JPH0615710B2 - Method for forming synthetic resin film - Google Patents
Method for forming synthetic resin filmInfo
- Publication number
- JPH0615710B2 JPH0615710B2 JP61206764A JP20676486A JPH0615710B2 JP H0615710 B2 JPH0615710 B2 JP H0615710B2 JP 61206764 A JP61206764 A JP 61206764A JP 20676486 A JP20676486 A JP 20676486A JP H0615710 B2 JPH0615710 B2 JP H0615710B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- temperature
- substrate
- processing chamber
- synthetic resin
- 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 - Fee Related
Links
- 229920003002 synthetic resin Polymers 0.000 title claims description 20
- 239000000057 synthetic resin Substances 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 19
- 239000000178 monomer Substances 0.000 claims description 43
- 239000002994 raw material Substances 0.000 claims description 40
- 239000000758 substrate Substances 0.000 claims description 33
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 10
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 239000010408 film Substances 0.000 description 25
- 229920000642 polymer Polymers 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 1
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Physical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、例えば半導体素子の絶縁膜、パツシベーシヨ
ン膜、ソフトエアー防止膜や液晶表示素子の液晶配向
膜、液体や気体の分離膜等の各種合成樹脂被膜の形成方
法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention relates to various kinds of insulating films for semiconductor devices, passivation films, soft air prevention films, liquid crystal alignment films for liquid crystal display devices, liquid or gas separation films, and the like. The present invention relates to a method for forming a synthetic resin film.
（従来の技術） 従来、この種の合成樹脂被膜の形成方法としては、合成
樹脂の原料モノマーを適当な溶媒に溶かしてこれを基体
上で重合させるいわゆる湿式法、合成樹脂ポリマー自体
を基体上に蒸着させるいわゆるポリマー蒸着法或いは合
成樹脂の原料モノマーをプラズマ状態にしてプラズマ中
の基体で重合させるプラズマ重合法等が知られている。(Prior Art) Conventionally, as a method of forming a synthetic resin film of this type, a so-called wet method of dissolving a raw material monomer of a synthetic resin in an appropriate solvent and polymerizing the same on a substrate, a synthetic resin polymer itself on a substrate A so-called polymer vapor deposition method in which vapor deposition is performed, a plasma polymerization method in which a raw material monomer of a synthetic resin is put into a plasma state and polymerized on a substrate in plasma, and the like are known.
（発明が解決しようとする問題点） しかしながら、前記従来法は湿式法の場合は極めて薄い
膜が得られ難く、また基体に対する合成樹脂被膜の密着
性が不十分で、しかも溶媒の添加、除去、回収等の工程
が入るために不純物の混入が起りやすいという不都合を
有し、またポリマー蒸着法の場合は解重合と共に分解が
起つたりして重合度が十分でないという不都合を有し、
またプラズマ重合法の場合は原料モノマー自体が分解し
たりして合成樹脂の分子設計が困難で、しかも合成樹脂
が架橋構造を含むために比較的剛直な被膜しか得られな
いという不都合を有する。(Problems to be Solved by the Invention) However, in the conventional method, it is difficult to obtain an extremely thin film in the case of the wet method, and the adhesion of the synthetic resin film to the substrate is insufficient, and further, addition and removal of the solvent, There is a disadvantage that impurities are likely to be mixed due to the steps such as recovery, and in the case of the polymer vapor deposition method, there is a disadvantage that the degree of polymerization is not sufficient due to decomposition with depolymerization,
Further, in the case of the plasma polymerization method, it is difficult to design the molecular weight of the synthetic resin because the raw material monomer itself is decomposed, and furthermore, since the synthetic resin contains a crosslinked structure, there is a disadvantage that only a relatively rigid coating film can be obtained.
かかる不都合を解消するものとして、真空処理室中で原
料モノマーを蒸発させて、これを基体上で重合するよう
にした合成樹脂被膜の形成方法が本出願人による特開昭
６１−７８４６３号において開示されており、かかる方
法によれば緻密で高純度且つ均一な膜厚の合成樹脂被膜
を基板に対する良好な密着性をもつて、しかも極めて薄
い膜を始め所望膜厚に容易に形成でき、更に原料モノマ
ーの選択によつて種々に分子設計された被膜の形成を行
なえるが、かかる方法において複雑な形状の基体に対し
てもその全面に均一に被膜を形成できるようにすること
が望まれる。As a solution to such a problem, a method for forming a synthetic resin film in which a raw material monomer is evaporated in a vacuum processing chamber and polymerized on a substrate is disclosed in Japanese Patent Laid-Open No. 61-78463 by the present applicant. According to such a method, a synthetic resin film having a high density and a high purity and a uniform film thickness can be easily formed to a desired film thickness including an extremely thin film with good adhesion to a substrate. A film having various molecular designs can be formed by selecting a monomer, but it is desired by such a method that a film having a complicated shape can be uniformly formed on the entire surface of the substrate.
（問題を解決するための手段） 本発明は前記要望を満たす合成樹脂被膜の形成方法を提
供することを目的とするもので、その発明は、真空処理
室中で原料モノマーを蒸発させて、これを基体上で重合
させることから成る合成樹脂被膜の形成方法において、
該真空処理室の真空度を１×１０-2Torr以下に設定する
と共に、該基体の温度を原料モノマーの蒸発温度を超え
る温度に設定し且つ該真空処理室の室壁内温度を該基体
の温度を超える温度に設定した状態で該原料モノマーを
蒸発させることを特徴とする。(Means for Solving the Problem) The present invention is intended to provide a method for forming a synthetic resin coating film that satisfies the above-mentioned needs, and the invention is to evaporate a raw material monomer in a vacuum processing chamber and In a method for forming a synthetic resin film, which comprises polymerizing
The degree of vacuum of the vacuum processing chamber is set to 1 × 10 −2 Torr or less, the temperature of the substrate is set to a temperature higher than the evaporation temperature of the raw material monomer, and the temperature inside the chamber wall of the vacuum processing chamber is set to the temperature of the substrate. It is characterized in that the raw material monomer is evaporated in a state of being set to a temperature exceeding the temperature.
ここで、真空処理室の真空度を１×１０-2Torr以下に設
定するのは、真空度が１×１０-2Torrを超えると、原料
モノマー同士が接触しやすくなり、原料モノマーを真空
処理室内に設けられた蒸発用容器から蒸発させる場合
は、該蒸発用容器の近傍の、また原料モノマーを真空処
理室の外部で蒸発させて、これを導入管を介して該直空
処理室内に導入する場合は、該導入管の流出口近傍の真
空処理室の室壁等に原料モノマーの一部が重合して付着
してしまい、原料モノマーが真空処理室の全空間に亘つ
て均一に分散せず、均一厚さの被膜が得られないからで
あるが、製造速度の観点から１×１０-6Torr程度までと
するのが好ましい。Here, the vacuum degree of the vacuum processing chamber is set to 1 × 10 −2 Torr or less, because when the vacuum degree exceeds 1 × 10 −2 Torr, the raw material monomers are likely to come into contact with each other, and the raw material monomer is vacuum treated. When evaporating from the evaporation container provided inside the chamber, the raw material monomer near the evaporation container and outside the vacuum processing chamber are evaporated, and this is introduced into the direct air processing chamber through the introduction pipe. In that case, a part of the raw material monomer is polymerized and adhered to the chamber wall of the vacuum processing chamber in the vicinity of the outlet of the introduction pipe, and the raw material monomer is uniformly dispersed over the entire space of the vacuum processing chamber. However, it is not possible to obtain a film having a uniform thickness, but from the viewpoint of the production speed, it is preferable to set it to about 1 × 10 −6 Torr.
基体の温度を原料モノマーの蒸発温度を超える温度にす
るのは、原料モノマー単独では基体上に付着しないよう
にして、主として基体に衝突すると同時に該基体上で重
合する原料モノマーで順次均一な組成の合成樹脂被膜が
形成されるようにするためである。尚、原料モノマーが
２種以上の場合には、該基体の温度はこれら原料モノマ
ーの蒸発温度のうち最高温度を越える温度に設定するこ
とになる。The temperature of the substrate is set to a temperature higher than the evaporation temperature of the raw material monomer so that the raw material monomer alone does not adhere to the substrate so that the raw material monomer mainly collides with the base material and is simultaneously polymerized on the base material so as to have a uniform composition. This is because the synthetic resin film is formed. When two or more raw material monomers are used, the temperature of the substrate is set to a temperature exceeding the maximum temperature among the evaporation temperatures of these raw material monomers.
また、真空処理室の室壁内面温度を基体の温度を超える
温度に設定するのは、原料モノマー或いはその重合物が
該室壁内面よりも基体に付着しやすいようにするためで
ある。Further, the temperature of the inner surface of the chamber wall of the vacuum processing chamber is set to a temperature higher than the temperature of the substrate so that the raw material monomer or its polymer is more likely to adhere to the substrate than the inner surface of the chamber wall.
（作用） 前記のような真空処理室の真空度と、基体並びに室壁内
面の温度設定によれば、蒸発した原料モノマーが、真空
処理室の全空間に亘つて均一に分散することとなり、主
として基体に衝突した原料モノマーのうち衝突と同時に
重合する原料モノマーで基体の全面に順次均一な組成の
重合樹脂被膜が形成される。(Function) According to the vacuum degree of the vacuum processing chamber and the temperature settings of the substrate and the inner surface of the chamber wall as described above, the evaporated raw material monomer is uniformly dispersed over the entire space of the vacuum processing chamber, and mainly Of the raw material monomers that have collided with the substrate, the raw material monomers that are polymerized at the same time as the collision form a polymerized resin film having a uniform composition over the entire surface of the substrate.
（実施例） 次に、添付図面に従つて本発明の実施例に付き説明す
る。(Example) Next, an example of the present invention will be described with reference to the accompanying drawings.
第１図は本発明方法を実施する装置の１例を示すもの
で、１はステンレス製容器から成る真空処理室を示し、
該処理室１内を外部の真空ポンプその他の真空排気系２
に接続すると共に、該処理室１の中央にステンレス製の
棒状体の保持部材３で、たて、よこ、厚さが１０cm×１
０cm×０．５cmのアルミ製の基体４を保持すると共に該
基体４の上方に、原料モノマーａ、ｂを蒸発させるため
の蒸発用容器５、５をその各蒸発口６を上向きにして設
けてある。また、該真空処理室１の外周に加熱用ヒータ
７を巻回し、該真空処理室１の室壁８の加熱によつて該
真空処理室１内を所望温度に加熱できるようにした。FIG. 1 shows an example of an apparatus for carrying out the method of the present invention, in which 1 shows a vacuum processing chamber composed of a stainless steel container,
An external vacuum pump or other vacuum exhaust system 2 is provided inside the processing chamber 1.
And a stainless steel rod-shaped holding member 3 at the center of the processing chamber 1 so that the vertical length, width and thickness are 10 cm × 1.
A 0 cm × 0.5 cm aluminum base 4 is held, and evaporation containers 5 and 5 for evaporating the raw material monomers a and b are provided above the base 4 with their evaporation ports 6 facing upward. is there. Further, a heater 7 for heating is wound around the outer periphery of the vacuum processing chamber 1 so that the inside of the vacuum processing chamber 1 can be heated to a desired temperature by heating the chamber wall 8 of the vacuum processing chamber 1.
ここで、当該装置による合成樹脂被覆の形成につき説明
する。Here, the formation of the synthetic resin coating by the apparatus will be described.
まず、真空処理室１を大気圧状態にして、蒸発用容器
５、５の一方に原料モノマーａとしてピロメリト酸二無
水物と、他方に原料モノマーｂとして４、４′−ジアミ
ノジフエニルエーテルとを各１ｇづつ充填する。First, the vacuum processing chamber 1 is brought to atmospheric pressure, and pyromellitic dianhydride is used as a raw material monomer a in one of the evaporation vessels 5 and 5, and 4,4′-diaminodiphenyl ether is used as a raw material monomer b in the other. Fill 1 g each.
次で、ヒータ７を１５０℃に加熱して、真空処理室１内
を１５０℃近くに昇温し、原料モノマーａ、ｂと基体４
とを夫々１５０℃近くに加熱する。かかる温度設定によ
れば、真空処理室１内を１×１０-4Torrに排気すると、
原料モノマーａ、ｂの消化は開始するが、該原料モノマ
ーａ、ｂ各単独では、基体４上にはもとより、室壁８の
内面８ａに付着しない。Next, the heater 7 is heated to 150 ° C. to raise the temperature in the vacuum processing chamber 1 to near 150 ° C., and the raw material monomers a and b and the substrate 4 are heated.
And are heated to near 150 ° C., respectively. According to such temperature setting, when the vacuum processing chamber 1 is evacuated to 1 × 10 −4 Torr,
Although the starting monomers a and b start to be digested, the starting monomers a and b alone do not adhere to the inner surface 8a of the chamber wall 8 as well as to the substrate 4.
次で、真空処理室１内を真空排気系２を介して１×１０
-4Torrに設定すると共にヒータ７を２００℃に加熱し
て、該処理室１内を徐々に２００℃近くに昇温し、原料
モノマーａ、ｂと基体４とを夫々徐々に２００℃近く加
熱する。かくして、原料モノマーａ、ｂは昇華するが、
原料モノマーａ、ｂ各単独では原料モノマーａ、ｂの昇
華温度以上となつている基体４や室壁８の内面８ａには
付着しないので、該処理室１内に原料モノマーａ、ｂが
均一に分散することとなり、しかも、室壁８の内面８ａ
はヒータ７によつて直接加熱されて即時に２００℃に昇
温し、基体４よりも常に高温状態となつており、原料モ
ノマーａ、ｂ或いは、その重合物は、室壁８の内面８ａ
よりは基体４の方に付着しやすい状態となつており、該
原料モノマーａ、ｂによつて基体４の全面に均一な膜厚
でもつて、しかも化学量論的な組成比で、ポリイミドの
重合樹脂被膜が形成された。Next, the inside of the vacuum processing chamber 1 is passed through the vacuum exhaust system 2 to 1 × 10
-4 Torr and heating the heater 7 to 200 ° C. to gradually raise the temperature of the inside of the processing chamber 1 to near 200 ° C. and gradually heat the raw material monomers a and b and the substrate 4 to near 200 ° C. To do. Thus, the raw material monomers a and b sublime,
Since each of the raw material monomers a and b alone does not adhere to the substrate 4 or the inner surface 8a of the chamber wall 8 which has a temperature not lower than the sublimation temperature of the raw material monomers a and b, the raw material monomers a and b are uniformly distributed in the processing chamber 1. Will be dispersed, and moreover, the inner surface 8a of the chamber wall 8
Are heated directly by the heater 7 and instantly heated to 200 ° C. so that the temperature is always higher than that of the substrate 4. The raw material monomers a and b or the polymer thereof are the inner surface 8 a of the chamber wall 8.
It is more likely to adhere to the substrate 4 than to the substrate 4, and the raw material monomers a and b allow the polyimide 4 to be polymerized with a uniform film thickness over the entire surface of the substrate 4 and with a stoichiometric composition ratio. A resin film was formed.
（発明の効果） このように、本発明の合成樹脂被膜の形成方法によれ
ば、真空処理室の真空度を１×１０-2Torr以下に設定す
ると共に、基体の温度を原料モノマーの蒸発温度を超え
る温度に設定し且つ該真空処理室の室壁内面温度を該基
体の温度を超える温度に設定した状態で該原料モノマー
を蒸発させるようにしたので、原料モノマーが基体の全
周囲に亘つて均一に分散することとなり、基体の形状、
大きさにかかわりなく、その全面に均一な合成樹脂被膜
を形成できる効果を有する。(Effect of the Invention) As described above, according to the method for forming a synthetic resin film of the present invention, the degree of vacuum in the vacuum processing chamber is set to 1 × 10 −2 Torr or less, and the temperature of the substrate is set to the evaporation temperature of the raw material monomer. Since the raw material monomer is vaporized in a state in which the temperature of the raw material is set to a temperature higher than that and the temperature of the inner wall surface of the vacuum processing chamber is set to a temperature higher than the temperature of the substrate, the raw material monomer is spread over the entire circumference of the substrate. It will be dispersed evenly, the shape of the substrate,
It has the effect that a uniform synthetic resin film can be formed on the entire surface regardless of the size.
図面は本発明合成樹脂被膜の形成方法を実施するための
装置の一例の截断面図である。 １……真空処理室、２……真空排気系 ４……基体、７……ヒータ ８ａ……室壁内面、ａ、ｂ……原料モノマーThe drawing is a cross-sectional view of an example of an apparatus for carrying out the method for forming a synthetic resin film of the present invention. 1 ... Vacuum processing chamber, 2 ... Vacuum exhaust system 4 ... Substrate, 7 ... Heater 8a ... Chamber wall inner surface, a, b ... Raw material monomer
Claims (1)
て、これを基体上で重合させることから成る合成樹脂被
膜の形成方法において、該真空処理室の真空度を１×１
０-2Torr以下に設定すると共に、該基体の温度を原料モ
ノマーの蒸発温度を超える温度に設定し且つ該真空処理
室の室壁内面温度を該基体の温度を超える温度に設定し
た状態で該原料モノマーを蒸発させることを特徴とする
合成樹脂被膜の形成方法。1. A method for forming a synthetic resin film comprising evaporating a raw material monomer in a vacuum processing chamber and polymerizing the monomer on a substrate, wherein the vacuum degree in the vacuum processing chamber is 1 × 1.
The temperature is set to 0 −2 Torr or less, the temperature of the substrate is set to a temperature higher than the evaporation temperature of the raw material monomer, and the inner wall temperature of the vacuum processing chamber is set to a temperature higher than the temperature of the substrate. A method for forming a synthetic resin film, which comprises evaporating a raw material monomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61206764A JPH0615710B2 (en) | 1986-09-04 | 1986-09-04 | Method for forming synthetic resin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61206764A JPH0615710B2 (en) | 1986-09-04 | 1986-09-04 | Method for forming synthetic resin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6362869A JPS6362869A (en) | 1988-03-19 |
| JPH0615710B2 true JPH0615710B2 (en) | 1994-03-02 |
Family
ID=16528699
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61206764A Expired - Fee Related JPH0615710B2 (en) | 1986-09-04 | 1986-09-04 | Method for forming synthetic resin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0615710B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560402A (en) * | 2012-02-10 | 2012-07-11 | 肇庆市振华金冠真空设备有限公司 | Method for coating reflection cup of car lamp |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5343904B2 (en) * | 1973-05-11 | 1978-11-24 | ||
| JPS6178463A (en) * | 1984-09-25 | 1986-04-22 | Ulvac Corp | Formation of synthetic resin film |
-
1986
- 1986-09-04 JP JP61206764A patent/JPH0615710B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6362869A (en) | 1988-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4624867A (en) | Process for forming a synthetic resin film on a substrate and apparatus therefor | |
| Wu et al. | Surface-modified hydrophilic membranes in membrane distillation | |
| JPH08509421A (en) | Selective permeable membrane formed by plasma polymerization of gas | |
| JPH1092800A (en) | Evaporation source and vacuum treatment chamber provided with evaporation source, and forming method of organic compound film | |
| JP3863934B2 (en) | Method for forming polymer thin film | |
| JP2619399B2 (en) | Method for producing polyimide film | |
| JPS6178463A (en) | Formation of synthetic resin film | |
| JPH0718000B2 (en) | Method for forming synthetic resin film | |
| JPH0615710B2 (en) | Method for forming synthetic resin film | |
| US4360393A (en) | Vapor deposition of H3 PO4 and formation of thin phosphorus layer on silicon substrates | |
| JPS60197730A (en) | Formation of polyimide film | |
| JPH0726023A (en) | Method for producing organic polymer thin film | |
| JPH04236769A (en) | Film forming device | |
| JP3773587B2 (en) | Purification method for organic compound monomers | |
| JPH0776416B2 (en) | Method for forming polyimide resin coating | |
| JPH0445259A (en) | Film forming device | |
| JPH0668151B2 (en) | Vacuum contact surface treatment method inside vacuum member | |
| JP3745051B2 (en) | Film thickness measurement method | |
| Linkov et al. | Composite carbon-polyimide membranes | |
| JPH04341559A (en) | Production of synthetic resin coating film | |
| JPH0615711B2 (en) | Method for forming polyimide resin coating | |
| JPS61219028A (en) | Formation of liquid crystal orienting film | |
| JPH05132763A (en) | Omnidirectional and simultaneous vapor-deposition polymerization device | |
| JPH0521214B2 (en) | ||
| JPS5824374B2 (en) | Silicon oxide film production method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees |