CN100458433C - 测定熔融金属或熔渣中氧活度的测量装置 - Google Patents
测定熔融金属或熔渣中氧活度的测量装置 Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
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- 229910004261 CaF 2 Inorganic materials 0.000 claims 2
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Abstract
本发明涉及测定熔融金属或熔渣中氧活度的测量装置，该装置具有一个测量头，该测量头置于承载管的一端，测量头上放置一电化学测量电池。该电化学测量电池具有固态的电解质管，电解质管一端闭合，其包含闭合端处的基准物质和电极。其中电极从固态电解质管的另一端伸出。本发明还涉及相应的固态电解质管。本发明的特征在于固态电解质管的外表面具有锆酸钙和氟化物的混合物涂层。
Description
技术领域
本发明涉及测定熔融金属或熔渣中氧活度的测量装置，该装置具有一个测量头，该测量头置于承载管的一端，测量头上置有一电化学测量电池。该电化学测量电池具有一端闭合的固态电解质管，电解质管包含位于闭合端处的标准物质和电极，其中电极从固态电解质管的另一端伸出。此外，本发明还涉及用于电化学测量电池的固态电解质管。
背景技术
这类装置是已知的，如已在DE 31 52 318 C2中公开。在该文件中描述的传感器用于测量熔融金属中的氧浓度。类似的测量装置也在US3,578,578、DE28 10 134 A1或者DE 26 00 103 C2中公开。
发明内容
除了氧，还需要对熔融金属中的其它物质进行测量。因此，本发明的目的在于提供一种简单的测量装置以及相应的固态电解质管，采用该装置不仅能对氧含量进行测量，同时也能对其它元素的浓度进行测定。
该目的是通过固态电解质管的外表面具有的锆酸钙和氟化物的混合涂层来实现的。已经显示利用该涂层可测定熔融物中诸如硫、硅、或碳的浓度。该作用可这样解释：液态金属中的硫与来自于锆酸钙中的CaO反应，生成反应产物氧，然后测量固态电解质表面的氧活度变化，其值与硫相关。该测量装置可用于熔融金属或熔渣，尤其适用于测定钢或铁的熔融物中硫、硅、或碳的浓度。由此获得一种快速的测定。除了电化学测量电池外，如果该测量装置还具有温度传感器，例如热电偶，则也可测量熔融金属的温度。硅与硫含量相关。碳可通过熔融金属的硅-碳热平衡而计算得。
利用本发明的测量装置可省去实验室中的样品分析，因而大大节省了生产过程中所需的时间，进而可改进并加快生产过程。
根据本发明的有利的实施方式，氟化物优选CaF2、NaF、SrF2、BaF2、MgF2中的至少一种。化学计量的锆酸钙利于测量的高灵敏度。氟化物在锆酸钙中的重量比为2-10％，该值依据锆酸钙的颗粒结构而定。涂层厚度优选为约10～100μm，尤其优选为30μm。当使用温度越高(例如，在脱硫步骤前)时，需要的涂层越薄。这种情况下，其响应时间也越短。当使用温度越低(例如，在脱硫步骤后)时，需要的涂层越厚。则其响应时间也相应延长。
固态电解质管优选是稳定的ZrO2。涂层也可仅部分覆盖固态电解质管的外表面，其中至少涂布装有标准物质的这部分电解质管的外表面。下面参考附图对本发明的一个实施方式进行阐述。
附图说明
图1是测量装置；
图2是固态电解质管的横截面；
图3是Celox HM跟踪测量；
图4是Celox HM测量数据。
具体实施方式
图1仅显示了承载管的最初状态。该测量装置具有承载管1，其内有测量头2，其中测量头2通过接触元件3将承载管1内部与测量和数值计算装置相连的供应线相连接。
在测量头的浸入端，除了热电偶4，还有固态电解质管5。热电偶4和固态电解质管5被防护帽6包围，在测量头浸入熔融物，尤其是熔融的钢或铁之前或进入期间，该防护帽起到保护热电偶4和固态电解质管5的作用。
图2所示为固态电解质管的截面。其是由稳定的二氧化锆制备而成，内部有铬和二氧化铬混合物组成的标准物质7。在该混合物上面的填充物质8为诸如氧化铝的物质。在固态电解质管的中央置有钼棒作为电极9。电极9从固态电解质管5的开口端伸出。该开口端由帽10闭合，其中填充物质8的上端是通气的接合剂11。该固态电解质管5被钢帽12所包围，在电解质管浸入熔融金属期间，该钢帽12也起到保护电解质管的作用。然后钢帽镕化，暴露出固态电解质管5上的涂层13。该涂层优选为锆酸钙和氟化镁的混合物。
在熔融物中CaO与硫反应生成CaS，释放出氧，氧的活度可以借助于固态电解质管进行测定。
图3和图4显示了采用本发明装置进行测量的精确度，Celox S的精确度相当于试验室用的光谱测定。
Claims (10)
1.测定熔融金属或熔渣中氧活度的测量装置，该装置承载管的一端具有测量头，测量头上置有一电化学测量电池，该电化学测量电池具有一端闭合的固态电解质管，电解质管包含位于闭合端处的标准物质和电极，其中电极从固态电解质管的另一端伸出，其特征在于，固态电解质管(5)的外表面具有锆酸钙和金属氟化物的混合物涂层(13)，金属氟化物选自CaF2、NaF、SrF2、BaF2、MgF2中的至少一种。
2.根据权利要求1或2的测量装置，其特征在于，锆酸钙是化学计量的。
3.根据权利要求1所述的测量装置，其特征在于，涂层(13)的厚度为10～100μm。
4.根据权利要求1所述的测量装置，其特征在于涂层(13)仅部分覆盖固态电解质管(5)的外层。
5.用于电化学测量电池的一端闭合的固态电解质管，其特征在于，该电解质管的外表面具有锆酸钙和金属氟化物的混合物涂层(13)，金属氟化物选自CaF2、NaF、SrF2、BaF2、MgF2中的至少一种。
6.根据权利要求5的固态电解质管，其特征在于，锆酸钙是化学计量的。
7.根据权利要求5所述的固态电解质管，其特征在于，涂层(13)的厚度为10～100μm。
8.根据权利要求5所述的固态电解质管，其特征在于涂层(13)仅部分覆盖固态电解质管的外层。
9.权利要求1中的测量装置在测定熔融金属或熔渣中的硫、硅、或碳的含量中的应用。
10.权利要求1中的测量装置在测定钢或铁融融物中的硫、硅、或碳的含量中的应用。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10310387A DE10310387B3 (de) | 2003-03-07 | 2003-03-07 | Messeinrichtung zur Bestimmung der Sauerstoffaktivität in Metall- oder Schlackeschmelzen |
| DE10310387.2 | 2003-03-07 |
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| Publication Number | Publication Date |
|---|---|
| CN1527050A CN1527050A (zh) | 2004-09-08 |
| CN100458433C true CN100458433C (zh) | 2009-02-04 |
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| US (1) | US7141151B2 (zh) |
| EP (1) | EP1460416B8 (zh) |
| JP (1) | JP4054314B2 (zh) |
| KR (1) | KR100766618B1 (zh) |
| CN (1) | CN100458433C (zh) |
| AT (1) | ATE480768T1 (zh) |
| AU (1) | AU2004200389B2 (zh) |
| BR (1) | BRPI0400385B1 (zh) |
| CA (1) | CA2455467C (zh) |
| DE (2) | DE10310387B3 (zh) |
| ES (1) | ES2352182T3 (zh) |
| MX (1) | MXPA04002075A (zh) |
| PT (1) | PT1460416E (zh) |
| RU (1) | RU2282184C2 (zh) |
| TW (1) | TWI298392B (zh) |
| UA (1) | UA75693C2 (zh) |
| ZA (1) | ZA200401834B (zh) |
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| DE69824039T2 (de) | 1997-12-08 | 2005-08-18 | Lexigen Pharmaceuticals Corp., Lexington | Heterodimäre fusionsproteine zur verwendung für gezielte immuntherapie und allgemeine immunerregung |
| DE102004022763B3 (de) * | 2004-05-05 | 2005-09-15 | Heraeus Electro-Nite International N.V. | Messeinrichtung zur Bestimmung der Sauerstoffaktivität in Metall- oder Schlackeschmelzen |
| GB0421868D0 (en) * | 2004-10-01 | 2004-11-03 | Environmental Monitoring And C | Apparatus and method for measuring hydrogen concentration |
| DE102005019666B3 (de) * | 2005-04-26 | 2006-08-31 | Heraeus Electro-Nite International N.V. | Eintauchmesssonde |
| DE102005019665B3 (de) * | 2005-04-26 | 2006-08-31 | Heraeus Electro-Nite International N.V. | Eintauchmesssonde, insbesondere Einwurfmesssonde |
| DE102005060493B3 (de) * | 2005-12-15 | 2006-11-30 | Heraeus Electro-Nite International N.V. | Messsonde |
| DE102007004147A1 (de) | 2007-01-22 | 2008-07-24 | Heraeus Electro-Nite International N.V. | Verfahren zum Beeinflussen der Eigenschaften von Gusseisen sowie Sauerstoffsensor |
| GB0822734D0 (en) * | 2008-12-12 | 2009-01-21 | Environmental Monitoring And C | Method and apparatus for monitoring gas concentration |
| US8689650B2 (en) | 2009-04-28 | 2014-04-08 | Heraeus Electro-Nite Co., Llc | Immersible oxygen sensor for molten metals |
| US8806967B2 (en) * | 2009-04-28 | 2014-08-19 | Keystone Sensors, LLC | Immersible oxygen sensor for molten metals |
| RU2489711C1 (ru) * | 2011-12-26 | 2013-08-10 | Федеральное государственное бюджетное учреждение науки Институт высокотемпературной электрохимии Уральского отделения Российской Академии наук | Твердоэлектролитный датчик для измерения концентрации кислорода в газах и металлических расплавах |
| DE102012002027B4 (de) * | 2012-02-03 | 2013-09-12 | Heraeus Electro-Nite International N.V. | Messeinrichtung zur Bestimmung der Sauerstoffaktivität in Metall- oder Schlackeschmelzen |
| RU2545517C1 (ru) * | 2013-11-12 | 2015-04-10 | Открытое Акционерное Общество "Акмэ-Инжиниринг" | Ядерный реактор с жидкометаллическим теплоносителем, система для контроля термодинамической активности кислорода в таких реакторах и способ контроля термодинамической активности кислорода |
| JP6242261B2 (ja) * | 2014-03-27 | 2017-12-06 | 新日鐵住金株式会社 | 溶融金属中の硫黄測定センサー及びその製造方法 |
| CN106248760B (zh) * | 2016-09-09 | 2018-12-14 | 中广核研究院有限公司 | 测量液态金属中溶解氧活度的固相参比电极氧传感器 |
| CN107504989A (zh) * | 2017-08-16 | 2017-12-22 | 钟祥市中原电子有限责任公司 | 一种钢水定氧探头 |
| CN107389768A (zh) * | 2017-08-16 | 2017-11-24 | 钟祥市中原电子有限责任公司 | 一种用于钢水定氧电池的钼针 |
| CN111163878B (zh) | 2017-10-05 | 2022-02-25 | 维苏威耐火材料有限公司 | 用于确定熔融金属的化学成分的浸入式传感器 |
| EP3581913B1 (en) | 2018-06-12 | 2023-06-07 | Heraeus Electro-Nite International N.V. | Improved molten metal sampler |
| CN113466079B (zh) * | 2021-06-30 | 2023-05-16 | 重庆钢铁股份有限公司 | 一种钢渣成分含量检测方法 |
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| JPS5746155A (en) * | 1980-09-05 | 1982-03-16 | Nippon Kokan Kk <Nkk> | Measuring sensor for oxygen concentration for molten metal |
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| DE4135510C2 (de) * | 1991-10-28 | 1994-02-24 | Heraeus Electro Nite Int | Tauchsensor für Metallschmelzen |
| WO1996032636A1 (de) * | 1995-04-12 | 1996-10-17 | Heraeus Electro-Nite International N.V. | Verfahren zum messen einer elektrochemischen aktivität |
| DE19531661C2 (de) | 1995-04-12 | 2002-08-14 | Heraeus Electro Nite Int | Verfahren zum Messen einer elektrochemischen Aktivität |
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- 2003-03-07 DE DE10310387A patent/DE10310387B3/de not_active Expired - Fee Related
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2004
- 2004-01-14 KR KR1020040002580A patent/KR100766618B1/ko active IP Right Grant
- 2004-01-15 PT PT04000680T patent/PT1460416E/pt unknown
- 2004-01-15 EP EP04000680A patent/EP1460416B8/de not_active Expired - Lifetime
- 2004-01-15 ES ES04000680T patent/ES2352182T3/es not_active Expired - Lifetime
- 2004-01-15 DE DE502004011626T patent/DE502004011626D1/de not_active Expired - Lifetime
- 2004-01-15 AT AT04000680T patent/ATE480768T1/de active
- 2004-01-16 JP JP2004008974A patent/JP4054314B2/ja not_active Expired - Fee Related
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- 2004-01-29 AU AU2004200389A patent/AU2004200389B2/en not_active Ceased
- 2004-02-05 TW TW093102606A patent/TWI298392B/zh not_active IP Right Cessation
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- 2004-03-05 RU RU2004106715/28A patent/RU2282184C2/ru active
- 2004-03-08 CN CNB2004100282396A patent/CN100458433C/zh not_active Expired - Lifetime
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| US3758397A (en) * | 1970-07-15 | 1973-09-11 | Steel Corp | Apparatus for oxygen determination |
| JPS6052763A (ja) * | 1983-09-01 | 1985-03-26 | Sumitomo Alum Smelt Co Ltd | 溶融金属中の酸素濃度測定用センサ− |
| CN1367383A (zh) * | 2001-01-26 | 2002-09-04 | 贺利氏耐特电子国际有限公司 | 测定金属熔体或熔渣中氧活性用的测量装置 |
Also Published As
| Publication number | Publication date |
|---|---|
| BRPI0400385B1 (pt) | 2016-04-12 |
| EP1460416A2 (de) | 2004-09-22 |
| JP2004271517A (ja) | 2004-09-30 |
| KR100766618B1 (ko) | 2007-10-15 |
| ZA200401834B (en) | 2004-09-07 |
| JP4054314B2 (ja) | 2008-02-27 |
| RU2282184C2 (ru) | 2006-08-20 |
| EP1460416A3 (de) | 2004-11-03 |
| AU2004200389A1 (en) | 2004-09-23 |
| RU2004106715A (ru) | 2005-08-20 |
| DE10310387B3 (de) | 2004-07-22 |
| CA2455467A1 (en) | 2004-09-07 |
| CN1527050A (zh) | 2004-09-08 |
| ATE480768T1 (de) | 2010-09-15 |
| PT1460416E (pt) | 2010-12-09 |
| ES2352182T3 (es) | 2011-02-16 |
| US20040173473A1 (en) | 2004-09-09 |
| TW200417731A (en) | 2004-09-16 |
| CA2455467C (en) | 2007-08-21 |
| KR20040079834A (ko) | 2004-09-16 |
| AU2004200389B2 (en) | 2007-09-20 |
| EP1460416B8 (de) | 2011-01-26 |
| MXPA04002075A (es) | 2005-02-17 |
| TWI298392B (en) | 2008-07-01 |
| EP1460416B1 (de) | 2010-09-08 |
| UA75693C2 (en) | 2006-05-15 |
| DE502004011626D1 (de) | 2010-10-21 |
| BRPI0400385A (pt) | 2004-10-13 |
| US7141151B2 (en) | 2006-11-28 |
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