GB2278853A - Method for manufacturing thin-film EL device - Google Patents

Method for manufacturing thin-film EL device Download PDF

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Publication number
GB2278853A
GB2278853A GB9409752A GB9409752A GB2278853A GB 2278853 A GB2278853 A GB 2278853A GB 9409752 A GB9409752 A GB 9409752A GB 9409752 A GB9409752 A GB 9409752A GB 2278853 A GB2278853 A GB 2278853A
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United Kingdom
Prior art keywords
target
manganese
sputtering
film
light
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Granted
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GB9409752A
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GB9409752D0 (en
GB2278853B (en
Inventor
Hisato Katou
Tomoyuki Kawahima
Harutaka Taniguchi
Shinichi Nakamata
Kazuyoshi Shibata
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Fuji Electric Co Ltd
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Fuji Electric Co Ltd
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Publication date
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Publication of GB9409752D0 publication Critical patent/GB9409752D0/en
Publication of GB2278853A publication Critical patent/GB2278853A/en
Application granted granted Critical
Publication of GB2278853B publication Critical patent/GB2278853B/en
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    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/57—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing manganese or rhenium
    • C09K11/572—Chalcogenides
    • C09K11/574—Chalcogenides with zinc or cadmium
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
    • 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
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/12—Light sources with substantially two-dimensional radiating surfaces
    • H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source

Description

1 1 W 2278853 METHOD FOR MANUFACTURING THIN-FILM EL DEVICE The present
invention relates to a method for manufacturing a thin-film electroluminescence device (hereinafter referred to as an EL device) having a light-emitting layer that comprises zinc sulphide (ZnS) to which manganese (Mn) is added to provide the light-emitting centres.
Thin-film EL devices, which are totally solid flat display devices with high resolution and suitable for obtaining a large display screen, have recently drawn much attention. Thin-film EL devices have a dual insulated structure, as shown in Figure 1, in which a transparent electrode 2, a first insulation layer 3. an EL light-emitting layer 4, a second insulation layer 5. and a back electrode 6 are laminated on a glass substrate 1. Among these element layers, the light-emitting layer 4 in the EL device is formed with zinc sulphide (ZnS) as the base material, to which a small amount of manganese (M) is added to provide the lightemitting centres. Light is emitted from the EL device by applying an alternating electric field between the transparent electrode 2 and the back electrode 6. To obtain a luminance of 70 cd/M2 or higher which is acceptable in practice, the concentration of the light-emitting centre material in the light-emitting layer 4 should be optimal and the ratio of the Mn concentration to the total content of the light-emitting layer 4 expressed as Mn/(ZnSMn) should preferably be about 0.5% by weight (or in the range of from 0.4 to 0.6% by weight).
As the methods for forming this light-emitting layer of an EL device, the vacuum deposition method, the atomic layer epitaxial growth method (ALE method) which may be classified into the CW method, and the sputtering method have been investigated. Of these methods, the sputtering method offers the superior productivity, because a uniform film is grown by the sputtering method over a large area with high film growth rate. Among the miscellaneous variations of the sputtering method, a reactive sputtering method disclosed in 2 the Japanese laid open Patent S62-2713961 which employs a zinc (Zn) target and a hydrogen sulphide (H2S) gas, is evaluated to be one of the best suited film fabrication methods for obtaining a uniform and high quality light-emitting layer. The Japanese laid open Patent S62-271396 discloses that an excellent light-emitting layer is obtained by employing an inert sputtering gas containing from 5 to 20 volume % of hydrogen sulphide (H2S) and a substrate heated from 100 to 3500C. The Japanese laid open Patent S62-271396 discloses a Zn-Mn alloy target and numerically estimates a Mn concentration Mn/(ZnS+Mn) in the Zn-Mn alloy target to be 0.8% by weight for obtaining a liqht-emitting layer containing the optimum 0.5% by weight of Mn in Mn/(ZnS+Mn) concentration.
However, Ono pointed out low luminance of the light-emitting layer grown by the sputtering method in Acta Polytechnica Scandinavia, Applied Physics Series, No. 170 (5th International Workshop on Electroluminescence), pp.41-48. The inventors of the present invention discovered that this low luminance is caused by large discrepancy of the composition of the grown light-emitting layer from the composition of the sputtering target. The composition discrepancy is caused by differences in the physical properties of constituent zinc (Zn), sulphur (S) and manganese (Mn) elements relevant to the sputtering process including sputtering rate, vapour pressure etc.. Because the vapour pressures of zinc and manganese atoms are high and because zinc and manganese atoms vaporize again from the substrate surface especially when the substrate is heated up the elevated temperatures, Mn concentration in the light- emitting layer grown by the reactive sputtering method becomes much higher than that in the sputtering target. Figure 3 is a graph showing the relationship between the Mn/(ZnS+Mn) concentration ratio of light- emitting layer relative to the Mn/(ZnS+Mn) concentration in the target and the substrate temperature. In Figure 3, line 21 represents the Mn/(ZnS+Mn) concentration ratio for a target the surface of which is metallic and line 22 represents the Mn/(ZnS+Mn) concentration ratio for a target the surface of which is 3 sulphurized. We know from Figure 3 that the Mn concentration in the lightemitting layer is from 1.5 to 8 times higher than that in the target. We know also from Figure 3 that the Mn concentration in the light-emitting layer depends greatly on the substrate temperature and surface state of the target. Consequently, the luminance of the light-emitting layer grown from a target the surface of which is sulphurized is high. Therefore, the desired optimum Mn concentration of around 0.5% by weight in the lightemitting layer is not obtained by the reactive sputtering method in so far as a target is employed the Mn/Zn ratio of which coincides with the desired Mn/Zn ratio in the light-emitting layer.
In view of the foregoing, an. object of the present invention is to provide a method for manufacturing a thin-film EL device that facilitates growing by the reactive sputtering technique a ZnS light-emitting layer which contains an optimum Mn concentration.
The object of the present invention is achieved by a method for manufacturing a thin-film EL device that features growth of a lightemitting layer of the thin-film El device made of zinc sulphide and manganese added to donate light-emitting centres by a reactive sputtering technique that employs a sputtering gas containing a sulphur compound, and a target containing zinc and less than 0.5 weight percent of manganese contained at least in its surface layer.
The target, the surface of-which is sulphurized during sputtering process, contains at least in the surface layer from 0.3 to 0.4% by weight of Mn.
The target, the surface of which is not sulphurized during sputtering process, contains at least in the surface layer less than 0.1% by weight of Mn.
The target is fabricated by co-melting Zn and Mn.
The target is fabricated under a press machine by pressing a mixture of Zn powder and Mn powder to form a target tablet.
The target comprises an exposed Mn region disposed on a zinc substrate and the exposed Mn region has an area ratio of a predetermined percentage by weight of Mn multiplied by 0.96 relative to a total area of a sputtering surface of the target.
4 m The light-emitting layer that contains an optimum from 0.4 to 0.6% by weight of manganese is grown with an excellent reproducibility, by compensating beforehand the manganese content increase in the reactive sputtering process described in Figure 3 by setting the Mn concentration Mn/(ZnS+Mn) in the surface layer of the target at less than 0.5% by weight that is less than 0.8% by weight corresponding to the optimum 0.5% by weight of Mn/(ZnS+Mn) in the light-emittinq layer. In the usual temperature range, the optimum Mn concentration Mn/(ZnS+Mn) in the surface layer of the target is from 0.3 to 0.4% by weight when the target is sulphurized and less than 0.1% by weight when the target is not sulphurized.
The present invention will be described in detail hereinafter with reference to the accompanied drawings, in which:
Figure 1 is a cross sectional view showing the structure of the thin-film EL device manufactured by the method according to the present invention; Figure 2 is a cross sectional view schematically showing the configuration of the sputtering apparatus in which the thin-film EL device is manufactured; Figure 3 is a graph showing the relationship between the Mn/(ZnS+Mn) concentration ratio of light-emitting layer relative to the Mn/(ZnS+Mn) concentration in the target and the substrate temperature; Figure 4 is a diagram schematically showing the second sputtering target employed in a second method for manufacturing according to the present invention, in which Figure 4(a) shows a top plan view of the second sputtering target and Figure 4(b) shows a cross sectional view of the second sputtering target; and Figure 5 is a cross sectional view showing a third sputtering target employed in a third method for manufacturing according to the present invention.
The thin-film EL device manufactured by the method of the present invention possesses a dual insulation structure as shown in Figure 1. The thin-film EL device of Figure I comprises a glass substrate 1; a transparent electrode 2 made of ITO (indium tin oxide) j m and laminated on the substrate 1 to a thickness of 1700 A (A = 10-11m); a first insulation layer 3 made of tantalum pentoxide (Ta205) and laminated on the electrode 2 to a thickness of 400OA; an EL light-emitting layer 4 laminated on the insulation layer 3 to thickness of 700OA; a second insulation layer 5 made of Ta2Os and laminated on the light-emitting layer 4 to a thickness of 400OA; and an aluminium back electrode 6 laminated on the second insulation layer 5 to a thickness of 7000A.
Figure 2 is a sectional view schematically showing a sputtering apparatus in which the thin-film EL device is manufactured by the method of the present invention. The sputtering apparatus includes a reaction chamber 11 in which cathode 13 and an anode 14 are positioned oppositely facing to each other. A target 12 of 100mm in diameter and 5mm in thickness is coated on a surface of the cathode 13. The substrate I on which the transparent electrode 2 and the first insulation layer 3 are laminated is disposed on a surface of the anode 14. The cathode 13 is connected via a matching circuit 15 to a 13.56 MHz RF power supply 16, and the anode 14 is earthed.
For growing the liqht-emittinq layer 4, an alloy target (hereinafter referred to as the first target) prepared by melting zinc to which manganese is added and having 0.4% by weight of Mn in Mn/(Zn+Mn) concentration is employed in a first exemplary method according to the present invention for manufacturing the thin-film EL device. A sputtering gas containing an argon gas, to which 40% of H2S is added as a sulphur containing compound gas, is fed at the flow rate of 30 sccm (standard cm3/min) through a gas inlet 17 into the reaction chamber 11. The other sputtering parameters include the gas pressure of 10 mTorr, the substrate temperature of 3500 and the discharge power of 3 W/CM3. Under the sputtering conditions described above, the target surface is sulphurized. The grown light-emitting layer 4 is then heat treated in a vacuum furnace at 600-C.
6 W The light-emitting layer 4 thus obtained contains from 0.4 to 0.6% by weight of Mn in Mn/(Zn+Mn) concentration, and such results can be repeatably achieved. The thin-film EL device which employs such a lightemitting layer 4 shows high luminance of 200 cd/M2 under the applied alternating voltage of 60 Hz.
The Zn-Mn target may be fabricated from a mixture of Zn powder and Mn powder by pressing the mixture to form a target tablet, or by sintering the mixture to form a compact sintered target.
Figure 4 is a diagram schematically showing the sputtering target employed in a second exemplary method according to the present invention, in which Figure 4(a) shows a top plan view of the second sputtering target and Figure 4(b) shows a cross sectional view of the second sputtering target. As Figures 4(a) and 4(b) show, the sputtering target is a mosaic target which comprises a plurality of Mn cylinders 22 of 5mm in thickness and from 1 to 5mm in diameter embedded in a Zn substrate 21 so as to cover 0.38% of the entire area of a surface of the target by Mn. Since the density of Zn is 7.12 and that of Mn is 7.24, the area of the Mn sites of 0.38% corresponds to the Mn concentration of 0.4% by weight. By sulphurizing the surface of the second sputtering target, a lightemitting layer that contains the optimum Mn concentration of from 0.4 to 0.6% by weight in Mn/(Zn+Mn) concentration is obtained under the same layer growth conditions with the first embodiment including the heat treatment after the layer growth.
Figure 5 is a cross sectional view showing a third sputtering target employed in a third exemplary method according to the present invention. As Figure 5 shows, the third sputtering target comprises a plurality of circular Mn tablets 23 of 1 mm in thickness and from 1 to 5 mm in diameter disposed on the Zn substrate 21 so as to cover 0.38% of the entire area of a surface of the target by Mn. The third target facilitates finely tuning the Mn area ratio on a sputtering target and growing a light-emitting layer that contains the optimum concentration of Mn under the various substrate temperature.
j 4 7 Though in the embodiments described above, the light-emitting layers are grown from the targets the surfaces of which are sulphurized, it is clear from Figure 3 that a light-emitting layer of the optimum Mn concentration may be grown from a target that contains less than 0.1% by weight of Mn in its surface layer by preventing the surface of the target from sulphurization, for example, by controlling the mixing ratio of the H2S gas to the sputtering gas.
As has been explained so far, by the method for manufacturing according to the present invention that employs a Zn-Mn target containing less than 0.5% by weight of Mn in its surface layer and a sputtering gas containing sulphur, a light-emitting layer is obtained by the reactive sputtering technique that contains the optimum 0.5% by weight of Mn relative to the total amount of Mn and ZnS yielded by the reaction between Zn from the target and sulphur contained in the sputtering gas. The manufacturing method according to the present invention facilitates obtaining a thinfilm EL device that shows in practice a luminance of more than 100 cd/M2 or more than 150 cd/M2.
8

Claims (4)

1. A method for manufacturing a thin-film EL device, wherein a lightemitting layer of the thin-film EL device containing zinc sulphide and manganese added to donate light-emitting centres is grown by a reactive sputtering technique that employs a sputtering gas containing a sulphur compound, and a target containing zinc and less than 0.5 weight percent of manganese contained at least in a surface layer thereof.
2. A method as claimed in claim 1, wherein the surface of the target is sulphurized during sputtering and wherein the target contains at least in the surface layer thereof from 0.3 to 0.4 weight percent of manganese.
3. A method as claimed in claim 1, wherein the surface of the target is not sulphurized during sputtering and wherein the target contains at least in the surface layer thereof less than 0.1 weight percent of manganese.
4. A method as claimed in claim 1, wherein the target is fabricated by co-melting zinc and manganese. S. A method as claimed in claim 1, wherein the target is fabricated by pressing a mixture of zinc powder and manganese powder to form a target tablet. 6. A method as claimed in claim 1, wherein the target comprises an exposed manganese region disposed on a zinc substrate, the ratio of the area of the exposed manganese region to the area of a sputtering surface the target being 0.96 times the required weight percent of manganese in the target surface. 7. A method substantially as described herein with reference to Figure 2, Figure 4 or Figure 5 of the accompanying drawings. 8. A thin-film electroluminescence device made by a method substantially as described herein with reference to Figure 2, Figure 4 or Figure 5 of the accompanying drawings.
i w I
GB9409752A 1993-06-08 1994-05-16 Method for manufacturing thin-film electroluminescence device Expired - Fee Related GB2278853B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13629993 1993-06-08

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GB9409752D0 GB9409752D0 (en) 1994-07-06
GB2278853A true GB2278853A (en) 1994-12-14
GB2278853B GB2278853B (en) 1997-02-12

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GB (1) GB2278853B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2294585A (en) * 1994-08-18 1996-05-01 Ultra Silicon Techn Uk Ltd Thin film electroluminescent device
GB2306251A (en) * 1994-08-18 1997-04-30 Ultra Silicon Techn Uk Ltd Electroluminescent devices
US5910706A (en) * 1996-12-18 1999-06-08 Ultra Silicon Technology (Uk) Limited Laterally transmitting thin film electroluminescent device

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2026221A (en) * 1978-07-18 1980-01-30 Western Electric Co Electroluminescent devices
US4394601A (en) * 1973-07-05 1983-07-19 Sharp Kabushiki Kaisha ZnS:Mn Thin-film electroluminescent element with memory function
US4672266A (en) * 1983-10-25 1987-06-09 Sharp Kabushiki Kaisha Thin film light emitting element
EP0239120A2 (en) * 1986-03-27 1987-09-30 GTE Laboratories Incorporated Method of producing thin film electroluminescent structures
US4777099A (en) * 1986-10-03 1988-10-11 Olympus Optical Co., Ltd. Thin-film EL device
GB2271022A (en) * 1992-09-24 1994-03-30 Fuji Electric Co Ltd A method for manufacturing a thin-film el device

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05315075A (en) * 1992-05-07 1993-11-26 Fuji Electric Co Ltd Forming method for electroluminescence light emitting film
GB9324505D0 (en) * 1992-12-07 1994-01-19 Fuji Electric Co Ltd Method for preparing thin-film electro-luminescence element

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4394601A (en) * 1973-07-05 1983-07-19 Sharp Kabushiki Kaisha ZnS:Mn Thin-film electroluminescent element with memory function
GB2026221A (en) * 1978-07-18 1980-01-30 Western Electric Co Electroluminescent devices
US4672266A (en) * 1983-10-25 1987-06-09 Sharp Kabushiki Kaisha Thin film light emitting element
EP0239120A2 (en) * 1986-03-27 1987-09-30 GTE Laboratories Incorporated Method of producing thin film electroluminescent structures
US4777099A (en) * 1986-10-03 1988-10-11 Olympus Optical Co., Ltd. Thin-film EL device
GB2271022A (en) * 1992-09-24 1994-03-30 Fuji Electric Co Ltd A method for manufacturing a thin-film el device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2294585A (en) * 1994-08-18 1996-05-01 Ultra Silicon Techn Uk Ltd Thin film electroluminescent device
GB2306251A (en) * 1994-08-18 1997-04-30 Ultra Silicon Techn Uk Ltd Electroluminescent devices
GB2306251B (en) * 1994-08-18 1998-02-04 Ultra Silicon Techn Uk Ltd Improved luminous efficiency in a thin film EL device
GB2294585B (en) * 1994-08-18 1998-02-04 Ultra Silicon Techn Uk Ltd Improvements in and relating to electroluminescent devices
US5910706A (en) * 1996-12-18 1999-06-08 Ultra Silicon Technology (Uk) Limited Laterally transmitting thin film electroluminescent device

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Publication number Publication date
GB9409752D0 (en) 1994-07-06
GB2278853B (en) 1997-02-12
DE4419242A1 (en) 1994-12-22

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