinc itself which acts to seal all of the valve clearances.
  • the opposite end of the delivery pipe 4 is sealed by welding to the chamber wall so that air cannot enter the evaporator at this point so that-undesirable oxidation and deposits within the deposition system due to air leakage are avoided.
  • the valve body 7, the stem 9 and the frame 8 are all constructed of graphite, as already explained, all of the openings in and clearances between these respective members are graphite to graphite contact surfaces.
  • the zinc is maintained at a temperature of approximately 850 F., but is has been found that at all the working temperatures used with this process, zinc will not wet the graphite. Therefore, the zinc itself will act to seal the various clearances between the parts also preventing anyfluid leakage.
  • My invention contemplates the use of other materials in constructing the valve, such as silicon carbide, zirconia, alumina, Stellite 06, Molybdenum-30 percent Tungsten alloy, and others, but graphite is particularly suitable since it does' not require expensive casting and may be readily machined. Graphite will resist a large variety of liquid metals, acids, and other corrosive fluids and can withstand temperatures in excess of the evaporation temperatures of any metal which might be metered by the valve.
  • an improved method and means comprising a valve of simple and inexpensive construction, which selectively meters the flow of a liquid metal to a vacuum deposition chamber and which seals itself and the chamber in a superior manner without requiring complicated construction or special materials.
  • a system for metering the flow of a liquid metal from a reservoir comprising:
  • valve body of refractory material positioned in the reservoir below the level of the metal and having a passage therein for accommodating the flow of the metal between an inlet and an outlet below the level of the metal; an operator of refractory material in said passage for metering the flow of metal of said outlet;
  • conduit means connected to said outlet for conducting the metered metal out of said reservoir.
  • conduit means is of a chromium carbide treated steel.
  • said operator comprises a member having an opening therein, said member being movable in said passage to meter the flow of said metal in proportion to the degree of registration of said opening and said passage.
  • a system for metering the flow of liquid zinc between a reservoir and a chamber at a pressure below atmospheric comprising:
  • valve body of graphite positioned in the reservoir below the level of the zinc and having a first passage therein for accommodating the flow of the zinc between an inlet and an outlet in said body and a second passage intersecting said first passage between said inlet and said outlet;
  • heating means for maintaining the temperature of the 'zinc approximately within the range from 788 F. to 1200 F. such that the zinc will not wet the graphite, sealing the clearances between the valve body and the operator;
  • a system as claimed in claim 5 wherein said operator comprises a cylindrical column having an opening therein, said column being movable in said second passage to meter the flow of the zinc to the outlet in proportion to the degree of registration of said opening and said first passage.
  • a system for metering the flow of a liquid from a reservoir comprising:
  • valve body adapted to be positioned in the reservoir below the level of the liquid to be metered and having a passage therein for accommodating the flow of the liquid between an inlet and an outlet;
  • valve body and operator material being such that they are not wetted by the liquid so that no liquid enters and thus the liquid seals the clearances between the valve body and the operator;
  • conduit means connected to said outlet and extending out cv immersing the valve in the reservoir with all the of said reservoir for Conducting th liq i f m i w clearances and the outlet below the level of the liquid and with the other end of the conduit extending out of the 9.
  • valve material is graphite

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Details Of Valves (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US3559662D 1968-11-25 1968-11-25 Method and valve apparatus for metering the flow of liquid metal Expired - Lifetime US3559662A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US77860968A 1968-11-25 1968-11-25

Publications (1)

Publication Number Publication Date
US3559662A true US3559662A (en) 1971-02-02

Family

ID=25113895

Family Applications (1)

Application Number Title Priority Date Filing Date
US3559662D Expired - Lifetime US3559662A (en) 1968-11-25 1968-11-25 Method and valve apparatus for metering the flow of liquid metal

Country Status (4)

Country Link
US (1) US3559662A (de)
DE (1) DE1959148A1 (de)
FR (1) FR2024152A1 (de)
GB (1) GB1262388A (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4094337A (en) * 1974-10-18 1978-06-13 Delphi Instruments, Inc. Pressure regulator valve
US4290581A (en) * 1979-09-21 1981-09-22 Acf Industries, Incorporated Seat assembly for ball valves
US4904085A (en) * 1988-05-04 1990-02-27 Simmonds Precision Products, Inc. Polarimetric fiber optic sensor testing apparatus
US20060167416A1 (en) * 2004-11-23 2006-07-27 Mark Mathis Steerable device for accessing a target site and methods
US20170130854A1 (en) * 2014-06-11 2017-05-11 Tata Steel Nederland Technology B.V. Valve for high temperature liquid

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103363809B (zh) * 2013-07-25 2015-07-15 深圳市劲拓自动化设备股份有限公司 一种液态金属真空抽取装置及抽取方法

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4094337A (en) * 1974-10-18 1978-06-13 Delphi Instruments, Inc. Pressure regulator valve
US4290581A (en) * 1979-09-21 1981-09-22 Acf Industries, Incorporated Seat assembly for ball valves
US4904085A (en) * 1988-05-04 1990-02-27 Simmonds Precision Products, Inc. Polarimetric fiber optic sensor testing apparatus
US20060167416A1 (en) * 2004-11-23 2006-07-27 Mark Mathis Steerable device for accessing a target site and methods
US20170130854A1 (en) * 2014-06-11 2017-05-11 Tata Steel Nederland Technology B.V. Valve for high temperature liquid
JP2017519162A (ja) * 2014-06-11 2017-07-13 タタ、スティール、ネダーランド、テクノロジー、ベスローテン、フェンノートシャップＴａｔａ Ｓｔｅｅｌ Ｎｅｄｅｒｌａｎｄ Ｔｅｃｈｎｏｌｏｇｙ Ｂｖ 高温液体用バルブ
US10167972B2 (en) * 2014-06-11 2019-01-01 Tata Steel Nederland Technology B.V. Valve for high temperature liquid

Also Published As

Publication number Publication date
GB1262388A (en) 1972-02-02
FR2024152A1 (de) 1970-08-28
DE1959148A1 (de) 1970-06-11

Similar Documents

Publication Publication Date Title
US7294208B2 (en) Apparatus for providing gas to a processing chamber
US3559662A (en) Method and valve apparatus for metering the flow of liquid metal
US4178974A (en) Flow controller
TWI737718B (zh) 含有瀉流源的沉積系統及相關方法
NO137678B (no) Utformning av depotdrageer med en kjerne inneholdende aktivt stoff og overtrukket med en kappe
US11339876B2 (en) Butterfly valve
US5989722A (en) Reduced pressure device and method of making
EP1975927A2 (de) Vorrichtung und Verfahren zur Anwendung von Gleitbeschichtungen auf magnetischen Platten via Dampfströmungspfad, einschließlich einer wahlweise geöffneten oder geschlossenen Klappe
JPH01210670A (ja) 改良テーパー型ボールバルブ
Cho et al. Creation of extreme high vacuum with a turbomolecular pumping system: A baking approach
US3654374A (en) Apparatus for and method of de-waxing, presintering and sintering powdered metal compacts
US3743587A (en) Method for reactive sputter deposition of phosphosilicate glass
JPS56147756A (en) Synthetic method of urea using silicon carbide material in apparatus
JP2959951B2 (ja) 液循環式恒温装置
JPS6233762A (ja) 真空蒸着装置
US6115538A (en) Steam supplying apparatus and method for controlling same
JPS6278188A (ja) バブラ−シリンダ装置
GB1396507A (en) Cryostat
JP3234038B2 (ja) 半導体処理液用熱交換器
JPH0739630B2 (ja) 真空蒸着装置
JP3030458B1 (ja) 真空装置
US3812720A (en) Inhibitor to reduce mercury corrosion
JPH06229693A (ja) ヒートパイプの製造方法および製造装置
JPS63470A (ja) 真空装置
SU1030636A1 (ru) Газорегулируема теплова труба