JP2006349171A - Method of storing nitrogen trifluoride gas - Google Patents
Method of storing nitrogen trifluoride gas Download PDFInfo
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- JP2006349171A JP2006349171A JP2006161674A JP2006161674A JP2006349171A JP 2006349171 A JP2006349171 A JP 2006349171A JP 2006161674 A JP2006161674 A JP 2006161674A JP 2006161674 A JP2006161674 A JP 2006161674A JP 2006349171 A JP2006349171 A JP 2006349171A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L5/00—Gas handling apparatus
- B01L5/02—Gas collection apparatus, e.g. by bubbling under water
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L5/00—Gas handling apparatus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
- C01B21/0832—Binary compounds of nitrogen with halogens
- C01B21/0835—Nitrogen trifluoride
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Abstract
Description
本発明は、三フッ化窒素（ＮＦ３）ガスの貯蔵方法に関する。
さらに詳細には、本発明は、深絞りしごき（Deep Drawing Ironing）工法（以下、「ＤＤＩ工法」という）で製造されたクロム−モリブデン鋼製容器を用いることによるＮＦ３ガスの貯蔵方法に関する。
The present invention relates to a method for storing nitrogen trifluoride (NF 3 ) gas.
More specifically, the present invention relates to a method for storing NF 3 gas by using a chromium-molybdenum steel container manufactured by a deep drawing ironing method (hereinafter referred to as “DDI method”).
板金加工において、絞り型（Drawing Die）を用いて底付き円筒状の容器を作る加工方法をＤＤＩ工法という。
なお、ＤＤＩ工法は、深絞り加工法ともいうことがある。炭素工具鋼又は合金工具鋼の上下１組（パンチとダイス）からなっている金型を絞り型という。この絞り型（ダイス）を機械プレスに固定させ、型の間に板材を挟んだ後パンチを押すと、板材が延伸されながら底面と壁面が一体になるコップ状の円筒型容器が成形される。容器の上部を密封し、注入口にバルブを設置すると、ガス貯蔵用高圧容器が完成される。
In sheet metal processing, a processing method for producing a cylindrical container with a bottom using a drawing die is called a DDI method.
The DDI method may also be referred to as a deep drawing method. A die composed of a pair of upper and lower carbon tool steel or alloy tool steel (punch and die) is called a drawing die. When this drawing die (die) is fixed to a mechanical press, a plate material is sandwiched between the dies, and then a punch is pressed, a cup-shaped cylindrical container in which the bottom surface and the wall surface are integrated while the plate material is stretched is formed. When the upper part of the container is sealed and a valve is installed at the inlet, a high-pressure container for gas storage is completed.
ＮＦ３ガスは、半導体素子の製造の際にエッチング剤（etching agent）として用いられる高価な化学工業薬品である。ＮＦ３は、フッ素ガスとアンモニアとを直接反応させ、あるいは酸性フッ化アンモニウム（ＮＦ４・ＨＦ）とフッ素ガスとを反応させて製造することも、酸性フッ化アンモニウム溶融塩を電気分解して製造することもできる。一般に、ＮＦ３ガスは、高純度の液体状態に製造された後、２０〜５０Ｌの容器に高圧ガスの状態で充填してユーザーに供給されている。
ＮＦ３は、半導体素子構造の製造工程のエッチング剤として用いられるものなので、９９．９９％以上の高純度のものが要求される。
現在、半導体製造工程では、Ｎ２：ｍａｘ３ｐｐｍ、Ｏ２：ｍａｘ３ｐｐｍ、ＣＯ２：ｍａｘ１ｐｐｍ、ＣＦ４：ｍａｘ２０ｐｐｍ、Ｈ２Ｏ：ｍａｘ１ｐｐｍ、Ｎ２Ｏ：ｍａｘ１ｐｐｍ、ＨＦ：ｍａｘ１ｐｐｍの純度が保たれるＮＦ３ガスが要求されている。
NF 3 gas is an expensive chemical industrial chemical used as an etching agent in the manufacture of semiconductor devices. NF 3 can be produced by reacting fluorine gas and ammonia directly, or by reacting acid ammonium fluoride (NF 4 · HF) with fluorine gas, or by electrolyzing acid ammonium fluoride molten salt. You can also In general, NF 3 gas is supplied to a user after being manufactured in a high-purity liquid state and filled in a 20 to 50 L container in a high-pressure gas state.
Since NF 3 is used as an etchant in the manufacturing process of the semiconductor element structure, a high purity of 99.99% or more is required.
Currently, the semiconductor manufacturing process, N 2: max3ppm, O 2 : max3ppm, CO 2: max1ppm, CF 4: max20ppm, H 2 O: max1ppm, N 2 O: max1ppm, HF: NF 3 the purity of Max1ppm is maintained Gas is required.
ＮＦ３ガスは、反応性の高い気体の化学工業薬品であるので、保管又は流通過程で変質してはならないため、特殊な容器に充填して貯蔵することが一般的である。
従来のＮＦ３ガスを充填して貯蔵する容器としては、マンガン鋼で製造された容器が用いられている。このような用途として用いられるマンガン鋼製容器は、０．５〜１．５％のマンガンを含有するマンガン鋼からなるパイプを熱処理成形加工によって円筒状の密閉容器に作り、この容器の内部を研磨し洗浄するなどの工程を経て製造されたものである。
ＮＦ３を充填して貯蔵する容器として用いられるマンガン鋼製容器は、内面研磨によって内面粗さ（Ra）を１０μｍ以下に維持させ、洗浄、加熱及び真空作業によって内部の不純物を徹底的に除去してから使われる。
Since NF 3 gas is a highly reactive gaseous chemical industrial chemical, it must not be altered during storage or distribution, and therefore it is common to store it in a special container.
As a conventional container for filling and storing NF 3 gas, a container made of manganese steel is used. Manganese steel containers used for such applications are made by making a pipe made of manganese steel containing 0.5-1.5% manganese into a cylindrical sealed container by heat treatment molding, and polishing the interior of this container It is manufactured through a process such as cleaning.
Manganese steel containers used as containers for filling and storing NF 3 maintain inner surface roughness (Ra) of 10 μm or less by inner surface polishing, and thoroughly remove internal impurities by washing, heating and vacuum operations. Used after.
ところが、内部不純物が除去され、内面粗さ（Ra）が１０μｍ以下に加工処理されたマンガン鋼製容器であっても、ＮＦ３を充填して保管すると、時間の経過に伴ってＮＦ３ガスが酸性を示してくるという問題がある。ＮＦ３ガスが酸性を示すということは、ＮＦ３ガスが変質することである。
しかしながら、このようなＮＦ３ガスの変質原因は、未だその正確なメカニズムが解明されてはいないが、貯蔵容器内に存在する不純物、すなわち酸化鉄（ＦｅｘＯｙ）と水分、酸素による影響であると推測されており、酸性を示す主原因は、ＮＦ３ガスの変質により生成した硝酸による影響であると分析によって明らかになっている。
However, even if the container is made of manganese steel from which the internal impurities are removed and the inner surface roughness (Ra) is processed to 10 μm or less, if NF 3 is filled and stored, the NF 3 gas will increase with time. There is a problem of showing acidity. The fact that NF 3 gas is acidic means that NF 3 gas is altered.
However, alteration causes of such NF 3 gas is still Although the exact mechanism has not yet been elucidated, impurities present in the storage container, i.e. the iron oxide (Fe x O y) and moisture, the influence by oxygen It is speculated that there is an analysis, and it has been revealed by analysis that the main cause of acidity is the influence of nitric acid produced by the alteration of NF 3 gas.
ＮＦ３ガスが、充填容器の内部で硝酸に変質することを示す反応式は、次のとおりである。
現在、ＮＦ３ガス製造会社又はＮＦ３ガス使用会社で適用しているＮＦ３ガス規格には酸度が規定してあるが、これはＨＦのみを意味し、硝酸類を規定していないため、硝酸類は管理されていない。
このようにマンガン鋼製容器に充填・貯蔵されたＮＦ３ガスから硝酸が検出されるということは、マンガン鋼製容器がＮＦ３充填容器として適しないことを意味する。
したがって、ＮＦ３ガス製造会社又は使用会社は、長期保管の際に変質を起こさないＮＦ３貯蔵方法の開発が必要な実情にある。
For now, but the NF 3 gas standards that are applied in NF 3 gas manufacturers or NF 3 gas used company are defined acidity, this means only HF, but does not specify nitrates, nitrate Kinds are not managed.
Thus, the fact that nitric acid is detected from the NF 3 gas filled and stored in the manganese steel container means that the manganese steel container is not suitable as an NF 3 filled container.
Therefore, the NF 3 gas manufacturing company or the user company is in a situation where it is necessary to develop an NF 3 storage method that does not cause deterioration during long-term storage.
本発明者らは、従来の方法で製造されたマンガン鋼製容器にＮＦ３ガスを貯蔵する場合、容器の内部を研磨加工して粗さ（Ｒａ）を１０μｍ以下に低くしても、容器内面の組織が緻密ではなく、その結果、微量の遊離鉄（isolated iron）成分や水分などの不純物が存在することになり、このような不純物がＮＦ３ガスと反応を起こしてＮＦ３ガスが変質するが、これに対しＤＤＩ工法で製造されたクロム−モリブデン鋼製容器を使用すると、長期保管の際にもＮＦ３ガスが変質を起こさないことを確認し、本発明を完成するに至った。
本発明は、このような問題点に鑑みてなされたもので、その目的とするところは、長期保管の際にも変質を起こさないＮＦ３ガスの貯蔵方法を提供することにある。
When the NF 3 gas is stored in a manganese steel container manufactured by a conventional method, the inventors of the present invention can reduce the roughness (Ra) to 10 μm or less by polishing the inside of the container and the inner surface of the container. As a result, a small amount of isolated iron component and impurities such as moisture are present, and these impurities react with NF 3 gas and NF 3 gas is altered. However, when a chromium-molybdenum steel container manufactured by the DDI method was used, it was confirmed that the NF 3 gas did not change even during long-term storage, and the present invention was completed.
The present invention has been made in view of such problems, and an object of the present invention is to provide a method for storing NF 3 gas that does not cause alteration even during long-term storage.
上記課題を解決するために、本発明は、ＤＤＩ工法で製造されたクロム−モリブデン鋼製容器を用いるＮＦ３ガスの貯蔵方法を提供するものである。 In order to solve the above-described problems, the present invention provides a method for storing NF 3 gas using a chromium-molybdenum steel container manufactured by the DDI method.
本発明のクロム−モリブデン鋼製容器を用いて充填して貯蔵されたＮＦ３ガスは、２年以上長期保管経過後にも変質しないという効果がある。 The NF 3 gas filled and stored using the chrome-molybdenum steel container of the present invention has an effect that it does not deteriorate after a long-term storage for 2 years or longer.
半導体製造工程において使用されるガスの場合、半導体の集積度が高くなるにつれて、要求されるガスの純度も益々高くなっており、これによりガスの充填容器に対する管理もさらに厳しくなっている。一般に、高純度用ガス充填容器は、充填後、容器の内面に付いている水分及び不純物粒子によるガスの汚染を防止するために、内面研磨工程によって、内面の粗さ（Ｒａ）を１０μｍ以下の水準に維持させ、次いで容器内部の異物を除去するための洗浄、乾燥、真空などの工程を経る。ところが、ＮＦ３ガスの場合、前記のような厳しい工程によって製造された貯蔵容器であっても、充填後、段々酸性化してしまうという問題が発生している。 In the case of a gas used in a semiconductor manufacturing process, as the degree of integration of the semiconductor increases, the purity of the required gas becomes higher and higher, so that the management of the gas filling container becomes more severe. Generally, a high-purity gas-filled container has an inner surface roughness (Ra) of 10 μm or less by an inner surface polishing step in order to prevent gas contamination due to moisture and impurity particles attached to the inner surface of the container after filling. Then, it is subjected to processes such as washing, drying, and vacuum for removing foreign substances inside the container. However, in the case of NF 3 gas, there is a problem that even if the storage container is manufactured by the strict process as described above, it is gradually acidified after filling.
本発明者らは、ＮＦ３ガスの場合、従来のマンガン鋼で製作した充填容器に充填する場合、硝酸化物系の不純物が形成されて製品の酸度（ｐＨ）が増加することを観察し、マンガン鋼ではなくクロム−モリブデン鋼を用いてＤＤＩ工法で製作した充填容器にＮＦ３ガスを充填すると、酸度の増加なしに高純度の製品が維持されることを見出した。すなわち、既存のマンガン鋼で製作した充填容器は、如何に内面を精密に加工し、厳しく洗浄乾燥させても、ＮＦ３ガスを充填する場合、時間の経過に伴って酸性物質が生成され、ガスから酸性域のｐＨが検知されるという問題点があった。しかしながら、ＤＤＩ工法で製造したクロム−モリブデン鋼製容器を用いて三フッ化窒素ガスを充填すると、いかなる汚染物の生成も全く観察されず、長期間保存の際にも製品の変質がないため、ＮＦ３の貯蔵容器として適することを見出し、本発明に至った。
このような現象は、クロム−モリブデン鋼の場合、一般なマンガン鋼製容器とは異なり、パイプではなく、鋼板を用いてＤＤＩ工法によって製作されるが、材質及び工法の特性上、マンガン鋼製容器とは異なり、別途の内面処理工程を経なくても表面が均一になり、５μｍ以下の粗さ（Ｒａ）を示し、内面処理工程を経る場合に１μｍ未満の表面粗さ（Ｒａ）を得ることができるという利点がある。
In the case of NF 3 gas, the present inventors have observed that when filling a conventional container made of manganese steel, a nitrate-based impurity is formed and the acidity (pH) of the product is increased. It has been found that high purity products can be maintained without increasing acidity when NF 3 gas is filled into a filling vessel manufactured by the DDI method using chromium-molybdenum steel instead of steel. That is, even if the filling container made of the existing manganese steel is processed with a precise inner surface and rigorously washed and dried, when filling with NF 3 gas, an acidic substance is generated with the passage of time. Therefore, there is a problem that the pH in the acidic range is detected. However, when nitrogen trifluoride gas is filled using a chromium-molybdenum steel container manufactured by the DDI method, no contamination is observed at all, and there is no deterioration of the product even during long-term storage. It has been found that it is suitable as a storage container for NF 3 and has led to the present invention.
In the case of chromium-molybdenum steel, such a phenomenon is produced by a DDI method using a steel plate instead of a pipe unlike a general manganese steel vessel. Unlike the above, the surface becomes uniform without going through a separate inner surface treatment step, showing a roughness (Ra) of 5 μm or less, and when passing through the inner surface treatment step, a surface roughness (Ra) of less than 1 μm is obtained. There is an advantage that can be.
マンガン鋼パイプを材料として用いて製作されるマンガン鋼製容器は、徹底的な内面処理工程を経ても、極めて微細な隙間の中に付いている水分や粒子などの不純物を完璧に除去することが難しく、隙間の内部表面に露出している遊離（isolated）鉄成分などと三フッ化窒素との反応によりフッ化鉄が生成される上、生成されたフッ化鉄が触媒作用してＮＦ３の分解をさらに加速化させることによりＮ２Ｏ又は酸性成分が増加する。
これに対し、本発明におけるように、クロム−モリブデン鋼板を主材料としてＤＤＩ工法で製造した容器の場合、鉄板の圧縮成形過程で鋼板内部の組織が極めて緻密になって鉄成分の焼結（Sintering）などの現象が現われ、内面処理工程を経なくても表面が均一かつ清浄な形状になる。このような特性は、マンガン鋼より表面の隙間など微細空間が減少して内面の不純物の除去が容易になる上、遊離鉄と微量不純物の量が減少することによりＮＦ３ガスの分解が抑えられるためであると推定される。
以下、実施例を挙げて本発明を具体的に説明する。
Manganese steel containers manufactured using manganese steel pipes can completely remove impurities such as moisture and particles in extremely fine gaps even after a thorough internal surface treatment process. It is difficult, and iron fluoride is generated by the reaction of isolated iron component exposed on the inner surface of the gap with nitrogen trifluoride, and the generated iron fluoride catalyzes the action of NF 3 By further accelerating the decomposition, N 2 O or acidic components are increased.
On the other hand, as in the present invention, in the case of a container manufactured by the DDI method using a chromium-molybdenum steel plate as a main material, the structure inside the steel plate becomes very dense during the compression molding process of the iron plate and the iron component is sintered (Sintering ) And the like appear, and the surface becomes uniform and clean without going through the inner surface treatment process. Such characteristics make it easier to remove impurities on the inner surface by reducing the fine space such as the gap between the surfaces than manganese steel, and also suppresses the decomposition of NF 3 gas by reducing the amount of free iron and trace impurities. It is presumed that.
Hereinafter, the present invention will be specifically described with reference to examples.
溶融塩状態の酸性フッ化アンモニウムの中にアンモニアとフッ素をガス状態で供給して不純物含有ＮＦ３ガスを製造し、このガスから精製工程を経て低温の液状高純度ＮＦ３を製造して貯蔵容器に気（液）体状態で受け取った。受け取ったＮＦ３ガスをマンガン鋼製充填容器とＤＤＩ工法で製造されたクロム−モリブデン鋼製充填容器にそれぞれ２０ｋｇずつ充填し、充填容器を常温に放置した後、時間経過によるＮＦ３ガスのｐＨの変化を測定した。
ここで、マンガン鋼製容器は、マンガン含量１．５ｗｔ％の容器を使用し、クロム−モリブデン鋼製容器は、クロム含量１．５ｗｔ％、モリブデン含量０．５ｗｔ％の容器を使用した。ガスクロマトグラフ（Ｖａｌｃｏ社製、ＰＤＤ検出器）を用いてＮ２Ｏを分析した。
ＨＮＯ３分析は、ＮａＯＨを用いる中和滴定により総酸度を測定し、その総酸度の値からＨＦの量を差し引いた値をＨＮＯ３の量として換算することにより行った。ＨＦの量は、Ｆイオン分析器を用いて分析し、ＨＮＯ３の存在は、硫酸及びＦｅＳＯ４を用いてCS２及びKI液を加え、希硫酸酸性液中でCS２層の色相が紫色に変化する陰イオン定性分析により確認した。
その結果を、表１及び表２に示した。
表１において、粗さは容器の内面粗さ（Ｒａ）を意味する。
Ammonia and fluorine are supplied in a gaseous state to ammonium acid fluoride in a molten salt state to produce an impurity-containing NF 3 gas, and a low temperature liquid high-purity NF 3 is produced from this gas through a purification process, and a storage container I received it in the state of gas (liquid). The received NF 3 gas was filled in 20 kg each into a manganese steel filling container and a chromium-molybdenum steel filling container produced by the DDI method, and after the standing of the filling container at room temperature, the pH of the NF 3 gas over time Changes were measured.
Here, the manganese steel container was a container having a manganese content of 1.5 wt%, and the chromium-molybdenum steel container was a container having a chromium content of 1.5 wt% and a molybdenum content of 0.5 wt%. N 2 O was analyzed using a gas chromatograph (Valco, PDD detector).
The HNO 3 analysis was performed by measuring the total acidity by neutralization titration using NaOH, and converting the value obtained by subtracting the amount of HF from the value of the total acidity as the amount of HNO 3 . The amount of HF is analyzed using an F ion analyzer, and the presence of HNO 3 is obtained by adding CS 2 and KI solution using sulfuric acid and FeSO 4 , and the hue of CS 2 layer becomes purple in dilute sulfuric acid acidic solution. Confirmed by changing anion qualitative analysis.
The results are shown in Tables 1 and 2.
In Table 1, the roughness means the inner surface roughness (Ra) of the container.
マンガン鋼で製作した充填容器では、時間が経過すると酸成分が検知されるが、これに対し、クロム−モリブデン鋼で製作した充填容器では、２年以上の時間を置いて測定しても何の変化も認められなかった。
一方、マンガン鋼で製作した容器の場合、内部粗さを１０μｍ以下にまで研磨した貯蔵容器では、ＮＦ３ガスの分解の程度は、内部粗さ２５μｍ以上の容器に貯蔵されたガスよりさらに少なかったが、ＤＤＩ工法で製作されたクロム−モリブデン鋼貯蔵容器よりは多かった。
また、表２のように貯蔵容器内のガス成分を分析した結果、マンガン鋼で作製した充填容器に充填されたＮＦ３ガスの場合、硝酸とフッ酸の量が多少増加し、これによりｐＨ低下することが確認された。
実際、容器内のＮＦ３ガス中に含まれるＮ２Ｏ量もマンガン鋼の貯蔵容器では時間とともに増加する傾向を示したが、クロム−モリブデンのＤＤＩ工法で製作された貯蔵容器に充填されたＮＦ３ガスでは、時間をおいても殆ど変わらずＮＦ３ガスは高純度を維持することを確認することができた。
本発明のＮＦ３ガスを充填して貯蔵する容器としては、クロム含量１．５〜２．０ｗｔ％、モリブデン含量０．２〜０．５ｗｔ％のクロム−モリブデン鋼のDDI工法で製作された容器が適することが明らかになった。
In packed containers made of manganese steel, acid components are detected over time, whereas in filled containers made of chrome-molybdenum steel, no matter what the measurement takes over two years. No change was observed.
On the other hand, in the case of a container made of manganese steel, in a storage container whose internal roughness is polished to 10 μm or less, the degree of decomposition of NF 3 gas was even less than the gas stored in a container having an internal roughness of 25 μm or more. However, it was more than the chromium-molybdenum steel storage container manufactured by the DDI method.
In addition, as a result of analyzing the gas components in the storage container as shown in Table 2, in the case of NF 3 gas filled in a filling container made of manganese steel, the amount of nitric acid and hydrofluoric acid slightly increased, thereby lowering the pH Confirmed to do.
In fact, the amount of N 2 O contained in the NF 3 gas in the container also tended to increase with time in the manganese steel storage container, but the NF filled in the storage container manufactured by the chromium-molybdenum DDI method was used. With 3 gases, it was confirmed that the NF 3 gas maintained high purity with little change over time.
As a container for filling and storing the NF 3 gas of the present invention, a container manufactured by the DDI method of chromium-molybdenum steel having a chromium content of 1.5 to 2.0 wt% and a molybdenum content of 0.2 to 0.5 wt%. Was found to be suitable.
Claims (2)
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| KR1020050050668A KR100660444B1 (en) | 2005-06-14 | 2005-06-14 | Storage method of Nitrogen trifluoride |
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| US (1) | US20060280642A1 (en) |
| JP (1) | JP2006349171A (en) |
| KR (1) | KR100660444B1 (en) |
| CN (1) | CN100460745C (en) |
| DE (1) | DE102005060954B4 (en) |
| IT (1) | ITBO20060030A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000257795A (en) * | 1999-03-10 | 2000-09-19 | Mitsui Chemicals Inc | Inner surface treatment method of high pressure gas container |
| JP3107715U (en) * | 2004-09-13 | 2005-02-03 | 中国工業株式会社 | High pressure gas container |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE737556C (en) * | 1935-01-06 | 1943-07-19 | Hoesch Ag | Chromium-molybdenum-iron alloy for corrosion-resistant objects, the production of which requires a high level of deep-drawing ability |
| US4578113A (en) * | 1983-05-19 | 1986-03-25 | Union Carbide Corporation | High strength steel |
| US5133928A (en) * | 1989-10-28 | 1992-07-28 | Chesterfield Cylinders Limited | Cylinder body of a steel composition |
| JP2927914B2 (en) * | 1990-08-31 | 1999-07-28 | 三井化学株式会社 | Method for producing nitrogen trifluoride gas |
| JP3068216B2 (en) * | 1990-12-28 | 2000-07-24 | 東北特殊鋼株式会社 | High cold forging electromagnetic stainless steel |
| JP2933826B2 (en) * | 1994-07-05 | 1999-08-16 | 川崎製鉄株式会社 | Chromium steel sheet excellent in deep drawing formability and secondary work brittleness and method for producing the same |
| TW336257B (en) * | 1996-01-30 | 1998-07-11 | Daido Hoxan Inc | A method of carburizing austenitic stainless steel and austenitic stainless steel products obtained thereby |
| DE10158258B4 (en) * | 2000-11-30 | 2012-08-23 | Hyundai Motor Co. | Shift control method for an automatic transmission of a vehicle |
| RU2182556C1 (en) * | 2001-09-28 | 2002-05-20 | Зао "Астор-Электроникс" | Method of obtaining nitrogen trifluoride |
| KR100428906B1 (en) * | 2001-11-05 | 2004-04-29 | 주식회사 소디프신소재 | Method for preparing of filling cylinder of highly pure nitrogen trifluoride(nf3) by treating the inner side of filling cylinder and filling cylinder prepared by the method |
| JP2003232495A (en) * | 2002-02-07 | 2003-08-22 | Mitsui Chemicals Inc | Charged high-purity high-pressure gas |
| ES2276047T3 (en) * | 2002-02-15 | 2007-06-16 | Benteler Automobiltechnik Gmbh | USE OF A STEEL ALLOY AS A PIPE MATERIAL FOR THE MANUFACTURE OF PRESSURE GAS CONTAINERS OR AS A MATERIAL FOR THE MANUFACTURE OF MOLDED PIECES IN STEEL LIGHT STRUCTURES. |
| JP3816841B2 (en) * | 2002-06-25 | 2006-08-30 | 日本パイオニクス株式会社 | Purifying agent and purifying method for gas containing nitrogen fluoride |
-
2005
- 2005-06-14 KR KR1020050050668A patent/KR100660444B1/en active IP Right Grant
- 2005-11-25 CN CNB2005100482999A patent/CN100460745C/en not_active Expired - Fee Related
- 2005-12-05 US US11/293,782 patent/US20060280642A1/en not_active Abandoned
- 2005-12-20 DE DE102005060954A patent/DE102005060954B4/en not_active Expired - Fee Related
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- 2006-01-17 IT IT000030A patent/ITBO20060030A1/en unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000257795A (en) * | 1999-03-10 | 2000-09-19 | Mitsui Chemicals Inc | Inner surface treatment method of high pressure gas container |
| JP3107715U (en) * | 2004-09-13 | 2005-02-03 | 中国工業株式会社 | High pressure gas container |
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| KR20060130281A (en) | 2006-12-19 |
| KR100660444B1 (en) | 2006-12-22 |
| DE102005060954A1 (en) | 2006-12-28 |
| ITBO20060030A1 (en) | 2006-12-15 |
| CN100460745C (en) | 2009-02-11 |
| CN1880830A (en) | 2006-12-20 |
| DE102005060954B4 (en) | 2008-07-31 |
| US20060280642A1 (en) | 2006-12-14 |
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