JP2009236738A - Metal specimen collection sampler and sampling method using it - Google Patents
Metal specimen collection sampler and sampling method using it Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 138
- 239000002184 metal Substances 0.000 title claims abstract description 138
- 238000005070 sampling Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005452 bending Methods 0.000 claims description 5
- 230000035939 shock Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 230000003628 erosive effect Effects 0.000 claims description 2
- 230000001112 coagulating effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 73
- 229910000831 Steel Inorganic materials 0.000 description 24
- 239000010959 steel Substances 0.000 description 24
- 238000007670 refining Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 8
- 239000002436 steel type Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052582 BN Inorganic materials 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000000275 quality assurance Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
- Treatment Of Steel In Its Molten State (AREA)
- Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
- Carbon Steel Or Casting Steel Manufacturing (AREA)
Abstract
Description
本発明は、金属の精錬過程において、工程管理を迅速、的確に行なうために金属成分を迅速に判別するのに用いる金属試料、特に、スパーク発光分光分析法、蛍光Ｘ線分析法、化学分析法による成分分析に好適な金属試料を迅速に採取するサンプラーと、そのサンプラーを用いるサンプリング方法に関するものである。 The present invention relates to a metal sample used for quickly discriminating a metal component in order to perform process control quickly and accurately in a metal refining process, in particular, spark emission spectroscopic analysis, fluorescent X-ray analysis, chemical analysis The present invention relates to a sampler that quickly collects a metal sample suitable for component analysis by, and a sampling method using the sampler.
金属の精錬過程においては、サンプラーで金属試料を採取し、分析機器で成分を分析し、金属の成分を管理または調整する。この管理・調整には、迅速・的確性が要求されるが、上記管理・調整を迅速・的確に行なうには、先ず、金属試料を迅速に採取し、迅速に分析に供する必要がある。 In the metal refining process, a metal sample is collected with a sampler, the components are analyzed with an analytical instrument, and the components of the metal are controlled or adjusted. This management / adjustment requires quickness / accuracy, but in order to perform the above-mentioned management / adjustment quickly / accurately, it is first necessary to quickly collect a metal sample and use it quickly for analysis.
従来の溶融金属試料の採取装置及び採取方法については、プローブ紙管の先端部に溶融金属を蓄積する部分が納入されており、当該プローブを溶融金属中に挿入することにより、蓋として作用していた紙部や金属箔が溶解することにより、溶融金属が試料採取容器中に自重で入り込む形（図４参照）が一般的であり、温度センサー、ガス試料採取部を併設できると言うメリットや、試料が採取成功率高く流入できる形状、材質を定義する提案が多かった。 As for the conventional molten metal sample collection device and collection method, a portion for accumulating molten metal has been delivered to the tip of the probe paper tube, and it has acted as a lid by inserting the probe into the molten metal. As the paper part and metal foil are dissolved, the molten metal enters the sample collection container by its own weight (see FIG. 4), and the merit that a temperature sensor and a gas sample collection part can be provided, There were many proposals to define the shape and material that allowed the sample to flow with a high success rate.
例えば、特許文献１には、プローブ紙管の先端部に二つ割金属採取容器、石英製試料採取管、及び溶鋼中の炭素含有率を測定するための熱電対が挿入され、溶鋼の測温と試料採取を兼用する溶融金属採取プローブが提案されている。また、特許文献２には、保護管の先端に、細長いガラス製の採取容器を取り付け、その突出部分を紙製のキャップで覆うことにより、溶融金属採取成功率が高く正確な分析値を得られる溶融金属採取プローブが提案されている。 For example, in Patent Document 1, a split metal sampling container, a quartz sample sampling tube, and a thermocouple for measuring the carbon content in molten steel are inserted at the tip of the probe paper tube, and the temperature of the molten steel is measured. There has been proposed a molten metal sampling probe that is also used for sampling. Further, in Patent Document 2, a long and narrow glass collection container is attached to the tip of a protective tube, and the protruding portion is covered with a paper cap, thereby obtaining a highly accurate analysis value of the molten metal collection success rate. Molten metal sampling probes have been proposed.
また、特許文献３には、溶融金属中に含まれる水素濃度を測定するために不活性ガスを溶融金属中に吹き込み、溶融金属中の溶存水素を不活性ガス中に拡散移行させてから、不活性ガスを回収し、水素ガス濃度を測定するプローブが提案されており、不活性ガス通路と金属管との接続部位における気密性を確保するべく、金属とセラミックス用ガラス質融着剤を保護スリーブと上記金属、セラミックス間の空隙に充填して外部からバーナーで過熱溶融して、更に保護スリーブを高温から守るための可撓式断熱スリーブを取り付けた提案がなされている。 In Patent Document 3, an inert gas is blown into the molten metal in order to measure the concentration of hydrogen contained in the molten metal, and the dissolved hydrogen in the molten metal is diffused and transferred into the inert gas. A probe that collects active gas and measures the concentration of hydrogen gas has been proposed, and a protective sleeve is used to protect the glass and the glassy fusion agent for ceramics in order to ensure airtightness at the connection between the inert gas passage and the metal tube. In addition, a proposal has been made in which a gap between the metal and ceramics is filled and melted by heating with a burner from the outside, and a flexible heat insulating sleeve is attached to protect the protective sleeve from high temperatures.
しかしながら、実際に溶融金属精錬業を営む現場においては、溶融金属を採取したくても、回りの精錬制御装置の立体障害を受けるため、プローブ紙管の先端に溶融金属採取容器を付属させただけの直線的な型式では溶融金属を採取できない場所が数多く存在するという問題点があった。 However, at the site where the molten metal refining industry actually operates, even if it wants to collect molten metal, it suffers from the steric hindrance of the surrounding refining control device, so only a molten metal collection container is attached to the tip of the probe paper tube. However, there is a problem that there are many places where molten metal cannot be collected.
更には、従来の紙管プローブ法は、溶融金属の中にプローブ先端を挿入した後、溶融金属が自らの自重で溶融金属採取容器の空間内に入り込んでくる力のみで溶融金属を挿入せしめているため、浸漬深さを稼げない場合には、内部まで溶融金属が入り込まず、試料形状不良となり精錬制御操業に遅延をきたす一因となっていた。 Furthermore, in the conventional paper tube probe method, after inserting the probe tip into the molten metal, the molten metal is inserted only by the force that the molten metal enters into the space of the molten metal collection container by its own weight. Therefore, when the immersion depth cannot be obtained, the molten metal does not enter the interior, and the sample shape becomes defective, which is a cause of delay in the refining control operation.
水素ガス濃度を測定するプローブの案は気密性を確保するために多大なコストと部品を使用する必要があり、繰返し分析には向かず、また、実際に品質保証に必須となる溶融金属をサンプリングできる構成は提案されていない。 The proposed probe for measuring the hydrogen gas concentration requires a great deal of cost and parts to ensure airtightness, is not suitable for repeated analysis, and actually samples the molten metal that is essential for quality assurance. A possible configuration has not been proposed.
しかし、近年の金属の精錬工程においては、成分管理・調整を迅速、的確に行なうことは不可欠のことであり、そのため、立体障害があるような場所からの溶融金属サンプリングを、迅速かつ、確実に採取できることが強く望まれている。 However, in recent metal refining processes, it is indispensable to perform component management / adjustment quickly and accurately. Therefore, sampling of molten metal from places with steric hindrance can be performed quickly and reliably. It is highly desired that it can be collected.
そこで、本発明は、このような問題に鑑みてなされたもので、その目的は、溶融金属採取場所の制約に影響を受けずに、成分分析に直ちに供し得る試料を採取することが可能な、新規かつ改良された金属試料迅速採取サンプラー及びそれを用いる迅速サンプリング方法を提供することにある。 Therefore, the present invention has been made in view of such problems, the purpose of which is not affected by the restrictions of the molten metal collection location, it is possible to collect a sample that can be immediately used for component analysis, It is an object of the present invention to provide a new and improved metal sample rapid sampling sampler and a rapid sampling method using the same.
本発明は、上述の問題を解決するためになされたものであり、その要旨は、以下のとおりである。 The present invention has been made to solve the above-described problems, and the gist thereof is as follows.
（１）溶融金属から金属試料を採取するサンプラーであって、前記溶融金属を採取して当該溶融金属を凝固させるサンプラー本体と、前記サンプラー内を真空吸引する吸引ポンプと、前記サンプラー本体と前記吸引ポンプとの間を接続し、少なくともフレキシブルパイプを含む接続部と、を備えることを特徴とする、金属試料採取サンプラー
（２）前記フレキシブルパイプが、耐熱性、耐曲げ特性、形状保持性を有し、電磁攪拌の影響を受けない材質であることを特徴とする、（１）に記載の金属試料採取サンプラー。
（３）前記フレキシブルパイプが、アルミニウム合金、ステンレス合金又は耐熱性プラスチックの少なくとも１種からなる可動型空孔管であることを特徴とする、（１）又は（２）に記載の金属試料採取サンプラー。
（４）前記サンプラー本体は、当該サンプラー本体の先端に溶融金属を吸引する中空管を更に備え、該中空管の材質が、耐熱衝撃性、耐熱性を有し、電磁力の影響を受けないものであることを特徴とする、（１）〜（３）のいずれか１項に記載の金属試料採取サンプラー。
（５）前記中空管が、石英ガラス管であることを特徴とする、（４）に記載の金属試料採取サンプラー。
（６）前記サンプラー本体は、当該サンプラー本体内の試料形成空間にガス抜き孔を有していることを特徴とする、（１）〜（５）のいずれか１項に記載の金属試料採取サンプラー。
（７）溶融金属にサンプラーを浸漬し、分析に供する金属試料を採取するサンプリング方法において、（ａ）（１）〜（６）のいずれか１項に記載の金属試料採取サンプラーを溶融金属に浸漬し、（ｂ）吸引ポンプでサンプラー内の試料形成空間に溶融金属を導き、冷却凝固させて、金属試料を形成し、（ｃ）上記サンプラーを引き上げて冷却した後、サンプラー本体から試料形成空間を剥離して、溶融金属凝固サンプルを得て、研磨、分析に供することを特徴とするサンプリング方法。
（８）前記金属試料採取サンプラーを挿入する挿入口から直線では望めない位置にある前記溶融金属に、前記金属試料採取サンプラーを挿入することを特徴とする、（７）に記載の迅速サンプリング方法。
(1) A sampler for collecting a metal sample from a molten metal, the sampler body collecting the molten metal and solidifying the molten metal, a suction pump for vacuum-suctioning the sampler, the sampler body, and the suction A metal sampling sampler (2), wherein the flexible pipe has heat resistance, bending resistance characteristics, and shape retention. The metal sampling sampler according to (1), characterized in that it is a material that is not affected by electromagnetic stirring.
(3) The metal sampling sampler according to (1) or (2), wherein the flexible pipe is a movable hole tube made of at least one of an aluminum alloy, a stainless alloy, or a heat-resistant plastic. .
(4) The sampler body further includes a hollow tube for sucking molten metal at the tip of the sampler body, and the material of the hollow tube has thermal shock resistance and heat resistance, and is affected by electromagnetic force. The metal sampling sampler according to any one of (1) to (3), wherein the sampler is not provided.
(5) The metal sample collection sampler according to (4), wherein the hollow tube is a quartz glass tube.
(6) The metal sample collection sampler according to any one of (1) to (5), wherein the sampler body has a gas vent hole in a sample formation space in the sampler body. .
(7) In a sampling method in which a sampler is immersed in molten metal and a metal sample is collected for analysis, (a) the metal sample sampling sampler according to any one of (1) to (6) is immersed in the molten metal (B) The molten metal is guided to the sample formation space in the sampler with a suction pump, and cooled and solidified to form a metal sample. A sampling method characterized by peeling and obtaining a molten metal solidified sample, and subjecting it to polishing and analysis.
(8) The rapid sampling method according to (7), wherein the metal sample collection sampler is inserted into the molten metal at a position that cannot be expected in a straight line from an insertion port through which the metal sample collection sampler is inserted.
本発明によれば、従来、直管のサンプラーでは、溶融金属採取が不可能であった立体障害の多い場所でも容易にサンプル採取が可能となった。 According to the present invention, it has become possible to easily collect a sample even in a place where there is a large amount of steric hindrance where it has been impossible to collect a molten metal with a straight pipe sampler.
また、サンプラーを溶融金属に浸漬させるだけでは自重で溶融金属を試料室に採取する力が不足していることを補うために、サンプラー紙管の内部を真空引きにすることにより、強制的にサンプル採取を行い、採取成功率飛躍的に高めることが可能となった。 Also, in order to compensate for the lack of force to collect molten metal in the sample chamber by its own weight simply by immersing the sampler in the molten metal, the sampler is forcibly sampled by evacuating the inside of the sampler paper tube. It was possible to increase the success rate of collection.
このように、本発明は、精錬工程における成分管理・調整において、顕著な効果をもたらすものである。したがって、本発明は、産業上の価値が極めて高いものである。 Thus, this invention brings about a remarkable effect in the component management and adjustment in a refining process. Therefore, the present invention has extremely high industrial value.
以下に添付図面を参照しながら、本発明の好適な実施の形態について詳細に説明する。なお、本明細書及び図面において、実質的に同一の機能構成を有する構成要素については、同一の符号を付することにより重複説明を省略する。 Exemplary embodiments of the present invention will be described below in detail with reference to the accompanying drawings. In addition, in this specification and drawing, about the component which has the substantially same function structure, duplication description is abbreviate | omitted by attaching | subjecting the same code | symbol.
発明者は、従来の溶融金属サンプラーが、例えばＲＨ二次精錬工程や、ＴＤ鋳込み工程での自動サンプリングに特化されたあまりに、溶融金属サンプラーの形状がプローブ紙管１２のストレートタイプから変化していないことに気付いた。そのため、ストレートタイプでは立体障害部に挿入できないという問題点を回避するために、サンプラー中央部を自由に折り曲げることができるフレキシブルパイプに変更することで課題を解決した。 The inventor indicated that the shape of the molten metal sampler has not changed from the straight type of the probe paper tube 12 because the conventional molten metal sampler is specialized in, for example, automatic sampling in the RH secondary refining process and TD casting process. I realized that. Therefore, in order to avoid the problem that the straight type cannot be inserted into the three-dimensional obstacle part, the problem has been solved by changing the central part of the sampler to a flexible pipe that can be bent freely.
また、サンプラーを溶融金属に浸漬させるだけでは自重で溶融金属を試料室１５に採取する力が不足していることに気付き、それを補うために、サンプラー紙管の内部を真空引きにすることにより、強制的にサンプル採取を行い、採取成功率を高めることを行なった。 In addition, by simply immersing the sampler in the molten metal, it is noticed that the force of collecting the molten metal into the sample chamber 15 by its own weight is insufficient, and in order to compensate for this, the inside of the sampler paper tube is evacuated. The sample was forcibly collected to increase the success rate of collection.
さらに、サンプラー紙管を溶融金属部分に直接浸漬させることにより、溶融金属そのものを汚染したりするのを防止するために、石英製チューブを先端に取り付けて、溶融金属に変動を与えることなく、迅速かつ綺麗な溶融金属を採取することにも成功した。 Furthermore, in order to prevent the molten metal itself from being contaminated by directly immersing the sampler paper tube in the molten metal part, a quartz tube is attached to the tip, so that the molten metal can be changed quickly without causing fluctuations. And we succeeded in collecting beautiful molten metal.
本発明者は、サンプラー本体と吸引ポンプとの間に設けるフレキシブルパイプの材質を実験した結果、耐熱性、耐曲げ特性、形状保持性を有し、電磁攪拌の影響を受けない材質が必要であり、アルミニウム合金、ステンレス合金、耐熱性プラスチックからなる可動型空孔管であれば、サンプリング作業時に、確実かつ安全に溶融金属を採取するための吸引用空間を保持できるフレキシブルパイプとなり得ることを明らかにした。 As a result of experimenting on the material of the flexible pipe provided between the sampler body and the suction pump, the present inventor needs a material that has heat resistance, bending resistance, shape retention, and is not affected by electromagnetic stirring. It is clear that a movable hole tube made of aluminum alloy, stainless steel, and heat-resistant plastic can be a flexible pipe that can hold a suction space for sampling molten metal reliably and safely during sampling operations did.
また、サンプラー本体先端に溶融金属を吸引する耐熱衝撃性、耐熱性を有し、電磁攪拌の影響を受けない材質の中空管の材質を替えて実験した結果、ガラス、窒化ホウ素、石英ガラス管が適していることを見出した。なお、本発明者の実験結果によれば、溶融金属が溶鋼の場合、石英ガラス中空管が好適である。 In addition, as a result of experiment with changing the material of the hollow tube that has the thermal shock resistance and heat resistance that attracts molten metal to the tip of the sampler body and is not affected by electromagnetic stirring, glass, boron nitride, quartz glass tube Found that is suitable. According to the experiment results of the present inventors, when the molten metal is molten steel, a quartz glass hollow tube is suitable.
以下、上記知見を踏まえながら、本発明に係る金属試料迅速採取サンプラー及び迅速サンプリング方法について、詳細に説明する。 The metal sample rapid sampling sampler and rapid sampling method according to the present invention will be described in detail below based on the above findings.
本発明の第１の実施形態に係る金属試料迅速採取サンプラーは、溶融金属から金属試料を採取するサンプラーであって、溶融金属を急冷凝固するサンプラー本体と、サンプラー本体内を真空吸引できる吸引ポンプと、サンプラー本体と吸引ポンプとの間を接続し、少なくともフレキシブルパイプを含む接続部と、を備えることを基本思想とする。 A metal sample rapid collection sampler according to the first embodiment of the present invention is a sampler that collects a metal sample from molten metal, a sampler body that rapidly solidifies the molten metal, and a suction pump that can vacuum-suck the sampler body. The basic idea is to connect the sampler body and the suction pump, and to include a connection portion including at least a flexible pipe.
図１に、上記金属試料迅速採取サンプラーの一態様を示す。図１に示すように、金属試料迅速採取サンプラーは、吸引ポンプ引手１、吸引開始レバー２、吸引ポンプ本体３、中空パイプ４、軸受筒５、フレキシブルパイプ６、装着金具７、紙管８、試料採取容器９及び試料採取パイプ１０によって構成されている。ここで、中空パイプ４、軸受筒５、フレキシブルパイプ６及び装着金具７が、上述の接続部に対応し、紙管８、試料採取容器９及び試料採取パイプ１０が、上述のサンプラー本体に対応する。 FIG. 1 shows an embodiment of the metal sample rapid collection sampler. As shown in FIG. 1, the metal sample quick sampling sampler includes a suction pump handle 1, a suction start lever 2, a suction pump body 3, a hollow pipe 4, a bearing cylinder 5, a flexible pipe 6, a mounting bracket 7, a paper tube 8, and a sample. A sampling container 9 and a sampling pipe 10 are used. Here, the hollow pipe 4, the bearing cylinder 5, the flexible pipe 6 and the mounting bracket 7 correspond to the above-described connecting portion, and the paper tube 8, the sampling container 9, and the sampling pipe 10 correspond to the above-described sampler body. .
吸引ポンプ引手１および吸引開始レバー２が設けられた吸引ポンプ本体３は、接続部を介してサンプラー本体内を真空吸引して、サンプラー本体内を低圧にする装置である。図１に示したように、吸引ポンプ本体３には中空パイプ４が接続されており、中空パイプ４の吸引ポンプ本体３に接続されていない端部には、軸受筒５を介してフレキシブルパイプ６が接続されている。フレキシブルパイプ６の他端には、軸受筒５を介して、サンプラー本体にフレキシブルパイプ６を接続するための装着金具７が接続されている。ここで、フレキシブルパイプ６は、上述のように軸受筒５を介して装着金具７に接続されていてもよく、フレキシブルパイプ６の他端に更に中空パイプが接続され、この中空パイプに装着金具７が接続されていてもよい。装着金具７は、試料採集容器９及び試料採取パイプ１０が設けられた紙管８に差し込まれる。 The suction pump main body 3 provided with the suction pump puller 1 and the suction start lever 2 is a device that evacuates the inside of the sampler main body through a connecting portion to lower the inside of the sampler main body. As shown in FIG. 1, a hollow pipe 4 is connected to the suction pump main body 3, and a flexible pipe 6 is connected to the end of the hollow pipe 4 not connected to the suction pump main body 3 via a bearing cylinder 5. Is connected. A mounting fitting 7 for connecting the flexible pipe 6 to the sampler body is connected to the other end of the flexible pipe 6 via the bearing cylinder 5. Here, the flexible pipe 6 may be connected to the mounting bracket 7 through the bearing cylinder 5 as described above, and a hollow pipe is further connected to the other end of the flexible pipe 6, and the mounting bracket 7 is connected to the hollow pipe. May be connected. The mounting bracket 7 is inserted into a paper tube 8 provided with a sample collection container 9 and a sample collection pipe 10.
ここで、試料採取容器９の構造については、一般的に利用されているような左右一対の半割りサンプルケースの中に、溶融金属を引き入れる流入路と空気抜け穴をもった、コイン状金属試料を得るような試料採取容器等を設置することができる。更に、発明者が特許文献４で示したような、溶融金属から金属試料を採取するサンプルケース体が、ケース体に設けた流入路から侵入してくる溶融金属を急冷凝固せしめる偏平な試料採取空間を一側面に備える左右１対の半割サンプルケースと、上記左右１対の半割サンプルケースの間に在って上記試料採取空間を区分し、サンプルケース体内に左右１対の試料採取空間を形成する溶融金属をはじく材質の空間分割板と、を備える試料採取ケースを用いると、従来の金属試料採取ケースに比べてより迅速な急冷凝固による迅速性の確保と試料の採取ミスを防止することが可能となる。 Here, regarding the structure of the sample collection container 9, a coin-shaped metal sample having an inflow path for drawing molten metal and an air vent hole in a pair of left and right halved sample cases as generally used is used. A sample collection container or the like can be installed. Further, as shown in Patent Document 4, the sample case body for collecting a metal sample from the molten metal is a flat sample collection space in which the molten metal entering from the inflow passage provided in the case body is rapidly cooled and solidified. The sample collection space is divided between a pair of left and right halved sample cases and a pair of left and right halved sample cases, and a pair of left and right sample collection spaces are provided in the sample case. Using a sampling case with a space dividing plate made of a material that repels the molten metal to be formed ensures quickness by rapid solidification and prevents sample sampling errors compared to conventional metal sampling cases. Is possible.
ここで、試料採取容器９は、溶融金属を的確に急冷凝固させ、均一な凝固組織を有する金属試料を得るために、抜熱能力に優れた材料で構成することが好ましい。抜熱能力に優れた材料として、例えば、鉄、鋼、アルミニウム、銅及びステンレス鋼のいずれか１種又は２種以上からなる材料を用いることが可能である。 Here, it is preferable that the sample collection container 9 is made of a material having an excellent heat removal capability in order to accurately and rapidly solidify the molten metal and obtain a metal sample having a uniform solidified structure. As a material excellent in heat removal capability, for example, a material composed of one or more of iron, steel, aluminum, copper, and stainless steel can be used.
まず、吸引ポンプ引手１を引き上げることにより、吸引ポンプ本体３の内部空間を低圧状態にしておく。次に、吸引ポンプの先端にある装着金具７を、紙管８に差し込むことにより接続され、かつ脱着が可能なように構成し、吸引準備が完了する。 First, the internal space of the suction pump body 3 is kept in a low pressure state by pulling up the suction pump handle 1. Next, the mounting bracket 7 at the tip of the suction pump is connected to the paper tube 8 so that it can be connected and detached, and preparation for suction is completed.
実際の溶融金属、例えば、溶鋼を採取する現場においては、その場、その場において、どのような立体障害があるのかにより、フレキシブルパイプ６の折り曲げ角度を変更する。フレキシブルパイプの折り曲げ角度は、採取時点で、溶鋼表面のパウダー層を突き抜ける深さと角度を計算した上で、予め手で折り曲げて調整しておき、複数回、同じ場所でサンプル採取テストを行っておくと、次回から固定したサンプル角度で、成功率高く、サンプルを採取することが可能となる。なお、紙管８の長さについては、余り長過ぎると溶鋼差込み部での立体障害となり易いため、できる限りコンパクトに長さや直径を小さくしておくことが望ましく、試料採取空間を確保できる最小限の長さであることが好ましい。 At the site where an actual molten metal, for example, molten steel is collected, the bending angle of the flexible pipe 6 is changed depending on the steric hindrance on the spot. The bending angle of the flexible pipe is calculated by calculating the depth and angle that penetrates the powder layer on the surface of the molten steel at the time of sampling. From the next time, it becomes possible to collect a sample at a fixed sample angle with a high success rate. As for the length of the paper tube 8, if it is too long, it is likely to cause a steric hindrance at the molten steel insertion portion. Therefore, it is desirable to make the length and diameter as small as possible, and to minimize the sampling space. It is preferable that it is the length of.
更に、どうしてもモールド上でフレキシブルパイプを折り曲げる必要があるような場所においては、フレキシブルパイプ本体を任意の角度に曲げて、溶鋼を採取し、その後に元の角度に戻すことができるような遠隔駆動部をパイプ中間から先端部分に備えることも可能である。 Furthermore, in places where it is necessary to bend the flexible pipe on the mold, a remote drive unit that can bend the flexible pipe body to an arbitrary angle, collect molten steel, and then return to the original angle. It is also possible to provide at the tip part from the middle of the pipe.
フレキシブルパイプ本体は、１５００℃近い溶鋼が直接通過する部分ではないものの、耐熱衝撃性、耐熱性等の高温箇所で使用する上での基本的特性が必要であり、低圧にした吸引ポンプ本体へサンプラー本体の空気が通過するだけの温度に耐えること、及び、使用する製鋼現場の雰囲気温度に耐えることが必要である。このような観点から、フレキシブルパイプ本体は、高温に晒されても熱で変形し難い、例えば、アルミニウム合金、ステンレス合金、耐熱性プラスチックの少なくとも１種からなる可動型空孔管であることが望ましい。 Although the flexible pipe body is not a part through which molten steel close to 1500 ° C passes directly, it must have basic characteristics for use in high-temperature locations such as thermal shock resistance and heat resistance. It is necessary to withstand the temperature at which the air of the main body passes and to withstand the atmospheric temperature of the steelmaking site to be used. From such a viewpoint, the flexible pipe body is not easily deformed by heat even when exposed to high temperatures, and is preferably a movable hole tube made of at least one of an aluminum alloy, a stainless alloy, and a heat resistant plastic. .
次に、溶融金属上面に断熱パウダー等がある場合は、パウダー層を突き抜けるように試料採取パイプ１０を差し込み、溶融金属の内部にまで浸漬させた後に、吸引開始レバー２を押すと、吸引ポンプ本体の低圧部と中空パイプ４及びフレキシブルパイプ６と紙管８までが接続され、試料採取容器９及び試料採取パイプ１０の内部が低圧状態となる。 Next, when there is a heat insulating powder or the like on the upper surface of the molten metal, the suction pipe body is inserted by inserting the sampling pipe 10 so as to penetrate the powder layer and immersing it into the molten metal, and then pressing the suction start lever 2. Are connected to the hollow pipe 4 and the flexible pipe 6 and the paper tube 8, and the inside of the sampling container 9 and the sampling pipe 10 is in a low pressure state.
このとき、溶融金属を吸引するための試料採取パイプ１０材質も金属不純物量の少ない材質で、耐熱衝撃性、耐熱性、耐溶融金属溶損性を有すると共に、近年の精錬制御高度化のために多用される電磁撹拌による電磁力の影響を受けない材質を用いることが好ましい。そのため、少なくとも溶鋼温度１６００℃でも溶けない耐熱性が必要であり、また、常温状態から溶鋼と直接接触しても壊れないようにするため、熱膨張係数が例えば１０−６／℃程度の小さな値となっていることが好ましい。例えば、石英ガラス板の他に、ガラス、窒化ホウ素管を用い得ること、またセラミックス管の表層に高温潤滑・離型材（例えば、窒化ホウ素、シリカ、アルミナ、ジルコニア、炭化珪素等のセラミックスパウダー）を塗布した管を用いることが可能である。なお、本発明者の実験結果によれば、溶融金属が溶鋼の場合、石英ガラス（熱膨張係数：５．６×１０−７／℃）が好適である。電磁力の影響を受ける材質溶融金属が溶鋼の場合、石英ガラスが好適である。一方、鉄等の磁性体を用いた場合、鋳型内に挿入する時点で磁場の影響を受け所望の部位に浸漬することができなくなるため、好ましくない。 At this time, the material of the sampling pipe 10 for sucking the molten metal is also a material having a small amount of metal impurities, and has thermal shock resistance, heat resistance, and resistance to molten metal erosion, and for the advancement of refining control in recent years. It is preferable to use a material that is not affected by electromagnetic force caused by electromagnetic stirring that is frequently used. Therefore, heat resistance that does not melt at least at a molten steel temperature of 1600 ° C. is necessary, and in order to prevent breakage even when directly in contact with molten steel from room temperature, the thermal expansion coefficient is a small value of about 10 −6 / ° C., for example. It is preferable that For example, in addition to quartz glass plates, glass and boron nitride tubes can be used, and high temperature lubrication / release materials (for example, ceramic powders such as boron nitride, silica, alumina, zirconia, silicon carbide) are used on the surface of the ceramic tube. It is possible to use a coated tube. According to the experiment results of the present inventors, when the molten metal is molten steel, quartz glass (thermal expansion coefficient: 5.6 × 10 −7 / ° C.) is suitable. When the molten metal affected by electromagnetic force is molten steel, quartz glass is preferred. On the other hand, when a magnetic material such as iron is used, it is not preferable because it cannot be immersed in a desired site under the influence of a magnetic field when inserted into the mold.
低圧状態の試料採取パイプ１０を通じて溶融金属が引きずり込まれ、試料採取容器９の二つ割急冷凝固空隙にて急冷凝固される。このとき試料採取容器９にはガス抜きのための穴を二つ以上設けておくことにより、上記低圧吸引を容易にする作用が生まれる。 Molten metal is drawn through the low-pressure sampling pipe 10 and rapidly solidified in the two-part rapid cooling solidification gap of the sampling container 9. At this time, the sample collection container 9 is provided with two or more holes for venting the gas, so that the low-pressure suction is facilitated.
紙管サンプラー本体に溶融金属を真空吸引した後は、紙管サンプラーを溶融金属から引き出し、別の場所で、紙管サンプラー本体８を空冷、もしくは水冷することにより金属を低温まで冷却する。 After the molten metal is vacuum-sucked into the paper tube sampler body, the paper tube sampler is pulled out from the molten metal, and the metal is cooled to a low temperature by cooling the paper tube sampler body 8 with air or water at another location.
その後、試料採取容器９内部の二つ割急冷凝固空隙を外し、溶融金属の凝固試料を得たら、通常の研磨作業を行い、発光分析、蛍光Ｘ線分析に供する。また、切り粉試料を採取して、化学分析に供することもできる。 Thereafter, the 20% rapidly cooled solidification gap inside the sampling container 9 is removed, and when a solidified sample of molten metal is obtained, a normal polishing operation is performed and it is subjected to emission analysis and fluorescent X-ray analysis. It is also possible to collect a chip sample for chemical analysis.
上記サンプラーの中でフレキシブルパイプ６の長さは、長過ぎると自重を支えきれず垂れ下がってしまう可能性があり、逆に短過ぎると柔軟性が得られないため、臨む場所のサンプリングが不可能となってしまう。そのため、フレキシブルパイプの長さは、１ｃｍから２００ｃｍほどの間に収めるのが良い。 If the length of the flexible pipe 6 in the sampler is too long, it may not be able to support its own weight and may hang down. On the other hand, if it is too short, the flexibility cannot be obtained. turn into. Therefore, it is preferable that the length of the flexible pipe be within a range of 1 cm to 200 cm.
次に、試料採取パイプ１０の長さについて検討した結果、短過ぎると溶鋼表層のパウダーを巻き込んでしまい、サンプリング不良となるため、最低限でも表層パウダー層を完全に貫通する長さ以上が必須である。例えば、厚さ１０ｃｍのパウダー層に斜め４５度の角度で進入させた場合は１５ｃｍ以上の長さが必要となる。一方、長過ぎる場合には、サンプラー先端を挿入するときに立体障害となる可能性が高くなる弊害が発生する。そのため、表層パウダー層等の不要部分を貫通させた後、長くて２０ｃｍ以内、好ましくは１０ｃｍ以内に止めることが、作業性を良好にして良質の溶融金属を採取できる条件となる。 Next, as a result of examining the length of the sampling pipe 10, if the length is too short, the powder on the surface of the molten steel is entrained, resulting in poor sampling. Therefore, at least the length that completely penetrates the surface powder layer is essential. is there. For example, when entering a 10 cm thick powder layer at an angle of 45 degrees, a length of 15 cm or more is required. On the other hand, if it is too long, there is a problem that the possibility of steric hindrance increases when the sampler tip is inserted. Therefore, after making unnecessary parts, such as a surface powder layer, penetrate, it is long and within 20 cm, preferably within 10 cm, which is a condition for improving workability and collecting good quality molten metal.
次に、本発明の実施例について説明するが、本発明は、実施例で採用した条件に限定されるものではない。 Next, examples of the present invention will be described, but the present invention is not limited to the conditions employed in the examples.
図１に示す構造のサンプラーを作製し、図２に示すように立体障害のある場所の代表として、溶鋼モールド鋳込み部にて、本実施形態に係る迅速サンプリング方法で溶鋼をサンプリングした。 A sampler having the structure shown in FIG. 1 was produced, and the molten steel was sampled by the rapid sampling method according to the present embodiment at a molten steel mold casting portion as a representative of a place having a steric hindrance as shown in FIG.
モールド部は、タンディッシュ部からモールド部に円柱状のノズルで溶鋼が挿入される。この場合、２２０ｍｍ角に１６０ｍｍφのノズルが挿入されると、実質的にサンプラーを挿入できるのは、６２ｍｍφしか許されない。また、高さ的にも２５０ｍｍ間隔しかないため、通常のストレート紙管タイプでは挿入することが実質不可能である。そのため、紙管の長さを１５５ｍｍ、直径を５０ｍｍ、試料採取パイプ先端長さを１０７ｍｍとコンパクトに設計し、後方より吸引ポンプで強制的に吸い上げることにより、溶融金属を容易に採取せしめることが可能となった。 Molten steel is inserted into the mold part from the tundish part to the mold part with a cylindrical nozzle. In this case, when a 160 mmφ nozzle is inserted in a 220 mm square, only a 62 mmφ is allowed to insert a sampler substantially. Further, since the height is only 250 mm, it is practically impossible to insert with a normal straight paper tube type. Therefore, the length of the paper tube is 155mm, the diameter is 50mm, the tip length of the sampling pipe is 107mm, and it is possible to collect the molten metal easily by forcibly sucking it up from the back with a suction pump. It became.
このサンプリング方法を用いて、タンディッシュ内の溶鋼が鋼種Ａから鋼種Ｂに移り変わる遷移状態における炭素量の変化を逐次採取、分析して評価した。その結果を図４に示す。ここで、図４において横軸は通過トン数を表しており、マイナスの値からゼロ点（リアルバウンダリー点）までが、本来、前の鋼種の溶鋼が全部通過してしまう点を示しており、ゼロ点からプラス側の値が、次に注がれた鋼種が通過したトン数を表している。左側が元々タンディッシュに挿入されていた鋼種Ａの炭素量０．２３％が徐々に高くなり、最終的には鋼種Ｂの炭素量０．３６％に移り変わる様が綺麗に採取できた。この結果より、鋼種Ａと鋼種Ｂの間で、鋼種判定上歩留落ちとなる部分を正確に判断できるようになり、異鋼種継ぎ目間の歩留落ちを最小限に留めることができるため、大幅なコスト削減に役立った。 Using this sampling method, changes in the carbon content in the transition state in which the molten steel in the tundish transitions from steel type A to steel type B were sequentially collected, analyzed, and evaluated. The result is shown in FIG. Here, the horizontal axis in FIG. 4 represents the passing tonnage, and from the negative value to the zero point (real boundary point), the point where all the molten steel of the previous steel grade originally passes. The value on the plus side from the zero point represents the tonnage through which the next poured steel grade has passed. The carbon content of steel type A, which was originally inserted in the tundish on the left side, gradually increased to 0.23%, and finally the carbon content of steel type B changed to 0.36%. From this result, it becomes possible to accurately determine the yield drop between the steel grade A and the steel grade B, and the yield drop between the different steel grade joints can be minimized. Helped to reduce costs.
このように、本実施形態に係るサンプリング方法によれば、立体障害があるような精錬制御工程においても、容易に溶融金属サンプルを採取でき、その結果から、精錬制御工程を高精度に制御でき得ることを示した。 As described above, according to the sampling method according to the present embodiment, it is possible to easily collect a molten metal sample even in a refining control process having a steric hindrance, and from the result, the refining control process can be controlled with high accuracy. Showed that.
以上、添付図面を参照しながら本発明の好適な実施形態について説明したが、本発明はかかる例に限定されないことは言うまでもない。当業者であれば、特許請求の範囲に記載された範疇内において、各種の変更例または修正例に想到し得ることは明らかであり、それらについても当然に本発明の技術的範囲に属するものと了解される。 As mentioned above, although preferred embodiment of this invention was described referring an accompanying drawing, it cannot be overemphasized that this invention is not limited to this example. It will be apparent to those skilled in the art that various changes and modifications can be made within the scope of the claims, and these are naturally within the technical scope of the present invention. Understood.
１ 吸引ポンプ引手
２ 吸引開始レバー
３ 吸引ポンプ本体
４ 中空パイプ
５ 軸受筒
６ フレキシブルパイプ
７ 装着金具
８ 紙管
９ 試料採取容器
１０ 試料採取パイプ
１１ プローブ紙管
１２ 紙管
１３ 接続ユニット
１４ 熱電対封入管
１５ 試料採取容器
１６ 耐火物
１７ 試料採取管
１８ キャップ
DESCRIPTION OF SYMBOLS 1 Suction pump handle 2 Suction start lever 3 Suction pump main body 4 Hollow pipe 5 Bearing cylinder 6 Flexible pipe 7 Mounting bracket 8 Paper tube 9 Sample collection container 10 Sample collection pipe 11 Probe paper tube 12 Paper tube 13 Connection unit 14 Thermocouple enclosure tube 15 Sampling container 16 Refractory 17 Sampling tube 18 Cap
Claims (8)
前記溶融金属を採取して当該溶融金属を凝固させるサンプラー本体と、
前記サンプラー内を真空吸引する吸引ポンプと、
前記サンプラー本体と前記吸引ポンプとの間を接続し、少なくともフレキシブルパイプを含む接続部と、
を備えることを特徴とする、金属試料採取サンプラー。 A sampler for taking a metal sample from a molten metal,
A sampler body for collecting the molten metal and solidifying the molten metal;
A suction pump for vacuum suction in the sampler;
Connecting between the sampler body and the suction pump, and including at least a flexible pipe;
A metal sampling sampler, comprising:
耐熱性、耐曲げ特性、形状保持性を有し、電磁攪拌の影響を受けない材質である
ことを特徴とする、請求項１に記載の金属試料採取サンプラー。 The flexible pipe is
2. The metal sampler sampler according to claim 1, wherein the metal sampler is a material having heat resistance, bending resistance and shape retention, and not affected by electromagnetic stirring.
アルミニウム合金、ステンレス合金又は耐熱性プラスチックの少なくとも１種からなる可動型空孔管である
ことを特徴とする、請求項１又は２に記載の金属試料採取サンプラー。 The flexible pipe is
The metal sampling sampler according to claim 1 or 2, wherein the metal sampler is a movable hole tube made of at least one of an aluminum alloy, a stainless alloy, and a heat resistant plastic.
前記中空管の材質は、耐熱衝撃性、耐熱性、耐溶融金属溶損性を有し電磁力の影響を受けないものである
ことを特徴とする、請求項１〜３のいずれか１項に記載の金属試料採取サンプラー。 The sampler body further comprises a hollow tube for sucking molten metal at the tip of the sampler body,
The material of the hollow tube has a thermal shock resistance, a heat resistance, and a molten metal erosion resistance, and is not affected by electromagnetic force. Metal sampling sampler as described in 1.
ことを特徴とする、請求項４に記載の金属試料採取サンプラー。 The metal sampling sampler according to claim 4, wherein the hollow tube is a quartz glass tube.
当該サンプラー本体内の試料形成空間にガス抜き孔を有している
ことを特徴とする、請求項１〜５のいずれか１項に記載の金属試料採取サンプラー。 The sampler body is
The metal sample collection sampler according to any one of claims 1 to 5, wherein a gas vent hole is provided in a sample formation space in the sampler body.
（ａ）請求項１〜６のいずれか１項に記載の金属試料採取サンプラーを溶融金属に浸漬し、
（ｂ）吸引ポンプでサンプラー内の試料形成空間に溶融金属を導き、冷却凝固させて、金属試料を形成し、
（ｃ）上記サンプラーを引き上げて冷却した後、溶融金属が凝固している試料形成空間をサンプラー本体から剥離して、溶融金属凝固サンプルを研磨、分析に供する
ことを特徴とする、サンプリング方法。 In a sampling method of immersing a sampler in molten metal and collecting a metal sample for analysis,
(A) Immerse the metal sampling sampler according to any one of claims 1 to 6 in molten metal,
(B) A molten metal is introduced into the sample formation space in the sampler with a suction pump, cooled and solidified to form a metal sample
(C) A sampling method, wherein after the sampler is pulled up and cooled, the sample forming space in which the molten metal is solidified is peeled off from the sampler body, and the molten metal solidified sample is polished and analyzed.
ことを特徴とする、請求項７に記載のサンプリング方法。
The sampling method according to claim 7, wherein the metal sample collection sampler is inserted into the molten metal at a position that cannot be expected in a straight line from an insertion port into which the metal sample collection sampler is inserted.
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| KR101919544B1 (en) * | 2016-12-23 | 2018-11-16 | 주식회사 포스코 | Apparstus for sampling molten |
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