EP0309657B1 - Pulverulent metal-containing material and process for the production of a protective layer - Google Patents

Pulverulent metal-containing material and process for the production of a protective layer Download PDF

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Publication number
EP0309657B1
EP0309657B1 EP88110585A EP88110585A EP0309657B1 EP 0309657 B1 EP0309657 B1 EP 0309657B1 EP 88110585 A EP88110585 A EP 88110585A EP 88110585 A EP88110585 A EP 88110585A EP 0309657 B1 EP0309657 B1 EP 0309657B1
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EP
European Patent Office
Prior art keywords
process according
metal powder
protective layer
remainder
hot gases
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
EP88110585A
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German (de)
French (fr)
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EP0309657A1 (en
Inventor
Hans-Theo Steine
Christofer Wasserman
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.)
ECG Immobilier SA
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Castolin SA
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Filing date
Publication date
Application filed by Castolin SA filed Critical Castolin SA
Priority to AT88110585T priority Critical patent/ATE67522T1/en
Publication of EP0309657A1 publication Critical patent/EP0309657A1/en
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Publication of EP0309657B1 publication Critical patent/EP0309657B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F22—STEAM GENERATION
    • F22B—METHODS OF STEAM GENERATION; STEAM BOILERS
    • F22B37/00—Component parts or details of steam boilers
    • F22B37/02—Component parts or details of steam boilers applicable to more than one kind or type of steam boiler
    • F22B37/04—Component parts or details of steam boilers applicable to more than one kind or type of steam boiler and characterised by material, e.g. use of special steel alloy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06—Metallic material
    • C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic

Definitions

  • the invention relates to a powdery material and to a method for producing corrosion-resistant protection on fin walls and superheater tubes in sulfur-containing hot gases which are used in combustion systems at surface temperatures of over 400 ° C.
  • the inventor has set himself the goal of improving the above-mentioned method while avoiding the identified shortcomings and of creating a suitable powdery material that can be used well and permanently in sulfur-containing hot gases.
  • a metal powder of a certain composition atomized from the melt flow and having a surface area of more than 200 cm 2 / g is applied with an autogenous flame spray burner at a gas flow rate between about 1000 to 3000 NL / h or 1500 to 2500 NL / h for the fuel gas.
  • the composition of the metal powder used here has Cr 15% to 35%, Mn 0.05% to 3%, Mo 0.05% to 5.0%, CO, 1% to 3%, Si O, 1% to 3% , Al 2% to 15% with a remainder of Fe.
  • Preferred ranges are Cr 20% to 30%, Mn 0.1% to 2%, Mo 0.1% to 4%, C 0.1% to 2.9%, Si 0.5% to 2%, Al 3 % to 10%, remainder Fe.
  • the layer has a uniform structure and is sprayed on without a primer.
  • the homogeneity and composition ensure good corrosion resistance in sulfur-containing hot gases with a sulfur content of more than 0.2% to 5%.
  • a steep tube boiler 10 for coal firing has a combustion chamber 14 with a burner 15 and a plurality of water tubes 16 on the boiler walls 17 above a deasher 12.
  • With 18 bulkhead superheaters are designated below a boiler drum 20, with 22 touch superheaters and with 24 feed water preheaters or economizers.
  • Air preheaters 26 are arranged on the right flank of FIG. 1 between the feed water preheaters 24 - in which the feed water is preheated with the exhaust gases of the boiler system while saving fuel and reducing the thermal stresses in the boiler. In those superheaters 18, 22, saturated steam is brought to a higher temperature without an increase in pressure, i.e. overheated.
  • Corrosion is mainly found on the burner 15 k , on the boiler wall 17 k and on the bulkhead superheater 18 k , the erosion phenomena however, below the combustion chamber 14 at 13 a , on the boiler wall at 17 a , on the soot blower 19 a of the bulkhead superheater 18, on the first contact superheaters 22 a in the flow direction x and on the preheater 24 a .
  • the temperatures in the corrosion and oxidation-loaded combustion chamber are approximately between 1000 ° and 1200 ° C (zone A), in zone B at approximately 700 ° C and in the area of the preheaters 24, 26 at approximately 400 ° C (zone C).
  • the powdery materials according to the invention are applied to fin walls and superheater tubes by thermal spraying, which are used at surface temperatures of far more than 400 ° C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Resistance Heating (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

A process for producing a corrosion-resistant protection on stabilizing wall surfaces and superheater tubes in sulfur-bearing hot gases which are used at surfaces temperatures of over 400 DEG C. in combustion installations, and a material in powder form which is suitable for that process, are intended to make it possible to use such wall surfaces and superheater tubes in sulfur-bearing hot gases in a good and durable fashion. For that purpose, to form a protective layer which is preferably from 0.2 to 1.5 mm in thickness, a metal powder which is sprayed out of a molten state, of a given composition, with a surface area of more than 200 cm2/g, is applied with an autogenous flame spray torch, with a quantitative gas flow rate of between about 1000 to 3000 NL/h, or 1500 to 2500 NL/h, for the combustion gas. The preferred composition of the metal powder used in Cr 15% to 35%, Mn 0.05% to 3%, Mo 0.05% to 5.0%, C 0.1% to 3%, Si 0.1% to 3%, Al 2% to 15%, with the balance Fe.

Description

Die Erfindung betrifft einen pulverförmigen Werkstoff sowie ein Verfahren zum Herstellen eines korrosionsfesten Schutzes an Flossenwänden und Ueberhitzerrohren in schwefelhaltigen Heißgasen, die bei Oberflächentemperaturen von über 400°C in Verbrennungsanlagen eingesetzt sind.The invention relates to a powdery material and to a method for producing corrosion-resistant protection on fin walls and superheater tubes in sulfur-containing hot gases which are used in combustion systems at surface temperatures of over 400 ° C.

An Flossenwänden, insbesondere von Großfeuerungsanlagen, beispielsweise in thermischen Kraftwerken, Müllverbrennungsanlagen od.dgl., treten in Abhängigkeit von dem eingesetzten flüssigen, gasförmigen oder festen Brennstoff in der Turbulenzzone der Flamme bzw. des Feuerballes starke Korrosionserscheinungen auf.On fin walls, in particular of large combustion plants, for example in thermal power plants, waste incineration plants or the like, depending on the liquid, gaseous or solid fuel used, severe corrosion phenomena occur in the turbulence zone of the flame or the fireball.

Die Entstehung dieses Korrosionsangriffes ist auf die oxydierende bzw. reduzierende Flamme und auf die verschiedenen Oxyde von Elementen in den Flammengasen wie z.B. SO₂ oder CO zurückzuführen. Bis heute werden an den stark korrodierten Stellen die Rohre bzw. Teile der Flossenwand herausgeschnitten und durch neue Teile ersetzt. Bei Verwendung von Plasma und Drahtspritzverfahren konnte ein solcher Austausch teilweise bzw. in begrenzten Fällen vermieden werden. Allerdings zeigten diese Beschichtungen unbefriedigend kurze Standzeiten bzw. bei Einsatz einer Haftschicht Ablöseerscheinungen.The origin of this corrosion attack is due to the oxidizing or reducing flame and to the various oxides of elements in the flame gases such as SO₂ or CO. To date, the pipes or parts of the fin wall have been cut out at the highly corroded areas and replaced with new parts. When using plasma and wire spraying, such an exchange could be avoided in part or in limited cases. However, these coatings showed unsatisfactorily short service lives or signs of detachment when an adhesive layer was used.

Besondere Erschwernisse entstehen durch die Größe der erforderlichen Spritzanlagen und den beim Spritzen auftretenden Geräuschpegel, der ein Arbeiten mit Gehörschutz notwendig macht. Auch die bei diesen Verfahren einzuhaltenden Spritzdistanzen zum Aufbringen einer konstanten Schicht sind beim Arbeiten in Kesselanlagen schwierig einzuhalten.Particular difficulties arise due to the size of the spraying equipment required and the noise level that occurs when spraying, which makes it necessary to work with hearing protection. The spraying distances for applying a constant layer, which are to be observed in these processes, are also difficult to maintain when working in boiler systems.

Gegen den Einsatz an sich bekannter autogener Flammspritzbrenner bestanden in der Fachwelt erhebliche Bedenken, weshalb derartige Geräte auf dem in Rede stehenden Gebiet nicht angewendet wurden.There were considerable concerns in the professional world against the use of autogenous flame spray burners, which is why such devices were not used in the field in question.

Angesichts dieser Gegebenheiten hat sich der Erfinder das Ziel gesetzt, das eingangs erwähnte Verfahren unter Meidung der erkannten Mängel zu verbessern sowie einen dafür geeigneten pulverförmigen Werkstoff zu schaffen, der in schwefelhaltigen Heißgasen gut und dauerhaft eingesetzt werden kann.In view of these circumstances, the inventor has set himself the goal of improving the above-mentioned method while avoiding the identified shortcomings and of creating a suitable powdery material that can be used well and permanently in sulfur-containing hot gases.

Bei dem erfindungsgemäßen Verfahren wird zur Bildung einer Schutzschicht -- von bevorzugt 0,2 bis 1,5 mm Dicke -- ein aus dem Schmelzfluß verdüstes Metallpulver bestimmter Zusammensetzung mit einer Oberfläche von mehr als 200 cm²/g mit einem autogenen Flammspritzbrenner aufgetragen bei einer Gasdurchflußmenge zwischen etwa 1000 bis 3000 NL/h bzw. 1500 bis 2500 NL/h für das Brenngas. Hierbei weist die Zusammensetzung des eingesetzten Metallpulvers Cr 15 % bis 35 %, Mn 0,05 % bis 3 %, Mo 0,05 % bis 5,0 %, C O,1 % bis 3 %, Si O,1 % bis 3 %, Al 2 % bis 15 % mit einem Rest Fe auf.In the method according to the invention, to form a protective layer - preferably 0.2 to 1.5 mm thick - a metal powder of a certain composition atomized from the melt flow and having a surface area of more than 200 cm 2 / g is applied with an autogenous flame spray burner at a gas flow rate between about 1000 to 3000 NL / h or 1500 to 2500 NL / h for the fuel gas. The composition of the metal powder used here has Cr 15% to 35%, Mn 0.05% to 3%, Mo 0.05% to 5.0%, CO, 1% to 3%, Si O, 1% to 3% , Al 2% to 15% with a remainder of Fe.

Bevorzugte Bereiche sind Cr 20 % bis 30 %, Mn 0,1 % bis 2 %, Mo 0,1 % bis 4 %, C 0,1 % bis 2,9 %, Si 0,5 % bis 2 %, Al 3 % bis 10 %, Rest Fe.Preferred ranges are Cr 20% to 30%, Mn 0.1% to 2%, Mo 0.1% to 4%, C 0.1% to 2.9%, Si 0.5% to 2%, Al 3 % to 10%, remainder Fe.

Die Schicht hat einen gleichmäßigen Aufbau und wird ohne Haftgrund aufgespritzt. Durch die Homogenität und die Zusammensetzung ist eine gute Korrosionsbeständigkeit in schwefelhaltigen Heißgasen mit einem Schwefelgehalt über 0,2 % bis 5 % gegeben.The layer has a uniform structure and is sprayed on without a primer. The homogeneity and composition ensure good corrosion resistance in sulfur-containing hot gases with a sulfur content of more than 0.2% to 5%.

Weitere Vorteile, Merkmale und Einzelheiten der Erfindung ergeben sich aus der nachfolgenden Beschreibung eines bevorzugten Ausführungsbeispiels sowie anhand der Zeichnung; diese zeigt in

Fig. 1
einen Steilrohrkessel im Querschnitt;
Fig. 2
eine schematisierte Wiedergabe des Steilrohrkessels.
Further advantages, features and details of the invention result from the following description of a preferred exemplary embodiment and from the drawing; this shows in
Fig. 1
a steep tube boiler in cross section;
Fig. 2
a schematic representation of the steep tube boiler.

Ein Steilrohrkessel 10 für Kohlefeuerung weist über einem Entascher 12 einen Feuerraum 14 mit Brenner 15 und eine Vielzahl von Wasserrohren 16 an den Kesselwänden 17 auf. Mit 18 sind Schottenüberhitzer unterhalb einer Kesseltrommel 20 bezeichnet, mit 22 Berührungsüberhitzer und mit 24 Speisewasservorwärmer oder Ekonomiser. Zwischen den Speisewasservorwärmern 24 -- in welchen mit den Abgasen der Kesselanlage das Speisewasser unter Einsparung von Brennstoff und Verringerung der Wärmespannungen im Kessel vorgewärmt wird -- sind an der rechten Flanke der Fig. 1 Luftvorwärmer 26 angeordnet. In jenen Ueberhitzern 18, 22 wird Sattdampf ohne Drucksteigerung auf eine höhere Temperatur gebracht, d.h. überhitzt.A steep tube boiler 10 for coal firing has a combustion chamber 14 with a burner 15 and a plurality of water tubes 16 on the boiler walls 17 above a deasher 12. With 18 bulkhead superheaters are designated below a boiler drum 20, with 22 touch superheaters and with 24 feed water preheaters or economizers. Air preheaters 26 are arranged on the right flank of FIG. 1 between the feed water preheaters 24 - in which the feed water is preheated with the exhaust gases of the boiler system while saving fuel and reducing the thermal stresses in the boiler. In those superheaters 18, 22, saturated steam is brought to a higher temperature without an increase in pressure, i.e. overheated.

Die Fig. 2 zeigt typische Belastungszonen für Korrosion (Index k) und Erosion (Index a). Korrosionen sind vornehmlich am Brenner 15k, an der Kesselwand 17k und an den Schottenüberhitzern 18k zu finden, die Erosionserscheinungen hingegen unterhalb des Feuerraums 14 bei 13a, an der Kesselwand bei 17a, am Rußbläser 19a des Schottenüberhitzers 18, an den in Strömungsrichtung x ersten Berührungsüberhitzern 22a sowie am Vorwärmer 24a. Zudem gibt es Erosionen an einer oberen Zugangsöffnung 30a.2 shows typical stress zones for corrosion (index k) and erosion (index a). Corrosion is mainly found on the burner 15 k , on the boiler wall 17 k and on the bulkhead superheater 18 k , the erosion phenomena however, below the combustion chamber 14 at 13 a , on the boiler wall at 17 a , on the soot blower 19 a of the bulkhead superheater 18, on the first contact superheaters 22 a in the flow direction x and on the preheater 24 a . There are also erosions at an upper access opening 30 a .

Die Temperaturen in dem korrosions- und oxidationsbelasteten Feuerraum liegen etwa zwischen 1000° und 1200° C (Zone A), in Zone B bei etwa 700° C sowie im Bereich der Vorwärmer 24, 26 bei etwa 400°C (Zone C).The temperatures in the corrosion and oxidation-loaded combustion chamber are approximately between 1000 ° and 1200 ° C (zone A), in zone B at approximately 700 ° C and in the area of the preheaters 24, 26 at approximately 400 ° C (zone C).

Die erfindungsgemäßen pulverförmigen Werkstoffe werden auf Flossenwände und Ueberhitzerrohre auf dem Wege des thermischen Spritzens aufgetragen, die bei Oberflächentemperaturen von weit mehr als 400° C eingesetzt sind.The powdery materials according to the invention are applied to fin walls and superheater tubes by thermal spraying, which are used at surface temperatures of far more than 400 ° C.

Claims (8)

  1. Process for the production of a corrosion resistant protective layer on finned walls and superheater tubes in sulphur-containing hot gases used in combustion plants at surface temperatures in excess of 400°C, characterised in that, in order to form a protective layer, a metal powder atomised from the melt having a surface area of more than 200 cm²/g and having the following composition

    Cr 15.0 % to 35.0 %
    Mn 0.05 % to 3 %
    Mo 0.05 % to 5 %
    C 0.1 % to 3 %
    Si 0.1 % to 3 %
    Al 2.0 % to 15 %
    Fe remainder,

    is applied by means of an oxyacetylene spray torch, at a combustible gas flow rate of between approximately 1000 and 3000 nl/h.
  2. Process according to claim 1, characterised by the application of a metal powder having the following composition:

    Cr 20.0 % to 30.0 %
    Mn 0.1 % to 2 %
    Mo 0.1 % to 4 %
    C 0.1 % to 2.9 %
    Si 0.5 % to 2 %
    Al 3 % to 10 %
    Fe remainder,

    said metal powder being applied by means of an oxyacetylene spray torch, at a combustible gas flow rate of between approximately 1000 and 3000 nl/h.
  3. Process according to claim 1 or claim 2, characterised by an oxyacetylene spray torch at 1500 to 2500 nl/h.
  4. Process according to one of claims 1 to 3, characterised in that the powder is used in a quantity of 3 to 10 kg/h, preferably 4 to 8 kg/h.
  5. Process according to one of claims 1 to 4, characterised by a spraying distance of 150 to 200 ± 50 mm.
  6. Process according to at least one of claims 1 to 5, characterised in that the layer is applied in a thickness of up to 0.2 to 1.5 mm.
  7. Material for carrying out the process according to at least one of the preceding claims, characterised by the following composition for the powdered material:

    Cr 15.0 % to 35.0 %, preferably 20 to 30 %,
    Mn 0.05 % to 3 %, preferably 0.1 % to 2 %,
    Mo 0.05 % to 5 %, preferably 0.1 % to 4 %,
    C 0.1 % to 3 %, preferably 0.1 % to 2.9 %,
    Si 0.1 96 to 3 %, preferably 0.5 & to 2 %,
    Al 2.0 % to 15 %, preferably 3 % to 10 %,
    Fe remainder.
  8. Material according to claim 7, characterised by a nonspherical grain shape.
EP88110585A 1987-07-08 1988-07-02 Pulverulent metal-containing material and process for the production of a protective layer Expired - Lifetime EP0309657B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88110585T ATE67522T1 (en) 1987-07-08 1988-07-02 POWDER METALLIC MATERIAL AND PROCESS FOR PRODUCING A PROTECTION.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3722532 1987-07-08
DE3722532 1987-07-08

Publications (2)

Publication Number Publication Date
EP0309657A1 EP0309657A1 (en) 1989-04-05
EP0309657B1 true EP0309657B1 (en) 1991-09-18

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EP88110585A Expired - Lifetime EP0309657B1 (en) 1987-07-08 1988-07-02 Pulverulent metal-containing material and process for the production of a protective layer

Country Status (5)

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US (1) US4935266A (en)
EP (1) EP0309657B1 (en)
AT (1) ATE67522T1 (en)
DE (1) DE3864963D1 (en)
ES (1) ES2025737T3 (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE8717405U1 (en) * 1987-07-08 1989-03-09 Castolin S.A., Lausanne-St. Sulpice, Waadt/Vaud Pipe for preheater and economizer
DE4104832A1 (en) * 1991-02-16 1992-08-20 Castolin Sa METAL DEVICE FOR CLOSING COOKING OVENS AND METHOD FOR THE PRODUCTION THEREOF
US6017591A (en) * 1996-11-14 2000-01-25 Ford Global Technologies, Inc. Method of making adherently sprayed valve seats
FR2795748B1 (en) * 1999-07-02 2002-03-01 Electricite De France IMPROVED SURFACE COATING COMPOSITION
US9546412B2 (en) 2008-04-08 2017-01-17 Federal-Mogul Corporation Powdered metal alloy composition for wear and temperature resistance applications and method of producing same
US9624568B2 (en) 2008-04-08 2017-04-18 Federal-Mogul Corporation Thermal spray applications using iron based alloy powder
US9162285B2 (en) 2008-04-08 2015-10-20 Federal-Mogul Corporation Powder metal compositions for wear and temperature resistance applications and method of producing same
CN106435399B (en) * 2016-10-21 2019-05-07 广东电网有限责任公司电力科学研究院 A kind of pipe fitting and its application
CN106636963B (en) * 2016-10-21 2019-02-12 广东电网有限责任公司电力科学研究院 A kind of alloy material

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4019875A (en) * 1973-07-06 1977-04-26 Metco, Inc. Aluminum-coated nickel or cobalt core flame spray materials
US4447503A (en) * 1980-05-01 1984-05-08 Howmet Turbine Components Corporation Superalloy coating composition with high temperature oxidation resistance
US4348433A (en) * 1981-04-06 1982-09-07 Eutectic Corporation Flame spray powder
US4361604A (en) * 1981-11-20 1982-11-30 Eutectic Corporation Flame spray powder
CH663219A5 (en) * 1984-01-31 1987-11-30 Castolin Sa FLAME INJECTION MATERIAL.
US4578115A (en) * 1984-04-05 1986-03-25 Metco Inc. Aluminum and cobalt coated thermal spray powder

Also Published As

Publication number Publication date
EP0309657A1 (en) 1989-04-05
DE3864963D1 (en) 1991-10-24
ATE67522T1 (en) 1991-10-15
ES2025737T3 (en) 1992-04-01
US4935266A (en) 1990-06-19

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