US3524745A - Photoconductive alloy of arsenic,antimony and selenium - Google Patents

Photoconductive alloy of arsenic,antimony and selenium Download PDF

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Publication number
US3524745A
US3524745A US609126A US3524745DA US3524745A US 3524745 A US3524745 A US 3524745A US 609126 A US609126 A US 609126A US 3524745D A US3524745D A US 3524745DA US 3524745 A US3524745 A US 3524745A
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selenium
arsenic
antimony
alloy
percent
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Peter J Cerlon
Mark B Myers
Evan J Felty
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Xerox Corp
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Xerox Corp
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/082—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and not being incorporated in a bonding material, e.g. vacuum deposited
    • G03G5/08207—Selenium-based
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/043—Photoconductive layers characterised by having two or more layers or characterised by their composite structure
    • G03G5/0433—Photoconductive layers characterised by having two or more layers or characterised by their composite structure all layers being inorganic

Definitions

  • This invention relates in general to the art of xerography, and in particular, to a new photosensitive element.
  • a member or plate which comprises a conductive backing such as, for example, a metallic surface having a photoconductive insulating layer thereon.
  • a suitable plate for this purpose is a metallic member overcoated with a layer of vitreous selenium.
  • Such a plate is characterized by being capable of receiving a satisfactory electrostatic charge and selectively dissipating such a charge when exposed to a light pattern, and in general, is largely sensitive to light in the blue-green spectral range.
  • Vitreous selenium for the most part has become the standard in commercial xerography, but many of its properties can be improved by the addition of alloying elements which enhance such properties as spectral response, light sensitivity, thermal stability, etc.
  • U.S. Pats. 2,803,542 to Ullrich and 2,822,300 to Mayer et al. both show the advantages of modifying vitreous selenium by the addition of appreciable amounts of arsenic in order to yield a wider range of spectral sensitivity, increase the overall photographic speed, and in general improve the stability of the photoconductive layer.
  • vitreous selenium shows a satisfactory sensitivity
  • the need for photoconductors exhibiting increased sensitivity and spectral response exceeding those of vitreous selenium is needed for high speed processes which require a plate having a very high degree of sensitivity or panchromativity due to the short time factor in rapid cycling.
  • a step in this direction involves the addition of antimony in appreciable amounts to selenium, such as that set forth in copending application Ser. No. 566,593 filed on July 20, 1966.
  • Vitreous alloys of antimony and selenium have been found to yield a photosensitive composition having a sensitivity factor up to 12 times greater than that of vitreous selenium, and in addition, having a relative response up to 3 times that of vitreous selenium in the blue-green spectral range.
  • the antimonyselenium system has enhanced xerographic speed, it does suffer from one disadvantage in that there is a relative lack of thermal stability with respect to crystallization.
  • vitreous arsenic-antimony-selenium alloy for use as a photoconductor.
  • These alloys are prepared in a manner similar to those vitreous photoconductive alloys of the arsenicselenium system such as those described in U.S. Pats. 2,803,542 and 2,822,300, already mentioned above, and in copending application Ser. No. 566,593. It has been discovered that a vitreous alloy of arsenic, antimony and selenium in an effective range of up to about 50 at. percent (48.7 wt. percent) arsenic, about 0.1 to 22 at. percent (0.15 to 31.0 Wt.
  • a preferred range of about up to about 45 at. percent (43.7 Wt. percent) arsenic, up to about 13 at. percent (18.8 wt. percent) antimony, and not less than about 55 at. percent (56.3 wt. percent) selenium has been found to yield the combination of optimum thermal stability and sensitivity.
  • the ratio of arsenic to antimony necessary in order to main tain maximum thermal stability should be in the order of about 2 to 4 at.
  • the arsenic should be present in an amount of at least about 0.5 at. percent (0.6 wt. percent) in order to impart appreciable thermal stability, while the antimony should be present in an amount of at least about 0.1 at. percent (0.15 wt. percent) to yield the desired sensitivity of spectral respouse.
  • FIG. 1 is a portion of the ternary diagram for antimony, arsenic and selenium.
  • FIG. 2 is a series of spectral response curves for a group of photoconductors including a ternary alloy of this invention
  • the ternary diagram illustrates the areas in which the alloy of antimony-arsenic-selenium exhibits the desired photoconductive properties and thermal stability.
  • the area below Curve ABC-D represents compositions having a preferred thermal stability.
  • Dotted lines I and K represent the boundaries for the minimum amounts of arsenic and antimony, respectively.
  • the arsenic should be present in an amount of at least about 0.5 at. percent (0.6 wt. percent) with the amount of antimony being at least about 0.1 at. percent (0.15 wt. percent).
  • the arsenic-antimony-selenium vitreous alloys of this invention may be prepared by any suitable techniques. Typical techniques are conventional single source evaporation and flash evaporation. In both evaporation techniques it is preferred that a prereaction of the constituents take place before evaporation in that it results in the formation of s'elenide compounds with more similar vapor pressures than the elemental constituents.
  • the starting alloys are prepared by weighing the elemental arsenic, antimony, and selenium, and vacuum sealing them in a silica glass ampul. The materials are heated at 600 C. for several hours then air cooled to room temperature.
  • the cooled alloy is completely poly-crystalline, a mixture of crystalline and amorphous phases, or completely amorphous.
  • the prereacted alloy is then ball milled to a fine particulate size of less than about 1 millimeter in diameter.
  • the crucibles may be made of any inert material such as quartz, molybdenum, or ceramic lined metal.
  • the arsenic-antimony-selenium alloy is maintained at a temperature to insure sufficient vapor for deposition in reasonable time. This temperature usually exceeds the melting point of the alloy.
  • a total evaporation time of about minutes at a temperature of about 400 C. under the above mentioned vacuum conditions results in the formation of an alloy layer about 20 to 40 microns in thickness.
  • a substrate is supported above the heating crucibles upon which the arsenic-antimony-selenium is evaporated.
  • the substrate is maintained at a relatively low temperature. Suitable substrate temperatures are from about 60 to 150 C.
  • Another typical method of evaporation includes flash evaporation under vacuum conditions similar to those defined in single source evaporation, wherein the prereacted alloy of arsenic-antimony-selenium having a particle size of about less than 1 millimeter in diameter is selectively dropped into a heated inert crucible maintained at a temperature from about 450 to 660 C.
  • the vapors formed by heating the mixture are evaporated upward onto a substrate supported about the crucible.
  • the alloy is dropped at a rate sufiicient to prevent the formation of an alloy pool in the crucible, and thus minimize the problem of fractional vaporization.
  • the substrate is maintained at a temperature in the range of about 60 to 150 C. This procedure is continued until the desired thickness of the vitreous arsenic-antimonyselenim photoconductor has been formed on the substrate.
  • the alloys of this invention may be conveniently formed on any substrate, conductive or insulating. This may be a metal plate such as brass, aluminum, gold, platinum, steel or the like.
  • the support member may be of any convenient thickness, rigid or flexible, in the form of a sheet, a web, a cylinder or the like, and may be coated with a thin layer of plastic. It may also comprise such materials as metallized paper, plastic or plastic covered with a thin coating of aluminum or copper iodide, or glass coated with a thin layer of partially transparent copper iodide, tin oxide, or gold. In certain cases, after formation to the alloy, the substrate may even be dispensed with, if desired.
  • the thickness of the arsenic-antimony-selenium photoconductor alloy layer is not critical.
  • the layer can be as thin as about 0.1 micron, or as great as 300 microns or more, but for most applications the thickness will generally be from about 20 to 80 microns.
  • the photoconductive alloy of this invention may be doped with a halogen such as iodine, chlorine or bromine in order to reduced residual voltage and in general enhance its electrical characteristics.
  • a halogen such as iodine, chlorine or bromine
  • the halogen dopant is usually present in amounts from about 10 parts per million up to 2 percent by weight.
  • the arsenicantimony-selenium alloy may be utilized in a layered configuration.
  • Typical configurations include a relatively thin layer of from about 0.1 to 5 microns of arsenicantimony-selenium alloy over a relatively thicker layer of vitreous selenium.
  • Another typical structure includes an alloy of arsenic-selenium such as that disclosed in U.S. Pat. 2,822,300 which may be used in place of selenium in the two layered configuration defined above. It should be understood that both layers of a two layered structure may be doped with a suitable halogen in order to enhance the electrical characteristics. Structures having more than two photoconductive layers are also included within the scope of this invention.
  • the arsenic-antimonyselenium alloy layer may also be formed at the substrate interface of a transparent substrate, and imaged by exposure through the substrate.
  • the arsenic-antimony-selenium alloy may be used alone or in conjunction with other photoconductive layers such as those defined above.
  • Example I A starting alloy is prepared by weighing elemental arsenic, antimony and selenium in the ratio of 18 wt. percent arsenic, 1 wt. percent antimony, and 81 wt. percent selenium and vacuum sealing the mixture in a silica glass ampul. The mixture is then heated to about 600 C. for about 2 hours in a rocking furnace and then cooled to room temperature. The resultant alloy is a solidified polycrystalline matrix of intermixed phases which is then ball milled into a relatively fine material less than about 1 mm. in diameter.
  • Example II A 40 micron alloy film of vitreous arsenic-antimonyselenium on an aluminum substrate comprising about 1 wt. percent antimony, 18 wt. percent arsenic, and 81 wt. percent selenium is prepared as follows: The prereacted alloy of Example I is placed in a shallow fiat 2 x 4 inch ceramic coated metal boat. The particulate alloy is evenly distributed over the surface of the boat. The boat is then placed into a vacuum chamber. A 4 x 5 inch aluminum plate is thoroughly cleaned and suspended in the vacuum chamber about 12 inches above the boat and maintained at a temperature of about 65 C. with a water cooled platen. The chamber is evacuated into a vacuum of about 10- millimeters of mercury.
  • the arsenic-antimony-selenium alloy is then evaporated onto the aluminum substrate by heating the boat to a temperature of about 400 C. for about 20 minutes.
  • the boat is then cooled to room temperature, the vacuum broken, and the arsenic-antimonyselenium alloy coated aluminum plate removed from the vacuum chamber.
  • the outer surface of the alloy layer of the plate formed in Example II contains a greater percentage of antimony than the interior of the alloy film, with the substrate surface of the alloy layer containing the least amount of antimony.
  • Example III The plate formed by the method of Example II is then imaged as follows in a xerographic mode: The plate is corona charged to a positive potential of about 300 volts, and then exposed to a 100 watt tungsten light source at a distance of about 16 inches for about /2 second to form a latent electrostatic image on the surface of the plate. The latent image is then developed by cascading electroscopic marking particles across the surface containing said image. The image is transferred to a sheet of paper and heat fused to make it permanent. An excellent reproduction of the original is obtained by this method.
  • Example IV A 25 micron layer of a vitreous arsenic-antimonyselenium alloy on an aluminum substrate is formed as follows: A prereacted alloy comprising about 12 wt. percent antimony, 28 wt. percent arsenic, and 60 wt. percent selenium is prepared by the method of Example I. The prereacted alloy is placed in a brass hopper containing a copper chute adapted to deliver the particulate alloy into a quartz crucible maintained below said hopper. The quartz crucible is surrounded with a resistance heater adapted to control the crucible at a temperature of about 600 C. An aluminum substrate is placed on a water cooled platen maintained at a temperature of about 70 C.
  • the aluminum substrate and platen are positioned about 12 inches above the quartz crucible.
  • a bell jar is then placed over the hopper, crucible, and substrate, and evacuated to a vacuum of about mm. of mercury, and the quartz crucible heated to a temperature of about 600 C.
  • the hopper door below the chute leading to the quartz crucible is opened allowing a small sample of the arsenic-antimonyselenium alloy to pour into the quartz crucible.
  • the alloy mixture rapidly evaporates causing vapors of arsenic, antimony and selenium to come into contact with the suspended aluminum substrate.
  • This process is continued for about 2 hours at which time a 25 micron layer of a vitreous antimony-arsenic-selenium alloy containing about 12 wt. percent antimony, 28 wt. percent arsenic, and 60 wt. percent selenium has been formed on the aluminum substrate.
  • the crucible is then allowed to cool at room temperature, the vacuum broken, and the coated substrate removed from the chamber.
  • Example V The alloy formed by Example IV is then imaged in the manner set forth in Example III. An excellent copy of the original is obtained by this method.
  • Examples VI-IX A series of four plates are prepared for a comparison of spectral response. All four plates contain a 40 micron layer of a photoconductor on an aluminum substrate.
  • Plate No. 1 comprises a 40 micron layer of vitreous selenium made according to the method set forth in US. Pat. 2,970,906.
  • Plate No. 2 comprises a 40 micron layer of an 18 wt. percent arsenic, 82 wt. percent selenium vitreous alloy doped with about 1000 ppm. of iodine formed by the method set forth in copending US. patent application 516,529, filed on Dec. 27, 1965.
  • Plate No. 3 comprises a vitreous alloy of 14 wt. percent antimony and 86 wt.
  • Plate No. 4 comprises the ternary alloy of Example I comprising about 1 wt. percent antimony, 18 wt. percent arsenic, and 81 wt. percent selenium which is doped with about 1000 p.p.m. of iodine.
  • the spectral response curves for each of plates 1-4 are then plotted and illustrated in FIG. 2.
  • the spectral response of the four plates is plotted at dilferent wavelengths.
  • E represents the energy in ergs/cm. required to discharge plate approximately 25 percent.
  • the plates were each tested at the various wavelengths by charging each plate to an initial field potential of about 15 volts per micron, and exposing each plate at the particular Wavelength to approximately 2X 10 photons per cm. second.
  • the arsenic-antimony-selenium plate of this invention at 4000 angstroms exhibits approximately twice the spectral response as that of vitreous selenium and the arsenicselenium alloy, and considerably greater response than that of the antimony-selenium binary alloy.
  • arsenic-antimony-selenium alloys prepared by this invention have an extended spectral response all the way out to about 7000 angstroms and enhanced response in the shorter wavelength region.
  • these alloys have improved thermal stability not attainable by that of antimony-selenium photoconductors, and in preferred ratios of arsenic to antimony, show a thermal stability exceeding that of vitreous selenium.
  • a thermally stable vitreous photoconductive alloy of arsenic, antimony, and selenium bounded by the area below the Curve ABCD of FIG. 1, and comprising at least about 0.5 atomic percent arsenic, and 0.1 atomic percent antimony.
  • a vitreous photoconductive alloy of arsenic, antimony, and selenium bounded by the area below Curve EFG-H of FIG. 1, and comprising at least about 0.5 atomic percent arsenic, and 0.1 atomic percent antimony.
  • a photosensitive element having a photoconductive insulating layer, said layer comprising a vitreous alloy of arsenic, antimony and selenium in a concentration of about 0.5 to 50 atomic percent arsenic, 0.1 to 22 atomic percent antimony and the balance substantially selenium in an amount of at least about 40 atomic percent.
  • a photosensitive element comprising a supporting substrate, a photoconductive insulating layer overlaying said substrate with said layer comprising a vitreous alloy of arsenic, antimony and selenium in a'concentration of about 0.5 to 50 atomic percent arsenic, 0.1 to 22 atomic percent antimony, and the balance substantially selenium in an amount of at least about 40 atomic percent.
  • a photosensitive element comprising a support member, a first photoconductive layer overlaying said support member, and a second photoconductive layer comprising an alloy of arsenic, antimony and selenium overlaying said first photoconductive layer, said second photoconductive layer having an alloy composition comprising about 0.5 to 50 atomic percent arsenic, 0.1 to 22 atomic percent antimony, and the balance substantially selenium in an amount of at least about 40 atomic percent.
  • said first photoconductive layer comprises an arsenic-selenium alloy.
  • a method of imaging comprising:
  • a xerographic plate having an electrically conductive support member and a photoconductive insulating layer thereon, said layer comprising a vitreous alloy of arsenic, selenium, and antimony, with arsenic being present in an amount from about 0.5 to 50 atomic percent, antimony in an amount from about 0.1 to 22 atomic percent and the balance substantially selenium in an amount of at least about 40 atomic percent.
  • arsenic being present in an amount from about 0.5 to 50 atomic percent, antimony in an amount from about 0.1 to 22 atomic percent and the balance substantially selenium in an amount of at least about 40 atomic percent.
  • a method of imaging comprising: (a) providing a xerographic plate having an electrically conductive support member and a photoconductive insulating layer thereon, said layer comprising a mony-selenium layer is overcoated with a second photoconductive layer.
  • arsenic being present in an amount from about 3 96-15 0.5 to 50 atomic percent, antimony in an amount 2962376 1/1960 96-45 from about 0.1 to 22 atomic percent, and the balance 66 962 3 en 96 1'5 selenium in an amount of at least about 40 atomic 1 ar can 96-45 25 age; 2x22; a -h e21;
  • a method of imaging comprising:

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
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US609126A 1967-01-13 1967-01-13 Photoconductive alloy of arsenic,antimony and selenium Expired - Lifetime US3524745A (en)

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BE (1) BE709132A (nl)
CH (1) CH495573A (nl)
DE (1) DE1608200B2 (nl)
ES (1) ES349235A1 (nl)
FR (1) FR1550902A (nl)
GB (1) GB1209971A (nl)
LU (1) LU55231A1 (nl)
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3772006A (en) * 1971-07-08 1973-11-13 Hoya Glass Works Ltd Amorphous material for active elements exhibiting a memory effect
US3867143A (en) * 1969-01-17 1975-02-18 Canon Kk Electrophotographic photosensitive material
US3904408A (en) * 1969-11-14 1975-09-09 Canon Kk Electrophotographic member with graded tellurium content
JPS536035A (en) * 1976-07-07 1978-01-20 Yamanashi Denshi Kogyo Kk Electrophotographic photosensitive element
US4097277A (en) * 1973-01-31 1978-06-27 Canon Kabushiki Kaisha Photosensitive member having layer of vinyl carbazole polymer containing antimony chalcogen compound of antimony and sulfur
US4780386A (en) * 1986-11-28 1988-10-25 Xerox Corporation Selenium alloy treatment
US4822712A (en) * 1988-04-08 1989-04-18 Xerox Corporation Reduction of selenium alloy fractionation
US4859411A (en) * 1988-04-08 1989-08-22 Xerox Corporation Control of selenium alloy fractionation
US5002734A (en) * 1989-01-31 1991-03-26 Xerox Corporation Processes for preparing chalcogenide alloys
US10191186B2 (en) 2013-03-15 2019-01-29 Schott Corporation Optical bonding through the use of low-softening point optical glass for IR optical applications and products formed

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3322494A1 (de) * 1983-06-22 1985-01-10 Valentina Fedorovna Leningrad Kokorina Optisches chalkogenidglas

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2803541A (en) * 1953-05-29 1957-08-20 Haloid Co Xerographic plate
US2803542A (en) * 1955-07-26 1957-08-20 Haloid Co Xerographic plate
US2962376A (en) * 1958-05-14 1960-11-29 Haloid Xerox Inc Xerographic member
US3041166A (en) * 1958-02-12 1962-06-26 Xerox Corp Xerographic plate and method
US3312548A (en) * 1963-07-08 1967-04-04 Xerox Corp Xerographic plates
US3312547A (en) * 1964-07-02 1967-04-04 Xerox Corp Xerographic plate and processes of making and using same
US3355289A (en) * 1962-05-02 1967-11-28 Xerox Corp Cyclical xerographic process utilizing a selenium-tellurium xerographic plate
US3372294A (en) * 1966-07-29 1968-03-05 Gen Electrodynamics Corp Camera tube target including porous photoconductive layer comprising antimony trisulfide, free antimony and copper phthalocyanine
US3427157A (en) * 1964-12-28 1969-02-11 Xerox Corp Xerographic process utilizing a photoconductive alloy of thallium in selenium

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2803541A (en) * 1953-05-29 1957-08-20 Haloid Co Xerographic plate
US2803542A (en) * 1955-07-26 1957-08-20 Haloid Co Xerographic plate
US3041166A (en) * 1958-02-12 1962-06-26 Xerox Corp Xerographic plate and method
US2962376A (en) * 1958-05-14 1960-11-29 Haloid Xerox Inc Xerographic member
US3355289A (en) * 1962-05-02 1967-11-28 Xerox Corp Cyclical xerographic process utilizing a selenium-tellurium xerographic plate
US3312548A (en) * 1963-07-08 1967-04-04 Xerox Corp Xerographic plates
US3312547A (en) * 1964-07-02 1967-04-04 Xerox Corp Xerographic plate and processes of making and using same
US3427157A (en) * 1964-12-28 1969-02-11 Xerox Corp Xerographic process utilizing a photoconductive alloy of thallium in selenium
US3372294A (en) * 1966-07-29 1968-03-05 Gen Electrodynamics Corp Camera tube target including porous photoconductive layer comprising antimony trisulfide, free antimony and copper phthalocyanine

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3867143A (en) * 1969-01-17 1975-02-18 Canon Kk Electrophotographic photosensitive material
US3904408A (en) * 1969-11-14 1975-09-09 Canon Kk Electrophotographic member with graded tellurium content
US3772006A (en) * 1971-07-08 1973-11-13 Hoya Glass Works Ltd Amorphous material for active elements exhibiting a memory effect
US4097277A (en) * 1973-01-31 1978-06-27 Canon Kabushiki Kaisha Photosensitive member having layer of vinyl carbazole polymer containing antimony chalcogen compound of antimony and sulfur
JPS536035A (en) * 1976-07-07 1978-01-20 Yamanashi Denshi Kogyo Kk Electrophotographic photosensitive element
US4780386A (en) * 1986-11-28 1988-10-25 Xerox Corporation Selenium alloy treatment
US4822712A (en) * 1988-04-08 1989-04-18 Xerox Corporation Reduction of selenium alloy fractionation
US4859411A (en) * 1988-04-08 1989-08-22 Xerox Corporation Control of selenium alloy fractionation
US5002734A (en) * 1989-01-31 1991-03-26 Xerox Corporation Processes for preparing chalcogenide alloys
US10191186B2 (en) 2013-03-15 2019-01-29 Schott Corporation Optical bonding through the use of low-softening point optical glass for IR optical applications and products formed

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LU55231A1 (nl) 1969-08-12
FR1550902A (nl) 1968-12-20
DE1608200B2 (de) 1977-02-24
SE328189B (nl) 1970-09-07
NL160663B (nl) 1979-06-15
NL160663C (nl) 1979-11-15
DE1608200A1 (de) 1971-02-25
BE709132A (nl) 1968-07-09
NL6800625A (nl) 1968-07-15
GB1209971A (en) 1970-10-28
ES349235A1 (es) 1969-09-16
NO127943B (nl) 1973-09-03
CH495573A (de) 1970-08-31

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