JPH0729086B2 - Coating film manufacturing method - Google Patents
Coating film manufacturing methodInfo
- Publication number
- JPH0729086B2 JPH0729086B2 JP61245723A JP24572386A JPH0729086B2 JP H0729086 B2 JPH0729086 B2 JP H0729086B2 JP 61245723 A JP61245723 A JP 61245723A JP 24572386 A JP24572386 A JP 24572386A JP H0729086 B2 JPH0729086 B2 JP H0729086B2
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- coating film
- resistance
- solvent
- composition
- polyborosiloxane resin
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Description
【発明の詳細な説明】 産業上の利用分野 本発明は、輻射型の暖房器や調理器、その他産業用設備
に使用する薄膜輻射体の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a thin film radiator used in a radiation type heater, a cooking device, and other industrial facilities.
従来の技術 従来、ポリボロシロキサン樹脂の塗膜は、高温下で使用
する電線の被覆用に用いられてきた。ポリボロシロキサ
ン樹脂の加熱硬化体は、耐熱性が高く、耐熱電線の被覆
材としては適している。しかしながら、現在のところ、
電線以外の用途はない。2. Description of the Related Art Conventionally, coating films of polyborosiloxane resin have been used for coating electric wires used at high temperatures. The heat-cured product of polyborosiloxane resin has high heat resistance and is suitable as a coating material for heat-resistant electric wires. However, at the moment,
There are no other uses than electric wires.
発明が解決しようとする問題点 上記ポリボロシロキサン樹脂の加熱硬化体はそれ自身の
耐熱性は優れてはいるが、400℃以上では造膜が困難
で、加えて多孔質であるために、高湿度や腐食性環境下
では基材によっては容易に腐食され、実用性が低い。Problems to be Solved by the Invention Although the heat-cured product of the polyborosiloxane resin described above has excellent heat resistance itself, it is difficult to form a film at 400 ° C. or higher, and in addition, it is highly porous. In a humidity or corrosive environment, it is easily corroded depending on the base material and is not practical.
さらに、任意機能を付与する目的で、適当な充填材をポ
リボロシロキサン樹脂に配合した時の、最適な調合条件
は全く不明である。Furthermore, the optimum blending conditions when a suitable filler is blended with the polyborosiloxane resin for the purpose of imparting an arbitrary function are completely unknown.
また、焼成温度に関しては、ポリボロシロキサン樹脂の
塗膜化に関する方法が、特開昭59−218844号公報に示さ
れている。この中で焼成条件に関しては600℃以上（例
えば、600℃にて５分）とあるが、使用環境に応じた条
件設定をすることが重要であり、焼成条件の選択を誤る
と、塗膜劣化が速まり、機器の寿命を短くする。使用環
境をあまり考慮することなく、広範囲の使用環境にわた
って良好な特性を有する焼成条件は全く不明である。Regarding the firing temperature, Japanese Patent Laid-Open No. 59-218844 discloses a method for forming a coating film of a polyborosiloxane resin. Of these, the firing conditions are 600 ° C or higher (for example, 5 minutes at 600 ° C), but it is important to set the conditions according to the operating environment. Will shorten the life of the equipment. The firing conditions that have good characteristics over a wide range of use environments are completely unknown, without giving much consideration to the use environment.
本発明は、かかる従来の問題を解消するもので、ポリボ
ロシロキサン樹脂の耐熱性を生かした耐熱性塗膜を得る
為に、充填材の配合量、溶剤配合量、焼成条件等を明確
にすることを目的としている。The present invention solves such a conventional problem, and clarifies the blending amount of the filler, the blending amount of the solvent, the firing conditions, etc. in order to obtain a heat-resistant coating film that takes advantage of the heat resistance of the polyborosiloxane resin. Is intended.
問題点を解決するための手段 上記問題点を解決するために、本発明の塗膜の製造方法
は、ポリボロシロキサン樹脂有機溶媒溶液100重量％
と、無機質40〜80重量部と、有機溶剤とから成る組成物
を、混合撹拌した後、前記組成物を任意基材上に塗布
し、酸化性雰囲気もしくは不活性雰囲気で450℃の温度
で焼成するものである。Means for Solving the Problems In order to solve the above problems, the method for producing a coating film of the present invention comprises a polyborosiloxane resin organic solvent solution 100% by weight.
And a composition consisting of 40 to 80 parts by weight of an inorganic substance and an organic solvent are mixed and stirred, and then the composition is applied onto an arbitrary substrate and baked at a temperature of 450 ° C. in an oxidizing atmosphere or an inert atmosphere. To do.
作用 本発明は上記の方法は以下の作用を有する。Actions The present invention has the following actions.
（１）無機質粉末でポリボロシロキサン樹脂の高温時の
造膜性が向上し、約1000℃でもクラックの発生なしに造
膜することができる。(1) The inorganic powder improves the film-forming property of the polyborosiloxane resin at high temperature, and the film can be formed without cracks even at about 1000 ° C.
（２）有機溶媒は、ポリボロシロキサン樹脂を溶解膨潤
させ、無機質粉末が分散しやすい状態とする。又、有機
溶媒により組成物粘度を、撹拌に適当な負荷となる様な
調整も可能。(2) The organic solvent dissolves and swells the polyborosiloxane resin so that the inorganic powder is easily dispersed. It is also possible to adjust the viscosity of the composition by using an organic solvent so that the composition is appropriately loaded for stirring.
（３）焼成温度は、塗膜の構造を大きく変える。室温か
ら200℃位までは溶剤が蒸発する程度で塗膜は有機質で
連続性がある。200℃を超えて450℃位になると殆ど無機
質の膜となる。これは、ポリボロシロキサン樹脂の構造
に起因するもので、600℃を超すと完全に無機質とな
る。このように膜の構造が変わると、硬度、耐温性、耐
食性も変わる。よって、450℃で加熱すると広範囲の環
境に適した塗膜を得ることができる。(3) The firing temperature greatly changes the structure of the coating film. From room temperature to around 200 ° C, the solvent is evaporated and the coating film is organic and continuous. When the temperature exceeds 200 ° C and reaches 450 ° C, it becomes an almost inorganic film. This is due to the structure of the polyborosiloxane resin and becomes completely inorganic above 600 ° C. When the structure of the film changes in this way, hardness, temperature resistance, and corrosion resistance also change. Therefore, when heated at 450 ° C, a coating film suitable for a wide range of environments can be obtained.
（４）組成物粘度は、塗装作業性に影響する。よって粘
度調整により作業性の向上が計られる。(4) The composition viscosity affects the coating workability. Therefore, the workability can be improved by adjusting the viscosity.
実施例 以下本発明の実施例について説明する。Examples Examples of the present invention will be described below.
ポリボロシロキサン樹脂として昭和電線電纜（株）のSM
P−32、溶剤としてトルエン、無機質粉末としてAl2O3と
ZrO2とFe2O3・CuO・Mn2O3とを選定し、第１表の条件
で、組成物を撹拌調合した。SM of Showa Electric Wire & Cable Co., Ltd. as polyborosiloxane resin
P-32, toluene as solvent, Al 2 O 3 as inorganic powder
ZrO 2 and Fe 2 O 3 .CuO.Mn 2 O 3 were selected, and the composition was stirred and blended under the conditions shown in Table 1.
上記組成物を、SUS430基材上に塗布後200℃10分、450℃
10分の乾燥・焼成を行い、諸物性を確認した。その結果
を第２表にまとめた。第２表中各種テスト内容について
は注釈した。 After coating the above composition on a SUS430 substrate, 200 ° C for 10 minutes, 450 ° C
After 10 minutes of drying and baking, various physical properties were confirmed. The results are summarized in Table 2. The contents of various tests in Table 2 are noted.
注１）硬度は鉛筆ひっかき硬度。 Note 1) Hardness is pencil scratch hardness.
注２）密着性はゴバン目テープ剥離テスト。Note 2) Adhesiveness is a peeling tape peeling test.
注３）耐湿性は高温、高湿で24Hr放置による。Note 3) Moisture resistance is based on leaving for 24 hours at high temperature and high humidity.
注４）耐汚染性は、高温、高湿で各種調味料を滴下し24
Hr放置による。Note 4) Contamination resistance is 24 hours after dropping various seasonings at high temperature and high humidity.
Hr left.
注５）耐溶剤性は、布に各種溶剤を含浸させ塗膜の摩耗
を荷重をかけて行う。Note 5) For solvent resistance, cloth is impregnated with various solvents and the coating film is abraded by applying a load.
第２表中、耐湿性、耐汚染性の△、×はそれぞれ少し異
常ありと、基材腐食による塗膜の剥離を示し、耐溶剤性
の△、×は摩耗による塗膜成分の布への付着の程度であ
る。当然、各項目につき（○）＞（△）＞（×）の順で
良好であることを示す。第１表、及び第２表から、焼成
条件一定の下での無機粉末の配合量、溶剤配合量の塗膜
物性に及ぼす影響がわかる。組成物２、３、４より無機
粉末配合量が多いと耐溶剤性が劣る（組成物４）のがわ
かる。これは、粉末の量が多すぎて、ポリボロシロキサ
ン樹脂が相対的に少なくなることにより、粉末が表面に
浮きでることによる。粉末量が極めて少ないと（例ば５
重量部以下）、造膜しないこともある。又、組成物１、
２から、溶剤が多すぎると耐湿性、耐汚染性に劣ること
がわかる。これは、焼成硬化の途中過程で溶剤の蒸発ス
ピードが、溶剤量に影響を受け、溶剤の多い方が、塗膜
がより多孔質化しやすいからと考えられる。In Table 2, Δ and × of moisture resistance and stain resistance are slightly abnormal, respectively, indicating peeling of the coating film due to corrosion of the base material, and Δ and × of solvent resistance are Δ and × of the coating component on the cloth due to abrasion. The degree of adhesion. As a matter of course, each item is shown to be good in the order of (◯)>(Δ)> (x). From Tables 1 and 2, the effects of the blending amount of the inorganic powder and the blending amount of the solvent under constant baking conditions on the physical properties of the coating film can be seen. It can be seen that the solvent resistance is inferior (composition 4) when the content of the inorganic powder is larger than those of the compositions 2, 3, and 4. This is because the amount of the powder is too large and the polyborosiloxane resin is relatively small, so that the powder floats on the surface. If the amount of powder is extremely small (eg 5
In some cases, the film is not formed. Also, composition 1,
From 2, it can be seen that when the amount of the solvent is too much, the moisture resistance and the stain resistance are poor. This is presumably because the evaporation rate of the solvent is affected by the amount of the solvent during the course of baking and curing, and the more the solvent is, the more easily the coating film becomes porous.
以上、第１表、第２表から、耐湿性、耐汚染性、硬度、
耐溶剤性に良好な塗膜を得るには、ポリボロシロキサン
樹脂（以下バインダ）100重量部に対し、無機粉末を５
〜100重量部、好ましくは40〜80重量部、溶剤を好まし
くは100〜120重量部の配合とすることが良い。As described above, from Table 1 and Table 2, moisture resistance, stain resistance, hardness,
To obtain a coating film with good solvent resistance, 5 parts of inorganic powder should be added to 100 parts by weight of polyborosiloxane resin (hereinafter referred to as binder).
-100 to 100 parts by weight, preferably 40 to 80 parts by weight, and the solvent is preferably 100 to 120 parts by weight.
次に組成物１〜４中、最も塗膜性能が良好な２について
焼成温度を変えて、評価した。乾燥は200℃、10分で一
定としている。第３表にその結果をまとめた。Next, among the compositions 1 to 4, 2 having the best coating film performance was evaluated by changing the firing temperature. Drying is kept constant at 200 ° C for 10 minutes. The results are summarized in Table 3.
第３表より450℃、10分位が最適であることがわかる。4
00℃では、バインダの有機分（フェニル基）が残るため
に、溶剤との強い親和性を示し耐溶剤性に劣る。これに
対して、450℃では、バインダの有機分（フェニル基）
が、400℃焼成に比較して微量ではあるが、適量残るこ
とと、塗膜の適度なセラミック化（無機質化）により、
高い耐湿性・耐汚染性・耐溶剤性をバランスよく示すも
のと考えられる。500℃以上になると、有機分（フェニ
ル基）は殆どなくなり耐溶剤性は良いが、多孔質になる
為に基材が腐食を受けやすくなり、耐湿性、耐汚染性は
劣る。第１図は塗膜の赤外反射スペクトルにより焼成温
度と塗膜中の残存有機分との関係を示したものである。
ここまで、説明したように、耐湿性、耐汚染性のテスト
では塗膜が劣化するのではなく、基材（金属）が、腐食
を受けて塗膜が剥離したりするのである。基材がセラミ
ック質であれば何の問題もないことも確認した。ポリボ
ロシロキサン樹脂の構造を次式に示した。 It can be seen from Table 3 that 450 ° C and 10 minutes are optimal. Four
At 00 ° C, since the organic component (phenyl group) of the binder remains, it shows strong affinity with the solvent and is inferior in solvent resistance. On the other hand, at 450 ° C, the organic content of the binder (phenyl group)
However, although it is a small amount compared to 400 ° C firing, an appropriate amount remains and due to the appropriate ceramicization (inorganization) of the coating film,
It is considered to have a good balance of high humidity resistance, stain resistance and solvent resistance. Above 500 ° C, organic components (phenyl groups) are almost eliminated and solvent resistance is good, but since it is porous, the base material is susceptible to corrosion, resulting in poor moisture resistance and stain resistance. FIG. 1 shows the relationship between the baking temperature and the residual organic content in the coating film by the infrared reflection spectrum of the coating film.
As described above, in the moisture resistance and stain resistance tests, the coating film does not deteriorate, but the base material (metal) is corroded and the coating film peels off. It was also confirmed that there was no problem if the base material was ceramic. The structure of the polyborosiloxane resin is shown in the following formula.
前記SMP−32は、上式のポリボロシロキサン樹脂が、Ｎ
−メチル−２−ピロリドン（NMP）とキシレンの混合溶
媒に溶解されたもので、前記組成物１〜８の塗布後の乾
燥によりNMP、キシレンが殆ど蒸発し、その後の焼成過
程により、樹脂中のフェニル基が徐々に分解消失し、塗
膜のセラミック化が進行するのである。SMP−32は、600
℃以上では完全にセラミック化し、加熱による重量減少
はないが、それ以下の温度では、その温度や焼成時間に
応じて、フェニル基の残留程度が異なる。その残留程度
により、耐湿性、耐汚染性、耐溶剤性、硬度に差がで
る。よって、厳しい腐食性環境では、第３表の通りに焼
成を450℃位で行うのがよい。又、特に厳しい腐食性環
境でなければ、450℃以上で焼成してもかまわない。塗
膜の使用環境が、800℃位で普通に加熱、放冷、あるい
は冷却というもので、特に腐食性環境でなければ、塗膜
の劣化等は殆ど見られないことも確認した。 In the SMP-32, the polyborosiloxane resin of the above formula is N
-Dissolved in a mixed solvent of methyl-2-pyrrolidone (NMP) and xylene, most of NMP and xylene are evaporated by the drying after coating the above Compositions 1-8, and the subsequent baking process causes The phenyl group gradually decomposes and disappears, and the coating film becomes ceramic. SMP−32 is 600
At temperatures above ℃, it becomes completely ceramic, and there is no weight loss due to heating, but at temperatures below that, the degree of residual phenyl groups varies depending on the temperature and firing time. Moisture resistance, stain resistance, solvent resistance, and hardness vary depending on the degree of residual. Therefore, in a severe corrosive environment, it is better to carry out firing at about 450 ° C as shown in Table 3. If it is not a particularly severe corrosive environment, it may be fired at 450 ° C or higher. It was also confirmed that the environment in which the coating film is used is that it is heated, cooled, or cooled normally at about 800 ° C., and that deterioration of the coating film is hardly seen unless it is a corrosive environment.
次に、組成物の粘度と不発揮分について説明する。撹拌
調合の操作により組成物温度が上昇し、溶剤分がいくか
ら揮発するために、撹拌後の組成物粘度と不揮発分は、
撹拌時間に比例して増加する。組成物の配合比によって
も大きく変化するが、代表的に組成物２の配合の場合、
粘度として50〜150CPS、不発揮分として50〜55％という
ところが好ましい。特に粘度は高すぎるとスプレー塗装
時の霧化が悪いとか、作業性が悪いなどの問題もあるの
で50〜150CPSが好ましい。Next, the viscosity and ineffectiveness of the composition will be described. Since the composition temperature rises by the operation of stirring and mixing, and the solvent content evaporates, the composition viscosity after stirring and the nonvolatile content are
It increases in proportion to the stirring time. Although it varies greatly depending on the composition ratio of the composition, typically in the case of the composition 2 composition,
It is preferable that the viscosity is 50 to 150 CPS and the ineffective portion is 50 to 55%. Particularly, if the viscosity is too high, there are problems such as poor atomization during spray coating and poor workability, so 50 to 150 CPS is preferable.
次に乾燥、焼成時の雰囲気について説明する。組成物を
構成する材料から、還元性雰囲気は、酸化物の不安定化
を引きおこすので好ましくない。よって、通常大気中
か、不活性雰囲気で行うとよい。Next, the atmosphere during drying and firing will be described. A reducing atmosphere is not preferable because it causes destabilization of the oxide due to the materials constituting the composition. Therefore, it is advisable to carry out the operation in the normal atmosphere or an inert atmosphere.
以上の様に、ポリボロシロキサン樹脂を使った組成物
を、適当な撹拌条件で混合し、基材上に塗膜を形成する
と、ポリボロシロキサン樹脂の耐熱性を生かした、新し
い耐熱性塗膜が得られ、種々の分野に応用できる。例え
ば、厳しい腐食性環境でなければ、700〜800℃での連続
使用が可能で、ヒートショックによる剥離もない。従来
は、前記SMP−32を電線に被覆して、耐熱電線として使
用していたが、これでは造膜性も悪く、耐湿性、耐汚染
性、硬度、密着性等いろいろな点で問題があったが、本
発明の塗膜の製造方法により上記問題点が解消できた。
第４表に、SMP−32と組成物２による塗膜の性能比較を
示す。焼成は200℃10分の乾燥の後、450℃10分とした。
基材は、0.5mm厚のSUS430板である。As described above, when a composition using a polyborosiloxane resin is mixed under appropriate stirring conditions to form a coating film on a substrate, a new heat resistant coating film that takes advantage of the heat resistance of the polyborosiloxane resin is obtained. Can be obtained and can be applied to various fields. For example, if it is not in a severely corrosive environment, it can be used continuously at 700 to 800 ° C and does not peel due to heat shock. Conventionally, the SMP-32 was used as a heat-resistant wire by coating the wire with a heat-resistant wire, but this has poor film-forming properties, and has various problems such as moisture resistance, stain resistance, hardness, and adhesion. However, the above problems can be solved by the method for producing a coating film of the present invention.
Table 4 shows a performance comparison of the coating films of SMP-32 and Composition 2. Firing was performed at 200 ° C. for 10 minutes and then at 450 ° C. for 10 minutes.
The base material is a SUS430 plate having a thickness of 0.5 mm.
発明の効果 以上説明した様に、本発明の塗膜の製造方法によれば、
配合、撹拌、焼成を最適化することにより、 （１）ポリボロシロキサン樹脂の耐熱性を十分に生かせ
るので、今までの塗膜にない高耐熱性をもち、かつ広範
囲の環境に適した塗膜が得られる。 Effects of the Invention As described above, according to the method for producing a coating film of the present invention,
By optimizing the blending, stirring, and firing, (1) the heat resistance of the polyborosiloxane resin can be fully utilized, so it has a high heat resistance not seen in conventional paint films and is suitable for a wide range of environments. Is obtained.
（２）充填材料（無機質粉末）を任意に選定すれば、塗
膜への機能付加が可能で、応用分野が大きく広がる。(2) By arbitrarily selecting the filling material (inorganic powder), it is possible to add a function to the coating film, which greatly expands the field of application.
などの効果がある。And so on.
第１図は塗膜の焼成温度と残存有機分（フェニル基）と
の関係を示す塗膜の赤外反射スペクトル図である。FIG. 1 is an infrared reflection spectrum diagram of the coating film showing the relationship between the baking temperature of the coating film and the residual organic content (phenyl group).
───────────────────────────────────────────────────── フロントページの続き (72)発明者 礒谷 守 大阪府門真市大字門真1006番地 松下電器 産業株式会社内 (56)参考文献 特開 昭59−218844（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Mamoru Isotani 1006 Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Industrial Co., Ltd. (56) Reference JP-A-59-218844 (JP, A)
Claims (1)
リボロシロキサン樹脂を20〜60重量％含むポリボロシロ
キサン樹脂有機溶媒溶液100重量部と、Ｂ、Mg、A1、S
i、Ca、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ｙ、Zr、L
a、Ce、Prのうち少なくとも一種以上の酸化物または窒
化物40〜80重量部と、有機溶剤とから成る組成物を、基
材に塗布し、酸化性雰囲気もしくは不活性雰囲気で乾燥
の後、450℃の温度で焼成し塗膜を得る塗膜の製造方
法。1. 100 parts by weight of a polyborosiloxane resin organic solvent solution containing 20 to 60% by weight of a polyborosiloxane resin composed of Si, B, O and a phenyl group, and B, Mg, A1 and S.
i, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, L
a, Ce, 40 to 80 parts by weight of at least one oxide or nitride of Pr, and a composition comprising an organic solvent, applied to a substrate, after drying in an oxidizing atmosphere or an inert atmosphere, A method for producing a coating film by baking at a temperature of 450 ° C.
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61245723A JPH0729086B2 (en) | 1986-10-16 | 1986-10-16 | Coating film manufacturing method |
| KR1019870010165A KR900009035B1 (en) | 1986-09-19 | 1987-09-14 | Coating composition |
| CA 546912 CA1318744C (en) | 1986-09-19 | 1987-09-15 | Coating composition for ir radiation heating |
| EP19870113578 EP0260683B1 (en) | 1986-09-19 | 1987-09-17 | Coating composition for ir radiation heating |
| DE3788392T DE3788392T2 (en) | 1986-09-19 | 1987-09-17 | Coating composition for heating by infrared radiation. |
| AU78640/87A AU575752B2 (en) | 1986-09-19 | 1987-09-18 | Coating composition for ir radiation heating |
| US07/209,638 US4824730A (en) | 1986-09-19 | 1988-06-21 | IR Radiation heating element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61245723A JPH0729086B2 (en) | 1986-10-16 | 1986-10-16 | Coating film manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63258683A JPS63258683A (en) | 1988-10-26 |
| JPH0729086B2 true JPH0729086B2 (en) | 1995-04-05 |
Family
ID=17137842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61245723A Expired - Lifetime JPH0729086B2 (en) | 1986-09-19 | 1986-10-16 | Coating film manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0729086B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650882A (en) * | 2018-12-28 | 2019-04-19 | 河南省锅炉压力容器安全检测研究院 | A kind of fiber liner composite coating and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59218844A (en) * | 1983-05-27 | 1984-12-10 | 松下電器産業株式会社 | Infrared radiation coating |
-
1986
- 1986-10-16 JP JP61245723A patent/JPH0729086B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650882A (en) * | 2018-12-28 | 2019-04-19 | 河南省锅炉压力容器安全检测研究院 | A kind of fiber liner composite coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63258683A (en) | 1988-10-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |