JPH02173617A - Electroluminescence element - Google Patents
Electroluminescence elementInfo
- Publication number
- JPH02173617A JPH02173617A JP63327885A JP32788588A JPH02173617A JP H02173617 A JPH02173617 A JP H02173617A JP 63327885 A JP63327885 A JP 63327885A JP 32788588 A JP32788588 A JP 32788588A JP H02173617 A JPH02173617 A JP H02173617A
- Authority
- JP
- Japan
- Prior art keywords
- oxygen
- film
- diamond
- carbon
- contg
- 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.)
- Granted
Links
- 238000005401 electroluminescence Methods 0.000 title abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 239000007789 gas Substances 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 7
- -1 CH3OH and C2H5OH Chemical class 0.000 abstract description 3
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 19
- 238000010586 diagram Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000001017 electron-beam sputter deposition Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Electroluminescent Light Sources (AREA)
- Luminescent Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はダイヤモンド状炭素膜を用いた電界発光素子に
関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an electroluminescent device using a diamond-like carbon film.
（従来の技術）
従来、発光表示材料である薄膜型の電界発光（ＥＬ）素
子材料としては、ＺｎＳ、 ＺｎＣｄ５、Ｚｎ５ｅ、
ＣａＳ、 ＳｒＳ等の母材に、Ｃｕ％Ｍｎ、希土類、弗
化物等の添加剤を加えたものが公知である。(Prior Art) Conventionally, thin film type electroluminescent (EL) element materials that are light emitting display materials include ZnS, ZnCd5, Zn5e,
It is known that additives such as Cu%Mn, rare earths, and fluorides are added to base materials such as CaS and SrS.
（発明が解決しようとしている問題点）薄膜型ＥＬ素子
の発光層は、抵抗加熱、電子ビーム蒸着或いはスパッタ
法により生成するが、膜の構造欠陥等のため特に湿度に
弱く、発光が不安定であり劣化するという欠点があり、
Ａ−ｆＫ面をも包みこむ防湿膜を必要とするという問
題があった。(Problem to be solved by the invention) The light-emitting layer of a thin-film EL element is produced by resistance heating, electron beam evaporation, or sputtering, but due to structural defects in the film, it is particularly vulnerable to humidity and the light emission is unstable. There is a drawback that it deteriorates,
There is a problem in that a moisture-proof film that also covers the A-fK surface is required.
かかる耐湿性の聞届を解決するために、発光層をダイヤ
モンド状炭素膜で形成したＥＬ素子が＾ｐｐ１． Ｐｈ
ｙｓ、 ＬｅｔＬ、［５３（１９） ９月、１９８８年
］に開示されている。In order to solve the problem of moisture resistance, an EL element in which the light-emitting layer is formed of a diamond-like carbon film has been developed. Ph
ys, LetL, [53(19) September, 1988].
かかるＥＬ素子は、従来材料を用いたＥＬ′：Ａ子に比
べ耐湿性に優れたものであるが、印加電圧が高く、低輝
度で発行寿命も短いという欠点を有する。Although such an EL element has better moisture resistance than EL':A elements using conventional materials, it has the disadvantages of high applied voltage, low brightness, and short emitting life.
そこで１本発明のＩＮ的は、上記従来技術の問題点を解
決し、耐湿性に優れ、低印加電圧でも高輝度、長寿命で
あり、しかもより短波長側に発光するＥＬ素子を提供す
ることにある。Therefore, one objective of the present invention is to solve the above-mentioned problems of the prior art, and to provide an EL element that has excellent moisture resistance, high brightness even at low applied voltage, long life, and emits light at a shorter wavelength. It is in.
（問題点を解決するための手段） 上記目的は以下の本発明によって達成される。(Means for solving problems) The above objects are achieved by the present invention as described below.
すなわち、本発明は、酸素を含有するダイヤモンド状炭
素１漠を発光層に用いたことを特徴とするＥＬ素子であ
る。That is, the present invention is an EL device characterized in that diamond-like carbon containing oxygen is used in the light-emitting layer.
（好ましい実施態様）
次に好ましい実施態様により本発明を更に詳しく説明す
る。(Preferred Embodiments) Next, the present invention will be explained in more detail with reference to preferred embodiments.
本発明に用いられるダイヤモンド状炭素（ＤＬＬ：）膜
とは１発光色に対して透明であることが必要であり、可
視光領域をカバーするためにはＥｇｏｐＬが１．５ｅｖ
以上、更に好ましくは２．ＯｅＶ以上が良い。又、絶縁
耐圧が充分あり、発光中心を励起する電子を十分加速す
ることが出来るためには抵抗率が１０９乃至１０′３Ω
Ｃ１が好ましい。又、化学的に安定で１１！２質の低下
が生じないものが良い。The diamond-like carbon (DLL) film used in the present invention must be transparent for one emission color, and EgopL is 1.5ev to cover the visible light region.
Above, more preferably 2. OeV or higher is better. In addition, in order to have sufficient dielectric strength and to be able to sufficiently accelerate the electrons that excite the luminescent center, the resistivity must be 109 to 10'3Ω.
C1 is preferred. In addition, it is preferable to use one that is chemically stable and does not cause deterioration in 11!2 quality.
この様なりＬＣＩＱは、カーボンブラックやグラツシー
カーボンとは異なり、ＳＰ２炭素の膜中混在比が少なく
、又、二重結合共役系が小さいことが必要となる。それ
故に長距離的にはアモルファス構造であっても、短距離
的にはダイヤモンド構造をとり、ＳＰ３炭素主体による
膜である。又、ＥＯ等で見た結晶成分の有無については
本発明においては問題ではない。In this way, unlike carbon black or glassy carbon, LCIQ requires that the mixture ratio of SP2 carbon in the film is small and that the double bond conjugated system is small. Therefore, even if it has an amorphous structure over a long distance, it has a diamond structure over a short distance, and is a film mainly composed of SP3 carbon. Furthermore, the presence or absence of crystal components as seen by EO etc. is not a problem in the present invention.
該Ｄ【、ＣＢ！２の生成方法は、スパッタ法、イオンビ
ーム蒸着法等のＰＶＤ法や、ＲＦプラズマＣｖＤ法、直
流グロー放電法等のＣＶＯ法が使用できる。The D [, CB! As the generation method 2, a PVD method such as a sputtering method or an ion beam evaporation method, or a CVO method such as an RF plasma CVD method or a DC glow discharge method can be used.
ＤＬＣ膜に酸素を含有させる方法は、原料ガスにＣ１１
３０１１、Ｃ，１１，０１１等のアルコール類、（Ｃ８
４）２ＧＯ１（Ｃａｌｌｓ） ＧＯ等のケトン類やＣＯ
やＣＯ，等の炭素と酸素元素を含有するガスを用いる方
法、０２や１１２０等の酸素を含有するガス雰囲気或い
はプラズマ中でＤＬＣＩＩ！２の生成を行なう方法、更
にはＤＬＣＩＩＱ生成後、０２や１１２０雰囲気或いは
プラズマ近傍で酸化する方法がある。酸素含有ｌｉｔは
５ａｖａ■％以下、好ましくは０．１ａｖａｍ％以十が
好ましく、５ａｖａｍ％を越えると構造が不安定となり
、繰り返し耐久性が低下し、又、含酸素ガスを混合して
用いる場合は特に成膜速度が低下し、一方、０．１ａｖ
ａｍ％以下では発光強度が低下する。The method of incorporating oxygen into the DLC film is to add C11 to the raw material gas.
Alcohols such as 3011, C, 11,011, (C8
4) 2GO1 (Calls) Ketones such as GO and CO
A method using a gas containing carbon and oxygen elements such as 02 or 1120, or a method using a gas containing oxygen such as 02 or 1120, or in a plasma or DLCII! There is a method of generating DLCIIQ, and a method of oxidizing in an atmosphere of 02 or 1120 or near plasma after the generation of DLCIIQ. The oxygen content is preferably 5 ava% or less, preferably 0.1 avam% or more. If it exceeds 5 avam%, the structure becomes unstable and the repeated durability decreases. In particular, the deposition rate decreased, while 0.1av
If it is less than am%, the emission intensity decreases.
（実施例）
次に実施例及び比較例により本発明を更に具体的に説明
する。(Example) Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples.
実施例１
第１図は、本発明のＥＬ素子の形成に用いた装置の概略
図を示すものである。磁場を印加した空胴共振３２に原
料ガスとマイクロ波を導入して放電させ、空胴共振器２
から吹き出したプラズマにより成膜室ｌに設置した基板
フ上に成膜を行なうものである。Example 1 FIG. 1 shows a schematic diagram of an apparatus used to form an EL element of the present invention. Raw material gas and microwaves are introduced into the cavity resonator 32 to which a magnetic field is applied to cause a discharge, and the cavity resonator 2
A film is formed on a substrate placed in a film forming chamber 1 using plasma blown out from the film forming chamber 1.
原料ガスとしてＧＩＬ／ＩＩ□１０□をＩ／Ｉ１０．１
の混合物として導入し、マイクロ波（２，４５Ｇｌｌｚ
）２００Ｗとし、磁場は最大強度１ 、５００Ｇａｕｓ
ｓ ％ＥＣＲ条件を満たす８７５ Ｇａｕｓｓが空胴共
振器出口端から１ｃｍ内側に設定して放電した。圧力は
０．０５Ｔｏｒｒとし、基板温度２００℃に保持した。GIL/II□10□ as raw material gas I/I10.1
was introduced as a mixture of
) 200W, and the magnetic field has a maximum strength of 1, 500 Gauss.
875 Gauss satisfying the s %ECR condition was set 1 cm inside from the outlet end of the cavity resonator and discharged. The pressure was 0.05 Torr, and the substrate temperature was maintained at 200°C.
第２図は本発明のＥＬ素子の構成図を示す。ガラス基板
１４上に透明電極ＩＴＯ１３を１，０００人の厚ミニ、
絶縁膜１１ｆ０２１２を２，０００人の厚みに成膜した
後、ＰＩ＆素含有ＤＬＣ膜の発光層１１を０．８μｍの
厚みに成膜し、背面電極１０としてＡＩｔを１，０００
人の厚みに蒸着した。FIG. 2 shows a block diagram of the EL element of the present invention. Transparent electrode ITO 13 on glass substrate 14, 1,000mm thick,
After forming an insulating film 11f0212 to a thickness of 2,000 μm, a light-emitting layer 11 of PI and element-containing DLC film was formed to a thickness of 0.8 μm, and an AIt film of 1,000 μm was formed as a back electrode 10.
It was deposited to the thickness of a person.
第３図は生成したＤＬＣ膜のＩｎスペクトルを示す。こ
のＩｎスペクトルでは１，７００ｃｍ−’付近に−Ｃ−
Ｏに由来する吸収が認められ、膜中に酸素が安定に存在
していることがわかる。燃焼法による化学分析法による
酸素含有ｆｉｔは１ａｖａ−％であった。又、該ＯＬＣ
ＩＩＱのＥｇｏｐＬは２．８ｅｖであ７た。FIG. 3 shows the In spectrum of the produced DLC film. In this In spectrum, -C-
Absorption originating from O is observed, indicating that oxygen stably exists in the film. The oxygen content fit determined by chemical analysis using the combustion method was 1 ava-%. Also, the OLC
EgopL of IIQ was 7 at 2.8ev.
次にこの素子の両電極間に周波数３にＩｌｚの交流電場
を印加したところ、１００Ｖより発光を開始し２００ｖ
で飽和した。このときの発光色は第４図の発光スペクト
ルが示す様に黄緑色であ７た。Next, when an alternating current electric field of Ilz was applied at frequency 3 between both electrodes of this element, it started emitting light at 100V and reached 200V.
It was saturated. The color of the emitted light at this time was yellow-green, as shown in the emission spectrum of FIG.
実施例２
実施例１と同様の装置を用い、実施例１と同構成の基板
（ガラス／ＩＴＯ／ＩＩｆＯ□）に、原料ガスとしてｅ
１１４ガスを導入し、マイクロ波出力１００Ｗ、磁場は
実施例１と同じにし、圧力５ｘｔｏ−’Ｔｏｒｒとして
放電を行ない発光層を形成した。基板温度は２００℃に
保持し、基板バイアス−４００Ｖを印加した。ＤＬＣｒ
ｆ；＆を１μｍの厚みに成膜した後放電を止め、基板温
度を８０℃に保持し、水をバブリングした後の酸素ガス
を導入し４０時間保持した。その後＾２電棒付けを行な
った。このとき（７）ＤＬ（：膜）ＥｇｏｐＬ ハ２
、３ ｅＶ”ｔ’あった。コノ発光素子の両電極間に実
施例１と同条件の交流電場を印加したところ実施例１と
同様の発光を確認した。尚、この素子において、その発
光層の酸素含有ｈ【は３ａｔｏａ＋％で、ＩＲスペクト
ルで−Ｃ−Ｏの吸収ピークの増加率が飽和した後は１ケ
月経過後でも発光強度は低下しなかった。Example 2 Using the same apparatus as in Example 1, e was applied as a raw material gas to a substrate (glass/ITO/IIfO□) having the same configuration as in Example 1.
114 gas was introduced, the microwave output was 100 W, the magnetic field was the same as in Example 1, and a discharge was performed at a pressure of 5 x to' Torr to form a light-emitting layer. The substrate temperature was maintained at 200°C, and a substrate bias of -400V was applied. DLCr
After forming f; After that, I attached ^2 electric rods. At this time, (7) DL (: membrane) EgopL Ha2
, 3 eV"t'. When an alternating current electric field under the same conditions as in Example 1 was applied between both electrodes of the light-emitting device, light emission similar to that in Example 1 was confirmed. In this device, the light-emitting layer The oxygen content h was 3atoa+%, and the emission intensity did not decrease even after one month had passed after the increase rate of the -C-O absorption peak in the IR spectrum was saturated.
比較例！
実施例２と同様にして１＆膜したＤＬＣ膜を、放電を止
めた後酸化せずに比較例のＥＬ素子を作成した。このと
きのＤＬＣｎＱは１１（スペクトルで−Ｃ・０吸収ピー
クは検出されなか７た。このＥＬ素子を実施例１と同条
件で発光させたところ、僅かに発光するものの、実施例
１及び２のＥＬ素子と比較すると、その輝度は１／１０
０以下であった。Comparative example! An EL element of a comparative example was prepared by using a DLC film formed as a 1& film in the same manner as in Example 2 without oxidizing it after stopping the discharge. DLCnQ at this time was 11 (-C.0 absorption peak was not detected in the spectrum). When this EL element was made to emit light under the same conditions as in Example 1, it emitted light slightly, but compared to Examples 1 and 2. Compared to EL elements, its brightness is 1/10
It was less than 0.
実施例３
実施例１と同じ装置を用い原料ガスを［：２１１．７（
：０〜１７Ｉ混合比で導入し、圧力９ Ｘ １０−３Ｔ
ｏｒｒに保持し、基板バイアス−１００Ｖとし、他は実
施例１と同条件にしてＤＬＣ膜の成膜を行なった。Ｅｇ
ｏｐｔは２．２ｅＶであった。＾１電極付けした後実施
例１と同条件で測定した発光スペクトルは第４図と類似
し、酸素含打晴は５ａｔｏｍ％であワた。発光強度が半
減する時間は５，０００時間であった。Example 3 Using the same equipment as Example 1, the raw material gas was heated to [:211.7(
: Introduced at a mixing ratio of 0 to 17I, pressure 9 x 10-3T
The DLC film was formed under the same conditions as in Example 1 except that the substrate bias was kept at -100V. Eg
opt was 2.2 eV. The emission spectrum measured under the same conditions as in Example 1 after attaching the ^1 electrode was similar to that shown in FIG. 4, and the oxygen content was 5 atom %. The time required for the luminescence intensity to decrease by half was 5,000 hours.
（発明の効果）
以上説明した様にＥＬ素子の発光層に酸素を含有するＤ
ＬＣＩＩ＜１を用いることにより、耐環境性、特に湿度
に対し、発光強度の劣化がない長寿命の信頼性の高いＥ
Ｌ素子を実現出来る様になった。(Effect of the invention) As explained above, D containing oxygen in the light emitting layer of the EL element
By using LCII < 1, it is possible to achieve long-life and highly reliable E with no deterioration in luminous intensity, especially against humidity.
It became possible to realize an L element.
第１図 本発明を実施した装置概略図
第２図 本発明を実施したＥＬ素ｆ・構成図第３図 Ｄ
ｌ、Ｃ発光層のＩＲスペクトル図第４図 発光スペクト
ル図
１−−−−−成１１Ｑ室 ２−−−−−空洞共振
器３−−−−−−電磁石 ４−−−−−−ガス導
入［１５−−−−−マイクロ波導波管 ６・・・・・
・排気ロア・−・−基 板 ８−−−−−−直流
電源１０−・・−背面電極 １１−−−−−発光［Ｉ
ＬＣ層！２−・−絶縁層 １３−・・−透明電極１
４・−・・・ガラス基板
第１図
第３図
第２し１
波数（（Ｊ−’）
第４図
波長（ｒｕｍ）Fig. 1 Schematic diagram of the device implementing the present invention Fig. 2 Configuration diagram of the EL element f implementing the present invention Fig. 3 D
IR spectrum diagram of l, C luminescent layer Figure 4 Emission spectrum diagram 1 ------- Formation 11Q chamber 2 ------- Cavity resonator 3 ------- Electromagnet 4 ------- Gas introduction [15---Microwave waveguide 6...
・Exhaust lower --- Board 8 ------ DC power supply 10 --- Back electrode 11 --- Light emission [I
LC layer! 2--Insulating layer 13--Transparent electrode 1
4... Glass substrate Figure 1 Figure 3 Figure 2 1 Wave number ((J-') Figure 4 Wavelength (rum)
Claims (2)
用いたことを特徴とする電界発光素子。(1) An electroluminescent device characterized in that a diamond-like carbon film containing oxygen is used as a light emitting layer.
載の電界発光素子。(2) The electroluminescent device according to claim 1, wherein the oxygen concentration is 5 atom% or less.
Priority Applications (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63327885A JP2614097B2 (en) | 1988-12-27 | 1988-12-27 | EL device |
| DE68928245T DE68928245T2 (en) | 1988-12-27 | 1989-12-27 | Device emitting light by electric field |
| EP93203387A EP0588449B1 (en) | 1988-12-27 | 1989-12-27 | Electric field light-emitting device |
| EP89313589A EP0377320B1 (en) | 1988-12-27 | 1989-12-27 | Electric field light-emitting device |
| DE68928319T DE68928319T2 (en) | 1988-12-27 | 1989-12-27 | Device emitting light by electric field. |
| US07/457,864 US5210430A (en) | 1988-12-27 | 1989-12-27 | Electric field light-emitting device |
| AT93203387T ATE156648T1 (en) | 1988-12-27 | 1989-12-27 | LIGHT EMITTING DEVICE BY ELECTRICAL FIELD |
| AT89313589T ATE156324T1 (en) | 1988-12-27 | 1989-12-27 | LIGHT EMITTING DEVICE BY ELECTRICAL FIELD |
| US07/929,916 US5275967A (en) | 1988-12-27 | 1992-08-17 | Electric field light-emitting device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63327885A JP2614097B2 (en) | 1988-12-27 | 1988-12-27 | EL device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02173617A true JPH02173617A (en) | 1990-07-05 |
| JP2614097B2 JP2614097B2 (en) | 1997-05-28 |
Family
ID=18204068
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63327885A Expired - Fee Related JP2614097B2 (en) | 1988-12-27 | 1988-12-27 | EL device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2614097B2 (en) |
-
1988
- 1988-12-27 JP JP63327885A patent/JP2614097B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2614097B2 (en) | 1997-05-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |