JPH0294289A - Manufacture of thin film type electroluminescence element - Google Patents
Manufacture of thin film type electroluminescence elementInfo
- Publication number
- JPH0294289A JPH0294289A JP63245638A JP24563888A JPH0294289A JP H0294289 A JPH0294289 A JP H0294289A JP 63245638 A JP63245638 A JP 63245638A JP 24563888 A JP24563888 A JP 24563888A JP H0294289 A JPH0294289 A JP H0294289A
- Authority
- JP
- Japan
- Prior art keywords
- emitting layer
- thin film
- light emitting
- layer
- degree
- 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.)
- Pending
Links
- 239000010409 thin film Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000005401 electroluminescence Methods 0.000 title 1
- 238000001704 evaporation Methods 0.000 claims abstract description 22
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 10
- 238000005566 electron beam evaporation Methods 0.000 claims description 11
- 239000010408 film Substances 0.000 claims description 5
- 239000004020 conductor Substances 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 238000000313 electron-beam-induced deposition Methods 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 7
- 238000009413 insulation Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910019695 Nb2O6 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000002784 hot electron Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、デイスプレィ装置などに利用される薄膜形
のエレクトロルミネッセンス（以下、ＥＬという）素子
、とくにＺｎＳ：Ｓｍ、Ｆからなる発光層を有して発光
三原色の一つである赤色発光を行う上記ＥＬ素子の製造
法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a thin-film electroluminescent (hereinafter referred to as EL) element used in display devices, etc., and particularly to a thin-film electroluminescent (hereinafter referred to as EL) element having a light-emitting layer made of ZnS:Sm, F. The present invention relates to a method for manufacturing the above-mentioned EL element that emits red light, which is one of the three primary colors of light.
一般に、薄膜形ＥＬ素子は、少なくとも表示側が透明で
かつ通常はどちらか一方がパターン化された一対の電極
間に、発光層と誘電層とが配設された構造を有しており
、上記誘電層が発光層の片側のみに設けられた卓絶縁形
ならびに同じく両側に設けられた二重絶縁形のものが知
られており、また発光層が一層に限らす誘電層を介して
二層以上に積層されたものもある。In general, a thin film EL element has a structure in which a light emitting layer and a dielectric layer are disposed between a pair of electrodes that are transparent at least on the display side and usually one of which is patterned. A desk insulation type in which the layer is provided on only one side of the light emitting layer and a double insulation type in which the layer is provided on both sides are known. Some are laminated.
このようなＥＬ素子の駆動は、交流駆動方式では、両電
極間に交流電圧を印加することにより、発光層にその発
光開始しきい値電界以上の電界をかけて発光させ、この
発光色を表示側の表面に表出させることにより、所定パ
ターンの表示を行わせるものである。In the AC driving method, such an EL element is driven by applying an AC voltage between both electrodes to apply an electric field equal to or higher than the threshold electric field for starting light emission to the light emitting layer, causing it to emit light, and displaying the color of the emitted light. By exposing the side surface, a predetermined pattern is displayed.
ところで、上記発光層を構成する発光体材料には、通常
ＺｎＳやＣａＳなどの蛍光体からなる母材中に少量の発
光付活剤を配合したものが使用されており、この発光付
活剤の種類によって特有の発光色が示される。たとえば
、光の三原色に近い発光色が得られる発光体材料として
は、赤色発光ではＺｎＳ ： Ｓｍ、Ｆ、緑色発光では
ＺｎＳ：Ｔｂ、Ｆ、青色発光ではＺｎＳ：Ｔｍ、Ｆがそ
れぞれ代表的なものとして知られている（文献不詳）。By the way, the luminescent material constituting the luminescent layer is usually a base material made of a phosphor such as ZnS or CaS mixed with a small amount of luminescent activator. Each type exhibits a unique emitted color. For example, typical luminescent materials that produce luminescent colors close to the three primary colors of light include ZnS:Sm, F for red luminescence, ZnS:Tb, F for green luminescence, and ZnS:Tm, F for blue luminescence. It is known as (document unknown).
しかしながら、とくに赤色発光を行う発光体材料である
ＺｎＳ：Ｓｍ、Ｆに関しては、従来より輝度向上のため
に発光層形成に採用する各種真空中薄膜形成法の条件を
始めとして種々の検討〔たとえば、Ｊ、Ｊ、八、Ｐ、
（１９８４）Ｐ、 ６など〕が行われているが、現状で
は１ＫＩＩｚ駆動における最大輝度が２００ｃｄ≠
ためにカラーデイスプレィなどの赤色発光用ＥＬ素子と
しては輝度不足で実用性がなかった。However, with regard to ZnS:Sm, F, which is a luminescent material that emits red light in particular, various studies have been conducted, including the conditions of various thin film formation methods in vacuum, which are conventionally adopted for forming luminescent layers to improve brightness [e.g. J, J, 8, P,
(1984) P, 6], but currently the maximum brightness in 1KIIz drive is 200 cd≠, so the brightness is insufficient and it is not practical as an EL element for red light emission such as a color display.
この発明は、上述の状況に鑑み、赤色発光用の発光体材
料としてＺｎＳ：Ｓｍ、Ｆを使用して、かつ高輝度で実
用性充分な薄膜形ＥＬ素子の製造法を提供することを目
的としている。In view of the above-mentioned circumstances, the present invention aims to provide a method for manufacturing a thin film EL element that uses ZnS:Sm, F as a luminescent material for red light emission and is highly luminous and has sufficient practicality. There is.
この発明者らは、上記の目的を達成するために鋭意検討
を重ねた結果、ＺｎＳ：Ｓｍ、Ｆからなる発光層を有す
るＥＬ素子の輝度がこの発光層の結晶性と発光中心濃度
つまりＳｍ（サマリウム）濃度によって大きく影響され
、この発光層の形成手段として電子ビーム蒸着法を採用
した場合には上記結晶性が形成雰囲気の真空度と密接に
相関し、この真空度と発光層中のＳｍ７１度を特定値に
設定することにより、従来では得られなかった高輝度の
赤色発光が達成されることを見い出し、この発明をなす
に至った。As a result of intensive studies to achieve the above object, the inventors found that the brightness of an EL element having a light emitting layer made of ZnS:Sm,F depends on the crystallinity of the light emitting layer and the concentration of light emitting centers, that is, Sm( When electron beam evaporation is adopted as a means of forming this luminescent layer, the crystallinity is closely correlated with the vacuum degree of the formation atmosphere, and this vacuum degree and the Sm in the luminescent layer are 71 degrees Celsius. The present inventors have discovered that by setting the value to a specific value, it is possible to achieve high-intensity red light emission that could not be obtained in the past, and have thus come up with the present invention.
すなわち、この発明は、少なくとも一方が透明である一
対の電極間にＺｎＳ：Ｓｍ、Ｆからなる発光層と誘導体
層とが介在されてなる薄膜形ＥＬ素子の製造法において
、上記発光層を、電子ビム蒸着法によってＳｍおよびＦ
を含有するＺｎＳを蒸発源として真空度５Ｘ１０−ｈＴ
ｏｒｒ以下の雰囲気中で成膜して形成し、かつ層中のＳ
ｍ？ｍ度を０．２〜１．０モル％の範囲とすることを特
徴とする薄膜形ＥＬ素子の製造法に係るものである。That is, the present invention provides a method for manufacturing a thin film EL device in which a light emitting layer made of ZnS:Sm,F and a dielectric layer are interposed between a pair of electrodes, at least one of which is transparent. Sm and F by beam evaporation method
Vacuum degree 5X10-hT using ZnS containing as evaporation source
It is formed by forming a film in an atmosphere below orr, and the S in the layer is
M? The present invention relates to a method for manufacturing a thin film EL element, characterized in that the m degree is in the range of 0.2 to 1.0 mol%.
また、この発明では、上記電子ビーム蒸着法における蒸
発源のＳｒｒ＋？ａ度を０．１〜１．５モル％の範囲と
した構成を好適態様としている。Further, in the present invention, Srr+? A preferred embodiment is a configuration in which the a degree is in the range of 0.1 to 1.5 mol%.
この発明においては、前記の如＜ＺｎＳ：Ｓｍ。 In this invention, as described above <ZnS:Sm.
Ｆからなる発光層を電子ビーム蒸着法により形成するに
あたり、形成雰囲気の真空度を５Ｘ１０Ｔｏｒｒ以下と
し、かつ形成される発光層中のＳｍ ？Ｍ度を０．２〜
１．０モル％に設定することにより、高い発光輝度を実
現する。When forming a light-emitting layer made of F by electron beam evaporation, the degree of vacuum in the formation atmosphere is set to 5×10 Torr or less, and Sm? M degree from 0.2
By setting it to 1.0 mol%, high luminescence brightness is achieved.
すなわち、上記真空度に関しては、後述する実施例１に
おいて発光層形成時の真空度を種々変えて他の条件は形
成される発光層中のＳ ｍ ７＠度が等しくなるように
同一に設定して作製されたＥＬ素子につき、その真空度
と結晶性および輝度を示す第１表から明らかなように、
真空度が高くなるほど結晶性が向上すると同時に輝度も
高くなる傾向が認められており、とくに真空度が５Ｘ１
０−６Ｔｏｒｒ以下では非常に高い輝度が得られること
が判明している。この理由は、発光層形成時の真空度が
高くなるほど蒸着粒子のエネルギーが高くなり、これに
伴って蒸着面での結晶粒の成長が活発化するとともに不
純物原子の混入量が減少する結果、形成される発光層の
結晶性が向上して発光効率を高めるように作用し、とく
に上記特定値以下の高真空条件で上記作用が顕著に発現
されるものと考えられる。That is, regarding the above degree of vacuum, in Example 1 to be described later, the degree of vacuum during the formation of the light emitting layer was varied, and the other conditions were set the same so that the S m 7@ degree in the formed light emitting layer was equal. As is clear from Table 1, which shows the degree of vacuum, crystallinity, and brightness of EL devices manufactured using
It has been observed that the higher the degree of vacuum, the better the crystallinity and the higher the brightness, especially when the degree of vacuum is 5X1.
It has been found that very high brightness can be obtained at 0-6 Torr or less. The reason for this is that the higher the degree of vacuum during formation of the emissive layer, the higher the energy of the evaporated particles, which in turn activates the growth of crystal grains on the evaporation surface and reduces the amount of impurity atoms mixed in. It is considered that the crystallinity of the light-emitting layer is improved and the luminous efficiency is increased, and the above-mentioned effect is particularly noticeable under high vacuum conditions below the above-mentioned specific value.
一方、発光層中のＳｍｔｆｆｉ度に関しては、後述する
実施例２において発光層形成時に真空度以外の条件を種
々変化させることによって作製した上記Ｓｍ濃度が異な
るＥＬ素子のＳｍ？Ｍ度−輝度の相関を示す第２図から
明らかなように、５ｍ９７４度が０．２〜１．０モル％
の範囲よりも低くなっても高くなってもともに著しい輝
度低下を生じることが確認されている。これは、Ｓｍ濃
度が０．２モル％より少なくなるとＳｍ発光中心とホッ
トエレクトロンとの衝突励起の確率低下により、逆に１
．０モル％より多くなると濃度消光により、それぞれ輝
度低下が著しくなるものと考えられる。On the other hand, regarding the Smtffi degree in the light emitting layer, the Sm? As is clear from Figure 2, which shows the correlation between M degree and brightness, 5m974 degree is 0.2 to 1.0 mol%.
It has been confirmed that a significant decrease in brightness occurs when the brightness is lower or higher than the range of . When the Sm concentration is less than 0.2 mol%, the probability of collisional excitation between Sm emission centers and hot electrons decreases, and conversely, 1
．． It is considered that when the amount exceeds 0 mol %, the luminance decreases significantly due to concentration quenching.
なお、形成される発光層中のＳｍ濃度は、使用する蒸発
源中のＳｍ濃度のほか、この蒸発源の形態、大きさ（ベ
レットでは粒度）、密度、作製方法ならびに蒸着時の基
板温度、成膜速度、電子ビム強度、基板位置の如き各種
条件によっても変化する。したがって、この発明では、
発光層中のＳｍｆ１４度が０．２〜１．０モル％の範囲
となるように蒸発源の種類と蒸着条件を適宜選択すれば
よいが、とくに蒸発源中のＳｍ７１度は通常０．ｌ〜１
．５モル％程度とすることが推奨される。The Sm concentration in the light emitting layer formed depends on the Sm concentration in the evaporation source used, as well as the form, size (particle size for pellets), density, manufacturing method, substrate temperature during evaporation, and formation of the evaporation source. It also changes depending on various conditions such as film speed, electron beam intensity, and substrate position. Therefore, in this invention,
The type of evaporation source and vapor deposition conditions may be appropriately selected so that the Smf 14 degrees in the light emitting layer is in the range of 0.2 to 1.0 mol%, but in particular, the Sm 71 degrees in the evaporation source is usually 0.2 to 1.0 mol%. l~1
．． It is recommended that the content be about 5 mol%.
なお、蒸発源の作製は、一般にＺｎＳ粉末に所要量のＳ
ｍ Ｆ ：＋粉末を均一に添加混合し、この混合物を
加圧成形してペレット状やディスク状などの所要形状と
することによって行われる。In addition, to prepare the evaporation source, generally a required amount of S is added to ZnS powder.
This is carried out by uniformly adding and mixing m F :+ powder, and press-molding this mixture into a desired shape such as a pellet shape or a disk shape.
電子ビーム蒸着によって発光層を形成するには、基板と
蒸発源を蒸着チャンバー内にセットし、チャンバー内を
真空度５Ｘ１０−６Ｔｏｒｒ以下の不活性ガス雰囲気と
して、基板温度を２００〜２５０℃程度に設定した上で
、蒸発源に電子ビームを照射して加熱蒸発させればよい
。このとき、成膜速度は通常ｌＯＯ〜６００ 人／分程
度、最終的に得られる発光層の厚みを３．０００〜７，
０００人程度に設定すればよい。To form a light-emitting layer by electron beam evaporation, set the substrate and evaporation source in a evaporation chamber, create an inert gas atmosphere in the chamber with a vacuum level of 5 x 10-6 Torr or less, and set the substrate temperature to about 200 to 250 °C. After that, the evaporation source may be heated and evaporated by irradiating the evaporation source with an electron beam. At this time, the film formation rate is usually about 100 to 600 persons/min, and the thickness of the final luminescent layer is 3,000 to 7,000 people/min.
The number may be set to about 000 people.
第１図はこの発明によって作製される二重絶縁形の赤色
発光ＥＬ素子の一例を示すものである。FIG. 1 shows an example of a double insulation type red light emitting EL device manufactured according to the present invention.
図において、１はガラス製の基板であり、その一方の表
面にインジウム−スズ複合酸化物（以下、ＩＴＯという
）やフッ素を含む酸化スズなどの透明性導電材料の薄膜
からなる表示側電極２が形成されている。この表示側電
極２上には順次、第１の誘電層３、前記のＺｎＳ：Ｓｍ
、Ｆからなる発光層４、第２の誘電層５、Ａ１薄膜また
は上記透明性導電材料の薄膜からなる背面側電極６が積
層形成されている。In the figure, 1 is a glass substrate, on one surface of which a display-side electrode 2 made of a thin film of a transparent conductive material such as indium-tin composite oxide (hereinafter referred to as ITO) or fluorine-containing tin oxide is disposed. It is formed. On this display side electrode 2, a first dielectric layer 3, the above-mentioned ZnS:Sm
, a second dielectric layer 5, and a back side electrode 6 made of an A1 thin film or a thin film of the transparent conductive material described above.
ここで、第１および第２の誘電層３．５の構成材料とし
ては、既存の絶縁材料をいずれも使用でき、たとえば’
ｌ”ａ２ ｏｓ 、Ａｌｚ Ｏｔ 、 Ｙ２０ｗｌ 。Here, any existing insulating material can be used as the constituent material of the first and second dielectric layers 3.5, such as '
l”a2 os, Alz Ot, Y20wl.
ＳｉＯ□、Ｓ ５３Ｎｐ 、ＴＩ Ｏ□、Ｎｂ２Ｏ６、
ＢａＴｉ０． 、ＳｒＴｉＯ３、ＰｂＴｉ０：＋などが
挙げられ、各誘電層で異なるものを使用してもよい。ま
た、画成電層３．５の一方もしくは両方を、構成材料の
異なる２層以上の積層物としても差し支えない。SiO□, S53Np, TIO□, Nb2O6,
BaTi0. , SrTiO3, PbTi0:+, etc., and different materials may be used for each dielectric layer. Furthermore, one or both of the definition electrode layers 3.5 may be a laminate of two or more layers made of different constituent materials.
各層の厚さは、画成電層３，５では３，０００〜７．０
００人程度、側電極２．６では１，０００〜３゜０００
人程度である。なお、これら各層の形成手段としては、
電子ビーム蒸着や抵抗加熱蒸着の如き真空蒸着法、高周
波スパッタリングの如きスパッタリング法、イオンブレ
ーティング法などの既存の種々の真空中薄膜形成法を使
用材料種に応じて適宜採用できる。The thickness of each layer is 3,000 to 7.0 for the definition layers 3 and 5.
00 people, 1,000 to 3°000 for side electrode 2.6
It is about the size of a person. Note that the means for forming each of these layers are as follows:
Various existing vacuum thin film forming methods such as vacuum evaporation methods such as electron beam evaporation and resistance heating evaporation, sputtering methods such as high frequency sputtering, and ion blating methods can be employed as appropriate depending on the type of material used.
上記構成のＥＬ素子では、発光層４にその発光開始しき
い値電界を超える電界がかかりうる電圧を側電極２．６
間に印加することにより、発光層４がＺｎＳ：Ｓｍ、Ｆ
に基づく赤色に発光する。In the EL element having the above configuration, a voltage that can apply an electric field exceeding the emission start threshold electric field to the light emitting layer 4 is applied to the side electrodes 2.6.
By applying a voltage between
It emits red light based on
そして、この赤色発光はＩＫＩ（ｚ駆動で４００ｃｄ／
ｄ以上という高輝度を示すものとなる。And this red light emission is IKI (400 cd/ in z drive)
It exhibits high brightness of d or more.
なお、この発明は、上述した二重絶縁形のＥＬ素子のほ
か、卓絶縁形のＥＬ素子や、一方の電極をパターンの異
なる２層以上の多層構造としたＥＬ素子にも適用可能で
ある。In addition to the above-mentioned double insulation type EL element, the present invention is also applicable to a table insulation type EL element and an EL element in which one electrode has a multilayer structure of two or more layers with different patterns.
この発明の製造法によれば、ＺｎＳ：Ｓｍ、Ｆからなる
発光層を特定条件の電子ビーム蒸着によって形成し、か
つこの発光層中のＳ ｍ ’濃度を特定範囲に設定する
ことから、上記発光体材料を使用した発光層を有する従
来のＥＬ素子では達成されなかった高い発光輝度を示し
てカラーデイスプレィなどとして実用性充分な薄膜形Ｅ
Ｌ素子を提供できる。According to the manufacturing method of the present invention, a light-emitting layer made of ZnS:Sm, F is formed by electron beam evaporation under specific conditions, and the S m ' concentration in this light-emitting layer is set within a specific range. Thin-film type E exhibits high luminance that could not be achieved with conventional EL elements that have a light-emitting layer made of organic material, making it practical for use in color displays, etc.
L elements can be provided.
また、上記方法において、蒸発源のＳ ｍ ’０％度を
０．１〜１．５モル％の範囲とした場合は、上記特定範
囲のＳｍ１１度を有する発光層を容易に形成できる利点
がある。In addition, in the above method, when the Sm'0% degree of the evaporation source is set in the range of 0.1 to 1.5 mol%, there is an advantage that a light emitting layer having an Sm11 degree within the above specific range can be easily formed. .
以下、この発明を実施例によって具体的に説明する。 Hereinafter, the present invention will be specifically explained with reference to Examples.
実施例１
縦３４龍、横３４１重、厚さｌ、 ｌ ＊＊のガラス製
基板の一面側に電子ビーム蒸着法によりＩＴＯ薄膜から
なる厚さ２．０００人の表示側電極を形成し、ついでこ
の電極上に順次、スパッタリング法によりＴ ａ ｚ
Ｏｓからなる厚さ４，０００人の第１の誘電層、電子ビ
ーム蒸着法によりＺｎＳ：Ｓｍ、Ｆからなる厚さ５，０
００人の発光層、スパッタリング法により’ｒａｚｏｓ
からなる厚さ４，０００人の第２の誘電層、抵抗加熱蒸
着法によりＡＩ薄膜からなる厚さ１，５００人の所定パ
ターンの背面側電極を積層形成して、第１図で示す構造
のＥＬ素子を作製した。Example 1 A display-side electrode made of an ITO thin film with a thickness of 2,000 mm was formed on one side of a glass substrate measuring 34 mm long, 341 mm wide, and 1 and 1 ** thick by electron beam evaporation, and then On this electrode, T a z
A first dielectric layer 4,000 thick consisting of Os, 5,000 thick consisting of ZnS:Sm,F by electron beam evaporation
00 luminescent layer, 'razos' by sputtering method
A second dielectric layer with a thickness of 4,000 layers and a back electrode of a predetermined pattern with a thickness of 1,500 layers made of an AI thin film were laminated using a resistance heating evaporation method to form the structure shown in An EL device was produced.
このとき、電子ビーム蒸着法による発光層の形成を、基
板温度２２０℃、成膜速度３００Ａ／分として、真空度
のみを下記第１表に記載されるように種々変更した条件
下で行い、いずれも発光層中のＳｍ？１度が０．３モル
％である試料１１ｈｌ〜７のＥＬ素子を作製した。At this time, the formation of the light emitting layer by electron beam evaporation was carried out at a substrate temperature of 220°C, a film formation rate of 300 A/min, and only the degree of vacuum was varied as shown in Table 1 below. Also Sm in the luminescent layer? EL elements of samples 11hl to 7 in which 1 degree was 0.3 mol % were fabricated.
これらＥＬ素子について、発光層の結晶性を示すＸ線回
折半値幅と１Ｋｌｌｚ駆動による最大発光輝度を測定し
たところ、つぎの第１表の結果が得られた。For these EL elements, the half width of X-ray diffraction, which indicates the crystallinity of the light emitting layer, and the maximum luminance by driving at 1 Kllz were measured, and the results shown in Table 1 below were obtained.
第 １
表
第１表の結果から、発光層形成時の真空度と発光層の結
晶性および発光輝度とが密接に相関しており、真空度が
高くなるほど結晶性が向上して高輝度が得られ、とくに
この発明の方法である真空度５Ｘ１０−ｂＴｏｒｒ以下
で作製したＥＬ素子隘５〜７はこれらより真空度の低い
条件で作製したＥＬ素子ｍ１〜４に比較して格段に高い
輝度を発現することが明らかである。Table 1 From the results in Table 1, the degree of vacuum during formation of the light emitting layer is closely correlated with the crystallinity and luminance of the light emitting layer, and the higher the degree of vacuum, the better the crystallinity and the higher the brightness. In particular, the EL elements 5 to 7 produced using the method of the present invention at a vacuum level of 5 x 10-b Torr or less exhibit much higher luminance than the EL elements m1 to 4 produced at lower vacuum conditions. It is clear that
実施例２
電子ビーム蒸着法による発光層の形成に際し、真空度を
５Ｘ１０−６Ｔｏｒｒとし、他の条件（主として蒸発源
のＳｍ７１度）を種々変更して発光層のＳｍ濃度を種々
異ならせた以外は、実施例１と同様にして多数のＥＬ素
子を作製した。Example 2 When forming a light-emitting layer by electron beam evaporation, the degree of vacuum was set to 5X10-6 Torr, and other conditions (mainly Sm of the evaporation source at 71 degrees) were variously changed to vary the Sm concentration of the light-emitting layer. A large number of EL devices were manufactured in the same manner as in Example 1.
これらＥＬ素子について、発光層のＳ ｍ ？ａ度をＩ
ＣＰＳ（プラズマ発光分光分析）にて測定するとともに
、１ＫＩｌｚ駆動による最大発光輝度を測定した。その
結果、上記Ｓｍ濃度と最大発光輝度との間にほぼ第２図
で示す関係があることが判った。Regarding these EL elements, the S m ? of the light emitting layer? degree a degree
In addition to measuring by CPS (plasma emission spectroscopy), the maximum luminance was measured by driving at 1Klz. As a result, it was found that there is a relationship approximately shown in FIG. 2 between the Sm concentration and the maximum luminance.
なお、図中の最大発光輝度は３ｍ７．ｉ７ｉ度１．２モ
ル％の発光層による輝度を基準とした相対値で示してい
る。The maximum luminance in the figure is 3m7. It is shown as a relative value based on the luminance due to the luminescent layer having i7i degree of 1.2 mol %.
第２図の結果から、発光層中のＳ ｍ ｆＱ度が０．２
〜１．０モル％の範囲にある場合に高い発光輝度が得ら
れ、この範囲よりも少なくても、また多くても輝度低下
が著しくなることが判る。From the results shown in Figure 2, the S m fQ degree in the light emitting layer is 0.2.
It can be seen that high luminance is obtained when the content is in the range of 1.0 mol %, and even if the content is less than or greater than this range, the luminance decreases significantly.
実施例３
電子ビーム蒸着法による発光層の形成に際し、蒸発源の
Ｓｍ濃度および真空度を下記第２表に示す値とした以外
は、実施例１と同様にしてＥＬ素子Ａ−Ｅを作製した。Example 3 EL devices A-E were produced in the same manner as in Example 1, except that the Sm concentration of the evaporation source and the degree of vacuum were set to the values shown in Table 2 below when forming the light emitting layer by electron beam evaporation. .
このＥＬ素子Ａ−Ｅについて、実施例２と同様にして発
光層中のＳｍ濃度を測定した結果を第２表に示すととも
に、ＩＫＨｚ駆動による輝度−電圧特性の測定結果を第
３図に示す。Table 2 shows the results of measuring the Sm concentration in the light emitting layer of EL elements A to E in the same manner as in Example 2, and FIG. 3 shows the results of measuring the brightness-voltage characteristics by IKHz driving.
第 ２ 表
第３図の結果から、この発明の製造法によるＥＬ素子Ａ
では最大輝度４ＱＯｃｄ／ｒｔｆに達する高輝度が得ら
れてかつ輝度の立ち上がりが急峻である特性を示すのに
対し、蒸着時の真空度および発光層中のＳｍｔｌｉＡ度
のいずれか一方でもこの発明の規定範囲を外れる条件で
得られるＥＬ素子Ｂ−Ｅは到達輝度が低く輝度の立ち上
がりも緩やかで実用性に乏しいことが判る。From the results shown in Table 2 and Figure 3, it can be seen that EL element A manufactured by the manufacturing method of the present invention
In this case, high brightness reaching a maximum brightness of 4QOcd/rtf can be obtained and the rise in brightness is steep. It can be seen that the EL elements B-E obtained under conditions outside the range have low achieved brightness and a slow rise in brightness, and are therefore impractical.
第１図はこの発明の製造法によって作製される薄膜形エ
レクトロルミネッセンス素子の構造例を示す断面図、第
２図は実施例２で作製された同上素子の発光層中のＳｍ
濃度と最大発光輝度との相関図、第３図は実施例３で作
製されたＥＬ素子の輝度−電圧特性図である。
２・・・表示側電極、３・・・誘電層、４・・・発光層
、５・・・誘電層、６・・・背面側電極
特許出願人 日立マクセル株式会社
第１
第２図FIG. 1 is a cross-sectional view showing an example of the structure of a thin film electroluminescent device manufactured by the manufacturing method of the present invention, and FIG. 2 shows Sm in the light emitting layer of the same device manufactured in Example 2.
A correlation diagram between concentration and maximum luminance, and FIG. 3 is a luminance-voltage characteristic diagram of the EL element manufactured in Example 3. 2...Display side electrode, 3...Dielectric layer, 4...Light emitting layer, 5...Dielectric layer, 6...Back side electrode Patent applicant Hitachi Maxell Ltd. 1 Figure 2
Claims (2)
Ｓ：Ｓｍ，Ｆからなる発光層と誘電層とが介在されてな
る薄膜形エレクトロルミネツセンス素子の製造法におい
て、上記発光層を、電子ビーム蒸着法によつてＳｍおよ
びＦを含有するＺｎＳを蒸発源として真空度５×１０＾
−＾６Ｔｏｒｒ以下の雰囲気中で成膜して形成し、かつ
層中のＳｍ濃度０．２〜１．０モル％の範囲とすること
を特徴とする薄膜形エレクトロルミネツセンス素子の製
造法。(1) Zn between a pair of electrodes, at least one of which is transparent
S: In a method for manufacturing a thin film electroluminescent device having a light emitting layer and a dielectric layer interposed between Sm and F, the light emitting layer is coated with ZnS containing Sm and F by an electron beam evaporation method. Vacuum degree 5×10^ as evaporation source
- A method for manufacturing a thin film electroluminescent device, characterized in that the film is formed in an atmosphere of 6 Torr or less, and the Sm concentration in the layer is in the range of 0.2 to 1.0 mol%.
にある請求項（１）に記載の薄膜形エレクトロルミネツ
センス素子の製造法．(2) The Sm concentration of the evaporation source is 0. The method for producing a thin film electroluminescent device according to claim 1, wherein the amount is in the range of 1 to 1.5 mol%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63245638A JPH0294289A (en) | 1988-09-29 | 1988-09-29 | Manufacture of thin film type electroluminescence element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63245638A JPH0294289A (en) | 1988-09-29 | 1988-09-29 | Manufacture of thin film type electroluminescence element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0294289A true JPH0294289A (en) | 1990-04-05 |
Family
ID=17136635
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63245638A Pending JPH0294289A (en) | 1988-09-29 | 1988-09-29 | Manufacture of thin film type electroluminescence element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0294289A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0414398U (en) * | 1990-05-28 | 1992-02-05 | ||
| JPH0414397U (en) * | 1990-05-28 | 1992-02-05 |
-
1988
- 1988-09-29 JP JP63245638A patent/JPH0294289A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0414398U (en) * | 1990-05-28 | 1992-02-05 | ||
| JPH0414397U (en) * | 1990-05-28 | 1992-02-05 |
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