TW461925B - An electrode preparation process improved by applying ultrasound for ammonia ion detection - Google Patents

Abstract

An electrode preparation process is improved by applying ultrasound to increase active surface area of a metal film formed on the electrode and enhance its sensing ability for ammonia ion. The preparation process includes: using an ion exchange membrane of Nafion(R), and forming the metal film on the ion exchange membrane of Nafion(R) by impregnation-reduction method applying ultrasound in the meantime.

Description

46192? V. Description of the invention (1) Field of invention, especially the use of impregnation reduction method. This case relates to the preparation of an ammonium ion sensing electrode with an electrode. 乂 Background of the invention ^ ^ ^ (lmpregnation-red! JctiOn method) M S Isolation: The electrode is prepared on the exchange membrane. It is widely used in construction and can be used. The prepared electrode is in the form of a membrane, which is a flat environment. It can also be used. The device has a special structure. Or hand-to-hand dragger β B has its convenience in use. In addition, because the electrode-like skin has a characteristic of allowing specific ions to pass through, it is widely used in such analysis as Xianlang Etc. However, the two aspects of electricity produced by: quality: 僖 :: batteries, electrolyzed water, and electrochemical reduction method =, restriction 'make the performance of traditional impregnated B Li \ electricity can not be effectively improved. Qi Ribo has been applied to promote the quality transmission in the ultrasonic cleaning # Rong good. The political fruit, and also successfully applied ultrasound application 偟 ° σ; In view of this, the present invention will be immersion reduction to prepare the electrode method In the use of ultra-thin: to further improve the efficiency of the prepared electrode. Sorrow for the inherent defects of the reduction method. Summary of the invention The present invention lies in: ^ A method for preparing a thunder wave to increase the surface area of a metal film. The process uses-supersonic and increases the sensing t area of one of the electrodes formed in the electrode. 'And μ <' The process includes

£: \ Zongrong \ Hongxian \ Revision. Oral payment Page 4 46192 ^ V. Description of the invention (2) Membrane replacement; using an impregnation reduction method to form the metal membrane on the ion exchange membrane; and using the Ultrasound is carried out in the impregnation reduction method. The ultrasound has a frequency and an energy. The sensing capability of the electrode includes a current sensitivity and a recovery time. The ion-father changing membrane is a Nafion series, including: a Nafion⑻NR50,-

Nafion (R) 117, a Nafion (R) 324, a Nafion (R) 417 and — Nafion (R) 423. The above electrode manufacturing process, wherein the impregnation reduction method includes: preparing a metal solution, the metal solution includes platinum, gold, and silver solutions, etc. The ion exchange membrane is immersed in the metal solution for a period of time, and the first period is 0 to 120 minutes' for ion exchange to produce a gold-exchange thin film; and to prepare a reducing solution, soak the metal ion into the reducing solution for a second period of time. At 120 minutes, the reducing solution is a NaBH4 solution, and the process is performed for one day, and the metal thin film is formed on the ion exchange membrane to form the electrode, wherein the frequency range of the ultrasonic wave is ^. kHζ ′. The energy range is 0 to 1000 wa 11 s; the electrode system is two, which can be applied to a sensor, a fuel cell, and a hydroelectric body for analysis. > Electrolysis and an electrochemistry This case can be understood by the following chart and detailed description, a foot of ice into the picture: Figure 1 ·· The device diagram of the electrode preparation in this case;

Λ6 1 92Γ V. Description of the invention (3) " —:-^ 3: Cyclic voltammogram of the electrode prepared by the second method and the traditional method. The conditions for performing the n-pass test were: 1MH2S04,25. 2v (vs g / AgCl) '100mV / s and 10 cycies. Figure 3: The amine ion sensing device used when the electrode prepared in this case and the traditional method is used as a sensor; Figure 4. When the electrode prepared in this case and the traditional method is used as a sensor, the amine is detected separately, , The resulting current changes. Sensing conditions: 0.001M NH4OH, 25 ° c, latm, 0.03V (vs. Ag / AgC 1) ^ 1 〇m 1 / min flow rate; Figure 5. Electrodes and traditional methods for changing ultrasonic energy production in this case When the two-pole method prepared is used as a sensor, the amine ions are separately detected, and the current obtained is double. Sensing conditions: 0.00lM NH4〇H, 25〇c, latv, 0.03v (vs. now rate. '= Ray: break with Pt Μ ° ° M impregnation ^, β. A not added during the loading process Ultrasound, electrode in this case (-in the process #: b-187.5 watts; c-225. 0 watts d-262 watts; e-300.0 watts; f-337. 5 watts;., One, this case changes the preparation of ultrasonic energy The results of the cyclic voltammetry experiment of the electrode and electrode '. The cyclic voltammetry: ^ 1MH2S〇- 25 ^-^^. 2V (vs. Ag / AgC〇; ^^ _ Page 6 E: \ Zongrong \ 洪 先 \ Revision.pt (j 46 1 92r V. Description of the invention ⑷ ^ and 10 cycles. Description of content: The impregnated reduction method is used to prepare electrodes such as clams, fuel cells, and ion exchange membrane electrodes. The metal ion crosses $ 2 for electrochemical analysis, etc. However, the original agent is used to reduce metal ions. ^ The original membrane impregnation reduction method is also used in the replacement of the membrane or the reduction solution. The limitation of f to mass transfer makes the limit 'As a result, the efficiency cannot be increased by increasing the surface area. The mass transfer effect is controlled in order to improve the effectiveness of the present invention in using ultrasound to improve the prepared electrode. Take the car: Jiashi surface area, and then increase the early and good performance. The results are explained. One of the implementation examples, the use of beauty: Duon Corporation's ion-exchange membrane Nanon Μ, such as Ξ — — U7 lost in-impregnation In the reduction tank, the 0.01M Pt (II) (NH4) C12 solution was introduced from the left of the mouth, and the tank was placed in a C water bath for 30 minutes to exchange metal ions to the surface of Nanon 7 and then, The tank was taken out from the water, and the pt (丨 丨 ^ NH4 +) C 込 solution was drained. After being rinsed with deionized water, NaBH4 was injected to perform a reduction reaction, so that metal ions exchanged to the surface of Nafion 117 were reduced to a metal on the thallium. The thin film is prepared as a metal-ion exchange rubidium electrode; during the above reaction, an ultrasonic wave is applied according to the design. The traditional method electrode: a_ The electrode is not added in the process (the ultrasonic wave is applied in the process): b_187 5 watts; c-225.0 watts; d-262. 5 watts; e-300. 0

Ε · \ Zongrong \ Hongxian \ Revised Edition ptd Page 7 46192 ^ V. Description of the Invention (5) watts; f-337.5 watts; of which, Ultrasonic Density: Secondary System = Small, Temperature, Geometric Configuration, Ultra Acoustic wave: The size of the radioactivity may vary depending on factors such as J solution, reducing solution, and process time. It is based on production = 9ycllc voltammetry is often used to measure the active surface area of the ion exchange membrane electrode.) 'Conditions of the cyclic voltammetry And lcycles. The results are shown in Fig. 2. lg \ 100 mV / s oxygen… between the horizontal axis === to === 7 two positive:; charge =: how much, depending on the percentage — the weight of the work is proportional to the area of the reaction The reaction area is the active surface area of the electrode (the active surface U is the same. In the case of the same experiment, the higher the oxidation peak is, the more the oxidation between the horizontal axis and the botanical: the more the amount of charge provided by the oxide oxidation, the more the oxidation The larger the material, the larger the active surface area of the electrode, as shown in this figure :: Lei Case: The oxidation peak of electricity produced by the method is significantly higher than the oxidation peak of the traditional method, which shows that The electrode produced by the method in this case has a larger area than the electrode produced by the traditional method. The more accurate number can be calculated by the following formula [j · H. Ye and ρ. S. Fedkiw.

Electrochim. Acta, 41, 221 (1996)]: Active surface area (cm2) (1) = number of surface charges (c) x l (cm2) / 210 (VC)

4 6 19 2? V. Description of the invention (6)

The specific active surface area is determined by dividing the 'active L * winter active surface area by 3.8 cm, and detailed results are shown in Table 1. ^ Example 2 of the second embodiment, the device '2 belongs, the sub-exchange membrane electrode is assembled-sensing the full sound β 雷雷 代' first electrode, a platinum private counter electrode and Ag / Ag are placed in the groove connected to the other side of the membrane (： 1, ^. ^ 1 Introduce the same range of ooiM ΜΗ40 相同 solution, the obtained == shown in Figure 4, from this figure, we can see that when the J method produced by the method is urgently used as a sensor, its current is sensitive ^ ) Is significantly higher than the electrode (4.2 " A) made by the traditional method, but should be equal to two η " 1. . 1 U) is significantly less than the electrode made by the traditional method of the third embodiment. The electrode prepared by the method of the present invention will be used as the electrode of He Qi ^, and the ultrasonic energy according to the method 3 of Example 1 will be used to detect the difference. The results are shown in Figure 4. From this figure, it can be seen that although the lack of electrode Π increases = small changes with the energy of the ultrasonic wave, however, using the second case: Force 2 "Using ultrasonic & while preparing the electrode, the prepared electrode has no: U ί current In terms of sensitivity or short response time, it is due to the electrode prepared by the traditional method. As mentioned above, the process of the present invention uses an ultrasonic wave to impregnate the reduction 4, 6 1 9 2 Γ 5. Description of the invention ( 7) A metal-ion exchange membrane electrode is prepared by the method. Because the ultrasonic wave has the function of promoting mass transmission, the electrode prepared by the process has a large active surface area, which can improve the performance of the electrode. The main point of the invention is that in order to protect the creative effort, this case may be modified by anyone who is familiar with the technology, but it is not as bad as the protection of the patent scope attached.

ΕΛ 宗 荣 \ 洪 先 \ Revision.ptd Page 10

Claims (1)

Use a Naf ion⑴ series ion exchange membrane; π ^ week / make a metal solution, soak the Naf inon (R) series ion exchange membrane; = metal solution order, apply ultrasound for a first period of time, perform ionization The role of the parent to generate a metal ion exchange film; and, + preparing a reducing solution 'soaking the metal ion exchange film in the reducing bath' applying an ultrasonic wave for a second time to perform a reduction reaction to generate the metal film To form the electrode. 2. The electrode manufacturing process according to item 1 of the scope of the patent application, wherein the ammonium ion sensing capability includes a current sensitivity (Sens 丨 t i v 丨 ty) and a response time (recovery time). 3. The electrode manufacturing process according to item 1 in the scope of patent application, wherein the Nafi ON (R) series includes: a Nafion (R) NR50, a Nafion (R) 117, a Naiion (R) 324, a Nafion ( R) 417 and a Nafion (R) 423. 4. The electrode manufacturing process according to item 1 of the scope of patent application, wherein the metal solution includes platinum, gold, silver, and other solutions. 5. The process of electrode according to item 4 of the patent application, wherein the metal solution includes a platinum solution. 6. The electrode manufacturing process according to item 1 of the scope of patent application, wherein the first period of time is 0 to 120 minutes. 7. The manufacturing process of the electrode according to item 1 of the patent application scope, wherein the reducing solution is a NaBH4 aqueous solution. E: \ Zongrong \ Hongxian \ Revision.Ptd Page 11 4 6 19 2? · Patent application range paragraph 8 · The process of electrode described in item 1 of the patent application range, where the first time is 0 to 120 minutes . 9) The process of electrode according to item 1 of the patent application range, wherein the frequency of the ultrasonic wave is 5 to 1000 kHz. Shi declared that the electrification π described in the first item of the patent scope, where the energy range is 0, the structure of the dry cold milk sensing state, η, such as the scope of patent application Watts. The conductor can be used in the process of electrode fabrication. The f * & _ any ~ sensing, VAi ,, must be electrode system-an electrochemical analysis. Fuel cell