CN117887310A - Ink for sweat sensor, preparation method and application - Google Patents
Ink for sweat sensor, preparation method and application Download PDFInfo
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- 210000004243 sweat Anatomy 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title abstract description 25
- 239000013543 active substance Substances 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 30
- 229920000877 Melamine resin Polymers 0.000 claims description 27
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 102000004190 Enzymes Human genes 0.000 claims description 18
- 108090000790 Enzymes Proteins 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- 229920001661 Chitosan Polymers 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 12
- 229920000557 Nafion® Polymers 0.000 claims description 12
- 239000002033 PVDF binder Substances 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 230000036541 health Effects 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical compound CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 239000004800 polyvinyl chloride Substances 0.000 claims description 6
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 108090000854 Oxidoreductases Proteins 0.000 claims description 4
- 102000004316 Oxidoreductases Human genes 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- -1 sodium tetraphenylborate Chemical compound 0.000 claims description 4
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 3
- 108010092464 Urate Oxidase Proteins 0.000 claims description 3
- 229930003270 Vitamin B Natural products 0.000 claims description 3
- 229930003268 Vitamin C Natural products 0.000 claims description 3
- HFKJQIJFRMRSKM-UHFFFAOYSA-N [3,5-bis(trifluoromethyl)phenoxy]boronic acid Chemical compound OB(O)OC1=CC(C(F)(F)F)=CC(C(F)(F)F)=C1 HFKJQIJFRMRSKM-UHFFFAOYSA-N 0.000 claims description 3
- 235000019155 vitamin A Nutrition 0.000 claims description 3
- 239000011719 vitamin A Substances 0.000 claims description 3
- 235000019156 vitamin B Nutrition 0.000 claims description 3
- 239000011720 vitamin B Substances 0.000 claims description 3
- 235000019154 vitamin C Nutrition 0.000 claims description 3
- 239000011718 vitamin C Substances 0.000 claims description 3
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- 102000004366 Glucosidases Human genes 0.000 claims description 2
- 108010056771 Glucosidases Proteins 0.000 claims description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims description 2
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 claims description 2
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229940045997 vitamin a Drugs 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 27
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 abstract description 22
- 239000008103 glucose Substances 0.000 abstract description 22
- 229930003231 vitamin Natural products 0.000 abstract description 16
- 235000013343 vitamin Nutrition 0.000 abstract description 16
- 239000011782 vitamin Substances 0.000 abstract description 16
- 229940088594 vitamin Drugs 0.000 abstract description 16
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 11
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 abstract description 10
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 abstract description 10
- 229940116269 uric acid Drugs 0.000 abstract description 10
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 abstract description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 7
- 239000010931 gold Substances 0.000 abstract description 7
- 229910052737 gold Inorganic materials 0.000 abstract description 7
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 abstract description 5
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 abstract description 5
- 239000008101 lactose Substances 0.000 abstract description 5
- 238000001259 photo etching Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 2
- 230000002503 metabolic effect Effects 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 103
- 229940088598 enzyme Drugs 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000007639 printing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 150000003722 vitamin derivatives Chemical class 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
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- 239000000126 substance Substances 0.000 description 5
- 108010015776 Glucose oxidase Proteins 0.000 description 4
- 239000004366 Glucose oxidase Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229940116332 glucose oxidase Drugs 0.000 description 4
- 235000019420 glucose oxidase Nutrition 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 150000003460 sulfonic acids Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 229960001031 glucose Drugs 0.000 description 3
- KAVKNHPXAMTURG-UHFFFAOYSA-N n-(4-bromonaphthalen-1-yl)acetamide Chemical compound C1=CC=C2C(NC(=O)C)=CC=C(Br)C2=C1 KAVKNHPXAMTURG-UHFFFAOYSA-N 0.000 description 3
- 239000008363 phosphate buffer Substances 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 210000001124 body fluid Anatomy 0.000 description 2
- 239000010839 body fluid Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 108010025188 Alcohol oxidase Proteins 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
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- 229920006255 plastic film Polymers 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
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Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses ink for a sweat sensor, the sweat sensor, a preparation method and application, and relates to the field of sensor preparation. The sweat sensor ink disclosed by the invention comprises conductive ink with improved conductivity and active ink with active substances, is suitable for continuous printing-drying process, has great production efficiency, and can reduce the cost by about 80% compared with a photoetching gold electrode. The obtained sensor has good conductivity, high sensitivity and rich detection function, can detect metabolic micromolecules such as glucose, lactose, uric acid and the like, and microelements such as sodium ions, potassium ions, vitamins and the like, and has good application prospect.
Description
Technical Field
The invention relates to the field of sensor preparation, in particular to ink for a sweat sensor, the sweat sensor, a preparation method and application.
Background
With the progress of technology and the improvement of living standard of people, health problems are becoming a focus of attention. Over a decade recently, wearable devices have been rapidly developed, and light weight, intelligence and convenience in measuring physical signs of the wearable devices have been improved obviously, and various watches and bracelets have been accepted by people gradually.
Among other things, sensitive electronics and sensors are important components of wearable devices, playing a vital role in health monitoring. Currently, commercial wearable sensors detect human activities and vital signs, such as step numbers, temperature, heart rate, blood pressure, etc., based on physical sensing. However, the physical sensor cannot deeply penetrate into the physiological information of the human body at the molecular level, in this aspect, the biological sensor can detect ions and small molecules in body fluid (including sweat, saliva, urine, tears and the like) in a noninvasive manner, so that the health state of the individual can be dynamically tracked, and the physical sensor can more comprehensively detect the health state of the individual, and is a main development direction of the sensor.
Sweat is a liquid secreted by sweat glands, and has the advantages of easy acquisition, convenient sampling and the like compared with other body fluids. Meanwhile, sweat contains a plurality of markers related to human physiological states, such as electrolyte ions, metabolites, nutrients, medicines and the like. Therefore, the sensing technology based on sweat detection gradually becomes an important development direction in the field of new generation wearable health monitoring. Correspondingly, the wearable sweat sensor continuously and closely monitors biomarkers in sweat by being attached to the skin surface, and builds a bridge for in-situ sweat detection and real-time feedback of body information. Therefore, the wearable sweat sensing technology has wide application prospects in the fields of sports health management, noninvasive detection, disease diagnosis, personalized medical treatment and the like in the future.
The key to wearable sweat sensing technology is the development of high performance sweat sensors. Although they have received increasing attention over the last decades, a series of advances have been made, but are still in the laboratory's initial stage of research, and their development and use face numerous scientific challenges. For example: (1) the sweat sensor has insufficient sensitivity and unstable dynamic monitoring accuracy; (2) the sweat sensor has single function and can not monitor various physiological information at the same time; (3) the sweat sensor has a complex preparation method and is difficult to produce and apply in large scale.
Wei Gao et al (Fully integrated wearable sensor arrays for multiplexed in situ perspiration analysis. Nature, 2016, 529, 509-514) from the university of California, U.S. university of California constructed gold electrodes and conductive traces on a flexible polyethylene terephthalate substrate by photolithographic techniques, and fabricated a sweat sensor array based thereon to monitor Na in sweat + 、K + Glucose, lactic acid, and the like. However, on one hand, the method firstly adopts the photoetching technology to construct a gold electrode and a conductive circuit on a flexible substrate, and then the sensitive active substances are dropwise added on the gold electrode layer by layer, so that the preparation method is very complex, and high-purity gold is needed, and the price is high, so that the large-scale production is difficult; on the other hand, the sweat sensor prepared by the report has insufficient sensitivity, can only reach 2.35 nA/mu M, and can not monitor substances (such as vitamins and amino acids) with low concentration in sweat, so that the application range is limited.
Donghua university Hou Chengyi et al (A highly integrated sensing paper for wearable electrochemical sweat analysis, biosensors and Bioelectronics, 2021, 174, 112828) first synthesized Ti 3 C 2 T x MXene material, then screen printing Ti 3 C 2 T x The MXene material is printed on paper to obtain a flexible electrode substrate, and then sensitive active substances are dropwise added on the flexible electrode substrate layer by layer to prepare the glucose and lactose sensor, so that glucose and lactose in sweat can be monitored. However, the report also has the problems of low efficiency, poor precision and the like, and is not beneficial to large-scale production; and because the common MXene material is adopted, the sensitivity of the prepared sweat sensor is not high enough, only 2.4 nA/mu M can be achieved, substances (such as vitamins and amino acids) with low concentration in sweat can not be monitored, only glucose and lactose in sweat can be monitored, the function is single, and the requirements of modern noninvasive detection can not be met.
Therefore, a simple and efficient method is developed, the sweat sensor with high performance and multiple functions is prepared, and the sweat sensor has an important pushing effect on the development of wearable sweat sensing technology and the progress of noninvasive medical treatment.
Disclosure of Invention
To solve the problems encountered in the development of sweat sensors described above, a first aspect of the present invention provides an ink for sweat sensors.
The ink for sweat sensor disclosed by the invention comprises conductive ink and active ink.
Wherein the conductive ink is a solution of melamine modified MXene (MXene-MA), carbon black and polyvinylidene fluoride in N-methylpyrrolidone.
The active ink is a solution containing an active substance, wherein the active substance is an enzyme or a component that can form a selectively permeable membrane. The sensor obtained after printing the active ink is decomposed or penetrated through a specific substance by enzyme or selective penetration membrane to cause the change of an electric signal, thereby realizing the detection of the specific substance.
Preferably, the MXene is selected from Ti 3 C 2 T x 、Ti 2 CT x 、Ti 3 CNT x 、V 2 CT x 、Nb 2 CT x 、Zr 3 C 2 T x 、TiNbCT x 、Nb 4 C 3 T x One or more of the following.
Preferably, dropwise adding a solution of melamine into the solution of MXene, and stirring to obtain the melamine modified MXene, wherein the mass ratio of Mxene to melamine is 5-100:1. The temperature of the reaction is not critical and may be generally carried out at any temperature between 15 and 30 ℃.
In the invention, the conductivity and rheological property of the ink can be adjusted by adjusting the type of MXene and the modification degree of MA so as to optimize the sensitivity and the stability of the final sensor. Wherein, the MA modified MXene is mainly used as an intermediate tie, so that the combination between the MXene and an active substance (such as biological enzyme) is enhanced, and the MA modification degree (i.e. the mass ratio of MA to the MXene-MA) has great influence on printing ink and printing electrodes. For example, trace MA modification has weaker reinforcement effect, excessive MA modification can weaken conductivity of the MXene, and experiments optimize that the mass ratio of MA to the MXene-MA is 1% -8% conveniently.
Preferably, the enzyme is one or more of a glucosidase, a lactate enzyme, a uricase, a vitamin C enzyme, a vitamin A enzyme, a vitamin B enzyme, and an alcohol oxidase.
Preferably, the components forming the selective permeable membrane are one or two of sodium tetra (3, 5-di (trifluoromethyl) phenyl) borate or sodium tetraphenyl borate and dioctyl sebacate, so that the selective permeability is formed for Na or K elements, and the Na and K elements in sweat are detected.
Preferably, enzyme and chitosan are added into a phosphoric acid buffer solution to be stirred and dissolved to obtain a mixed solution, then Nafion solution is added into the mixed solution in a dropwise manner, and the active ink is obtained after uniform stirring. This step is not required for the reaction temperature and is usually carried out at room temperature.
It is further preferred that the mass ratio of enzyme, chitosan and Nafion solution is (0.4-3): 1-1.6): 1.
Preferably, the components capable of forming the selective permeable membrane are added into tetrahydrofuran to obtain a mixed solution, then polyvinyl chloride is added into the mixed solution, and the active ink is obtained after uniform stirring.
It is further preferable that the mass ratio of the sodium tetrakis (3, 5-bis (trifluoromethyl) phenyl) borate or the sodium tetraphenylborate, dioctyl sebacate, polyvinyl chloride and tetrahydrofuran is (1-20): 40-60): 30-80): 500.
In the invention, different sweat sensors are prepared, and different active substance inks are required to be configured. By adjusting the composition and content of the active substance, the kind of substance detected by the sensor and the detection sensitivity can be regulated.
In a second aspect of the present invention, there is provided a sweat sensor obtained using the ink for sweat sensor described above. Specifically, the substrate of the sweat sensor is a flexible film, and a conductive layer and an active layer are sequentially printed on the flexible film. Namely, a conductive layer is printed on the flexible film, and then an active layer is printed on the conductive layer. Wherein the conductive layer and the active layer are printed using the conductive ink and the active ink, respectively.
The invention is not limited to the flexible film, and any plastic film with excellent flexibility and thermal stability suitable for manufacturing the sensor can be selected. In view of production cost and processability, a polyimide film or a polyphenylene sulfide film is preferable.
In a third aspect of the present invention, there is provided a method for manufacturing the sweat sensor, which is a continuous printing method having high printing efficiency.
Specifically, the prepared conductive ink and the prepared active ink are respectively added into two ink rollers, and in the continuous printing process, a flexible polymer film passes through the conductive ink rollers and is printed with a layer of MXene-MA conductive ink; and then the film passes through an active ink roller, and a layer of active substance is printed on the conductive layer pattern, so that the sensor printed with the conductive layer and the active substance is obtained.
Preferably, a high temperature dryer is provided after the conductive ink cylinder and a low temperature dryer is provided after the active ink cylinder.
Further preferably, the temperature of the high temperature dryer is 80-110℃and the temperature of the low temperature dryer is 20-40 ℃.
In the invention, the pattern of the finally obtained sensor array can be adjusted by designing the shape of the ink outlet of the ink cylinder; by controlling the drying temperature and speed of the ink, the microstructure and sensitivity of the sensor can be adjusted.
In a fourth aspect the invention provides the use of a sweat sensor as described above, i.e. in a health monitoring or detection device, e.g. a wearable device, such as a bracelet, a watch.
The ink for sweat sensor disclosed by the invention and the sweat sensor prepared by the ink have the following remarkable advantages.
Firstly, the production efficiency can be obviously provided, and compared with the traditional method for preparing the electrode by photoetching and preparing the sensor by dropwise adding the active substances layer by layer, the ink developed by the invention is suitable for a continuous printing-drying process, can realize the continuous production of the sensor array, and can improve the production efficiency by tens of times.
Secondly, the production cost is greatly reduced. The sensor electrode is prepared by adopting high-purity gold in the traditional process, and the cost is high. Compared with the photoetching gold electrode, the cost of the series of melamine modified MXene-based conductive ink disclosed by the invention can be reduced by about 80%.
Thirdly, the printed electrode has good conductivity. After the melamine is used for modifying the MXene, the dispersibility of the MXene in printing ink can be improved, so that the printing electrode has high conductivity. Through a comparison experiment, the conductivity of the electrode printed by the common MXene conductive ink is about 825S/m, and the conductivity of the electrode printed by the melamine modified MXene conductive ink disclosed by the invention is up to 9631S/m, so that the conductivity is improved by 1067%.
Fourthly, the sensitivity and stability of the sensor are obviously improved. The melamine modified MXene can be firmly combined with active substances, and the printed sensor array has high sensitivity and excellent stability. Through experiments, the sensitivity of the glucose sensor printed by adopting the common MXene conductive ink is 2.1 nA/mu M, while the sensitivity of the glucose sensor printed by adopting the melamine modified MXene conductive ink reaches 9.8 nA/mu M, the sensitivity is improved by 367%, and the detection limit is 0.01 mu M.
Fifthly, the detection function is rich. According to different active substances, the ink and the sensor can detect micro-elements such as glucose, lactose, uric acid and the like, sodium ions, potassium ions, zinc ions, calcium ions, hydrogen ions and the like, vitamins A, vitamin B, vitamin C and the like.
Drawings
FIG. 1 shows Ti as obtained in example 1 of the present invention 3 C 2 T x And Ti is 3 C 2 T x -a comparison photograph after MA has been left to stand for one week;
FIG. 2 is a graph comparing the conductivities of flexible electrodes printed with the conductive inks of example 2 and comparative example 2;
FIG. 3 is a graph showing the comparison of the sensitivity of sweat sensors obtained in examples 3 to 6 and comparative example 2 to simulated sweat of different glucose, vitamin, uric acid and sodium ion concentrations (a is a graph showing the comparison of the sensitivity of simulated sweat of different glucose, b is a graph showing the comparison of the sensitivity of simulated sweat of different vitamin, c is a graph showing the comparison of the sensitivity of simulated sweat of different uric acid, d is a graph showing the comparison of the sensitivity of simulated sweat of different sodium ion concentrations;
FIG. 4 is a schematic diagram of the apparatus of the print sensor used in example 7;
fig. 5 is a schematic diagram of a sensor array patterned in different ways (a is a schematic diagram of a sensor array, b is a schematic diagram of a sensor array, c is a schematic diagram of a sensor array, and c is a schematic diagram of a sensor array).
Detailed Description
The technical scheme of the invention is further described by the following drawings and examples:
example 1: an ink for a sensor for detecting glucose in sweat, comprising a conductive ink and an active ink.
The configuration method of the conductive ink comprises the following steps:
(1) Preparation of MXene material: ti is mixed with 3 AlC 2 The powder was added to a mixed solution of LiF and HCl, followed by heating and stirring at 35℃for 24℃ 24 h, during which process Ti 3 AlC 2 Al of (C) is gradually etched away to obtain a two-dimensional layered MXene material Ti 3 C 2 T x ；
(2) Preparation of MXene-MA: to Ti 3 C 2 T x Dropwise adding melamine solution into the solution, and stirring at room temperature for a period of time to obtain melamine modified MXene (Ti) 3 C 2 T x -MA), wherein as reactants Ti 3 C 2 T x The mass ratio of the Ti to the melamine is 30:1, and the obtained Ti 3 C 2 T x In MA, the mass fraction of melamine is 3.2%;
(3) Configuration of conductive ink: ti to be prepared 3 C 2 T x And (3) dispersing MA, carbon black and polyvinylidene fluoride (PVDF) in the mass ratio of 7:2:1 in N-methyl pyrrolidone (NMP), and uniformly stirring to obtain the conductive ink.
The preparation method of the active ink comprises the following steps: adding a certain amount of glucose oxidase and chitosan into phosphate buffer salt solution (PBS buffer solution), fully stirring at room temperature for dissolution, then dripping a certain amount of perfluorinated sulfonic acid type polymer solution (Nafion solution) into the mixed solution, and uniformly stirring to obtain the active ink, wherein the mass ratio of the glucose oxidase to the chitosan to the Nafion is 1:1.2:1.
FIG. 1 shows the obtained Ti 3 C 2 T x And Ti is 3 C 2 T x Macroscopic comparison of MA after one week of rest, it can be seen that Ti 3 C 2 T x The dispersibility of MA is obviously better than that of Ti 3 C 2 T x Which helps to improve the conductivity of the electrode.
As comparative example 1, an ink for a sensor for detecting glucose in sweat was prepared, which is different from example 1 in that MXene (Ti 3 C 2 T x ) I.e. without melamine modification.
Example 2: a sensor for detecting glucose in sweat is prepared by printing the conductive ink and the active ink obtained in the embodiment 1 on a polyimide flexible film in sequence, and assembling the sensor. Specifically, conductive ink is printed on a flexible film to obtain a first flexible electrode, and then active ink is printed to obtain the sweat sensor.
As comparative example 2, a sensor for detecting glucose in sweat, which is different from example 2 in that the conductive ink and the active ink obtained in comparative example 1 of example 1 were printed on a flexible film, a glucose-sensitive sweat sensor was obtained.
Fig. 2 is a graph comparing the conductivities of the first flexible electrode test printed with the conductive inks of example 2 and comparative example 2. The conductive ink of example 2 gave an electrode conductivity as high as 9631S/m, which was 1067% higher than the electrode conductivity (825S/m) of comparative example 2.
Example 3: an ink for a sensor for detecting glucose in sweat, comprising a conductive ink and an active ink.
The configuration method of the conductive ink comprises the following steps:
(1) Preparation of MXene material: will V 2 AlC powder is added to the mixed solution of LiF and HCl, followed by heating and stirring at 35 ℃ for 24 h, during which process V 2 Al of AlC is gradually etched to obtain two-dimensional layered MXene V 2 CT x ；
(2) Preparation of MXene-MA: to V 2 CT x Dropwise adding melamine solution into the solution, and stirring at room temperature for a period of time to obtain melamine modified MXene (V) 2 CT x -MA), wherein the mass fraction of MA is 8%;
(3) Configuration of conductive ink: v to be prepared 2 CT x And (3) dispersing MA, carbon black and polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone (NMP) according to a ratio of 7:2:1, and uniformly stirring to obtain the high-conductivity ink.
The preparation method of the active ink comprises the following steps: adding a certain amount of glucose oxidase and chitosan into phosphate buffer salt solution (PBS buffer solution), fully stirring at room temperature for dissolution, then dripping a certain amount of perfluorinated sulfonic acid type polymer solution (Nafion solution) into the mixed solution, and uniformly stirring to obtain the active ink, wherein the mass ratio of the glucose oxidase to the chitosan to the Nafion is 0.4:1:1.
Example 4: an ink for a sensor for detecting vitamins in sweat, comprising a conductive ink and an active ink.
The configuration method of the conductive ink comprises the following steps:
(1) Preparation of MXene material: ti is mixed with 3 AlC 2 The powder was added to a mixed solution of LiF and HCl, followed by heating and stirring at 35℃for 24℃ 24 h, during which process Ti 3 AlC 2 Al of (C) is gradually etched away to obtain two-dimensional layered MXene (Ti 3 C 2 T x ）；
(2) Preparation of MXene-MA: to Ti 3 C 2 T x Dropwise adding melamine solution into the solution, and stirring at room temperature for a period of time to obtain melamine modified MXene (Ti) 3 C 2 T x -MA), wherein the mass fraction of MA is 1%;
(3) Configuration of conductive ink: ti to be prepared 3 C 2 T x And (3) dispersing MA, carbon black and polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone (NMP) according to a ratio of 7:2:1, and uniformly stirring to obtain the high-conductivity ink.
The preparation method of the active ink comprises the following steps: adding a certain amount of vitamin oxidase and chitosan into phosphate buffer salt solution (PBS buffer solution), fully stirring at room temperature for dissolution, then dripping a certain amount of perfluorinated sulfonic acid type polymer solution (Nafion solution) into the mixed solution, and uniformly stirring to obtain the active ink, wherein the mass ratio of the vitamin oxidase to the chitosan to the Nafion is 1:1.2:1.
Example 5: an ink for a sensor for detecting uric acid in sweat, comprising a conductive ink and an active ink;
the configuration method of the conductive ink comprises the following steps:
(1) Preparation of MXene material: ti is mixed with 3 AlC 2 The powder was added to a mixed solution of LiF and HCl, followed by heating and stirring at 35℃for 24℃ 24 h, during which process Ti 3 AlC 2 Al of (C) is gradually etched away to obtain two-dimensional layered MXene (Ti 3 C 2 T x ）；
(2) Preparation of MXene-MA: to Ti 3 C 2 T x Dropwise adding melamine solution into the solution, and stirring at room temperature for a period of time to obtain melamine modified MXene (Ti) 3 C 2 T x -MA), wherein the mass fraction of MA is 5%;
(3) Configuration of conductive ink: ti to be prepared 3 C 2 T x And (3) dispersing MA, carbon black and polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone (NMP) according to a ratio of 7:2:1, and uniformly stirring to obtain the high-conductivity ink.
The preparation method of the active ink comprises the following steps: adding a certain amount of urate oxidase and chitosan into phosphate buffer solution (PBS buffer solution), fully stirring at room temperature for dissolution, then dripping a certain amount of perfluorinated sulfonic acid type polymer solution (Nafion solution) into the mixed solution, and uniformly stirring to obtain the active ink, wherein the mass ratio of urea oxidase to chitosan to Nafion is 0.7:1.5:1.
Example 6: an ink for a sensor for detecting sodium ions in sweat, comprising a conductive ink and an active ink.
The configuration method of the conductive ink comprises the following steps:
(1) Preparation of MXene material: ti is mixed with 3 AlC 2 The powder was added to a mixed solution of LiF and HCl, followed by heating and stirring at 35℃for 24℃ 24 h, during which process Ti 3 AlC 2 Al of (C) is gradually etched away to obtain two-dimensional layered MXene (Ti 3 C 2 T x ）；
(2) Preparation of MXene-MA: to Ti 3 C 2 T x Dropwise adding melamine solution into the solution, and stirring at room temperature for a period of time to obtain melamine modified MXene (Ti) 3 C 2 T x -MA), wherein the mass fraction of MA is 6.5%;
(3) Configuration of conductive ink: ti to be prepared 3 C 2 T x And (3) dispersing MA, carbon black and polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone (NMP) according to a ratio of 7:2:1, and uniformly stirring to obtain the high-conductivity ink.
The preparation method of the active ink comprises the following steps: adding a certain amount of sodium tetrakis (3, 5-bis (trifluoromethyl) phenyl) borate and dioctyl sebacate into tetrahydrofuran, fully stirring at room temperature for dissolution, then adding a certain amount of polyvinyl chloride into the mixed solution, and uniformly stirring to obtain the active ink, wherein the ratio of the sodium tetrakis (3, 5-bis (trifluoromethyl) phenyl) borate to the dioctyl sebacate to the tetrahydrofuran to the polyvinyl chloride is 1:60:30:500.
The results of the sensor ink for detecting glucose, detecting vitamins, detecting uric acid, and detecting sodium ions in sweat obtained in examples 3 to 6 above are shown in FIG. 3; FIG. 3 is a comparison of the sensitivity of the sweat sensors of examples 3-6 and obtained by comparative example 2 to simulated sweat at different glucose, vitamin, uric acid, and sodium ion concentrations, showing that the greater the difference in current with concentration, the more sensitive the sensor.
Wherein a of fig. 3 is a sensitivity comparison of simulated sweat at different glucose concentrations; b is the sensitivity contrast of simulated sweat at different vitamin concentrations; c is the sensitivity contrast of simulated sweat at different uric acid concentrations; d is the sensitivity contrast of simulated sweat at different sodium ion concentrations;
as shown in FIG. 3, the sensitivity of the glucose sensor printed by the common MXene conductive ink in FIG. a is 2.1 nA/mu M, and the sensitivity of the glucose sensor printed by the melamine modified MXene conductive ink reaches 9.8 nA/mu M, which improves 367%.
As shown in fig. 3, the vitamin sensor sensitivity shown in fig. b was 1.1 nA/μm and 3.9nA/μm, respectively;
as shown in FIG. 3, the uric acid sensor sensitivity shown in FIG. c was 2.0 nA/. Mu.M and 6.5 nA/. Mu.M, respectively;
as shown in fig. 3, the sensitivity of the sodium ion sensor shown in fig. d is 61 nA/double and 21 nA/double, respectively, wherein the double is that of the concentration, and the concentration is an exponential relationship;
has excellent effects on detecting glucose, vitamins, uric acid and sodium ions.
Example 7: the preparation method of the sensor for detecting vitamins in sweat comprises the steps of using the equipment shown in fig. 4, respectively filling the conductive ink and the active ink in the embodiment 4 into corresponding ink rollers, taking a flexible polyphenylene sulfide film as a substrate of the sensor, and sequentially passing the flexible film through the conductive ink roller, a high-temperature dryer, the active ink roller and a low-temperature dryer to obtain the sensor printed with the conductive layer and the active layer, wherein the temperature of the high-temperature dryer is 110 ℃, and the temperature of the low-temperature dryer is 20 ℃.
Example 8: the preparation method of the sensor for detecting sodium ions in sweat comprises the steps of respectively filling the conductive ink and the active ink in the embodiment 6 into corresponding ink rollers, taking a polyimide flexible film as a substrate of the sensor, and sequentially passing the flexible film through the conductive ink roller, a high-temperature dryer, the active ink roller and a low-temperature dryer to obtain the sensor printed with the conductive layer and the active layer, wherein the temperature of the high-temperature dryer is 80 ℃, and the temperature of the low-temperature dryer is 30 ℃.
By designing the shape of the ink outlet of the two ink cylinders, the pattern of the final sensor array can be adjusted, as shown in fig. 5, where a is the sensor array schematic diagram one; b is a second sensor array schematic diagram; c is a sensor array schematic diagram III; designed according to actual needs.
Example 9: a wristband having the sensor for detecting vitamins in sweat obtained in example 7 mounted therein, which can detect vitamin content in sweat when a wearer moves.
Claims (10)
1. An ink for a sweat sensor, the ink comprising a conductive ink and an active ink; the conductive ink is an N-methyl pyrrolidone solution of melamine modified MXene, carbon black and polyvinylidene fluoride; the active ink is a solution containing an active substance, wherein the active substance is an enzyme or a component that can form a selectively permeable film.
2. The ink of claim 1 wherein the MXene is selected from the group consisting of Ti 3 C 2 T x 、Ti 2 CT x 、Ti 3 CNT x 、V 2 CT x 、Nb 2 CT x 、Zr 3 C 2 T x 、TiNbCT x 、Nb 4 C 3 T x One or more of the following.
3. The ink according to claim 1 or 2, wherein the melamine modified MXene is obtained by dropping the melamine solution into the MXene solution and stirring the solution, wherein the mass ratio of MXene to melamine is 5-100:1.
4. The ink of claim 1, wherein the ink is,
the enzyme is one or more of a glucosidase, a lactate enzyme, a uricase, a vitamin C enzyme, a vitamin A enzyme, a vitamin B enzyme and an ethanol oxidase;
the components capable of forming the selective permeable membrane are one or two of sodium tetra (3, 5-di (trifluoromethyl) phenyl) borate or sodium tetraphenyl borate and dioctyl sebacate.
5. The ink according to claim 1 or 4, wherein,
when the active substance is enzyme, adding the active substance and chitosan into a phosphoric acid buffer solution, stirring and dissolving to obtain a mixed solution, then dripping Nafion solution into the mixed solution, and stirring uniformly to obtain the active ink;
when the active substance is a component capable of forming a selectively permeable membrane, adding the active substance into tetrahydrofuran to obtain a mixed solution, then adding polyvinyl chloride into the mixed solution, and uniformly stirring to obtain the active ink.
6. The ink according to claim 5, wherein,
the mass ratio of the enzyme to the chitosan to the Nafion is (0.4-3): 1-1.6): 1;
the mass ratio of the sodium tetra (3, 5-di (trifluoromethyl) phenyl) borate or the sodium tetraphenylborate, the dioctyl sebacate, the polyvinyl chloride and the tetrahydrofuran is (1-20): 40-60): 30-80): 500.
7. The sweat sensor is characterized in that a substrate of the sweat sensor is a flexible film, and a conductive layer and an active layer are sequentially printed on the flexible film; the conductive layer and the active layer are printed using the conductive ink and the active ink described in claim 1, respectively.
8. The method for manufacturing a sweat sensor according to claim 7, wherein the flexible film is printed by a conductive ink roller and an active ink roller in sequence, so as to obtain the sensor printed with the conductive layer and the active layer.
9. The method of claim 8, wherein a high temperature dryer is provided after the conductive ink cylinder and a low temperature dryer is provided after the active ink cylinder, the high temperature dryer having a temperature of 80-110 ℃ and the low temperature dryer having a temperature of 20-40 ℃.
10. The use of the sweat sensor of claim 7, wherein the sweat sensor is used in a health monitoring or detection device.
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