JP2955385B2 - Manufacturing method of steel wire for glass reinforcement with excellent high temperature properties - Google Patents
Manufacturing method of steel wire for glass reinforcement with excellent high temperature propertiesInfo
- Publication number
- JP2955385B2 JP2955385B2 JP9846391A JP9846391A JP2955385B2 JP 2955385 B2 JP2955385 B2 JP 2955385B2 JP 9846391 A JP9846391 A JP 9846391A JP 9846391 A JP9846391 A JP 9846391A JP 2955385 B2 JP2955385 B2 JP 2955385B2
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- Prior art keywords
- steel wire
- glass
- present
- strength
- high temperature
- 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.)
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Description
【0001】[0001]
【産業上の利用分野】建築ならびに自動車産業界で使用
しているガラスは安全性を考慮しガラスの強化と破損時
の飛散防止のため、ガラスの中に鋼線を封入している。
本発明はこのガラス補強用鋼線の製造方法に関するもの
であり、詳しくは高温特性の優れたガラス補強用鋼線を
提供するものである。[Industrial application] Glass used in the construction and automotive industries has a steel wire enclosed in the glass in order to strengthen the glass and prevent scattering when broken in consideration of safety.
The present invention relates to a method for manufacturing a glass reinforcing steel wire, and more specifically, to provide a glass reinforcing steel wire having excellent high-temperature characteristics.
【0002】[0002]
【従来の技術】ガラス封入後に生じる鋼線界面近傍の気
泡や割れは商品価値を著しく低下させるため従来から多
くの検討がなされている。例えば、鋼線の表面疵を減少
して割れ起点を減少させる方法や特公昭42−169で
は鋼線表面のパーライト組織を球状化セメンタイト化し
て気泡発生および割れを抑制する方法などがある。ま
た、特公昭47−1474では水蒸気処理と燐酸処理を
組み合わせた方法が提案されている。また、この方法は
鋼線の成分によって効果が著しく変化することが判明し
てきた。特開昭52−11117は気泡発生に関して基
本的な検討をおこなっているがこの方法では割れに関し
ては発生頻度がばらつくなどの問題点が残されている。
いずれにせよ、こうした従来技術では割れの問題は完全
に解消されているとは言えず最終検査工程のチェックで
降格となる不良が発生している。この傾向は特に磨きガ
ラス(透明ガラス)で生じている。2. Description of the Related Art Many studies have been made on air bubbles and cracks near the steel wire interface after glass encapsulation, which significantly reduce the commercial value. For example, there is a method of reducing the crack origin by reducing the surface flaw of the steel wire, and Japanese Patent Publication No. Sho 42-169 discloses a method of suppressing the generation of bubbles and cracking by making the pearlite structure on the surface of the steel wire into spheroidized cementite. Japanese Patent Publication No. 47-1474 proposes a method combining steam treatment and phosphoric acid treatment. In addition, it has been found that the effect of this method varies significantly depending on the composition of the steel wire. Japanese Patent Application Laid-Open No. 52-11117 makes a basic study on the generation of air bubbles, but this method still has a problem that the frequency of occurrence of cracks varies.
In any case, the problem of cracking cannot be completely solved by such a conventional technique, and a failure that is demoted in a check in the final inspection process occurs. This is especially true for polished glass (clear glass).
【0003】このように従来の技術はガラスの中に如何
に鋼線を整合させて封入しうるかと言う観点から発泡あ
るいは割れ防止に関する技術が主体を占めていた。しか
しながら従来の網入りガラスは常温の場合あまり問題と
ならないが、火災が発生した場合、現状の鋼線の高温強
度ではガラスが脱落しやすいため、2次災害の発生およ
び延焼が生じ易くなるなどの問題点が残され、高温にお
ける強度の向上を期待する要求が高まってきた。As described above, the prior art mainly occupies a technique relating to foaming or crack prevention from the viewpoint of how to align and enclose a steel wire in glass. However, conventional meshed glass is not a problem at room temperature, but when a fire occurs, the glass tends to fall off at the current high-temperature strength of steel wire, which causes secondary disasters and fire spread. Problems remain, and demands for improvement in strength at high temperatures have increased.
【0004】[0004]
【発明が解決しようとする課題】そこで、本発明者らは
ガラス封入用鋼線の高温強度を向上させ、火災時のガラ
スの脱落率を低減し、火災時の2次災害の防止を計ると
いう本来目的に着眼を置いた研究に着手した。ガラス補
強用鋼線は基本的に低炭素を指向しなければならないた
め、高温での鋼線の強化は主にフェライトの固溶強化を
狙う必要があった。SUMMARY OF THE INVENTION Accordingly, the inventors of the present invention intend to improve the high-temperature strength of the steel wire for glass encapsulation, reduce the falling-off rate of glass in a fire, and prevent a secondary disaster in a fire. We have begun research that originally focused on the purpose. Since the steel wire for glass reinforcement basically has to be oriented to low carbon, it was necessary to strengthen the steel wire at a high temperature mainly for solid solution strengthening of ferrite.
【0005】このためMoを単独に添加させて種々研究
を行なったがMo単独では高温において強度の上昇は無
添加の場合より向上はするがその効果が持続できないこ
とがわかった。そこで本発明者らは高温での強化持続時
間の延長をはかるため、他の元素との複合効果を模索し
た結果、Nbを添加することにより大幅な強度の向上な
らびその効果が持続する時間がふえるとの知見を得た。
その理由はNbCの析出強化とMoの固溶強化の複合作
用によるものと考えられる。[0005] For this reason, various studies were conducted by adding Mo alone, but it was found that Mo alone increases the strength at high temperatures compared to the case without Mo, but cannot maintain its effect. Therefore, the present inventors sought a composite effect with other elements in order to extend the duration of strengthening at high temperatures, and as a result, by adding Nb, the strength was significantly improved and the time during which the effect was maintained increased. I got the knowledge.
The reason is considered to be due to the combined action of precipitation strengthening of NbC and solid solution strengthening of Mo.
【0006】[0006]
【課題を解決するための手段】本発明は、C:0.02
0%以下、Mn:0.2〜0.4%、Al:0.003
%以下、Al%/N%:1.3以下、Mo:0.1%〜
0.5%、Nb:0.005%〜0.06%、Cr:
0.1〜0.5%、Cu:0.05〜0.2%にNiを
Cu量の1/3〜1/2添加し、残部は不可避的不純物
からなる鋼成分の鋼片を線材圧延したのち、所定のサイ
ズまで伸線加工を施し、最終工程で鋼線表面にめっきを
施すことを特徴とする高温特性の優れたガラス補強用鋼
線の製造方法、である。According to the present invention, C: 0.02
0% or less, Mn: 0.2 to 0.4%, Al: 0.003
% Or less, Al% / N%: 1.3 or less, Mo: 0.1% or more
0.5%, Nb: 0.005% to 0.06%, Cr:
0.1 to 0.5%, Cu: 0.05 to 0.2%, Ni is added to 1/3 to 1/2 of the amount of Cu, and the remainder is a steel rod of a steel component consisting of unavoidable impurities. After that, a method for producing a glass reinforcing steel wire having excellent high-temperature characteristics, comprising drawing a wire to a predetermined size and plating the surface of the steel wire in a final step.
【0007】[0007]
【作用】Cは鋼線の強度を支配する元素であるが、ガラ
ス補強用鋼線の場合、過剰の添加はガラス封入時に気泡
発生を誘発しやすくするため、上限を0.020%に抑
える必要がある。また、これ以上の添加になると常温で
の強度が増し鋼線を編網する際、成形後のスプリングバ
ックが大きくなり金網のハンドリングが行いにくくなる
ためである。C is an element that controls the strength of the steel wire. However, in the case of a steel wire for reinforcing glass, the upper limit must be suppressed to 0.020% because excessive addition easily induces the generation of bubbles at the time of sealing the glass. There is. Further, if it is added more than this, the strength at normal temperature increases, and when knitting the steel wire, the springback after forming becomes large, and it becomes difficult to handle the wire mesh.
【0008】Mnは脱酸元素でありまた、熱間脆性を抑
制させる効果がある。上限を0.4%としたのはこれ以
上の添加は鋼線の常温強度を不必要に高め、編網工程の
作業性を損なうためである。下限を0.2%にした理由
は、これ以下では伸線工程で実施するバット溶接性が悪
くなるためである。Mn is a deoxidizing element and has an effect of suppressing hot brittleness. The upper limit is set to 0.4% because the addition of more than that unnecessarily increases the room temperature strength of the steel wire and impairs the workability of the knitting net process. The reason for setting the lower limit to 0.2% is that if it is less than 0.2%, the butt weldability performed in the wire drawing process will be poor.
【0009】Alは脱酸元素としてよく用いられるが同
時に窒化アルミニウムを形成するため、鋼線の再結晶挙
動に対して影響の大きい元素である。従って、本発明で
はきわめて重要な意味を持つ。Alが0.003%を越
えるとAlNが多く生成し、ガラス封入時点の再結晶粒
成長が不均一になり、粗大粒と微細粒の混粒組織となり
やすく一定張力制御がきわめて難しくなる。このため、
ガラスに封入する位置制御が不安定となり、冷却段階で
ガラスが割れるなどの問題を引き起こすため、上限を
0.003%とした。Although Al is often used as a deoxidizing element, it forms aluminum nitride at the same time, and therefore has a large effect on the recrystallization behavior of steel wires. Therefore, the present invention has a very important meaning. If the content of Al exceeds 0.003%, a large amount of AlN is generated, the growth of recrystallized grains at the time of enclosing the glass becomes nonuniform, and a mixed grain structure of coarse grains and fine grains is easily formed, and it is extremely difficult to control the constant tension. For this reason,
The upper limit is set to 0.003% because the position control of sealing the glass becomes unstable, causing problems such as breaking of the glass during the cooling stage.
【0010】NはAlと反応してAlNとなる元素であ
る。作用はAlの限定理由で述べたとおりである。Al
/Nを1.3以下に調整するのは、これ以上のNを含有
すると再結晶の粒成長を阻害し、スムースな粒成長が期
待できなくなり、このため、Alの場合と同様に鋼線を
一定の張力で封入することが困難になるためである。N is an element that reacts with Al to form AlN. The effect is as described for the limitation of Al. Al
The reason why / N is adjusted to 1.3 or less is that if N is contained more than this, the grain growth of recrystallization is hindered, so that smooth grain growth cannot be expected. This is because it becomes difficult to enclose with a constant tension.
【0011】Moは本発明の中で高温特性を向上させる
ために用い、Nbと同様に本発明において重要な役割を
有する元素である。Moの固溶強化による高温特性の改
善のためには、少なくとも0.1%の添加が必要であ
る。上限を0.5%にしたのはMoが高価であることお
よびこれ以上の添加では効果が飽和するためである。Mo is an element used in the present invention for improving high-temperature characteristics and has an important role in the present invention like Nb. In order to improve the high temperature characteristics by solid solution strengthening of Mo, it is necessary to add at least 0.1%. The upper limit is set to 0.5% because Mo is expensive and the effect is saturated when Mo is added further.
【0012】NbはTiと同様に窒化物および炭化物形
成元素である。本発明におけるNbの役割はC,Nを固
定して常温における時効を小さくし、鋼線強度のばらつ
きを小さくするほか、NbCによる析出強化作用で高温
強度を維持させるために用いる。下限を0.005%と
した理由はこれ以下では前述の効果が現われないためで
ある。上限を0.06%にしたのは微細炭化物の量が増
えるため、ガラス封入時に鋼線表面に露出する頻度が高
まり、Cと同様に発泡現象が現われるためである。Nb is a nitride and carbide forming element like Ti. The role of Nb in the present invention is used to fix C and N to reduce aging at room temperature, reduce variations in steel wire strength, and maintain high-temperature strength by the precipitation strengthening action of NbC. The reason why the lower limit is set to 0.005% is that below this value, the above-mentioned effects are not exhibited. The upper limit is set to 0.06% because the amount of fine carbides increases, so that the frequency of exposure to the steel wire surface during glass encapsulation increases, and a foaming phenomenon appears as in C.
【0013】Crは炭化物を形成するため、鋼中のCの
固定に用いて気泡発生防止を行なうために使用するがC
rの添加によっても高温の強度を向上できる。このた
め、その効果を発揮するため最小量として0.1%を添
加する。上限を0.5%としたのはこれ以上の過剰添加
では効果が飽和するためである。Since Cr forms carbides, it is used to fix C in steel and is used to prevent bubbles from being generated.
High temperature strength can also be improved by adding r. Therefore, 0.1% is added as a minimum amount to exhibit the effect. The upper limit is set to 0.5% because the effect is saturated when added in excess.
【0014】Cuは鋼に固溶して強度を高めるとともに
耐食性を向上させる元素である。本発明においてはCu
は耐食性を向上させるために用いる。ガラス補強線は封
入される前にめっきをすることにより鋼線の表面は優れ
た耐食性を有している。しかしながら、ガラスに封入さ
れた後、ガラスを定尺に裁断される場合に不可避的に切
断面が生じる。この切断された鋼線の断面の耐食性を向
上させることを目的に添加するものである。下限を0.
05%としたのはこれ以下では耐食性の向上が期待でき
ないためである。一方、耐食性を高めるにはCuの添加
量を増やすことが有効であるが極度の添加は常温におけ
る機械的性質の強度を不必要に上げるため、上限を0.
2%にした。Cu is an element that forms a solid solution with steel to increase strength and corrosion resistance. In the present invention, Cu
Is used to improve corrosion resistance. The surface of the steel wire has excellent corrosion resistance by plating the glass reinforcing wire before being enclosed. However, when the glass is cut into a fixed size after being sealed in the glass, a cut surface is inevitably generated. It is added for the purpose of improving the corrosion resistance of the cross section of the cut steel wire. Set the lower limit to 0.
The reason for setting it to 05% is that if it is less than this, improvement in corrosion resistance cannot be expected. On the other hand, it is effective to increase the amount of Cu added to increase the corrosion resistance, but the extreme addition unnecessarily increases the strength of the mechanical properties at room temperature.
2%.
【0015】NiはCu含有鋼の場合、熱間で生じる鋼
片の表面割れを防止するために用いる。この効果を得る
ために最低添加量はCu量の1/3必要であり、上限は
この効果が飽和するCu添加量の1/2とした。In the case of Cu-containing steel, Ni is used to prevent surface cracks of the steel slab that occur during hot working. To obtain this effect, the minimum addition amount is required to be 1/3 of the Cu amount, and the upper limit is set to 1/2 of the Cu addition amount at which this effect is saturated.
【0016】補強用鋼線の製造工程の最終段階にめっき
を行なう。めっき方法は特に規定しないが鋼線表面の平
滑性の高い電気めっきの方が好ましい。さらに詳しくは
ガラスとの濡れ性を考慮するとCrめっきが好ましい。
その他、電気Niめっきなども効果がある。すなわち、
鋼線表面とガラスが直接触れない方法でガラスとの濡れ
性のよいものであれば、鋼線表面に発生する気泡および
冷却時の熱収縮にともなう割れを防止できる。これらの
特性を有するめっきはすべて本発明の対象となる。次に
実施例について述べる。[0016] Plating is performed in the final stage of the manufacturing process of the reinforcing steel wire. Although the plating method is not particularly limited, electroplating with high smoothness on the surface of the steel wire is preferable. More specifically, Cr plating is preferable in consideration of wettability with glass.
In addition, electric Ni plating is also effective. That is,
As long as the steel wire surface does not come into direct contact with the glass and has good wettability with the glass, it is possible to prevent air bubbles generated on the steel wire surface and cracks due to heat shrinkage during cooling. All platings having these properties are the subject of the present invention. Next, examples will be described.
【0017】[0017]
【実施例】表1に示す鋼はすべて250ton転炉にて
溶製したもので、その後連続鋳造にて500×300m
mの鋳片とし、その後122mm角の鋼片とした。その
後、線材圧延を実施して5.5mmの線材とした。さら
に伸線加工を行い最終の鋼線径を0.57mmとした。EXAMPLES All the steels shown in Table 1 were melted in a 250 ton converter, and then continuously cast to 500 × 300 m.
m, and then a 122 mm square steel slab. After that, wire rolling was performed to obtain a 5.5 mm wire. Further, wire drawing was performed to make the final steel wire diameter 0.57 mm.
【0018】表1に示すNo1〜No6が本発明法で用
いた鋼を示す。一方、比較法としてNo7〜No9を示
す。No7は本発明法に対しCr、Cu、Niの添加の
ないもの。No8はCr、Mo、Nbの添加のないも
の。No9はMo、Nb、Cu、Niは添加していない
もので最終めっきも行なっていない水準である。表1に
示すめっき処理は電気Crめっきを実施したものであ
る。No. 1 to No. 6 shown in Table 1 indicate steels used in the method of the present invention. On the other hand, No. 7 to No. 9 are shown as comparative methods. No. 7 does not include Cr, Cu and Ni in the method of the present invention. No. 8 has no Cr, Mo and Nb added. No. 9 is a level in which Mo, Nb, Cu, and Ni are not added and final plating is not performed. The plating treatment shown in Table 1 was performed by electrochromic plating.
【0019】次に評価の方法について説明する。表2に
は常温および600℃×1時間保定を行なった結果を示
す。ガラス封入後の外観観察は目視観察により割れの発
生状況を観察した。鋼線端部の割れ発生はJISZ23
71に規定された塩水噴霧試験を行い試験後の割れ発生
状況を目視観察した。表3には実際の火災を想定した放
水テスト結果について示している。試験条件は表3に記
載したものを用い、ガラスの脱落に至るまでの時間を測
定した。Next, an evaluation method will be described. Table 2 shows the results of holding at room temperature and at 600 ° C. for 1 hour. The appearance of the glass-filled glass was observed by visual observation to determine the occurrence of cracks. The occurrence of cracks at the end of the steel wire is JISZ23
A salt spray test specified in No. 71 was performed, and the occurrence of cracks after the test was visually observed. Table 3 shows the results of the water discharge test assuming an actual fire. Using the test conditions described in Table 3, the time until the glass came off was measured.
【0020】[0020]
【表1】 [Table 1]
【0021】[0021]
【表2】 [Table 2]
【0022】表2の結果から、本発明法は本発明の目的
である高温強度が従来法のNo7〜9のものと比較して
明らかに向上していることがわかる。また、比較材の中
でNo7はMo、Nbを含有しているため高温強度は良
好であるが、Cu、Niの添加がないため、本発明法の
ように封入後の鋼線端部の錆による割れを防止できてい
ない。No8、9はいずれも高温強度が本発明法より低
い。これはMo、Nbの添加がないためである。また、
ガラスに封入後の割れ観察においても本発明法のNo1
〜6のものには割れが観察されず、きわめて封入性の優
れた鋼線であることがわかる。From the results shown in Table 2, it can be seen that the high temperature strength, which is the object of the present invention, is clearly improved in the method of the present invention as compared with those of Nos. 7 to 9 of the conventional method. Further, among the comparative materials, No. 7 has high strength at high temperature because it contains Mo and Nb. However, since there is no addition of Cu and Ni, there is no rust at the end of the steel wire after sealing as in the method of the present invention. Cracking due to cracking was not prevented. Nos. 8 and 9 both have lower high-temperature strength than the method of the present invention. This is because there is no addition of Mo and Nb. Also,
Observation of cracks after sealing in glass
No cracks were observed in samples Nos. 6 to 6, indicating that the steel wire was extremely excellent in encapsulation.
【0023】[0023]
【表3】 [Table 3]
【0024】また、表3に示す放水テストの結果は高温
における強度が本発明法のものが優れていることを示
す。この結果は鋼線単線の高温強度を測定した表2の結
果とよく対応していることがわかる。このように本発明
法によって製造した鋼線は封入性、端部防食性ならびに
高温強度が従来法より高位安定したガラス補強用鋼線と
なっていることがわかる。The results of the water discharge test shown in Table 3 show that the high-temperature strength of the method of the present invention is excellent. It can be seen that the results correspond well with the results in Table 2 in which the high-temperature strength of a single steel wire was measured. Thus, it can be seen that the steel wire manufactured by the method of the present invention is a steel wire for glass reinforcement in which the encapsulation property, the edge corrosion prevention property and the high-temperature strength are higher and more stable than the conventional method.
【0025】これらの特性は従来法では達成できなかっ
たので、本発明法の関連分野への貢献はきわめて大きい
ものである。特に、高層建築が今後ますます増加するこ
とが予想されるため、高温特性を備えた網入りガラスは
火災時の延焼防止に役立つものとなる。Since these characteristics could not be achieved by the conventional method, the contribution of the method of the present invention to the related field is extremely large. In particular, since high-rise buildings are expected to increase more and more in the future, netted glass having high-temperature characteristics will be useful for preventing fire spread in a fire.
【0026】[0026]
【発明の効果】本発明のガラス補強用鋼線は高温での強
度持続時間が長い。本発明のガラス補強用鋼線を用いる
ことにより高温特性の優れた網入りガラスの製造が可能
となった。またガラス封入製造工程が安定で、割れや発
泡のない網入りガラスが製造できる。本発明の鋼線を使
用した網入りガラスは、火災が発生した場合、2次災害
ならびに火災の延焼を減少させる効果が発揮できる。The steel wire for reinforcing glass of the present invention has a long strength duration at high temperatures. By using the steel wire for glass reinforcement of the present invention, it has become possible to produce a netted glass having excellent high-temperature characteristics. In addition, the glass encapsulation manufacturing process is stable, and it is possible to manufacture meshed glass free from cracks and foaming. The netted glass using the steel wire of the present invention can exhibit the effect of reducing secondary disasters and fire spread when a fire occurs.
【0027】[0027]
フロントページの続き (56)参考文献 特開 平2−77523(JP,A) 特開 昭52−113358(JP,A) 特開 昭53−94317(JP,A) 特開 平4−285120(JP,A) 特開 平4−288919(JP,A) (58)調査した分野(Int.Cl.6,DB名) C21D 7/00 - 7/10 C03B 13/12 C03C 27/00 - 27/02 C22C 38/00 - 38/60 Continuation of front page (56) References JP-A-2-77523 (JP, A) JP-A-52-113358 (JP, A) JP-A-53-94317 (JP, A) JP-A-4-285120 (JP, A) (A) JP-A-4-288919 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) C21D 7/00-7/10 C03B 13/12 C03C 27/00-27/02 C22C 38/00-38/60
Claims (1)
0.2〜0.4%、Al:0.003%以下、
Al%/N%:1.3以下、Mo:0.1%〜0.5
%、 Nb:0.005%〜0.06%、Cr:
0.1〜0.5%、 Cu:0.05〜0.2%にNi
をCu量の1/3〜1/2添加し、残部は不可避的不純
物からなる鋼成分の鋼片を線材圧延したのち、所定のサ
イズまで伸線加工を施し、最終工程で鋼線表面にめっき
を施すことを特徴とする高温特性の優れたガラス補強用
鋼線の製造方法。C: 0.020% or less; Mn:
0.2-0.4%, Al: 0.003% or less,
Al% / N%: 1.3 or less, Mo: 0.1% to 0.5
%, Nb: 0.005% to 0.06%, Cr:
0.1-0.5%, Cu: 0.05-0.2% Ni
Is added to 1/3 to 1/2 of the amount of Cu, and the remainder is made by rolling a steel slab of steel components consisting of unavoidable impurities, then drawing to a predetermined size, and plating the steel wire surface in the final process A method for producing a glass reinforcing steel wire having excellent high-temperature characteristics, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9846391A JP2955385B2 (en) | 1991-04-30 | 1991-04-30 | Manufacturing method of steel wire for glass reinforcement with excellent high temperature properties |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9846391A JP2955385B2 (en) | 1991-04-30 | 1991-04-30 | Manufacturing method of steel wire for glass reinforcement with excellent high temperature properties |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04329825A JPH04329825A (en) | 1992-11-18 |
| JP2955385B2 true JP2955385B2 (en) | 1999-10-04 |
Family
ID=14220385
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9846391A Expired - Fee Related JP2955385B2 (en) | 1991-04-30 | 1991-04-30 | Manufacturing method of steel wire for glass reinforcement with excellent high temperature properties |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2955385B2 (en) |
-
1991
- 1991-04-30 JP JP9846391A patent/JP2955385B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04329825A (en) | 1992-11-18 |
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