TWI582419B - Method for manufacturing nano-palladium containing biosensor strip - Google Patents

Method for manufacturing nano-palladium containing biosensor strip Download PDF

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TWI582419B
TWI582419B TW104131793A TW104131793A TWI582419B TW I582419 B TWI582419 B TW I582419B TW 104131793 A TW104131793 A TW 104131793A TW 104131793 A TW104131793 A TW 104131793A TW I582419 B TWI582419 B TW I582419B
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palladium
layer
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test piece
reagent
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TW201712331A (en
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陳科儒
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阮彥力
陳科儒
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含有奈米鈀之生物感測試片的製造方法 Method for producing biosensor test piece containing nano palladium

本發明係有關於一種生物感測試片的製造方法,尤指一種以奈米鈀作為電極材料且含有奈米鈀之生物感測試片的製造方法。 The present invention relates to a method for producing a biosensor test piece, and more particularly to a method for producing a biosensor test piece containing nanopalladium as an electrode material and containing nano palladium.

利用生物感測試片(例如:血糖試片)來做日常生活的血糖監測,已成為糖尿病患用來自我監控血糖數值不可或缺的事情。生物感測試片主要由基板、電極、隔離層、反應層、和蓋板等結構所組成,其中又以電極結構最為重要。目前市面上常見的電極製造方式有,濺鍍、蒸鍍、或印刷等。在濺鍍或蒸鍍形成電極的過程中,先將金屬沉積在基板上後,再利用雷雕或蝕刻來形成電極圖案,圖案化以外的金屬則會被去除,不僅造成了金屬浪費,其製程也較為複雜,使得加工成本昂貴。 The use of biosensor test strips (eg, blood glucose test strips) for daily blood glucose monitoring has become an indispensable part of diabetes patients' self-monitoring blood glucose levels. The biosensor test piece is mainly composed of a substrate, an electrode, an isolation layer, a reaction layer, and a cover plate, and the electrode structure is most important. Currently, common electrode manufacturing methods on the market include sputtering, evaporation, or printing. In the process of forming an electrode by sputtering or vapor deposition, after depositing metal on the substrate, the electrode pattern is formed by laser etching or etching, and the metal other than the pattern is removed, which not only causes waste of metal, but also processes thereof. It is also complicated, making the processing cost expensive.

在傳統上,利用印刷技術來製造電極的方式為,將導電碳粉及銀漿印於基板上以形成電極導電層。然而,利用此作法所形成的電極導電層,電阻的抗穩定性不佳,且碳粉容易吸收空氣中的水分而影響了量測數值的準確度。隨著科技的進步,印刷技術也隨之改良,利用改良的印刷技術形成電極的方式為,將導電膠體印刷在基板上以形成導電膠體層,再利用化學鍍的方式將金屬鍍於導電膠體層上以製成電極。但導電膠體單價相當高昂,且油墨 顆粒大的問題使得印刷品質難以改善,導致電極圖案的邊緣容易形成鋸齒狀,更進一步造成了量測精準度與穩定度不佳的問題。 Traditionally, electrodes have been fabricated using printing techniques by printing conductive carbon powder and silver paste onto a substrate to form an electrode conductive layer. However, the electrode conductive layer formed by this method has poor resistance to electrical resistance, and the carbon powder easily absorbs moisture in the air and affects the accuracy of the measured value. With the advancement of technology, printing technology has also been improved. The method of forming electrodes by using improved printing technology is to print conductive paste on the substrate to form a conductive colloid layer, and then electroless plating the metal on the conductive colloid layer. The top is made into an electrode. But the price of conductive colloid is quite high, and the ink The problem of large particles makes the printing quality difficult to improve, and the edges of the electrode pattern are easily formed into a zigzag shape, which further causes the problem of poor measurement accuracy and stability.

基於上述,本發明人研發了一種含有奈米鈀之生物感測試片的製造方法,以奈米鈀作為電極材料,因其粒徑小,藉由印刷技術將含有奈米鈀的奈米鈀膠體直接在基板上精確地印刷出所需的電極圖案,不須像傳統的圖案化製程,還要再去除多餘的金屬。而且,藉由奈米鈀膠體配合印刷方法所製作出來的電極圖案層的厚度很薄,僅有1-4微米。藉由本發明的含有奈米鈀之生物感測試片的製造方法,可以形成具有高精確度且高品質的電極圖案層,不僅不會造成金屬的浪費,還能夠降低生產成本,解決了傳統製程上所面臨的問題。 Based on the above, the present inventors have developed a method for producing a biosensing test piece containing nano palladium, which uses nanopalladium as an electrode material, and has a nanopalladium colloid containing nano palladium by a printing technique because of its small particle size. The desired electrode pattern is accurately printed directly on the substrate without the need to remove excess metal like a conventional patterning process. Moreover, the thickness of the electrode pattern layer produced by the nano palladium colloidal printing method is very thin, only 1-4 μm. By the method for manufacturing a nano-palladium-containing biosensor test piece of the present invention, an electrode pattern layer having high precision and high quality can be formed, which not only causes waste of metal, but also can reduce production cost and solve the conventional process. The problem facing.

本發明其中一實施例提供一種含有奈米鈀之生物感測試片的製造方法,其步驟包括:提供一基板;將一奈米鈀膠體印刷於基板上,用以形成一具有一預定圖案之電極圖案層,其中奈米鈀膠體含有一鈀化合物;將含有電極圖案層之基板浸入一第一試劑中,用以使奈米鈀膠體中的鈀化合物還原成一鈀金屬;清洗含有第一試劑的電極圖案層,再立即浸入一第二試劑中,用以在電極圖案層上形成一第一金屬層;清洗含有第二試劑的第一金屬層,再立即浸入一第三試劑中,用以在第一金屬層上形成一第二金屬層,並製得一電極導電層;將一絕緣層對應地設置在電極導電層上,且於絕緣層上定義一開口,以裸露出部分電極導電層;將一反應層設置在絕緣層的開口內,且反應層與電極導電層電性連接,其中反應層的大小與絕緣層的開口的大小相對應;以及將一保護片對應地覆蓋在設置有反應層的絕緣層上,並裸露出部分電極導電層,以完成一含有奈米鈀之生物感測試片,其中保護片的 長度較電極導電層的長度短。 An embodiment of the present invention provides a method for manufacturing a biosensing test piece containing nano palladium, the method comprising: providing a substrate; printing a nano palladium colloid on the substrate to form an electrode having a predetermined pattern a pattern layer, wherein the nano palladium colloid comprises a palladium compound; the substrate containing the electrode pattern layer is immersed in a first reagent for reducing the palladium compound in the nanopalladium colloid to a palladium metal; and the electrode containing the first reagent is washed The pattern layer is immediately immersed in a second reagent for forming a first metal layer on the electrode pattern layer; the first metal layer containing the second reagent is washed, and then immediately immersed in a third reagent for use in a second metal layer is formed on a metal layer, and an electrode conductive layer is formed; an insulating layer is correspondingly disposed on the electrode conductive layer, and an opening is defined on the insulating layer to expose a portion of the electrode conductive layer; The reaction layer is disposed in the opening of the insulating layer, and the reaction layer is electrically connected to the electrode conductive layer, wherein the size of the reaction layer corresponds to the size of the opening of the insulating layer; Correspondingly sheet overlying the insulating layer is provided with a reaction layer, and the exposed conductive portion of the electrode layer to complete a palladium containing nano biosensor test strip, wherein the protective sheet The length is shorter than the length of the electrode conductive layer.

本發明的有益效果可以在於,藉由本發明實施例所提供的含有奈米鈀之生物感測試片的製造方法,以奈米鈀作為電極材料,因其粒徑小,將含有奈米鈀的奈米鈀膠體印刷在基板上(例如:網版印刷)時,其所形成的電極圖案層邊緣的鋸齒狀結構,會比習知使用碳墨或銀膠的網版印刷所形成之鋸齒狀結構來得小。而且直接把奈米鈀膠體直接精確地印刷在基板形成所需的電極圖案,不須像傳統的圖案化製程,還要再去除多餘金屬的步驟。本發明利用奈米鈀膠體配合印刷方法所製作出來的電極圖案層的厚度很薄,僅有1-4微米。藉由本發明的含有奈米鈀之生物感測試片的製造方法,可以形成具有高精確度且高品質的電極圖案層,不僅不會造成金屬的浪費,還能夠降低生產成本,解決了傳統製程上所面臨的問題。此外,相較於傳統碳電極,本發明含有奈米鈀膠體的電極之生物感測試片所得到之血糖量測結果,亦具有穩定性高且變異數小的優點,因此其可靠度及信賴度亦較高。 The beneficial effects of the present invention may be that the nano palladium-containing biosensor test piece is provided by the embodiment of the present invention, and nano palladium is used as an electrode material, and the nanometer palladium-containing naphthalene is contained because of its small particle size. When the palladium colloid is printed on a substrate (for example, screen printing), the zigzag structure of the edge of the electrode pattern layer formed by the colloidal structure of the electrode is smaller than the zigzag structure formed by screen printing using carbon ink or silver paste. . Moreover, the nanopalladium colloid is directly and accurately printed on the substrate to form a desired electrode pattern, and the step of removing excess metal is not required as in the conventional patterning process. The thickness of the electrode pattern layer produced by the nanopalladium colloid-matching printing method of the present invention is very thin, only 1-4 micrometers. By the method for manufacturing a nano-palladium-containing biosensor test piece of the present invention, an electrode pattern layer having high precision and high quality can be formed, which not only causes waste of metal, but also can reduce production cost and solve the conventional process. The problem facing. In addition, compared with the conventional carbon electrode, the blood glucose measurement result obtained by the biosensing test piece of the electrode containing the nano palladium colloid has the advantages of high stability and small variation, so reliability and reliability are obtained. Also higher.

為使能更進一步瞭解本發明的特徵及技術內容,請參閱以下有關本發明的詳細說明與附圖,然而所附圖式僅提供參考與說明用,並非用來對本發明加以限制者。 For a better understanding of the features and technical aspects of the present invention, reference should be made to the accompanying drawings.

1‧‧‧生物感測試片 1‧‧‧Biosensor test piece

10‧‧‧基板 10‧‧‧Substrate

20‧‧‧電極導電層 20‧‧‧electrode conductive layer

201‧‧‧電極圖案層 201‧‧‧electrode pattern layer

202‧‧‧第一金屬層 202‧‧‧First metal layer

203‧‧‧第二金屬層 203‧‧‧Second metal layer

30‧‧‧絕緣層 30‧‧‧Insulation

301‧‧‧開口 301‧‧‧ openings

40‧‧‧反應層 40‧‧‧Reaction layer

50‧‧‧保護片 50‧‧‧protection film

X‧‧‧第一方向 X‧‧‧ first direction

圖1為本發明一實施例中含有奈米鈀之生物感測試片的製造方法之流程圖;圖2為本發明一實施例中含有奈米鈀之生物感測試片的立體分解示意圖;以及圖3為本發明一實施例中含有奈米鈀之生物感測試片的III-III區域之剖面圖。 1 is a flow chart showing a method for producing a biosensing test piece containing nano palladium according to an embodiment of the present invention; and FIG. 2 is a perspective exploded view showing a biosensor test piece containing nano palladium according to an embodiment of the present invention; 3 is a cross-sectional view of a III-III region of a biosensor test piece containing nanopalladium according to an embodiment of the present invention.

以下是通過特定的具體實例來說明本發明所揭露有關“含有奈米鈀之生物感測試片的製造方法”的實施方式,本領域技術人員可由本說明書所揭示的內容瞭解本發明的優點與功效。本發明可通過其他不同的具體實施例加以施行或應用,本說明書中的各項細節亦可基於不同觀點與應用,在不悖離本發明的精神下進行各種修飾與變更。另外,本發明的圖式僅為簡單示意說明,並非依實際尺寸的描繪,先予敘明。以下的實施方式將進一步詳細說明本發明的相關技術內容,但所揭示的內容並非用以限制本發明的技術範疇。 The following is a specific embodiment to illustrate an embodiment of the present invention relating to a "method of producing a nano-palladium-containing biosensor test piece", and those skilled in the art can understand the advantages and effects of the present invention from the contents disclosed in the present specification. . The present invention can be implemented or applied in various other specific embodiments, and various modifications and changes can be made without departing from the spirit and scope of the invention. In addition, the drawings of the present invention are merely illustrative and are not described in terms of actual dimensions. The following embodiments will further explain the related technical content of the present invention, but the disclosure is not intended to limit the technical scope of the present invention.

請參閱圖1至圖3所示,圖1為本發明一實施例中含有奈米鈀之生物感測試片1的製造方法之流程圖、圖2為本發明一實施例中含有奈米鈀之生物感測試片1的立體分解示意圖、以及圖3為本發明一實施例中含有奈米鈀之生物感測試片1的III-III區域之剖面圖。 1 to FIG. 3, FIG. 1 is a flowchart of a method for manufacturing a bio-sensing test sheet 1 containing nano-palladium according to an embodiment of the present invention, and FIG. 2 is a view showing a method for preparing nano-palladium according to an embodiment of the present invention. A schematic exploded view of the biosensor test piece 1 and a cross-sectional view of the III-III region of the biosensor test piece 1 containing nanopalladium according to an embodiment of the present invention.

本發明實施例提供一種含有奈米鈀之生物感測試片1的製造方法,其包含以下步驟:提供一基板10;將一奈米鈀膠體印刷於基板10上,用以形成一具有一預定圖案之電極圖案層201,其中奈米鈀膠體含有一鈀化合物;將含有電極圖案層201的基板10浸入一溫度為常溫之第一試劑中3至5分鐘,用以使奈米鈀膠體中的鈀化合物還原成一鈀金屬,其中第一試劑為一金屬化還原試劑;清洗含有第一試劑的電極圖案層201,其清洗步驟重複2至3次後,再立即浸入一溫度介於50至80℃之間的第二試劑中2至5分鐘,用以在電極圖案層201上形成一第一金屬層202,其中第二試劑為一含有鎳的化學鍍液,且第一金屬層202為鎳層;清洗含有第二試劑的第一金屬層202,其清洗步驟重複兩次後,再立即浸入一溫度介於45至85℃之間的第三試劑中1至5分鐘,用以在第一金屬層202上形成一第二金屬層203,清洗含有第三試劑的第二 金屬層203,其清洗步驟重複兩次後,製得一電極導電層20,其中第三試劑為一含有鈀、金或是鉑的化學鍍液,且第二金屬層203可為一鈀層、一金層、或是一鉑層;將一絕緣層30對應地設置在第二金屬層203上,且於絕緣層30上定義一開口301,以裸露出部分電極導電層20,其中所述開口沿著一第一方向X貫穿絕緣層30;將一反應層40設置在絕緣層30的開口301內,且反應層40與電極導電層20電性連接,其中反應層40的大小與絕緣層30的開口301的大小相對應;以及將一保護片50對應地覆蓋在設置有反應層40的絕緣層30上,並裸露出部分電極導電層20,以完成一含有奈米鈀之生物感測試片1,其中保護片的長度較電極導電層的長度短。 An embodiment of the present invention provides a method for manufacturing a bio-sensing test sheet 1 containing nano-palladium, comprising the steps of: providing a substrate 10; and printing a nano-palladium colloid on the substrate 10 to form a predetermined pattern. The electrode pattern layer 201, wherein the nano palladium colloid contains a palladium compound; the substrate 10 containing the electrode pattern layer 201 is immersed in a first reagent at a normal temperature for 3 to 5 minutes for palladium in the nanopalladium colloid The compound is reduced to a palladium metal, wherein the first reagent is a metallization reducing reagent; the electrode pattern layer 201 containing the first reagent is washed, and the cleaning step is repeated 2 to 3 times, and then immediately immersed in a temperature of 50 to 80 ° C. 2 to 5 minutes between the second reagent to form a first metal layer 202 on the electrode pattern layer 201, wherein the second reagent is a nickel-containing electroless plating solution, and the first metal layer 202 is a nickel layer; Cleaning the first metal layer 202 containing the second reagent, the cleaning step is repeated twice, and then immediately immersed in a third reagent at a temperature between 45 and 85 ° C for 1 to 5 minutes for use in the first metal layer Forming a second gold on 202 Layer 203, a third reagent containing the second washing After the metal layer 203 is repeated twice, the electrode conductive layer 20 is prepared. The third reagent is an electroless plating solution containing palladium, gold or platinum, and the second metal layer 203 can be a palladium layer. a gold layer or a platinum layer; an insulating layer 30 is correspondingly disposed on the second metal layer 203, and an opening 301 is defined on the insulating layer 30 to expose a portion of the electrode conductive layer 20, wherein the opening The insulating layer 30 is inserted through a first direction X; a reactive layer 40 is disposed in the opening 301 of the insulating layer 30, and the reactive layer 40 is electrically connected to the electrode conductive layer 20, wherein the size of the reactive layer 40 and the insulating layer 30 are The opening 301 has a corresponding size; and a protective sheet 50 is correspondingly covered on the insulating layer 30 provided with the reaction layer 40, and a part of the electrode conductive layer 20 is exposed to complete a bio-sensing test piece containing nano palladium. 1, wherein the length of the protective sheet is shorter than the length of the conductive layer of the electrode.

更進一步地,於本發明實施例中,清洗含有第一試劑的電極圖案層201以及清洗含有第二試劑的第一金屬層202步驟包括:先用蒸餾水清洗,用以去除所述第一試劑和所述第二試劑;以及再用丙酮清洗,用以去除所述電極圖案層和所述第一金屬層上的蒸餾水。由於本發明實施例是利用化學鍍溼式製程,於單位時間內可以形成多張的預定金屬膜,製造流程簡單且快速,大幅降低生產成本。 Further, in the embodiment of the present invention, the step of cleaning the electrode pattern layer 201 containing the first reagent and cleaning the first metal layer 202 containing the second reagent comprises: first washing with distilled water to remove the first reagent and And the second reagent; and the acetone is further washed to remove the electrode pattern layer and the distilled water on the first metal layer. Since the embodiment of the present invention utilizes an electroless plating process, a plurality of predetermined metal films can be formed in a unit time, and the manufacturing process is simple and rapid, and the production cost is greatly reduced.

較佳地,本發明實施例的含有奈米鈀之生物感測試片1的基板10為一絕緣材料,其可以是玻璃、玻璃纖維板、氧化鋁陶瓷、氧化鋯陶瓷、聚苯乙烯(Polystyrene,PS)、聚對苯二甲酸乙二醇酯(Polyethylene terephthalate,PET)、聚碳酸酯樹脂(Polycarbonate,PC)、聚丙烯(Polypropylene,PP)、聚乙烯(polyethylene,PE)、丙烯腈-丁二烯-苯乙烯共聚物(Acrylonitrile-Butadiene-Styrene,ABS)、聚碸(Polyethersulfon,PES)、聚醯亞胺(Polyimide,PI)、聚醚醯亞胺(Polyetherimide, PEI)、聚醯胺醯亞胺(Polyamide-imide,PAI)、熱塑性彈性體(Thermoplastic,TPE)、聚乳酸(polylacticacid,PLA)、或其組合。 Preferably, the substrate 10 of the nano-palladium-containing biosensor test piece 1 of the embodiment of the present invention is an insulating material, which may be glass, fiberglass board, alumina ceramic, zirconia ceramic, polystyrene (Polystyrene, PS). ), polyethylene terephthalate (PET), polycarbonate resin (Polycarbonate, PC), polypropylene (PP), polyethylene (PE), acrylonitrile-butadiene -Acrylonitrile-Butadiene-Styrene (ABS), Polyethersulfon (PES), Polyimide (PI), Polyetherimide (Polyetherimide, PEI), Polyamide-imide (PAI), Thermoplastic (TPE), Polylactic acid (PLA), or a combination thereof.

由於奈米鈀膠體的顆粒小,其粒徑大小僅有300-500奈米(nm),且其所含有的鈀化合物的粒徑大小更僅有20-30奈米(nm),藉由此特性,本發明的奈米鈀膠體具有良好的延展性,當利用一印刷機將奈米鈀膠體印刷於基板10上時,可以得到很薄的電極圖案層201,其厚度僅有1-4微米(μm)。然而,使用傳統的導電銀油墨或導電碳油墨來印刷時,導電銀油墨的墨膜厚度需達到6微米(μm)以上,而導電碳油墨的墨膜厚度需達到12微米(μm)以上,才能提供良好的導電品質。再者,相較於傳統的導電銀油墨或導電碳油墨的墨膜厚度,形成本發明僅有1-4微米(μm)的電極圖案層201所需使用的材料相對較少,因此生產成本可以降低。 Since the nanopalladium colloid has a small particle size, the particle size is only 300-500 nanometers (nm), and the palladium compound contained therein has a particle size of only 20-30 nanometers (nm). The nanopalladium colloid of the present invention has good ductility. When a nanopalladium colloid is printed on the substrate 10 by a printing machine, a very thin electrode pattern layer 201 having a thickness of only 1-4 μm can be obtained. (μm). However, when printing with a conventional conductive silver ink or conductive carbon ink, the thickness of the ink film of the conductive silver ink needs to be 6 micrometers (μm) or more, and the thickness of the ink film of the conductive carbon ink needs to be 12 micrometers (μm) or more. Provides good electrical conductivity. Furthermore, compared to the ink film thickness of the conventional conductive silver ink or conductive carbon ink, the material for forming the electrode pattern layer 201 of only 1-4 micrometers (μm) of the present invention is relatively small, so the production cost can be reduce.

更進一步地,本發明實施例之奈米鈀膠體的主要成分為,氯化鈀、氯化烯丙基鈀二聚物、硝酸鈀、氧化鈀、乙酸鈀、硫酸鈀、或其組合。奈米鈀膠體由0.005-1%的鈀化合物、10-30%的固形物、15-25%的滑石粉、和55-65%的溶劑所組成。其中,固形物可為環氧樹脂,溶劑可為丙酮、丁酮、環己酮、甲基異丁酮、或二異丁酮,但本發明不以此為限。另外,本發明奈米鈀膠體除了能夠使化學鍍液進行氧化還原的反應之外,還可增加基板10及第一金屬層202間的附著能力,用以加強電極導電層20的結構。 Further, the main components of the nanopalladium colloid of the present invention are palladium chloride, allyl palladium chloride dimer, palladium nitrate, palladium oxide, palladium acetate, palladium sulfate, or a combination thereof. The nano palladium colloid consists of 0.005-1% palladium compound, 10-30% solids, 15-25% talc, and 55-65% solvent. The solid matter may be an epoxy resin, and the solvent may be acetone, methyl ethyl ketone, cyclohexanone, methyl isobutyl ketone or diisobutyl ketone, but the invention is not limited thereto. Further, in addition to the reaction of redoxing the electroless plating solution, the nano palladium colloid of the present invention can increase the adhesion between the substrate 10 and the first metal layer 202 to enhance the structure of the electrode conductive layer 20.

於本發明實施例中,所使用印刷機可以是一凸版印刷機、一平版印刷機、一凹版印刷機、或一網版印刷機。其印刷技術可以應用網板印刷技術、噴墨技術技術、轉印技術技術、壓印技術技術、或其他塗佈技術等。印刷機主要由裝版、塗墨、壓印、輸紙(包括摺疊)等機構組成。它的工作原理是:先將要印刷的文字和圖像製成印版,裝在印刷機上,然後由人工或印刷機把墨塗敷於印版 上有文字和圖像的地方,再直接或間接地轉印到紙或其他承印物(如紡織品、金屬板、塑膠、皮革、木板、玻璃、或陶瓷)上,從而複製出與原稿相同的印刷品。本發明利用印刷技術來印刷出所需的電極圖案層201,不需像蝕刻、微影製程、或雷射雕刻等技術一樣,在圖案化後還須把多餘的金屬去除掉,才得到預定的圖案成品,因此本發明的製造方法較為簡便,可省略去除多餘金屬的步驟,也較不會浪費金屬材料。 In the embodiment of the present invention, the printing machine used may be a letterpress printing machine, a lithographic printing machine, a gravure printing machine, or a screen printing machine. Its printing technology can be applied to screen printing technology, inkjet technology, transfer technology, imprint technology, or other coating technology. The printing machine is mainly composed of a plate loading, ink coating, embossing, and paper feeding (including folding). It works by first making a plate of the text and image to be printed, mounting it on a printing press, and then applying the ink to the plate by a manual or printing machine. Where text and images are placed, directly or indirectly transferred to paper or other substrates (such as textiles, metal sheets, plastic, leather, wood, glass, or ceramics) to replicate the same print as the original . The invention utilizes printing technology to print the desired electrode pattern layer 201, without the need of etching, lithography process, or laser engraving, etc., after the patterning, the excess metal must be removed to obtain the predetermined Since the pattern is finished, the manufacturing method of the present invention is relatively simple, and the step of removing excess metal can be omitted, and the metal material is not wasted.

在形成預定圖案的電極圖案層201後,將含有電極圖案層201之基板10所浸入的第一試劑為金屬化還原試劑,其主要成分包含氫氧化鈉30-40%、硼氫化鈉10-15%、以及純水35-45%,使用時以純水稀釋30至100倍後使用。金屬化還原試劑用以使奈米鈀膠體中的鈀化合物還原成鈀金屬,鈀金屬為分散的微小顆粒,其粒徑大小為20-30奈米,且鈀化合物還原成所述鈀金屬的化學式如下:1. Pd2++4NaBH4+7H2O→Pd0+Na2B4O7+2Na++15H2 After the electrode pattern layer 201 of the predetermined pattern is formed, the first reagent immersed in the substrate 10 including the electrode pattern layer 201 is a metallization reducing reagent, and the main component thereof contains 30-40% of sodium hydroxide and 10-15% of sodium borohydride. %, and 35-45% of pure water, used 30 to 100 times diluted with pure water after use. The metallization reducing reagent is used to reduce the palladium compound in the nanopalladium colloid to palladium metal, the palladium metal is a dispersed fine particle having a particle size of 20-30 nm, and the palladium compound is reduced to the chemical formula of the palladium metal. As follows: 1. Pd 2+ +4NaBH 4 +7H 2 O→Pd 0 +Na 2 B 4 O 7 +2Na + +15H 2

2. Pd2++(CH3)2-NH-BH3+3H2O→Pd0+(CH3)2-NH+H3BO3+2H++2H2 2. Pd 2+ +(CH 3 ) 2 -NH-BH 3 +3H 2 O→Pd 0 +(CH 3 ) 2 -NH+H 3 BO 3 +2H + +2H 2

較佳地,本發明的絕緣層30的開口301用以提供一反應區域並設置反應層40和電極導電層20電性連接,而絕緣層30開口外的其它部位則用來保護並隔絕電極導電層20被反應液體所汙染,而影響量測結果。本發明實施例所使用的絕緣層30材料可以是,玻璃、玻璃纖維板、氧化鋁陶瓷、氧化鋯陶瓷、聚苯乙烯(Polystyrene,PS)、聚對苯二甲酸乙二醇酯(Polyethylene terephthalate,PET)、聚碳酸酯樹脂(Polycarbonate,PC)、聚丙烯(Polypropylene,PP)、聚乙烯(polyethylene,PE)、丙烯腈-丁二烯-苯乙烯共聚物(Acrylonitrile-Butadiene-Styrene,ABS)、聚碸 (Polyethersulfon,PES)、聚醯亞胺(Polyimide,PI)、聚醚醯亞胺(Polyetherimide,PEI)、聚醯胺醯亞胺(Polyamide-imide,PAI)、熱塑性彈性體(Thermoplastic,TPE)、聚乳酸(polylacticacid,PLA)、或其組合。 Preferably, the opening 301 of the insulating layer 30 of the present invention is used to provide a reaction region and the reactive layer 40 and the electrode conductive layer 20 are electrically connected, and other portions outside the opening of the insulating layer 30 are used to protect and insulate the electrode from conduction. Layer 20 is contaminated by the reaction liquid and affects the measurement results. The material of the insulating layer 30 used in the embodiments of the present invention may be glass, fiberglass board, alumina ceramic, zirconia ceramic, polystyrene (PS), polyethylene terephthalate (PET). ), Polycarbonate (PC), Polypropylene (PP), Polyethylene (PE), Acrylonitrile-Butadiene-Styrene (ABS), Poly碸 (Polyethersulfon, PES), Polyimide (PI), Polyetherimide (PEI), Polyamide-imide (PAI), Thermoplastic (TPE), Polylactic acid (PLA), or a combination thereof.

本發明實施例的含有奈米鈀之生物感測試片1之反應層40具有一生物化學試劑,當一待測液滲入反應層40後,會發生電化學反應以產生一電子訊號。舉例來說,用在測量血糖時,反應層40為具葡萄糖氧化酶的反應層40,而血液中的葡萄糖會與葡萄糖氧化酶會在此區域產生反應,當血液滲入具有葡萄糖氧化酶的反應層40後,血液中的葡萄糖會進行氧化還原反應而產生電流,電流的大小與血液中的血糖濃度成正比,藉由血糖測試儀測得電流訊號強弱,進而換算成血液中的葡萄糖濃度,再於血糖測試儀的螢幕上顯示出來。 The reaction layer 40 of the nano-palladium-containing biosensor test piece 1 of the embodiment of the present invention has a biochemical reagent. When a liquid to be tested penetrates into the reaction layer 40, an electrochemical reaction occurs to generate an electronic signal. For example, when measuring blood glucose, the reaction layer 40 is a reaction layer 40 having glucose oxidase, and glucose in the blood reacts with glucose oxidase in this region when the blood penetrates into a reaction layer having glucose oxidase. After 40, the glucose in the blood undergoes a redox reaction to generate a current. The magnitude of the current is proportional to the blood glucose concentration in the blood. The blood signal is measured by the blood glucose tester, and then converted into the blood glucose concentration. The blood glucose tester is displayed on the screen.

〔實施例的可行功效〕 [Effective effect of the embodiment]

綜上所述,本發明的有益效果可以在於,本發明實施例所提供的一種含有奈米鈀之生物感測試片的製造方法,以奈米鈀作為電極材料,因其粒徑小,將含有奈米鈀的奈米鈀膠體印刷在基板上(例如:網版印刷)時,其所形成的電極圖案層201邊緣的鋸齒狀結構,會比習知使用碳墨或銀膠的網版印刷所形成之鋸齒狀結構來得小。而且直接把奈米鈀膠體直接精確地印刷在基板形成所需的電極圖案,不須像傳統的圖案化製程,還要再去除多餘金屬的步驟。本發明利用奈米鈀膠體配合印刷方法所製作出來的電極圖案層的厚度很薄,僅有1-4微米。藉由本發明的含有奈米鈀之生物感測試片的製造方法,可以形成具有高精確度且高品質的電極圖案層,不僅不會造成金屬的浪費,還能夠降低生產成本,解決了傳統製程上所面臨的問題。此外,相較於傳統碳電極,本發明 含有奈米鈀膠體的電極之生物感測試片所得到之血糖量測結果,亦具有穩定性高且變異數小的優點,因此其可靠度及信賴度亦較高。 In summary, the beneficial effects of the present invention may be that a method for manufacturing a bio-sensing test piece containing nano-palladium according to an embodiment of the present invention uses nano-palladium as an electrode material, and the particle size thereof is small, and will contain When the nano palladium colloid of nano palladium is printed on a substrate (for example, screen printing), the zigzag structure of the edge of the electrode pattern layer 201 formed by it is formed by screen printing using a carbon ink or a silver paste. The zigzag structure is small. Moreover, the nanopalladium colloid is directly and accurately printed on the substrate to form a desired electrode pattern, and the step of removing excess metal is not required as in the conventional patterning process. The thickness of the electrode pattern layer produced by the nanopalladium colloid-matching printing method of the present invention is very thin, only 1-4 micrometers. By the method for manufacturing a nano-palladium-containing biosensor test piece of the present invention, an electrode pattern layer having high precision and high quality can be formed, which not only causes waste of metal, but also can reduce production cost and solve the conventional process. The problem facing. Furthermore, the present invention is compared to a conventional carbon electrode The blood glucose measurement results obtained by the biosensing test piece of the electrode containing the nano palladium colloid have the advantages of high stability and small variation, and thus the reliability and reliability are also high.

以上僅為本發明的較佳可行實施例,非因此侷限本發明的專利範圍,故舉凡運用本發明說明書及圖式內容所做的等效技術變化,均包含於本發明的保護範圍內。 The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Therefore, equivalent technical changes made by the present invention and the contents of the drawings are included in the scope of the present invention.

指定代表圖為流程圖,故無符號簡單說明。 The designated representative diagram is a flow chart, so no symbol is simply stated.

Claims (17)

一種含有奈米鈀之生物感測試片的製造方法,其步驟包括:提供一基板;將一奈米鈀膠體印刷於所述基板上,用以形成一具有一預定圖案之電極圖案層,其中所述奈米鈀膠體含有一鈀化合物;將含有所述電極圖案層之所述基板浸入一第一試劑中,用以使所述奈米鈀膠體中的所述鈀化合物還原成一鈀金屬;清洗含有所述第一試劑的所述電極圖案層,再立即浸入一第二試劑中,用以在所述電極圖案層上形成一第一金屬層;清洗含有所述第二試劑的第一金屬層,再立即浸入一第三試劑中,用以在所述第一金屬層上形成一第二金屬層,並製得一電極導電層;將一絕緣層對應地設置在所述電極導電層上,且於所述絕緣層上定義一開口,以裸露出部分的所述電極導電層;將一反應層設置在所述絕緣層的所述開口內,且所述反應層與所述電極導電層電性連接,其中所述反應層的大小與所述絕緣層的所述開口的大小相對應;以及將一保護片對應地覆蓋在設置有所述反應層的所述絕緣層上,並裸露出部分的所述電極導電層,以完成一含有奈米鈀之生物感測試片,其中所述保護片的長度較所述電極導電層的長度短。 A method for manufacturing a bio-sensing test piece containing nano-palladium, comprising the steps of: providing a substrate; and printing a nano-palladium colloid on the substrate to form an electrode pattern layer having a predetermined pattern, wherein The nano palladium colloid contains a palladium compound; the substrate containing the electrode pattern layer is immersed in a first reagent for reducing the palladium compound in the nanopalladium colloid to a palladium metal; The electrode pattern layer of the first reagent is immediately immersed in a second reagent for forming a first metal layer on the electrode pattern layer; cleaning the first metal layer containing the second reagent, Immediately immersed in a third reagent for forming a second metal layer on the first metal layer, and preparing an electrode conductive layer; an insulating layer is correspondingly disposed on the electrode conductive layer, and An opening is defined on the insulating layer to expose a portion of the electrode conductive layer; a reactive layer is disposed in the opening of the insulating layer, and the reactive layer is electrically connected to the electrode conductive layer ,its The size of the reaction layer corresponds to the size of the opening of the insulating layer; and a protective sheet is correspondingly covered on the insulating layer provided with the reaction layer, and a portion of the electrode is exposed a conductive layer to complete a biosensing test piece containing nanopalladium, wherein the length of the protective sheet is shorter than the length of the conductive layer of the electrode. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述基板為一絕緣材料,其是玻璃、玻璃纖維板、氧化鋁陶瓷、氧化鋯陶瓷、聚苯乙烯、聚對苯二甲酸乙二醇酯、聚碳酸 酯樹脂、聚丙烯、聚乙烯、丙烯腈-丁二烯-苯乙烯共聚物、聚碸、聚醯亞胺、聚醚醯亞胺、聚醯胺醯亞胺、熱塑性彈性體、聚乳酸、或其組合。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the substrate is an insulating material, which is glass, glass fiber board, alumina ceramic, zirconia ceramic, polystyrene, poly pair. Ethylene phthalate, polycarbonate Ester resin, polypropylene, polyethylene, acrylonitrile-butadiene-styrene copolymer, polyfluorene, polyimine, polyetherimine, polyamidimide, thermoplastic elastomer, polylactic acid, or Its combination. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述電極圖案層的厚度為1-4微米。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the electrode pattern layer has a thickness of from 1 to 4 μm. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述奈米鈀膠體的主要成分為氯化鈀、氯化烯丙基鈀二聚物、硝酸鈀、氧化鈀、乙酸鈀、硫酸鈀、或其組合。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the main component of the nanopalladium colloid is palladium chloride, allyl palladium chloride dimer, palladium nitrate, palladium oxide. , palladium acetate, palladium sulfate, or a combination thereof. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述奈米鈀膠體由0.005-1%的鈀化合物、10-30%的固形物、15-25%的滑石粉、和55-65%的溶劑所組成。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the nano palladium colloid is composed of 0.005-1% of a palladium compound, 10-30% of a solid matter, and 15-25% of a talc. Powder, and 55-65% solvent. 如請求項4所述之含有奈米鈀之生物感測試片的製造方法,其中所述奈米鈀膠體的粒徑大小為300-500奈米。 The method for producing a nano-palladium-containing biosensor test piece according to claim 4, wherein the nanopalladium colloid has a particle size of 300 to 500 nm. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述第一試劑為一金屬化還原試劑,其主要成分包含氫氧化鈉30-40%、硼氫化鈉10-15%、以及純水35-45%。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the first reagent is a metallization reducing reagent, and the main component thereof comprises sodium hydroxide 30-40%, sodium borohydride 10- 15%, and pure water 35-45%. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述鈀金屬為分散的微小顆粒,其粒徑大小為20-30奈米。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the palladium metal is dispersed fine particles having a particle size of 20 to 30 nm. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述第二試劑為一含有鎳的化學鍍液。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the second reagent is an electroless plating solution containing nickel. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述第一金屬層為一鎳層。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the first metal layer is a nickel layer. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述第三試劑為一含有鈀、金或是鉑的化學鍍液。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the third reagent is an electroless plating solution containing palladium, gold or platinum. 如請求項1所述之含有奈米鈀之生物感測試片的製造方法,其中所述第二金屬層為一鈀層、一金層、或是一鉑層。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the second metal layer is a palladium layer, a gold layer, or a platinum layer. 如請求項1述之含有奈米鈀之生物感測試片的製造方法,其中所述絕緣層的材料為玻璃、玻璃纖維板、氧化鋁陶瓷、氧化鋯陶瓷、聚苯乙烯、聚對苯二甲酸乙二醇酯、聚碳酸酯樹脂、聚丙烯、聚乙烯、丙烯腈-丁二烯-苯乙烯共聚物、聚碸、聚醯亞胺、聚醚醯亞胺、聚醯胺醯亞胺、熱塑性彈性體、聚乳酸、或其組合。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the insulating layer is made of glass, glass fiber board, alumina ceramic, zirconia ceramic, polystyrene, or polyethylene terephthalate. Glycol ester, polycarbonate resin, polypropylene, polyethylene, acrylonitrile-butadiene-styrene copolymer, polyfluorene, polyimine, polyetherimide, polyamidimide, thermoplastic elastomer Body, polylactic acid, or a combination thereof. 如請求項1述之含有奈米鈀之生物感測試片的製造方法,其中所述開口沿著一第一方向貫穿所述絕緣層。 A method of producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the opening penetrates the insulating layer along a first direction. 如請求項1述之含有奈米鈀之生物感測試片的製造方法,其中所述反應層具有一生物化學試劑,當一待測液滲入所述反應層後,會發生電化學反應以產生一電子訊號。 The method for producing a biosensitivity test piece containing nanopalladium according to claim 1, wherein the reaction layer has a biochemical reagent, and when a liquid to be tested penetrates into the reaction layer, an electrochemical reaction occurs to generate a Electronic signal. 如請求項1述之含有奈米鈀之生物感測試片的製造方法,其中將所述奈米鈀膠體印刷於所述基板上的步驟為,利用一印刷機進行印刷,所述印刷機可為一凸版印刷機、一平版印刷機、一凹版印刷機、或一網版印刷機。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the step of printing the nano palladium colloid on the substrate is performed by using a printing machine, and the printing machine may be A letterpress printer, a lithographic printer, a gravure press, or a screen printer. 如請求項1述之含有奈米鈀之生物感測試片的製造方法,其中清洗含有所述第一試劑的所述電極圖案層以及清洗含有所述第二試劑的所述第一金屬層的步驟包括:先用蒸餾水清洗,用以去除所述第一試劑和所述第二試劑;以及再用丙酮清洗,用以去除所述電極圖案層和所述第一金屬層上的所述蒸餾水。 The method for producing a nano-palladium-containing biosensor test piece according to claim 1, wherein the step of cleaning the electrode pattern layer containing the first reagent and cleaning the first metal layer containing the second reagent The method comprises: first washing with distilled water to remove the first reagent and the second reagent; and washing with acetone to remove the distilled water on the electrode pattern layer and the first metal layer.
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Publication number Priority date Publication date Assignee Title
CN100545305C (en) * 2007-05-29 2009-09-30 南京工业大学 A kind of activating process of nonmetal basal body chemical plating
CN103995030A (en) * 2010-10-26 2014-08-20 佑泰电子股份有限公司 Method for manufacturing electrochemical detection test piece

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Publication number Priority date Publication date Assignee Title
CN100545305C (en) * 2007-05-29 2009-09-30 南京工业大学 A kind of activating process of nonmetal basal body chemical plating
CN103995030A (en) * 2010-10-26 2014-08-20 佑泰电子股份有限公司 Method for manufacturing electrochemical detection test piece

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Title
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