JPS6358153A - Method for measuring minute amount of oxygen in molten metal in vacuum - Google Patents
Method for measuring minute amount of oxygen in molten metal in vacuumInfo
- Publication number
- JPS6358153A JPS6358153A JP61200003A JP20000386A JPS6358153A JP S6358153 A JPS6358153 A JP S6358153A JP 61200003 A JP61200003 A JP 61200003A JP 20000386 A JP20000386 A JP 20000386A JP S6358153 A JPS6358153 A JP S6358153A
- Authority
- JP
- Japan
- Prior art keywords
- vacuum
- tube
- oxygen
- molten metal
- standard electrode
- 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.)
- Pending
Links
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 20
- 239000001301 oxygen Substances 0.000 title claims abstract description 20
- 239000002184 metal Substances 0.000 title claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 8
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 8
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004568 cement Substances 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
見訓勿技権分災
本発明は、真空中の溶融金属中の微量酸素を測定する方
法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for measuring trace amounts of oxygen in molten metal in vacuum.
見訓夏従来技秀
現在、溶融金属中の酸素濃度を測定する方法として、ジ
ルコニア固体電解質からなる酸素センサが、用いられて
いる。例えば、溶融金属中の酸素は、特開昭５６−７７
７５２号のごとく、ジルコニア固体電解質を用いたもの
が、使用されている。Currently, an oxygen sensor made of a zirconia solid electrolyte is used as a method for measuring the oxygen concentration in molten metal. For example, oxygen in molten metal is
No. 752 uses a zirconia solid electrolyte.
しかし、これらは、真空中での溶融金属中の酸素濃度を
測定するものではなく、真空中での前記微量の酸素濃度
を測定する方法は、何ら開示されていない。However, these do not measure the oxygen concentration in molten metal in vacuum, and no method for measuring the minute amount of oxygen concentration in vacuum is disclosed.
本発明者等は、上記真空中での微量酸素濃度を計測する
方法として、以下の発明をなした。The present inventors have made the following invention as a method for measuring the trace oxygen concentration in a vacuum.
光：ｔへ構−戊
即ち、本発明は、固体電解質からなるタンマン管の内壁
の界面が、外気の影響を受けないように、ガラスシール
を標準極の上部に配置することを特徴とする真空中の溶
融金属中の微量酸素を測定する方法に関する。In other words, the present invention is a vacuum system characterized in that a glass seal is placed above the standard electrode so that the interface of the inner wall of the Tammann tube made of a solid electrolyte is not affected by the outside air. This invention relates to a method for measuring trace amounts of oxygen in molten metal.
９Ｌ！Ｊｌ勿退盗煎脱里
本発明の対象となる溶融金属は、鉄鋼、銅、亜鉛等及び
これらの合金の溶融状態におけるものである。9L! Molten metals to which the present invention is applied include steel, copper, zinc, etc., and alloys thereof in a molten state.
さらに、真空中下における微量の酸素についての測定方
法に関するものである。Furthermore, the present invention relates to a method for measuring trace amounts of oxygen in a vacuum.
真空とは、１Ｏ−２Ｔｏｒｒ以下の高真空までも含むも
のである。Vacuum includes even a high vacuum of 10-2 Torr or less.
さらに微量酸素とは、ｌｐｐｍ以下である。Further, trace oxygen is 1 ppm or less.
ただ、微量酸素を対象とするからと言って、１１００ｐ
ｐ前後等高濃度を測定できないということではない。However, just because the target is trace oxygen, it is 1100p.
This does not mean that high concentrations such as before and after p cannot be measured.
固体電解質は、ＺｒＯ２−Ｃａｂ、ＺｒＯ２−Ｍｇｏ等
のセラミックを用いる。ＺｒＯ□−ＣａＯの場合、Ｃａ
Ｏが１−１％前後の部分安定化ジルコニアが好ましい。As the solid electrolyte, ceramics such as ZrO2-Cab and ZrO2-Mgo are used. In the case of ZrO□-CaO, Ca
Partially stabilized zirconia with an O content of around 1-1% is preferred.
これをタンマン管状に形成し、溶融金属と接する外殻と
する。This is formed into a Tamman tube shape and serves as an outer shell that comes into contact with the molten metal.
さらに標準極としては、例えば、Ｎ ｉ −Ｎ ｉ Ｏ
粉からなるもの等を用いる。この場合、粉状の標準極を
用いるとすれば、上記タンマン管の内部に配置させるが
、タンマン管と標準極との接触を良くするため、静水圧
で加圧し、接触を良くさせることが好ましい。Furthermore, as a standard electrode, for example, N i -N i O
Use something made of powder. In this case, if a powdered standard electrode is used, it will be placed inside the Tammann tube, but in order to improve the contact between the Tammann tube and the standard electrode, it is preferable to apply hydrostatic pressure to improve the contact. .
この場合の圧は、５００〜２０００ ｋｇ／ｃＪの圧で
あることが好ましい。The pressure in this case is preferably 500 to 2000 kg/cJ.
また、標準極を通過し、タンマン管内壁に接する位置に
リード線を配置する。In addition, a lead wire is placed at a position that passes through the standard electrode and contacts the inner wall of the Tammann tube.
さらに、上記リード線と他の溶融金属中に埋め込んだ、
導線とを連結することにより、起電力を検知する。Furthermore, the above lead wire and other embedded in molten metal,
Electromotive force is detected by connecting it to a conductor.
本発明においては、特に標準極の上部にガラスシールを
することにより、固体電解質からなるタンマン管の内壁
の界面が、外気の影響を受けないようにシールすること
が重要な点である。In the present invention, it is particularly important to seal the interface of the inner wall of the Tammann tube made of solid electrolyte by placing a glass seal on the top of the standard electrode so that it is not affected by the outside air.
これにより、真空雰囲気下においても、精度の高い酸；
ａＩＡ度の検知が可能となるのである。This allows highly accurate acid even under a vacuum atmosphere;
This makes it possible to detect the degree of aIA.
本発明において得られる起電力から、計算により溶μ（
（金属中の酸素濃度を知るのである。From the electromotive force obtained in the present invention, the melt μ(
(Know the oxygen concentration in the metal.
Ｊｉ： ｌ！Ｉｊｊ、−Ｑ効−釆一
以上のように本発明を実施することにより、以下の効果
を有する。Ji: l! Ijj, -Q Effect - By carrying out the present invention as described above, the following effects can be obtained.
（］）真空雰囲気下（１０−２Ｔｏｒｒ以下）において
も大気圧下と同様に安定した測定値を得ることができる
。(]) Even under a vacuum atmosphere (10 −2 Torr or less), stable measurement values can be obtained in the same way as under atmospheric pressure.
（２）溶融金属中の１ ｐ ｐ ｍ以下の酸素濃度であ
っても精度良く、測定することができる。(2) Even oxygen concentrations of 1 ppm or less in molten metal can be measured with high accuracy.
（３）再現性においても良く、好ましい計測を持続する
ことができる。(3) Good reproducibility and favorable measurements can be maintained.
（４）対象の金属が、銅等のように低融点のものであれ
ば、使い捨てとすることなく、一定日数持続して計測す
ることができる。(4) If the target metal has a low melting point, such as copper, it can be measured continuously for a certain number of days without being disposable.
実施例
タフピッチ銅を溶解し、これを真空雰囲気下で脱酸処理
する際に、本発明の測定法を適用した。Example The measurement method of the present invention was applied to melting tough pitch copper and deoxidizing it in a vacuum atmosphere.
第１図をもって詳細に説明する。This will be explained in detail with reference to FIG.
第１図の（２）は、Ｚ ｒｏ□−１１ｍｏ Ｑ％Ｃａ○
からなるタンマン管である。この管の内側にＮ１−Ｎｊ
○粉（１）からなる標準極を設け、その上にガラスシー
ル（４）を行い、真空下でも、タンマン管内壁の界面が
、外気の影響を受けないようにする。(2) in Figure 1 is Z ro□-11mo Q%Ca○
It is a Tammann tube consisting of N1-Nj inside this tube
○A standard electrode made of powder (1) is provided, and a glass seal (4) is placed on top of it to prevent the interface of the inner wall of the Tammann tube from being affected by outside air even under vacuum.
タンマン管の内壁に接するようにｐｔからなるリード線
を設ける。このリード線と、他に配置したＭｏ線（図示
せず）と連続し、生じる起電力の変化を測定する。A lead wire made of PT is provided so as to be in contact with the inner wall of the Tammann tube. This lead wire is connected to another Mo wire (not shown), and the resulting change in electromotive force is measured.
タンマン管の上部には、アルミナ管（５）を配−４＝
置し、両者の接続部は、ジルコニアセメント（６）で接
続した。An alumina tube (5) was placed above the Tammann tube, and the connection between the two was connected with zirconia cement (6).
このようにして、真空処理された鋼中の酸素濃度を連続
して検知したが、得られた結果は、別にサンプリングし
て、分析により得られた酸素濃度と同じイ直であり、１
５０ｐｐｍから０．５ｐｐｍまで連続して正確な値を示
した。In this way, the oxygen concentration in the vacuum-treated steel was continuously detected, but the obtained results were the same as the oxygen concentration obtained by separate sampling and analysis.
Accurate values were continuously shown from 50 ppm to 0.5 ppm.
第１図は、本発明に係る酸素センサーを示す。
１は標準極、４はガラスシール、２は固体電解質を示す
。FIG. 1 shows an oxygen sensor according to the invention. 1 indicates a standard electrode, 4 indicates a glass seal, and 2 indicates a solid electrolyte.
Claims (1)
外気の影響を受けないように、ガラスシールを標準極の
上部に配置することを特徴とする真空中の溶融金属中の
微量酸素を測定する方法。(1) The interface of the inner wall of the Tammann tube made of solid electrolyte is
A method for measuring trace amounts of oxygen in molten metal in a vacuum, characterized by placing a glass seal on top of a standard electrode so as not to be affected by outside air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61200003A JPS6358153A (en) | 1986-08-28 | 1986-08-28 | Method for measuring minute amount of oxygen in molten metal in vacuum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61200003A JPS6358153A (en) | 1986-08-28 | 1986-08-28 | Method for measuring minute amount of oxygen in molten metal in vacuum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6358153A true JPS6358153A (en) | 1988-03-12 |
Family
ID=16417177
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61200003A Pending JPS6358153A (en) | 1986-08-28 | 1986-08-28 | Method for measuring minute amount of oxygen in molten metal in vacuum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6358153A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007024732A (en) * | 2005-07-19 | 2007-02-01 | Tokyo Yogyo Co Ltd | Oxygen sensor for oxygen-free copper and method for selecting oxygen sensor for copper |
| US20130042666A1 (en) * | 2011-08-17 | 2013-02-21 | Ecil Met Tec Ltda. | Immersion probe for analysis of gases in molten metal |
-
1986
- 1986-08-28 JP JP61200003A patent/JPS6358153A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007024732A (en) * | 2005-07-19 | 2007-02-01 | Tokyo Yogyo Co Ltd | Oxygen sensor for oxygen-free copper and method for selecting oxygen sensor for copper |
| JP4718264B2 (en) * | 2005-07-19 | 2011-07-06 | 東京窯業株式会社 | Oxygen sensor for oxygen-free copper |
| US20130042666A1 (en) * | 2011-08-17 | 2013-02-21 | Ecil Met Tec Ltda. | Immersion probe for analysis of gases in molten metal |
| US8833139B2 (en) * | 2011-08-17 | 2014-09-16 | Ecil Met Tec Ltda. | Immersion probe for analysis of gases in molten metal |
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