JP2021018065A - Gold electrode, electrochemical sensor using gold electrode, and method of manufacturing them - Google Patents
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Abstract
Description
本発明は、金電極および金電極を用いた電気化学センサ、並びにこれらの製造方法に関するものである。 The present invention relates to a gold electrode and an electrochemical sensor using the gold electrode, and a method for manufacturing the same.
貴金属である金は、高価であるが、低い電気抵抗率、広い電位窓を有する電極として、様々な分野でセンサ電極として使用されている（特許文献１、特許文献３、特許文献４）。
これらの金電極センサはインゴットで使用されるため金の使用量が多く、非常に高価である。
Gold, which is a noble metal, is expensive, but is used as a sensor electrode in various fields as an electrode having a low electrical resistivity and a wide potential window (Patent Document 1, Patent Document 3, Patent Document 4).
Since these gold electrode sensors are used in ingots, they use a large amount of gold and are very expensive.
一方、金は産出量が少なく、将来枯渇する恐れが大きい貴重な資源である為、金は家電製品、プリント基板などから種々の回収手段によって回収されている（例えば特許文献５）。 On the other hand, since gold is a valuable resource that is produced in a small amount and is likely to be exhausted in the future, gold is recovered from home appliances, printed circuit boards, etc. by various recovery means (for example, Patent Document 5).
貴重な資源である金の使用量を減らして、金電極を作製する方法として、基体金属への金めっきが考えられるが、金めっき膜に隙間が生じると、基体金属が露出するという問題がある。
例えば特許文献２に示されるように、ステンレス基体に金をめっきして作製した金電極を生体内に埋め込んだ場合、金めっき膜に隙間が生じると、ステンレスが露出し、ステンレスに含まれるニッケルが生体内で金属アレルギーを引き起こすおそれがある。
Gold plating on the base metal can be considered as a method for producing a gold electrode by reducing the amount of gold, which is a valuable resource, but there is a problem that the base metal is exposed when a gap is formed in the gold plating film. ..
For example, as shown in Patent Document 2, when a gold electrode produced by plating gold on a stainless steel substrate is embedded in a living body, if a gap is formed in the gold plating film, the stainless steel is exposed and nickel contained in the stainless steel is exposed. May cause metal allergies in the body.
そこで本発明は、低コストで、基体金属の露出がない金電極およびその製造方法を提供することを目的とする。更には金の使用量が少なく、基体金属の露出による金属アレルギーの恐れがない安全な金電極を用いた電気化学センサおよびその製造方法の提供を目的とする。 Therefore, an object of the present invention is to provide a gold electrode having no exposed base metal and a method for producing the same at low cost. Furthermore, it is an object of the present invention to provide an electrochemical sensor using a safe gold electrode which uses a small amount of gold and does not cause metal allergy due to exposure of the base metal, and a method for manufacturing the same.
上記の課題を解決するために、本発明者が鋭意検討を重ねた結果、以下に述べる解決手段を見出した。 As a result of diligent studies by the present inventor in order to solve the above problems, the following solution means have been found.
本発明に係る請求項１の発明は、
基体金属の表面に、炭素緻密膜、金めっき膜の順に積層されて成り、
前記炭素緻密膜が溶融塩電気炭素めっき膜で形成されていることを特徴とする金電極である。
The invention of claim 1 according to the present invention is
It is made by laminating a carbon dense film and a gold plating film on the surface of the base metal in this order.
The gold electrode is characterized in that the carbon dense film is formed of a molten salt electrocarbon plating film.
本発明に係る請求項２の発明は、
前記炭素緻密膜の厚さが１μｍ以上であることを特徴とする請求項１に記載の金電極である。
The invention of claim 2 according to the present invention is
The gold electrode according to claim 1, wherein the thickness of the carbon dense film is 1 μm or more.
本発明に係る請求項３の発明は、
測定試料の特定成分の濃度を検出する電気化学センサであって、
請求項１または２に記載の金電極を２つ、および、少なくとも電源部を有するセンサ制御部を備え、２つの前記金電極はそれぞれ電気的に前記電源部に接続されている、
ことを特徴とする電気化学センサである。
The invention of claim 3 according to the present invention
An electrochemical sensor that detects the concentration of a specific component of a measurement sample.
The two gold electrodes according to claim 1 or 2 and a sensor control unit having at least a power supply unit are provided, and the two gold electrodes are electrically connected to the power supply unit, respectively.
It is an electrochemical sensor characterized by this.
本発明に係る請求項４の発明は、
前記金電極の表面の少なくとも一部に感応物質が塗布されている、
ことを特徴とする請求項３に記載の電気化学センサである。
The invention of claim 4 according to the present invention
A sensitive substance is applied to at least a part of the surface of the gold electrode.
The electrochemical sensor according to claim 3, wherein the sensor is characterized by the above.
本発明に係る請求項５の発明は、
基体金属を準備する工程と、
前記基体金属の表面に溶融塩電気炭素めっきを実施して炭素緻密膜を形成する工程と、
前記炭素緻密膜表面に金めっきを実施して金めっき膜を形成する工程と、を有することを特徴とする請求項１または２に記載の金電極の製造方法である。
The invention of claim 5 according to the present invention
The process of preparing the base metal and
A step of forming a carbon dense film by performing molten salt electrocarbon plating on the surface of the substrate metal, and
The method for manufacturing a gold electrode according to claim 1 or 2, further comprising a step of forming a gold-plated film by performing gold plating on the surface of the carbon dense film.
本発明に係る請求項６の発明は、
請求項３または４に記載の電気化学センサを製造する方法であって、
２つの前記金電極を準備する工程と、
前記金電極それぞれを電気伝導体の一端と結合させて電気的に接続する工程と、
前記電気伝導体それぞれの他端を前記電源部と結合させて電気的に接続する工程と、
を有することを特徴とする電気化学センサの製造方法である。
The invention of claim 6 according to the present invention
The method for manufacturing the electrochemical sensor according to claim 3 or 4.
The process of preparing the two gold electrodes and
A process of connecting each of the gold electrodes to one end of an electric conductor and electrically connecting them.
A step of connecting the other ends of each of the electric conductors to the power supply unit and electrically connecting them.
It is a manufacturing method of an electrochemical sensor characterized by having.
本発明に係る金電極によれば、
前記溶融塩炭素電気めっき法では、基体金属表面に隙間のない緻密な炭素膜を形成することができる。すなわち、基体金属の露出がない炭素膜を形成することができる。これにより、例えば金めっき膜に隙間が生じたとしても、不活性な炭素緻密膜が露出して、基体金属の露出が生じない為、金属アレルギーの発生を防ぐことができる。また、厚さが薄い金めっき膜とすることで、金の使用量を削減でき、低コストで金電極が得られる。
According to the gold electrode according to the present invention
In the molten salt carbon electroplating method, a dense carbon film without gaps can be formed on the surface of the base metal. That is, it is possible to form a carbon film in which the base metal is not exposed. As a result, even if a gap is formed in the gold plating film, for example, the inert carbon dense film is exposed and the base metal is not exposed, so that the occurrence of metal allergy can be prevented. Further, by using a thin gold plating film, the amount of gold used can be reduced, and a gold electrode can be obtained at low cost.
また、本発明に係る電気化学センサによれば、
生体への埋め込みに適した、金属アレルギーの恐れのない電気化学センサが得られる。
Further, according to the electrochemical sensor according to the present invention.
An electrochemical sensor suitable for embedding in a living body and having no risk of metal allergy can be obtained.
以下、図を参照しながら本発明の実施形態を説明する。なお、重複する説明を省略するべく、図では同一又は類似の機能を発揮する構成要素には同一の符号を付している。
また、説明中に示す各部の外観や寸法、形状は一例であり、使用目的や測定試料の種類等の各種条件によって適宜変更してよい。
Hereinafter, embodiments of the present invention will be described with reference to the drawings. In addition, in order to omit duplicate description, the same reference numerals are given to the components exhibiting the same or similar functions in the drawings.
In addition, the appearance, dimensions, and shape of each part shown in the description are examples, and may be appropriately changed depending on various conditions such as the purpose of use and the type of measurement sample.
なお、本発明は、以下に述べる実施形態に限定されるものではなく、実施段階ではその
要旨を逸脱しない範囲で種々に変形することが可能である。また、各実施形態は適宜組み合わせて実施してもよく、その場合組み合わせた効果が得られる。更に、上記実施形態には種々の発明が含まれており、開示される複数の構成要件から選択された組み合わせにより種々の発明が抽出され得る。例えば、実施形態に示される全構成要件からいくつかの構成要件が削除されても、課題が解決でき、効果が得られる場合には、この構成要件が削除された構成が発明として抽出され得る。
The present invention is not limited to the embodiments described below, and can be variously modified at the implementation stage without departing from the gist thereof. In addition, each embodiment may be carried out in combination as appropriate, in which case the combined effect can be obtained. Further, the above-described embodiment includes various inventions, and various inventions can be extracted by a combination selected from a plurality of disclosed constituent requirements. For example, even if some constituent requirements are deleted from all the constituent requirements shown in the embodiment, if the problem can be solved and the effect is obtained, the configuration in which the constituent requirements are deleted can be extracted as an invention.
＜実施形態１＞
まず本発明の実施形態１に係る金電極について説明する。
図１は本発明の実施形態１に係る金電極の概略図である。
図１に示すように、金電極１の表面は、金めっき膜２に被覆されている。
<Embodiment 1>
First, the gold electrode according to the first embodiment of the present invention will be described.
FIG. 1 is a schematic view of a gold electrode according to the first embodiment of the present invention.
As shown in FIG. 1, the surface of the gold electrode 1 is covered with the gold plating film 2.
図２は図１に示す金電極１の断面の概略図である。
金電極１は、基体金属３、１μｍ以上の厚さの連続した炭素緻密膜５、金めっき膜２、の順に積層されている。
また、基体金属３は炭素緻密膜５によって完全に被覆されている。詳しくは後述するが、金めっき膜２の一部に傷が付く等により隙間が生じた場合でも、炭素緻密膜５が存在することで、基体金属が露出しないようにするためである。
FIG. 2 is a schematic cross-sectional view of the gold electrode 1 shown in FIG.
The gold electrode 1 is laminated in the order of the base metal 3, the continuous carbon dense film 5 having a thickness of 1 μm or more, and the gold plating film 2.
Further, the substrate metal 3 is completely covered with the carbon dense film 5. As will be described in detail later, this is to prevent the base metal from being exposed due to the presence of the carbon dense film 5 even when a gap is formed due to a part of the gold plating film 2 being scratched or the like.
金電極１は、図３のような工程で製造される。
具体的な製造工程としては、例えば次のようになる。
縦１ｍｍ、横３ｍｍ、奥行き３ｍｍの大きさの基体金属３を準備する工程Ａと、
基体金属３の表面全体に、溶融塩電気炭素めっきを実施して、１μｍ以上の厚さの連続した炭素緻密膜５で被覆する工程Ｂと、
炭素緻密膜５の表面に金をめっきして金めっき膜２を形成する工程Ｃと、
を実施することにより、金電極１が製造される。
The gold electrode 1 is manufactured by a process as shown in FIG.
The specific manufacturing process is as follows, for example.
Step A of preparing the base metal 3 having a size of 1 mm in length, 3 mm in width, and 3 mm in depth, and
Step B in which the entire surface of the substrate metal 3 is subjected to molten salt electrocarbon plating and coated with a continuous carbon dense film 5 having a thickness of 1 μm or more.
Step C of forming the gold-plated film 2 by plating the surface of the carbon dense film 5 with gold,
The gold electrode 1 is manufactured by carrying out the above.
金電極１の形状は特に制限はなく、どのような形状であっても構わない。図１のような四角柱でもよいし、あるいは球体や円柱などでもよい。電極としての使用目的に沿って適切な形状で設計することができる。またサイズも上記サイズに限定されない。 The shape of the gold electrode 1 is not particularly limited and may be any shape. It may be a quadrangular prism as shown in FIG. 1, or a sphere or a cylinder. It can be designed with an appropriate shape according to the purpose of use as an electrode. Also, the size is not limited to the above size.
基体金属３は、金属であれば特に制限はなく、単体金属であっても合金であってもよく、例えばステンレスを用いることができる。目的によっては腐食や変形がしにくい種類の金属を用いてよい。例えば生体センサとして用いる目的であれば、ステンレスのように安定した材料が好ましい。 The base metal 3 is not particularly limited as long as it is a metal, and may be a simple substance metal or an alloy. For example, stainless steel can be used. Depending on the purpose, a type of metal that is not easily corroded or deformed may be used. For example, for the purpose of using it as a biosensor, a stable material such as stainless steel is preferable.
炭素緻密膜５は、基体金属３の表面を完全に被覆することが好ましい。これは、基体金属３が露出しないようにするためであって、そのために炭素緻密膜５は、不活性物質である炭素を用い、さらに緻密な膜とすることで、傷が付く等のアクシデントがあっても簡単に基体金属３が露出しないようにする。
炭素緻密膜５の厚さは、基体金属３の表面を十分に被覆する厚さであればよい。金電極１において、金めっき膜２の一部に隙間が生じた際に基体金属３が露出しないためには、炭素緻密膜５の厚さは１μｍ以上が好ましい。
The carbon dense film 5 preferably completely covers the surface of the substrate metal 3. This is to prevent the substrate metal 3 from being exposed. Therefore, the carbon-dense film 5 uses carbon, which is an inert substance, and is made a denser film to prevent accidents such as scratches. Even if there is, the base metal 3 is not easily exposed.
The thickness of the carbon dense film 5 may be a thickness that sufficiently covers the surface of the base metal 3. In the gold electrode 1, the thickness of the carbon dense film 5 is preferably 1 μm or more so that the base metal 3 is not exposed when a gap is formed in a part of the gold plating film 2.
炭素緻密膜５は、前述のように不活性で緻密な膜が望ましく、本発明者らが鋭意検討した結果、溶融塩電気炭素めっきを用いて形成することとした。
溶融塩電気炭素めっきは公知の手段を用いてよいが、例えば特許第５１１２０１０号に示された方法を用いることができる。
この方法によれば、電解浴として溶融塩を用い、炭素含有イオンとしてカーバイドイオンを用い、陽極表面でカーバイドイオンを電気化学的に酸化させることにより、非常に緻密
な炭素膜を生成できる。
As described above, the carbon-dense film 5 is preferably an inert and dense film, and as a result of diligent studies by the present inventors, it was decided to form the carbon dense film 5 by using molten salt electrocarbon plating.
Known means may be used for molten salt electrocarbon plating, and for example, the method shown in Japanese Patent No. 5112010 can be used.
According to this method, a very dense carbon film can be formed by using a molten salt as an electrolytic bath, using a carbide ion as a carbon-containing ion, and electrochemically oxidizing the carbide ion on the surface of the anode.
以上説明したように、本発明に係る金電極によれば、基体金属が非常に緻密な炭素緻密膜に被覆されているため、基体金属が露出するおそれがなく、例えば電極表面の金めっき膜に隙間が生じたとしても、その下にある不活性な炭素緻密膜が露出するだけで、基体金属の露出が生じない。また、金めっき膜の厚さを薄くでき、金の使用量を削減できる。 As described above, according to the gold electrode according to the present invention, since the base metal is coated with a very dense carbon dense film, there is no possibility that the base metal is exposed, for example, on the gold plating film on the electrode surface. Even if a gap is generated, only the inactive carbon dense film under the gap is exposed, and the base metal is not exposed. In addition, the thickness of the gold plating film can be reduced, and the amount of gold used can be reduced.
＜実施形態２＞
次に、本発明の実施形態２に係る電気化学センサについて説明する。
図４は本発明の実施形態２に係る電気化学センサの概略図である。
図４に示すように電気化学センサ６は、２つの金電極１と電源部７とがそれぞれ電気伝導体８を介して結合して電気的に接続されている。電源部７には、表示部９、操作部１０などが接続されていてもよく、これらを一体としてセンサ制御部１２としてもよい。すなわちセンサ制御部１２には、金電極１に電力を供給する電源部７、センサの測定結果や測定条件を表示するための表示部９、測定作業を操作する操作部１０が備えられていてもよい。
センサ制御部１２はまた、記録機能や外部通信機能などを備えていてもよい。これらの機能により外部の印刷装置やＰＣ端末と接続することで、様々な操作を行うことができる。
<Embodiment 2>
Next, the electrochemical sensor according to the second embodiment of the present invention will be described.
FIG. 4 is a schematic view of the electrochemical sensor according to the second embodiment of the present invention.
As shown in FIG. 4, in the electrochemical sensor 6, two gold electrodes 1 and a power supply unit 7 are electrically connected to each other via an electric conductor 8. The display unit 9, the operation unit 10, and the like may be connected to the power supply unit 7, and these may be integrated into the sensor control unit 12. That is, even if the sensor control unit 12 includes a power supply unit 7 that supplies electric power to the gold electrode 1, a display unit 9 for displaying the measurement result and measurement conditions of the sensor, and an operation unit 10 for operating the measurement work. Good.
The sensor control unit 12 may also have a recording function, an external communication function, and the like. By connecting to an external printing device or PC terminal by these functions, various operations can be performed.
２つの金電極１の表面に、感応物質１１を塗布する等により密着させてもよい。感応物質１１は、特定物質に反応する物質であり、この特定物質で金電極を覆い、測定試料と接触させて、測定試料内に特定物質が含有されているか否かを検出することでセンシングするものである。 The surfaces of the two gold electrodes 1 may be brought into close contact with each other by applying a sensitive substance 11 or the like. The sensitive substance 11 is a substance that reacts with a specific substance, and the gold electrode is covered with this specific substance and brought into contact with the measurement sample to detect whether or not the specific substance is contained in the measurement sample for sensing. It is a thing.
感応物質１１としては、目的に合致する物質であれば特に制限はないが、例えば酸化スズ、グルコースオキシターゼなどを用いることができる。
酸化スズを感応物質とした場合は、本発明の電気化学センサにおいては呼気中のアルコール濃度を測定するセンサとして使用できる。またグルコースオキシターゼを感応物質ちとした場合は、グルコースセンサ（血糖値センサ）として使用できる。
センサとして用いる場合、例えば、ペースト状のパルプ繊維に酸化スズ、グルコースオキシターゼなどの感応物質を混入させ、乾燥してフイルム状の濾紙とし、金電極に密着させて用いることができる。
The sensitive substance 11 is not particularly limited as long as it is a substance that meets the purpose, but for example, tin oxide, glucose oxidase, or the like can be used.
When tin oxide is used as a sensitive substance, it can be used as a sensor for measuring the alcohol concentration in exhaled breath in the electrochemical sensor of the present invention. When glucose oxidase is used as a sensitive substance, it can be used as a glucose sensor (blood glucose level sensor).
When used as a sensor, for example, a paste-like pulp fiber may be mixed with a sensitive substance such as tin oxide or glucose oxidase, dried to form a film-like filter paper, and used in close contact with a gold electrode.
本発明の態様によれば、金電極の形状に加工された金属片、例えば縦１ｍｍ、横３ｍｍ、奥行き３ｍｍの直方体を、前述の溶融塩炭素電気めっき法を用いて、金属片の表面に１μｍ以上の厚さの連続した炭素緻密膜を形成し、さらにこの炭素緻密膜の上に金をめっきすることで、金の使用量を削減し、基体金属の露出のない、すなわち低コストで、生体センサとして用いた場合でも金属アレルギーのおそれの無い金電極を作製することができる。 According to the aspect of the present invention, a metal piece processed into the shape of a gold electrode, for example, a rectangular body having a length of 1 mm, a width of 3 mm, and a depth of 3 mm is placed on the surface of the metal piece by 1 μm by using the molten salt carbon electroplating method described above. By forming a continuous carbon-dense film with the above thickness and then plating gold on the carbon-dense film, the amount of gold used can be reduced, and the base metal is not exposed, that is, at low cost. Even when used as a sensor, a gold electrode without a risk of metal allergy can be produced.
また、上記方法で作製した金電極を図４に示したように電気化学センサ電極として用いることで、生体への埋め込みに適した、金属アレルギーのおそれの無い電気化学センサを得ることができる。 Further, by using the gold electrode produced by the above method as an electrochemical sensor electrode as shown in FIG. 4, it is possible to obtain an electrochemical sensor suitable for embedding in a living body and having no risk of metal allergy.
前記電気化学センサ６において、金電極１の表面に感応物質１１を塗布して、２つの金電極１それぞれに電気伝導体８を接続し、それぞれの電気伝導体８を電源部７に接続し、一方の金電極をアノード、他方の金電極をカソードとして、測定試料又は感応物質に電流又は電圧を印加することによって、前記測定試料の特定成分の濃度を測定することができる。
なお、上記感応物質は必ずしも必要ではなく、感応物質が無くても電気化学センサとして機能する。適宜その目的や必要とする感度に応じて感応物質を使用してよい。
In the electrochemical sensor 6, the sensitive substance 11 is applied to the surface of the gold electrode 1, the electric conductor 8 is connected to each of the two gold electrodes 1, and each electric conductor 8 is connected to the power supply unit 7. The concentration of a specific component of the measurement sample can be measured by applying a current or a voltage to the measurement sample or the sensitive substance with one gold electrode as the anode and the other gold electrode as the cathode.
The above-mentioned sensitive substance is not always necessary, and even if there is no sensitive substance, it functions as an electrochemical sensor. Sensitive substances may be used as appropriate according to the purpose and required sensitivity.
１…金電極
２…金めっき膜
３…基体金属
５…炭素緻密膜
６…電気化学センサ
７…電源部
８…電気伝導体
９…表示部
１０…操作部
１１…感応物質
１２…センサ制御部
1 ... Gold electrode 2 ... Gold plating film 3 ... Base metal 5 ... Carbon dense film 6 ... Electrochemical sensor 7 ... Power supply unit 8 ... Electric conductor 9 ... Display unit 10 ... Operation unit 11 ... Sensitive substance 12 ... Sensor control unit
Claims (6)
前記炭素緻密膜が溶融塩電気炭素めっき膜で形成されていることを特徴とする金電極。 It is made by laminating a carbon dense film and a gold plating film on the surface of the base metal in this order.
A gold electrode characterized in that the carbon dense film is formed of a molten salt electrocarbon plating film.
請求項１または２に記載の金電極を２つ、および、少なくとも電源部を有するセンサ制御部を備え、
２つの前記金電極はそれぞれ電気的に前記電源部に接続されている、
ことを特徴とする電気化学センサ。 An electrochemical sensor that detects the concentration of a specific component of a measurement sample.
The sensor control unit including the two gold electrodes according to claim 1 or 2 and at least a power supply unit.
The two gold electrodes are each electrically connected to the power supply unit.
An electrochemical sensor characterized by that.
ことを特徴とする請求項３に記載の電気化学センサ。 A sensitive substance is applied to at least a part of the surface of the gold electrode.
The electrochemical sensor according to claim 3.
前記基体金属の表面に溶融塩電気炭素めっきを実施して炭素緻密膜を形成する工程と、
前記炭素緻密膜表面に金めっきを実施して金めっき膜を形成する工程と、を有することを特徴とする請求項１または２に記載の金電極の製造方法。 The process of preparing the base metal and
A step of forming a carbon dense film by performing molten salt electrocarbon plating on the surface of the substrate metal, and
The method for manufacturing a gold electrode according to claim 1 or 2, further comprising a step of forming a gold-plated film by performing gold plating on the surface of the carbon dense film.
２つの前記金電極を準備する工程と、
前記金電極それぞれを電気伝導体の一端と結合させて電気的に接続する工程と、
前記電気伝導体それぞれの他端を前記電源部と結合させて電気的に接続する工程と、
を有することを特徴とする電気化学センサの製造方法。 The method for manufacturing the electrochemical sensor according to claim 3 or 4.
The process of preparing the two gold electrodes and
A process of connecting each of the gold electrodes to one end of an electric conductor and electrically connecting them.
A step of connecting the other ends of each of the electric conductors to the power supply unit and electrically connecting them.
A method for manufacturing an electrochemical sensor, which comprises.
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