KR100900771B1 - A oxidizing electrode for measuring organic materials - Google Patents

A oxidizing electrode for measuring organic materials Download PDF

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KR100900771B1
KR100900771B1 KR1020070063359A KR20070063359A KR100900771B1 KR 100900771 B1 KR100900771 B1 KR 100900771B1 KR 1020070063359 A KR1020070063359 A KR 1020070063359A KR 20070063359 A KR20070063359 A KR 20070063359A KR 100900771 B1 KR100900771 B1 KR 100900771B1
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dough
electrode
metal oxide
carbon
anode
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KR20080114110A (en
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강태영
조주영
황지현
차근식
남학현
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주식회사 아이센스
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

본 발명은 용액 중 산화 가능한 유기물질의 농도를 전기화학적으로 측정하는 산화전극에 관한 것으로 보다 구체적으로 전도성 탄소반죽에 금속산화물 분말을 균일하게 혼합한 탄소/금속산화물 반죽을 바탕전극에 바른 후 경화시켜 제조한 산화전극에 관한 것이다.The present invention relates to an anode for measuring the concentration of the oxidizable organic material in the solution electrochemically more specifically, the carbon / metal oxide dough uniformly mixed with a metal oxide powder in a conductive carbon dough is applied to the base electrode and cured It relates to a manufactured anode.

본 발명에 따른 산화전극은 유기물질을 안정적으로 산화시켜 발생하는 전류크기를 검출함으로써 유기물질 농도 측정에 사용할 수 있으며, 제작방법이 간단하여 저렴하게 대량 생산할 수 있는 산화전극을 제공하는 것이다.The anode according to the present invention can be used to measure the concentration of organic materials by detecting the current size generated by oxidizing the organic material stably, the manufacturing method is simple to provide an anode that can be mass-produced inexpensively.

산화전극, 유기물질, 탄소반죽, 금속산화물 Anode, organic material, carbon dough, metal oxide

Description

유기물질 측정을 위한 산화전극 및 그 제조방법{A oxidizing electrode for measuring organic materials}A oxidizing electrode for measuring organic materials and its manufacturing method

도 1은 본 발명의 일 실시예에 상응하는 산화전극 개략도이고,1 is a schematic diagram of an anode corresponding to an embodiment of the present invention,

도 2는 본 발명인 산화전극의 전기화학적 성질을 측정하기 위한 일반적인 장치도이고,2 is a general device diagram for measuring the electrochemical properties of the anode of the present invention,

도 3은 본 발명의 일 실시예에 상응하는 탄소/이산화납 반죽을 전극물질로 사용한 산화전극의 순환전압전류곡선이고,3 is a cyclic voltammogram of an anode using a carbon / lead dioxide paste as an electrode material according to one embodiment of the present invention,

도 4는 본 발명의 일 실시예에 상응하는 탄소/이산화납 반죽 전극의 대표적 유기물질인 글루코오스 농도에 따른 동적 감응 곡선과 검정 곡선이고,4 is a dynamic response curve and a calibration curve according to glucose concentration, which is a representative organic material of a carbon / lead dioxide dough electrode corresponding to one embodiment of the present invention,

도 5는 본 발명의 일 실시예에 상응하는 탄소/이산화납 반죽 전극의 다양한 유기물질에 대한 감응을 비교한 도표이다.5 is a chart comparing the response of the various organic materials of the carbon / lead dioxide dough electrode corresponding to an embodiment of the present invention.

-도면의 주요 부분에 대한 부호의 설명-Explanation of symbols on main parts of drawing

101: 전극물질 102: 바탕전극       101: electrode material 102: base electrode

103: 전극체 104: 연결선103: electrode body 104: connecting line

본 발명은 용액 중 산화 가능한 유기물질의 농도를 측정하는데 사용되는 산화 전극에 관한 것으로, 보다 구체적으로 전도성 탄소반죽에 금속산화물 분말을 혼합 교반한 전극 물질을 바탕전극에 도포하여 산화 전극을 제작함으로써 제작방법이 지극히 간단하며 저렴하게 대량 생산할 수 있는 산화전극에 관한 것이다.The present invention relates to an oxidizing electrode used to measure the concentration of oxidizable organic substances in a solution, and more particularly, by manufacturing an oxidizing electrode by applying an electrode material mixed with a metal oxide powder and mixed with a conductive carbon dough to a base electrode. The method relates to an anode which can be mass produced in a very simple and inexpensive manner.

전기화학적으로 다양한 유기물질들을 산화 분해하는 방법으로 물의 전기분해를 통해 생성된 산소를 산화제로서 사용하는 방법이 있다. 그러나 전기분해로 생성된 산소 산화제는 이론적으로 강한 산화력 가지고 있으나 유기물질 산화에 동력학적 반응속도가 매우 느려 다양한 유기물들을 산화시키는데 많은 어려움이 있다. As a method of oxidatively decomposing various organic materials electrochemically, there is a method of using oxygen generated through electrolysis of water as an oxidant. However, the oxygen oxidant produced by electrolysis has a strong oxidizing power in theory, but there are many difficulties in oxidizing various organic materials because the kinetics of the organic material oxidation are very slow.

따라서 상기 유기물질의 산화를 위한 전극을 다양한 금속산화물 전극으로 제작하는 것은 금속산화물이 전기화학적 촉매로서 산소전이반응을 빠르고 안정하게 유도하여 다양한 유기물질을 효과적으로 산화시키고 이에 발생하는 전류크기를 검출하여 다양한 유기물질의 농도를 측정할 수 있다. 그러나 상기 금속산화물 전극 제작에 있어 대부분 전기도금법을 사용하고 있어 제작방법이 매우 까다로운 과정을 가지며, 금속산화물이 전극에 형성되었다 하더라도 수명이 오래가지 않는 문제점이 있다. 또한, 오랜 수명을 위해 열처리를 이용한 졸-겔법이 사용되기는 하나 여전히 제작과정이 매우 복잡하여 비숙련 자에게는 재현성 있는 전극제작을 기대하기 어렵다.Therefore, the production of the electrode for the oxidation of the organic material with various metal oxide electrode is a metal oxide is an electrochemical catalyst to induce the oxygen transfer reaction quickly and stably to effectively oxidize various organic materials and detect the current size generated by The concentration of organic material can be measured. However, most of the metal oxide electrodes are manufactured by using an electroplating method, and thus, the manufacturing method has a very difficult process, and even though the metal oxide is formed on the electrode, the service life does not last long. In addition, although a sol-gel method using heat treatment is used for a long life, it is still difficult to expect a reproducible electrode production for an unskilled person because the manufacturing process is very complicated.

본 발명에 따른 기술적 과제는 다양한 유기물질을 효과적으로 산화 분해하고 안정적으로 산소전이반응이 유도되어 재현성 있게 유기물질 농도 측정할 수 있으 며, 제조방법이 지극히 단순하여 저렴하게 대량 생산할 수 있는 유기물질 산화전극을 제공하는 것이다.The technical problem according to the present invention is to effectively oxidatively decompose various organic materials and stably induce an oxygen transfer reaction to measure organic material concentrations reproducibly, and the manufacturing method is extremely simple and inexpensive mass production of organic material anodes. To provide.

상기 기술적 과제를 달성하기 위한 본 발명에 따른 산화전극은 전도성 탄소반죽에 금속산화물 분말을 균일하게 혼합한 탄소/금속산화물 반죽을 바탕전극에 바른 후 경화시켜 제조하는 것을 특징으로 한다.The electrode according to the present invention for achieving the above technical problem is characterized in that the carbon / metal oxide dough uniformly mixed with the metal oxide powder on the conductive carbon dough is applied to the base electrode and then hardened.

이하, 첨부된 도면을 참조하여 본 발명에 따른 산화전극에 대해 상세히 설명한다.Hereinafter, an anode according to the present invention will be described in detail with reference to the accompanying drawings.

도 1은 본 발명의 일 실시예에 상응하는 산화전극 개략도를 도시하고 있다.1 shows a schematic diagram of an anode corresponding to one embodiment of the present invention.

도 1에 도시되어 있는 것과 같이 전극물질(101)이 바탕전극(102)을 도포하고 있으며, 바탕전극(102)은 전극체(103) 내부에 구비되어 있는 연결선(104)과 전기적으로 접속되어 있다. 전극물질(101)의 전기화학적 반응을 통하여 생성되는 전류는 바탕전극(102)을 통해 연결선(104)으로 흐를 수 있다.
전극물질(101)은 전도성 탄소반죽에 금속산화물 분말을 균일하게 혼합하여 제작된다. 전도성 탄소반죽에 금속산화물 분말을 넣어 혼합 교반한 후, 롤밀(roll mill)로 균질화 작업을 수행한다. 균질화된 탄소/금속산화물 반죽을 바탕전극(102)에 도포하고, 도포한 탄소/금속산화물 반죽을 일정온도에서 열경화하여 산화전극을 제작한다.
바람직하게, 전도성 탄소반죽과 금속산화물 분말의 혼합 비율은 전도성 탄소반죽의 질량을 기준으로 20% 내지 70%의 금속산화물 분말을 혼합하여 교반하며, 금속산화물과 혼합 교반된 전도성 탄소 반죽을 10회 이상 롤밀로 균질화 작업을 수행한다. 또한, 도포한 탄소/금속산화물 반죽은 80℃ 내지 150℃에서 5분 내지 20분간 열경화시켜 산화전극을 제작된다. 금속산화물 분말로 납, 구리, 코발트, 니켈, 티타늄, 이리듐, 백금, 금, 루세늄 등의 산화물이 사용될 수 있다. 바탕전극(102)은 백금, 금, 은, 팔라듐 등의 금속을 사용할 수 있으며, 바람직하게는 백금을 바탕전극으로 사용할 수 있다. 전극체(103)는 절연성 재질을 사용한다.As shown in FIG. 1, the electrode material 101 is coated with the base electrode 102, and the base electrode 102 is electrically connected to the connection line 104 provided in the electrode body 103. . The current generated through the electrochemical reaction of the electrode material 101 may flow through the base electrode 102 to the connection line 104.
The electrode material 101 is made by uniformly mixing the metal oxide powder on the conductive carbon dough. After mixing and stirring the metal oxide powder in the conductive carbon dough, a homogenization operation is performed with a roll mill. The homogenized carbon / metal oxide dough is applied to the base electrode 102, and the coated carbon / metal oxide dough is thermoset at a predetermined temperature to produce an anode.
Preferably, the mixing ratio of the conductive carbon dough and the metal oxide powder is mixed by stirring 20% to 70% of the metal oxide powder based on the mass of the conductive carbon dough, and at least 10 times the mixed conductive carbon dough mixed with the metal oxide Homogenize the roll mill. In addition, the coated carbon / metal oxide dough is thermoset at 80 ° C. to 150 ° C. for 5 to 20 minutes to produce an anode. Oxides such as lead, copper, cobalt, nickel, titanium, iridium, platinum, gold and ruthenium may be used as the metal oxide powder. The base electrode 102 may be made of metal such as platinum, gold, silver, palladium, and preferably, platinum may be used as the base electrode. The electrode body 103 uses an insulating material.

도 2는 본 발명에 따른 산화전극의 전기화학적 성질을 측정하기 위한 3-전극계 장치도를 도시하고 있다.2 shows a three-electrode system diagram for measuring the electrochemical properties of an anode according to the present invention.

<실시예 1> 탄소/이산화납 반죽 전극의 순환전압전류 측정Example 1 Cyclic Voltammetry of a Carbon / Lead Dioxide Paste Electrode

탄소/이산화납 반죽을 전극물질로 하며, 백금을 바탕전극으로 하여 본 발명에 따른 산화 전극을 제조하였다. 탄소/이산화납 반죽은 50 질량% 탄소 반죽에 50 질량% 이산화납 분말을 혼합 교반하여 제작하였으며, 도 2의 장치에서 0.01M Na2SO4 용액내에 순환전압전류법을 수행하였다. An oxide electrode according to the present invention was prepared using carbon / lead dioxide dough as an electrode material and platinum as a base electrode. Carbon / lead dioxide dough was prepared by mixing and stirring 50 mass% lead dioxide powder in 50 mass% carbon dough, and cyclic voltammetry was performed in a 0.01 M Na 2 SO 4 solution in the apparatus of FIG. 2.

도 3은 탄소/이산화납 반죽을 전극물질로 하고 백극을 바탕전극으로 하며, 50질량% 탄소 반죽에 50질량% 이산화납 분말을 혼합 교반하여 제작된 산화전극의 순환전압전류곡선을 나타낸 것으로, 1.5V 이상에서는 산소발생반응의 산화피크가, 1.0~1.5V 사이에서는 산소전이반응의 산화피크를 보여주며 글루코오스 주입에 의해 1.0~1.5V 사이의 피크가 증가하는 것으로 보아 글루코오스가 산화 분해되어 전류 증가를 나타낸다. FIG. 3 shows a cyclic voltammogram of an anode prepared by mixing and stirring a carbon / lead dioxide dough as an electrode material and a white electrode as a base electrode, and mixing 50% by mass of 50% by mass of lead dioxide powder in a 50% by mass carbon paste. Above V, the peak of oxidation of oxygen generation reaction shows the peak of oxidation of oxygen transfer reaction between 1.0 and 1.5V and the peak between 1.0 and 1.5V increases due to glucose injection. Indicates.

<실시예 2> 탄소/이산화납 반죽 전극의 대표적 유기물질인 글루코오스의 농도에 따른 감응성 측정<Example 2> Sensitivity measurement according to the concentration of glucose which is a representative organic material of the carbon / lead dioxide dough electrode

탄소/이산화납 반죽을 전극물질로 하며, 백금을 바탕전극으로 하여 본 발명에 따른 산화 전극을 제조하였다. 탄소/이산화납 반죽은 탄소 반죽을 기준으로 이산화납 분말 양을 30 질량%, 50 질량%, 그리고 60 질량%로 각각 혼합 교반하여 산화전극을 제작하고 상기 도 2의 장치에서 0.01M Na2SO4 용액 내에 1.25V의 전압을 인가하여 글루코오스 농도에 따른 감응성을 측정하였다. An oxide electrode according to the present invention was prepared using carbon / lead dioxide dough as an electrode material and platinum as a base electrode. The carbon / lead dioxide dough is prepared by mixing and stirring the amount of lead dioxide powder at 30 mass%, 50 mass%, and 60 mass%, respectively, based on the carbon dough, and producing 0.01 M Na 2 SO 4 in the apparatus of FIG. The sensitivity of the glucose concentration was measured by applying a voltage of 1.25V in the solution.

도 4는 전극물질에 혼합된 이산화납 분말 양에 따른 탄소/이산화납 반죽 전극의 글루코오스에 대한 감응을 나타낸 것으로 첨가된 이산화납 분말의 양이 많을 수록 바탕전류 크기와 글루코오스 감응에 대한 전류크기가 증가하며 이산화납 분말 양이 60 질량% 차지하는 탄소/이산화납 반죽 전극은 200mg/L 글루코오스 농도까지 우수한 직선성(r2=0.99941)과 감응성를 나타낸다.Figure 4 shows the response of glucose to the carbon / lead dioxide dough electrode according to the amount of lead dioxide powder mixed in the electrode material as the amount of the added lead dioxide powder increases the current size for the background current and glucose response The carbon / lead dioxide dough electrode, which contains 60% by mass of lead dioxide powder, has excellent linearity (r 2 = 0.99941) and sensitivity up to 200 mg / L glucose concentration.

<실시예 3> 탄소/이산화납 반죽 전극의 다양한 유기물질에 대한 감응 비교Example 3 Response Comparison of Various Organic Materials of Carbon / Lead Dioxide Dough Electrode

탄소/이산화납 반죽을 전극물질로 하고 백금을 바탕전극하며, 탄소/이산화납 반죽은 탄소 반죽을 기준으로 이산화납 분말 양을 60 질량%로 혼합 교반하여 제작한 산화 전극으로 다양한 유기물질에 대해 전기화학적으로 산화 분해시 발생하는 전류크기를 측정하고 이를 소모되는 산소량으로 계산하여 비교하였다.Carbon / lead dioxide dough is used as electrode material and platinum-based electrode is used. Carbon / lead dioxide dough is an oxide electrode made by mixing and stirring 60% by mass of lead dioxide powder based on carbon dough. Chemically, the current magnitude generated during oxidative decomposition was measured and compared with the amount of oxygen consumed.

도 5는 탄소/이산화납 반죽 전극의 다양한 유기물질에 대한 감응을 비교한 도표를 나타낸 것으로 글루코오스를 포함하여 10가지의 다양한 유기물질을 측정하였으며 탄소/이산화납 반죽 전극이 전기화학적으로 다양한 유기물을 산화시킬 수 있으며, 수질의 화학적산소요구량(COD) 변화를 측정할 수 있다.FIG. 5 is a diagram comparing the response of various carbon / lead dioxide dough electrodes to various organic materials. Ten different organic materials including glucose were measured, and the carbon / lead dioxide electrode was oxidized electrochemically. It is possible to measure changes in chemical oxygen demand (COD) of water quality.

본 발명에 따른 유기물질 산화전극은 전도성 탄소반죽에 금속산화물 분말을 균일하게 혼합한 탄소/금속산화물 반죽을 바탕전극에 바른 후 경화시켜 제조하는 것으로 다양한 유기물질을 효과적으로 산화 분해하고 안정적으로 산소전이반응이 유도되어 재현성 있게 유기물질 농도 측정할 수 있으며, 제조방법이 지극히 단순하여 저렴하게 대량 생산할 수 있다.The organic material anode according to the present invention is prepared by applying a carbon / metal oxide paste uniformly mixed with a metal oxide powder on a conductive carbon dough to a base electrode and curing the organic material to effectively oxidatively decompose various organic materials and stably carry out an oxygen transfer reaction. This induced and reproducible organic matter concentration can be measured, and the manufacturing method is extremely simple and mass production at low cost.

Claims (5)

삭제delete 용액 중 산화 가능한 유기물질의 농도를 전기화학적으로 측정하는 산화전극 있어서, An electrode for measuring the concentration of the oxidizable organic material in the solution electrochemically, 전도성 탄소반죽에 금속산화물 분말을 혼합한 전극물질; 및An electrode material in which a metal oxide powder is mixed with a conductive carbon dough; And 상기 전극물질이 도포되어 있는 바탕전극을 포함하며,It includes a base electrode is coated with the electrode material, 상기 전극물질은 전도성 탄소반죽에 질량 퍼센트(%) 단위로 20% 내지 70%의 금속산화물 분말을 함유하는 반죽인 것을 특징으로 하는 산화전극.The electrode material is an anode, characterized in that the dough containing 20% to 70% of the metal oxide powder in a conductive carbon dough in mass percent (%) unit. 제 2 항에 있어서, 상기 금속산화물 분말에 사용되는 화합물은According to claim 2, wherein the compound used in the metal oxide powder 납, 구리, 코발트, 니켈, 티타늄, 이리듐, 백금, 금, 루세늄의 산화물인 것을 특징으로 하는 산화전극.An oxide electrode characterized in that the oxide of lead, copper, cobalt, nickel, titanium, iridium, platinum, gold, ruthenium. 제 2 항에 있어서, 상기 전극물질의 제조방법은 The method of claim 2, wherein the electrode material is manufactured. 전도성 탄소반죽에 질량 퍼센트(%) 단위로 20% 내지 70%의 금속산화물 분말을 균질하게 섞는 단계;Homogeneously mixing 20% to 70% of the metal oxide powder in conductive carbon dough by mass percent (%); 혼합된 탄소/금속산화물 반죽을 상기 바탕전극에 바르는 단계; 및Applying a mixed carbon / metal oxide dough to the base electrode; And 상기 탄소/금속산화물 반죽을 80℃ 내지 150℃에서 5분 내지 20분간 경화시켜 바탕전극에 고정하는 단계를 포함하는 것을 특징으로 하는 산화전극.And curing the carbon / metal oxide dough at 80 ° C. to 150 ° C. for 5 to 20 minutes to fix the carbon / metal oxide dough to a base electrode. 제 4 항에 있어서, 바탕전극의 재질은The material of claim 4, wherein the base electrode is made of a material. 백금, 금, 은, 팔라듐 인 것을 특징으로 하는 산화전극.An anode comprising platinum, gold, silver and palladium.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR810001459Y1 (en) * 1978-02-09 1981-10-06 호리바 마사오 Pole for measurement of oxidation and restoration potential
KR20040095996A (en) * 2003-05-07 2004-11-16 주식회사 엘지화학 production method of Pt-Ru catalyst for anode of direct methanol fuel cell
KR20070019972A (en) * 2003-12-23 2007-02-16 유니버시떼 드 몬트리얼 Process for preparing electroactive insertion compounds and electrode materials obtained therefrom
KR100781006B1 (en) 2000-08-09 2007-11-29 엠지 테크놀러지스 악티엔게젤샤프트 Method for catalytically producing organic substances by partial oxidation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR810001459Y1 (en) * 1978-02-09 1981-10-06 호리바 마사오 Pole for measurement of oxidation and restoration potential
KR100781006B1 (en) 2000-08-09 2007-11-29 엠지 테크놀러지스 악티엔게젤샤프트 Method for catalytically producing organic substances by partial oxidation
KR20040095996A (en) * 2003-05-07 2004-11-16 주식회사 엘지화학 production method of Pt-Ru catalyst for anode of direct methanol fuel cell
KR20070019972A (en) * 2003-12-23 2007-02-16 유니버시떼 드 몬트리얼 Process for preparing electroactive insertion compounds and electrode materials obtained therefrom

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