JPH0369157B2 - - Google Patents
Info
- Publication number
- JPH0369157B2 JPH0369157B2 JP61015390A JP1539086A JPH0369157B2 JP H0369157 B2 JPH0369157 B2 JP H0369157B2 JP 61015390 A JP61015390 A JP 61015390A JP 1539086 A JP1539086 A JP 1539086A JP H0369157 B2 JPH0369157 B2 JP H0369157B2
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- zns
- selenium
- sulfur
- film
- 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
Links
- 239000010409 thin film Substances 0.000 claims description 28
- 238000004519 manufacturing process Methods 0.000 claims description 12
- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 7
- 239000010408 film Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- LJSQFQKUNVCTIA-UHFFFAOYSA-N diethyl sulfide Chemical compound CCSCC LJSQFQKUNVCTIA-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 4
- 125000002524 organometallic group Chemical group 0.000 claims description 2
- RVIXKDRPFPUUOO-UHFFFAOYSA-N dimethylselenide Chemical compound C[Se]C RVIXKDRPFPUUOO-UHFFFAOYSA-N 0.000 claims 2
- 229940065287 selenium compound Drugs 0.000 claims 2
- 150000003343 selenium compounds Chemical class 0.000 claims 2
- 150000003464 sulfur compounds Chemical class 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 claims 1
- ALCDAWARCQFJBA-UHFFFAOYSA-N ethylselanylethane Chemical compound CC[Se]CC ALCDAWARCQFJBA-UHFFFAOYSA-N 0.000 claims 1
- 239000011669 selenium Substances 0.000 claims 1
- 238000000927 vapour-phase epitaxy Methods 0.000 claims 1
- 150000003752 zinc compounds Chemical class 0.000 claims 1
- 238000005401 electroluminescence Methods 0.000 description 19
- 239000000758 substrate Substances 0.000 description 7
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- -1 alkyl zinc Chemical compound 0.000 description 2
- 229910052798 chalcogen Inorganic materials 0.000 description 2
- 150000001787 chalcogens Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 description 2
- 229910000058 selane Inorganic materials 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Electroluminescent Light Sources (AREA)
- Luminescent Compositions (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、高輝度、高耐圧などの各特性を有
する多色の薄膜EL（Electro Luminescence）素
子の作製方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for manufacturing a multicolored thin film EL (Electro Luminescence) element having various characteristics such as high brightness and high breakdown voltage.
近時、薄膜EL素子の作製方法として、アルキ
ルジンクとH2Sまたはアルキルイオウなどを用い
た有機金属気相成長（Metal organic CVD；以
下、MOCVDと略称する。）法が高品質の薄膜を
均一にかつ大面積で安価に作製できる点で注目さ
れつつある。
Recently, metal organic chemical vapor deposition (hereinafter abbreviated as MOCVD) using alkyl zinc and H 2 S or alkyl sulfur has become a method for producing thin film EL devices, which allows for the production of uniform, high-quality thin films. It is attracting attention because it can be manufactured over a large area and at low cost.
ところで、本出願人は、1985年秋の応用物理学
会の予稿集P.590において、MOCVD法を用いて
黄橙色発光センタとなるMnの有機金属であるト
リカルボニルメチルシクロペンタジエニルMnを
反応炉導入時に加熱分解し、この分解ガスを基板
上にドーピングしてZnS：Mn薄膜EL素子を作製
する薄膜EL素子の作製方法を提案しており、こ
の薄膜EL素子は、5000cd／m2以上の高輝度、高
耐圧などの各特性を有するものである。 By the way, in Proceedings of the Japan Society of Applied Physics in the fall of 1985, page 590, the present applicant introduced tricarbonylmethylcyclopentadienyl Mn, an organometallic Mn that forms yellow-orange luminescent centers, into a reactor using the MOCVD method. We have proposed a method for manufacturing thin film EL devices in which ZnS:Mn thin film EL devices are fabricated by thermal decomposition and doping of the decomposed gas onto a substrate. , high withstand voltage, and other characteristics.
ところが、この種の薄膜EL素子の作製方法に
あつては、黄橙色の発光が得られるZnS：Mn薄
膜EL素子を高品質で作製されるものの、他の有
機金属、例えばTb（縁色発光センタ）、Sm（赤色
発光センタ）、Ce，Tm（青色発光センタ）などを
ZnSと合成することが困難で、たとえ合成できて
も固体となるため、蒸気圧による制御が難しく基
板上にドーピングできず、黄橙色以外の発光EL
素子を作製することができない問題があつた。
However, in the production method of this type of thin film EL device, although a high quality ZnS:Mn thin film EL device that can emit yellow-orange light is produced, other organic metals, such as Tb (fringe color luminescent center) are used. ), Sm (red emitting center), Ce, Tm (blue emitting center), etc.
It is difficult to synthesize with ZnS, and even if it can be synthesized, it becomes a solid, making it difficult to control by vapor pressure and making it impossible to dope it onto the substrate.
There was a problem that the device could not be manufactured.
そこで、この発明は、Mn，MnCl2，MnF2，
TbF3，SmF3，TmF3，CeF3，CeCl3からなる群
より選ばれた発光物質を減圧下の反応炉内で抵抗
加熱して蒸発させ基板上にドーピングしてZnS：
ＸまたはZnSe：Ｘ膜を形成することにより、上
記の問題点を解決するようにした。
Therefore, this invention provides Mn, MnCl 2 , MnF 2 ,
A luminescent substance selected from the group consisting of TbF 3 , SmF 3 , TmF 3 , CeF 3 , and CeCl 3 is evaporated by resistance heating in a reaction furnace under reduced pressure, and the substrate is doped with ZnS:
The above problems were solved by forming a X or ZnSe:X film.
〔実施例 １〕
発光センタ物質にTbF3をまた主原料にジメチ
ルジンク（DMZ）およびH2Sを使つてZnS：
TbF3からなる薄膜を第１図に示すような
MOCVD気相装置により作製した。[Example 1] ZnS using TbF 3 as the luminescent center material and dimethyl zinc (DMZ) and H 2 S as the main raw materials:
A thin film made of TbF 3 is made as shown in Figure 1.
Fabricated using MOCVD gas phase equipment.
このMOCVD気相装置は、円筒状の反応炉１
の上部にこの反応炉１内にDMZを供給するため
のノズル２とH2Sを供給するためのノズル３と、
電源４ａを備え、かつTbF3粉末が収容された抵
抗加熱用ヒータ４とがそれぞれ配設されてなるも
のである。また、この反応炉１の外周部には、反
応炉１内を加熱する高周波加熱コイル５が設けら
れ、反応炉１内には、SiCをコートしたグラフア
イトサセブタ６が設けられ、このグラフアイトサ
セブタ６上には、薄膜が形成される基板７が配置
されている。また、この反応炉１には、図示しな
い真空ポンプが配設されている。 This MOCVD gas phase equipment consists of a cylindrical reactor 1
A nozzle 2 for supplying DMZ into the reactor 1 and a nozzle 3 for supplying H2S into the reactor 1,
Each of them is equipped with a power source 4a and a resistance heater 4 containing TbF 3 powder. Further, a high-frequency heating coil 5 for heating the inside of the reactor 1 is provided on the outer periphery of the reactor 1, and a graphite susceptor 6 coated with SiC is provided inside the reactor 1. A substrate 7 on which a thin film is formed is arranged on the tosasebuta 6. Further, this reactor 1 is provided with a vacuum pump (not shown).
このような構成からなるMOCVD気相装置を
用い、次のような条件で基板７上にZnS：TbF3
膜を作製した。 ZnS:TbF 3 was deposited on the substrate 7 under the following conditions using a MOCVD vapor phase apparatus with such a configuration.
A membrane was prepared.
〔作製条件〕 基板７上の温度…約300℃、 反応炉１内の真空度…0.1Torr、 ノズル２から反応炉１へのDMZ導入速度… ２×10-6mol／min、 ノズル３から反応炉１へのH2S導入速度… 6.7×10-6mol／min、 TbF3の加熱温度…1150℃。[Fabrication conditions] Temperature on substrate 7: approx. 300°C, degree of vacuum in reactor 1: 0.1 Torr, DMZ introduction rate from nozzle 2 to reactor 1: 2×10 -6 mol/min, reaction starts from nozzle 3 H 2 S introduction rate into furnace 1: 6.7×10 -6 mol/min, TbF 3 heating temperature: 1150°C.
上記の〜の各条件に設定したところ、反応
炉１内においては、DMZとH2Sとが反応して基
板７上でZnSとして気相成長するとともに、この
ZnSからなる気相中に抵抗加熱用ヒータ４から蒸
発したTbF3分子が取り込まれてZnS−TbF3薄膜
を作製することができた。 When the above conditions are set, DMZ and H 2 S react in the reactor 1 and grow as ZnS on the substrate 7 in a vapor phase.
The TbF 3 molecules evaporated from the resistance heater 4 were incorporated into the ZnS gas phase, making it possible to fabricate a ZnS-TbF 3 thin film.
次に、上記のようにして得られたZnS：TbF3
膜上にSm2O3からなる薄膜を作製して二重絶縁
構造のEL素子を製造した。このEL素子の輝度−
電圧特性を調べ、その結果を第２図に示した。 Next, ZnS:TbF 3 obtained as above
A thin film made of Sm 2 O 3 was formed on the film to produce an EL device with a double insulation structure. The brightness of this EL element -
The voltage characteristics were investigated and the results are shown in FIG.
第２図から明らかなように、このEL素子は、
周波数5kHz、電圧195Vで4500cd／m2の輝度を示
す高輝度で高耐圧の縁色発光の素子であることが
わかつた。ZnS膜に取り込まれるTbF3の濃度は
抵抗加熱ヒータの温度、反応炉の真空度に依存す
る。最適温度をドーピングさせるためには、反応
炉内を減圧下（1Torr以下）にする必要がある。 As is clear from Figure 2, this EL element is
It was found to be a high-brightness, high-voltage, edge-color emitting device that exhibits a brightness of 4500 cd/m 2 at a frequency of 5 kHz and a voltage of 195 V. The concentration of TbF 3 incorporated into the ZnS film depends on the temperature of the resistance heater and the degree of vacuum in the reactor. In order to dope at the optimum temperature, it is necessary to reduce the pressure inside the reactor (below 1 Torr).
〔実施例 ２〕
発光センタ物質にMn、MnCl2、MnF2、
SmF3、TmF3、CeF3、CeCl3を用いた他は、実
施例１と同様にして各々ZnS：Mn、ZnS：
SmF3、ZnS：TmF3、ZnS：Ceの薄膜を作製し
た。そして、これらの薄膜上にSm2O3の絶縁層
を形成して二重絶縁構造のEL素子を製造した。[Example 2] Mn, MnCl 2 , MnF 2 ,
ZnS : Mn , ZnS :
Thin films of SmF 3 , ZnS:TmF 3 , and ZnS:Ce were fabricated. Then, an insulating layer of Sm 2 O 3 was formed on these thin films to produce an EL device with a double insulation structure.
これらのEL素子は、いずれも高輝度、高耐圧
の特性を示し、ZnS：Mnを用いたものでは、黄
橙色に、ZnS：SmF3を用いたものでは、赤色に、
ZnS：TmF3、ZnS：Ceを用いたものでは、青色
にそれぞれ発光する素子が得られた。 All of these EL elements exhibit high brightness and high breakdown voltage characteristics; those using ZnS:Mn have a yellow-orange color, and those using ZnS:SmF 3 have a red color.
When ZnS:TmF 3 and ZnS:Ce were used, elements that emitted blue light were obtained.
〔実施例 ３〕
主原料にジエチルジルク（DEZ）とH2S、
DMZと硫化ジエチル（DES）、DEZとDEZ、
DEZと硫化ジメチル（DMS）の組合せでZnS（カ
ルコゲン亜鉛）膜を得るようにし、他は実施例１
と同様にしてZnSに発光センタ物質が添加されて
なる薄膜をそれぞれ作製した。これらの薄膜は、
Sm2O3による二重絶縁構造としたことにより、
高輝度、高耐圧のEL素子となつた。[Example 3] Diethylzirc (DEZ) and H 2 S as main raw materials,
DMZ and diethyl sulfide (DES), DEZ and DEZ,
A ZnS (chalcogen zinc) film was obtained by a combination of DEZ and dimethyl sulfide (DMS), and the rest were as in Example 1.
In the same manner as above, thin films made of ZnS with a luminescent center substance added were prepared. These thin films are
By adopting a double insulation structure with Sm 2 O 3 ,
It has become an EL element with high brightness and high voltage resistance.
〔実施例 ４〕
実施例１で用いたZnSからなるカルコゲン薄膜
をZnSe−TbF3薄膜を作製した。この薄膜は、
Sm2O3による二重絶縁構造としたことにより、
高輝度、高耐圧のEL素子となつた。[Example 4] A ZnSe-TbF 3 thin film was fabricated from the chalcogen thin film made of ZnS used in Example 1. This thin film is
By adopting a double insulation structure with Sm 2 O 3 ,
It has become an EL element with high brightness and high voltage resistance.
また、ZnSe薄膜を作製する際の原料は、DMZ
とH2Se、DEZとH2Se、DMZとDESe、DMZと
DMSe、DEZとDESe、DEZとDMSeなどの組合
せが可能であることがわかつた。 In addition, the raw material for producing the ZnSe thin film is DMZ
and H2Se , DEZ and H2Se , DMZ and DESe, DMZ and
It was found that combinations such as DMSe, DEZ and DESe, and DEZ and DMSe are possible.
以上説明したように、この発明の方法によれ
ば、前述した各発光センタ物質を減圧状態でそれ
ぞれ加熱蒸発させせてガス化し、このガスをZnS
またはZnSe気相中に取り込ませることができる
ので、高輝度、高耐圧の各特性を有する多色の薄
膜EL素子を作製することができる。
As explained above, according to the method of the present invention, each of the above-mentioned luminescent center substances is heated and evaporated under reduced pressure to gasify, and this gas is converted into ZnS.
Alternatively, since it can be incorporated into the ZnSe gas phase, a multicolor thin film EL element having high brightness and high breakdown voltage characteristics can be produced.
また、この方法によつて得られた薄膜EL素子
は、膜厚が一定で、しかも面積の大きい安価なも
のとなる。 Furthermore, the thin film EL device obtained by this method has a constant film thickness, a large area, and is inexpensive.
第１図は、この発明の薄膜EL素子の作製方法
に好適に用いられるMOCVD成長装置の反応炉
を示す概略構成図、第２図は、この発明の薄膜
EL素子の作製方法によつて得られたZnS：TbF3
二重絶縁薄膜EL素子の輝度−電圧特性を示すグ
ラフである。
FIG. 1 is a schematic configuration diagram showing a reactor of an MOCVD growth apparatus suitably used in the method for producing a thin film EL device of the present invention, and FIG.
ZnS:TbF 3 obtained by the EL device manufacturing method
3 is a graph showing the brightness-voltage characteristics of a double-insulated thin film EL element.
Claims (1)
セレン化合物ガスを反応炉内で反応させ、同時に
発光センタとなる物質をドーピングする有機金属
気相成長法による薄膜EL発光膜の作製方法にお
いて、発光センタ物質Ｘを減圧下の反応炉内で抵
抗加熱して蒸発させることによりドーピングして
ZnS：ＸまたはZnSe：Ｘ膜を形成することを特
徴とする薄膜EL素子の作製方法。 ２ 発光センタ物質ＸがMn，MnCl2，MnF2，
TbF3，SmF3，TmF3，CeF3，CeCl3からなる群
より選ばれたものであることを特徴とする特許請
求範囲第１項記載の薄膜EL素子の作製方法。 ３ 有機亜鉛化合物ガスがジメチルジンクまたは
ジエチルジンクであることを特徴とする特許請求
範囲第１項記載の薄膜EL素子の作製方法。 ４ 硫黄化合物またはセレン化合物がH2S，
H2Se，ジメチルイオウ，ジエチルイオウ，ジメ
チルセレン，ジエチルセレンのいずれかであるこ
とを特徴とする特許請求範囲第１項記載の薄膜
EL素子の作製方法。[Claims] 1. A method for producing a thin EL light-emitting film by an organometallic vapor phase epitaxy method, in which an organozinc compound gas and a sulfur compound gas or a selenium compound gas are reacted in a reaction furnace, and at the same time, a substance to be a luminescent center is doped. In this method, the luminescent center substance X is doped by being evaporated by resistance heating in a reaction furnace under reduced pressure
A method for manufacturing a thin film EL device, characterized by forming a ZnS:X or ZnSe:X film. 2 The luminescent center substance X is Mn, MnCl 2 , MnF 2 ,
2. The method of manufacturing a thin film EL device according to claim 1, wherein the thin film EL device is selected from the group consisting of TbF 3 , SmF 3 , TmF 3 , CeF 3 and CeCl 3 . 3. The method for producing a thin film EL device according to claim 1, wherein the organic zinc compound gas is dimethyl zinc or diethyl zinc. 4 Sulfur compound or selenium compound is H 2 S,
The thin film according to claim 1, which is any one of H 2 Se, dimethyl sulfur, diethyl sulfur, dimethyl selenium, and diethyl selenium.
How to make an EL element.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61015390A JPS62176091A (en) | 1986-01-27 | 1986-01-27 | Manufacture of thin film el device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61015390A JPS62176091A (en) | 1986-01-27 | 1986-01-27 | Manufacture of thin film el device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62176091A JPS62176091A (en) | 1987-08-01 |
| JPH0369157B2 true JPH0369157B2 (en) | 1991-10-31 |
Family
ID=11887409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61015390A Granted JPS62176091A (en) | 1986-01-27 | 1986-01-27 | Manufacture of thin film el device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62176091A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009150764A1 (en) | 2008-06-09 | 2009-12-17 | 株式会社菊星 | Hair style treatment device |
| US9046860B2 (en) | 1995-03-27 | 2015-06-02 | Canon Kabushiki Kaisha | Coupling part, photosensitive drum, process cartridge and electrophotographic image forming apparatus |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6343292A (en) * | 1986-08-08 | 1988-02-24 | 日本電信電話株式会社 | Organic metal vapor phase growth system |
| JP2545694B2 (en) * | 1993-10-22 | 1996-10-23 | 日産自動車株式会社 | Method for manufacturing dispersed EL panel |
| JP4851875B2 (en) * | 2006-07-14 | 2012-01-11 | 川崎重工業株式会社 | Rear step mounting structure for motorcycle and motorcycle equipped with the rear step mounting structure |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6137857A (en) * | 1984-07-30 | 1986-02-22 | Seiko Epson Corp | Method and apparatus for preparation of thin phosphor film |
-
1986
- 1986-01-27 JP JP61015390A patent/JPS62176091A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6137857A (en) * | 1984-07-30 | 1986-02-22 | Seiko Epson Corp | Method and apparatus for preparation of thin phosphor film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9046860B2 (en) | 1995-03-27 | 2015-06-02 | Canon Kabushiki Kaisha | Coupling part, photosensitive drum, process cartridge and electrophotographic image forming apparatus |
| WO2009150764A1 (en) | 2008-06-09 | 2009-12-17 | 株式会社菊星 | Hair style treatment device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62176091A (en) | 1987-08-01 |
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