CN114588846A - Nano cellulose/Ti3C2TXComposite aerogel and preparation method and application thereof - Google Patents
Nano cellulose/Ti3C2TXComposite aerogel and preparation method and application thereof Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 125
- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 32
- 239000002131 composite material Substances 0.000 claims abstract description 82
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 59
- 229920002678 cellulose Polymers 0.000 claims abstract description 45
- 239000001913 cellulose Substances 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 46
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 23
- 238000007710 freezing Methods 0.000 claims description 22
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- 239000007788 liquid Substances 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 230000002457 bidirectional effect Effects 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 claims description 16
- 239000011775 sodium fluoride Substances 0.000 claims description 15
- 235000013024 sodium fluoride Nutrition 0.000 claims description 15
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000004108 freeze drying Methods 0.000 claims description 10
- 239000002121 nanofiber Substances 0.000 claims description 10
- 229920002201 Oxidized cellulose Polymers 0.000 claims description 9
- 229940107304 oxidized cellulose Drugs 0.000 claims description 9
- 238000010257 thawing Methods 0.000 claims description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
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- 230000008569 process Effects 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 3
- 241000609240 Ambelania acida Species 0.000 claims description 2
- 241000251557 Ascidiacea Species 0.000 claims description 2
- 229920002749 Bacterial cellulose Polymers 0.000 claims description 2
- 240000008564 Boehmeria nivea Species 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 125000003172 aldehyde group Chemical group 0.000 claims description 2
- 239000005016 bacterial cellulose Substances 0.000 claims description 2
- 239000010905 bagasse Substances 0.000 claims description 2
- 239000012520 frozen sample Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
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- 239000002994 raw material Substances 0.000 description 3
- 235000010086 Setaria viridis var. viridis Nutrition 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 244000304962 green bristle grass Species 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- -1 Polydimethylsiloxane Polymers 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 229910000077 silane Inorganic materials 0.000 description 1
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- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
The invention relates to nano-cellulose/Ti3C2TXThe composite aerogel is obtained by orderly and densely stacking a plurality of layers of wavy layered materials, wherein the layered materials are nano cellulose and Ti3C2TXUniformly mixing the components, and coating a layer of methyltrimethoxysilane on the surface of each layer of the layered material. The aerogel provided by the invention is light in weight, has a wave-shaped layered structure and hydrophobic property which are orderly stacked in the aerogel, has lasting high compression elasticity, has good pressure sensing performance, and is used for assembling a pressure sensor with the sensitivity as high as 4.05kPa‑1The 50ms response time and the pressure detection limit of 1Pa can be used for detecting physiological signals such as finger bending, heartbeat, sounding and the like, the defect that the conventional cellulose-based aerogel is poor in compression elasticity and difficult to practically apply is overcome, and the method has great application potential in the fields of multifunctional sensors and electronic skins.
Description
Technical Field
The invention belongs to the technical field of aerogel, and particularly relates to nano-cellulose/Ti3C2TXComposite aerogel and a preparation method and application thereof.
Background
The human skin can not only perceive external pressure, but also can perceive external temperature and humidity. The related researchers research the sensing materials and expect to realize the sensing function of the electronic skin. The conductive aerogel is widely applied to the field of sensors due to the advantages of ultra-light weight, rich pore structure, excellent compressibility and the like. The cellulose aerogel is widely used as a frame material for preparing the aerogel sensor due to the characteristics of greenness, no pollution, wide sources, good biocompatibility, light weight, good compressive strength and the like. However, cellulose aerogel has poor electrical conductivity, making it difficult to use as the only material for preparing electronic skin. In addition, the general cellulose aerogel has poor compression recovery performance due to random internal structure, and is difficult to meet the daily use requirement of electronic skin. Simultaneously, because the cellulose has abundant hydrophilic group, after absorbing the hydrone, the cellulose aerogel can make its inner structure take place to bond because powerful water tension under the effect of external force, finally destroys the structure of aerogel, and this makes the cellulose aerogel be difficult to use for a long time in practical application. Therefore, how to endow the cellulose composite aerogel with good compression performance and solve the problem of water absorption failure so that the aerogel keeps compression elasticity is a great challenge in the field of cellulose-based aerogels and has important significance for expanding the application of the cellulose-based aerogels.
Disclosure of Invention
The invention aims to solve the technical problem of providing the nano-cellulose/Ti aiming at the defects in the prior art3C2TXComposite aerogel andpreparation method and application thereof, and nano-cellulose/Ti3C2TXThe composite aerogel has high compression elasticity, has a pressure sensing function and has potential application prospects in the field of electronic skins.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
providing a nano-cellulose/Ti3C2TXThe composite aerogel is obtained by orderly and densely stacking a plurality of layers of waved layered materials, wherein the layered materials are nano-cellulose and Ti3C2TXUniformly mixing, and coating a layer of methyltrimethoxysilane (MTMS) on the surface of each layer of the layered material.
According to the scheme, the thickness of the wavy layered material is 0.1-1 mu m, and the distance between the layered materials is less than 200 mu m.
According to the scheme, the nano-cellulose/Ti3C2TXTi in composite aerogel3C2TXThe mass percentage of the component (A) is 10-70%.
The invention also comprises the nano-cellulose/Ti3C2TXThe preparation method of the composite aerogel comprises the following specific steps:
1) preparation of TEMPO oxidized cellulose nanofibers: adding TEMPO, natural fiber, NaBr and NaClO into deionized water, stirring uniformly, then dropwise adding NaOH solution to keep the pH value of the system at 9, carrying out oxidation reaction under the condition of stirring at room temperature, and then adding NaBH4Reducing incompletely oxidized aldehyde groups, performing suction filtration to neutrality after the reaction is finished, washing the obtained solid to neutrality, and dispersing the solid in deionized water to obtain dispersion liquid (TOCN dispersion liquid) of TEMPO oxidized cellulose nanofibers;
2) preparation of Ti3C2TX: adding sodium fluoride into concentrated hydrochloric acid, stirring until the sodium fluoride is completely dissolved to obtain an etching solution, and then adding Ti3AlC2Adding into etching solution for etching reaction, centrifuging with deionized water to wash the reaction solution after reaction, collecting precipitate, re-dispersing in deionized water, freezing in refrigerator, and taking out of the refrigeratorThawing, performing multiple circulating freeze thawing processes, ultrasonically dispersing the obtained dispersion liquid in nitrogen atmosphere, centrifuging the obtained suspension, and collecting upper layer dispersion phase to obtain Ti3C2TXA dispersion liquid;
3) nano cellulose/Ti3C2TXPreparing a composite aerogel: mixing the dispersion of TEMPO oxidized cellulose nano-fiber obtained in the step 1) and the Ti obtained in the step 2)3C2TXMixing the dispersion liquid and stirring uniformly, then performing bidirectional freezing on the obtained mixed liquid, and freeze-drying the frozen sample to obtain the TOCN/Ti3C2TXComposite aerogel, and the obtained TOCN/Ti3C2TXPlacing the composite aerogel and methyltrimethoxysilane in a vacuum drying oven, and heating to deposit the methyltrimethoxysilane to the TOCN/Ti3C2TXThe surface of the composite aerogel obtains the nano-cellulose/Ti with hydrophobic surface3C2TXComposite aerogel (M-TOCN/Ti)3C2TX)。
According to the scheme, the natural cellulose in the step 1) is one or more of cotton cellulose, wood pulp cellulose, ramie cellulose, bagasse cellulose, bacterial cellulose and ascidian cellulose.
According to the scheme, the TEMPO, the natural fiber, NaBr, NaClO and NaBH in the step 1)4The mass ratio of (1): 5-100: 5-100: 5-100: 5 to 100. Wherein natural fiber is used as fiber raw material, NaClO is used as oxidant, TEMPO is used as catalyst, NaBr is used as cocatalyst, NaBH4Is used as a reducing agent.
According to the scheme, the solid obtained in the step 1) is washed to be neutral and dispersed in deionized water, and the dispersion mode is one of mechanical stirring, high-pressure homogenization treatment, an ultrasonic cell disruptor, ball milling treatment and high-speed water impact treatment.
According to the scheme, the concentration of the dispersion liquid of the TEMPO oxidized cellulose nano-fibers in the step 1) is 0.1-2 wt%.
According to the scheme, the concentration of the concentrated hydrochloric acid in the step 2) is 5-12 mol/L, and the molar ratio of hydrochloric acid to sodium fluoride in the etching solution is 1-4: 1.
according to the scheme, the Ti in the step 2)3AlC2The mass ratio of the sodium fluoride to the sodium fluoride in the etching solution is 0.2-5: 1.
according to the scheme, the etching reaction temperature in the step 2) is 25-36 ℃, and the etching reaction time is 2-24 hours.
According to the scheme, the Ti in the step 2)3AlC2The particle size is 100 to 600 mesh.
According to the scheme, the number of the circulating freeze thawing times in the step 2) is 1-5.
According to the scheme, the Ti in the step 2)3C2TXThe concentration of the dispersion is 1-20 mg/mL. Step 2) etching off multilayer Ti by using a mixed solution of sodium fluoride and concentrated hydrochloric acid as an etchant3AlC2In order to obtain a multilayer Ti which is more easily peelable as a monolithic layer3C2TXFurther processing the multilayer Ti by using a freeze thawing method and ultrasound3C2TXTi exfoliated as a single layer3C2TX。
According to the scheme, Ti in the mixed solution in the step 3) is added3C2TXBased on the total mass of solids therein (TOCN and Ti)3C2TX) 10-70% of the total weight of the steel.
According to the scheme, the bidirectional freezing method in the step 3) comprises the following steps: and injecting the mixed solution into a bidirectional freezing mould, placing the bidirectional freezing mould on a wedge-shaped block, wherein the upper end of the wedge-shaped block is an inclined plane with an inclination angle of 15-30 degrees, the lower end of the wedge-shaped block is in contact with a round copper block, and placing the round copper block in liquid nitrogen to completely freeze the mixed solution for 1-4 hours.
The wedge-shaped block is made of Polydimethylsiloxane (PDMS). According to the scheme, the volume of the methyltrimethoxysilane in the step 3) is equal to the volume of the TOCN/Ti3C2TXThe mass ratio of the composite aerogel is 1-20 mL/g.
According to the scheme, the freeze drying temperature in the step 3) is-10 to-60 ℃, the vacuum degree is 20 to 40Pa, and the freeze drying time is 1 to 4 days.
According to the above scheme, step 3) of depositing methyltrimethoxysilane to TOCN/Ti3C2TXThe specific process conditions of the composite aerogel surface are as follows: reacting and depositing for 2-24 hours at 25-100 ℃ under vacuum condition.
The invention also includes the nano-cellulose/Ti3C2TXThe application of the composite aerogel in the field of sensors.
And a composition comprising the above nanocellulose/Ti3C2TXA composite aerogel sensor.
Compared with cellulose nanofibers obtained by other methods, the TEMPO oxidized cellulose nanofibers prepared by the method have the advantages of being easier to disperse (TOCN has oxidized carboxyl and negative charge, and the nano dispersion can be well realized due to electrostatic repulsion between the negative charges) and can also be used as a good dispersion body of two-dimensional nanosheets. And Ti3C2TXAs a good two-dimensional active conductive material, the Ti prepared by the invention has excellent conductivity and excellent electromagnetic shielding function3C2TXNot only the yield is improved, but also the obtained Ti3C2TXThe size is larger and the distribution is more concentrated. Finally, the nanocellulose (TOCN) and Ti are subjected to a bidirectional freeze drying method3C2TXPrepared into compressive elastic TOCN/Ti with orderly stacked wavy structures3C2TXThe conductive aerogel overcomes the defect of poor elasticity of cellulose-based aerogel. In order to prevent the loss of compression elasticity of the aerogel after absorbing water, hydrophobic methyltrimethoxysilane (MTMS) was further deposited on the surface of the elastic aerogel by thermal chemical vapor deposition to maintain its compression elasticity. The orderly stacked wavy layered structure may exhibit good compression elasticity. Since the water absorption characteristics of the cellulose material cause the loss of the compression elasticity of the aerogel, the defect that the performance of the cellulose aerogel is reduced due to the water absorption is overcome by simply depositing hydrophobic MTMS silane on the surface of the aerogel,the composite aerogel has hydrophobicity and compression elasticity, and is suitable for practical use of the sensor.
The invention has the beneficial effects that: 1. the invention provides nano-cellulose/Ti3C2TXThe composite aerogel is light in weight, has a wave-shaped layered structure and hydrophobic property which are orderly stacked in the composite aerogel, has lasting high compression elasticity (the compression strength is as high as 4.5KPa, and the compression strength can be kept at 92% under 300 times of 10% compression cycles), and the prepared nano-cellulose/Ti aerogel3C2TXThe composite aerogel also has good pressure sensing performance and is used for assembling a pressure sensor with the sensitivity as high as 4.05kPa-1The 50ms response time and the pressure detection limit of 1Pa can be used for detecting physiological signals such as finger bending, heartbeat, sounding and the like, the defect that the conventional cellulose-based aerogel is poor in compression elasticity and difficult to practically apply is overcome, and the method has great application potential in the fields of multifunctional sensors and electronic skins. 2. The preparation method provided by the invention has the advantages of simple process, convenience in operation, no pollution to the environment, low requirement on equipment in the whole process and contribution to industrial production.
Drawings
FIG. 1 shows Ti prepared in example 1 of the present invention3C2TXTEM images of the dispersion;
FIG. 2 is a graph of G-TOCN/Ti prepared in comparative examples 1 and 23C2TX-5 and B-TOCN/Ti3C2TX-5 aerogel compression elasticity test chart;
FIG. 3 shows M-TOCN/Ti prepared in example 13C2TX-SEM image of 10 composite aerogel;
FIG. 4 is the M-TOCN/Ti prepared in example 13C2TX-10 composite aerogel stress-strain plot;
FIG. 5 shows M-TOCN/Ti prepared in example 13C2TX-10 static contact angle photo of composite aerogel surface to water;
FIG. 6 shows M-TOCN/Ti prepared in examples 1 and 23C2TXCompoundingCurrent (I) -time (t) plot for aerogel sensor;
FIG. 7 shows M-TOCN/Ti prepared in example 23C2TX-30 stress-strain plots of composite aerogels;
FIG. 8 shows M-TOCN/Ti prepared in example 23C2TX-30 photo of composite aerogel on green bristlegrass;
FIG. 9 is a graph of current (I) versus time (t) for detecting finger bending for the sensor prepared in example 1;
fig. 10 is a graph of current (I) -time (t) curves of the sensor prepared in example 2 for detecting the pulse of a human body.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Comparative example 1
Preparation of TOCN/Ti3C2TXThe composite aerogel comprises the following steps:
1) preparation of TOCN dispersion: adding 2g of wood pulp cellulose, 0.032g of TEMPO and 0.2g of NaBr into 200mL of deionized water, magnetically stirring for dissolving, then adding 5.56mL of NaClO aqueous solution with the concentration of 5mmol/g, keeping the pH value of the system at 9.0 for oxidation reaction (reaction for 2h) under the titration condition of 0.5M NaOH solution, and adding 0.2g of NaBH after the reaction is finished4Continuing to perform reduction reaction, washing with deionized water after 3h, filtering to neutrality, adding deionized water for dispersion, mechanically stirring, and homogenizing under high pressure to obtain 0.5 wt% of TOCN dispersion solution with diameter of about 3nm and length of about 1 μm;
2) preparation of Ti3C2TX: adding 1.6g of sodium fluoride into 20mL of concentrated hydrochloric acid with the concentration of 12mol/L, stirring until the sodium fluoride is completely dissolved to obtain an etching solution, and then adding 1g of Ti into 5 batches in 5 minutes3AlC2Etching the raw materials (200 mesh in size) in etching solution, reacting at 36 deg.C for 24 hr, washing the reaction solution with deionized water, centrifuging at 3500rpm to pH 5, collecting precipitate, and dispersing in deionized waterFreezing in water at-20 deg.C for 12 hr, thawing in refrigerator, performing five cycles of freeze thawing, ultrasonically dispersing the obtained dispersion under nitrogen atmosphere for 30 min, centrifuging at 7000rpm for 0.5 hr, collecting upper dispersion phase to obtain Ti single layer or few Ti single layer3C2TXA dispersion, the concentration of the dispersion being set to 5 mg/mL;
3) preparation of TOCN/Ti3C2TXComposite aerogel: taking 19g of the TOCN dispersion prepared in the step 1) and 1mL of Ti prepared in the step 2)3C2TXDispersing the mixture, mixing and stirring for 6 hours to obtain a uniform mixed solution, wherein the TOCN and the Ti in the mixed solution3C2TXThe total mass of (A) is 100mg, and the mass ratio of TOCN: ti3C2TX95: 5, density of-5 mg/cm3Pouring the mixed solution into a small square plastic box mold of 3cm × 3cm × 3cm, freezing the mold in liquid nitrogen, and freeze-drying the frozen material at-60 deg.C under 30Pa for 24 hr to obtain freeze-dried G-TOCN/Ti3C2TXAnd (3) compounding the aerogel.
G-TOCN/Ti prepared by the comparative example3C2TXThe composite aerogel constitutes the main sensing element, G-TOCN/Ti3C2TXAnd respectively arranging copper foil electrodes on the upper surface and the lower surface of the composite aerogel, connecting the electrodes with a copper wire, and finally packaging to prepare the high-compression-elasticity flexible pressure sensor.
The mechanical properties of the aerogel were measured at room temperature using an MTS excepted E44 (China) electromechanical universal tester. G-TOCN/Ti3C2TXAerogels exhibit poor compression elasticity and do not recover after being deformed by force, as shown in figure 2 a. Mainly because the inside of the conventional freeze-dried aerogel is of a disordered structure and is easily damaged when being subjected to external pressure.
The G-TOCN/Ti prepared in this comparative example was measured in real time at a direct current voltage of 1V using an electrochemical workstation model CHI 660E3C2TXCurrent (I) -time (t) curve of composite aerogel with KH-01 stepping motor and dynamometer asThe auxiliary equipment performs a series of electrical signal response tests. The sensor can not generate electric signal response and has almost no sensing performance, mainly because of Ti in aerogel3C2TXThe content is too small, so that the composite aerogel has poor conductivity and no sensing performance.
Comparative example 2
Preparation of TOCN/Ti3C2TXThe composite aerogel comprises the following steps:
1) preparation of TOCN dispersion: the method of comparative example 1 was used to prepare a dispersion of TOCN at a concentration of 0.5 wt%;
2) preparation of Ti3C2TX: ti of 5mg/mL concentration was prepared by the method of comparative example 13C2TXA dispersion liquid;
3) preparation of TOCN/Ti3C2TXComposite aerogel: taking 19g of the TOCN dispersion prepared in the step 1) and 1mL of the Ti prepared in the step 2)3C2TXDispersing the mixture, mixing and stirring for 6 hours to obtain a uniform mixed solution, wherein the TOCN and the Ti in the mixed solution3C2TXThe total mass of (A) is 100mg, and the mass ratio of TOCN: ti (titanium)3C2TX95: 5, density of 5mg/cm3Pouring the mixed solution into a small plastic square box mold of 3cm multiplied by 3cm, placing the mold on a wedge-shaped block, wherein the upper end of the wedge-shaped block is an inclined plane with an inclination angle of 15 degrees, the lower end of the wedge-shaped block is contacted with a round copper block, placing the round copper block in liquid nitrogen for bidirectional freezing for 1h, and finally, freeze-drying the frozen material at the temperature of minus 60 ℃ and under the condition of 30Pa for 24h to obtain the bidirectional freeze-dried B-TOCN/Ti3C2TXAnd (3) compounding the aerogel.
B-TOCN/Ti prepared by the comparative example3C2TXComposite aerogel composition as the main sensing element, B-TOCN/Ti3C2TXAnd respectively arranging copper foil electrodes on the upper surface and the lower surface of the composite aerogel, connecting the electrodes with copper wires, and finally packaging to prepare the high-compression-elasticity flexible pressure sensor.
Adopts MTS excepted E44 (China) electromechanical universal testerThe mechanical properties of the composite aerogel, B-TOCN/Ti prepared in the comparative example, were measured at room temperature3C2TXThe aerogel shows good compression elasticity and can recover the original shape after being stressed and deformed, as shown in fig. 2b, mainly because the aerogel prepared by adopting the two-way freeze drying has an orderly stacked wavy layered structure and has excellent compression elasticity, but the compression elasticity of the aerogel gradually decreases along with the prolonging of the standing time in the air, and mainly because the strong water absorption of the cellulose causes the damage of the aerogel structure.
The TOCN/Ti prepared in this comparative example was measured in real time at a direct current voltage of 1V using a CHI 660E type electrochemical workstation3C2TXThe current (I) -time (t) curve of the composite aerogel shows that the sensor can not generate an electric signal response and has almost no sensing performance, mainly because of Ti in the aerogel3C2TXThe content is too small, so that the composite aerogel has poor conductivity and no sensing performance.
Example 1
Preparation of TOCN/Ti3C2TXThe composite aerogel comprises the following steps:
1) preparation of TOCN dispersion: adding 2g of wood pulp cellulose, 0.032g of TEMPO and 0.2g of NaBr into 200mL of deionized water, magnetically stirring for dissolving, then adding 5.56mL of NaClO aqueous solution with the concentration of 5mmol/g, keeping the pH value of the system at 9.0 for oxidation reaction (reaction for 2h) under the titration condition of 0.5M NaOH solution, and adding 0.2g of NaBH after the reaction is finished4Continuing to perform reduction reaction, washing with deionized water after 3h, filtering to neutrality, adding deionized water for dispersion, mechanically stirring, and homogenizing under high pressure to obtain 0.5 wt% of TOCN dispersion solution with diameter of about 3nm and length of about 1 μm;
2) preparation of Ti3C2TX: adding 1.6g of sodium fluoride into 20mL of concentrated hydrochloric acid with the concentration of 12mol/L, stirring until the sodium fluoride is completely dissolved to obtain an etching solution, and then adding 1g of Ti into 5 batches in 5 minutes3AlC2Etching the raw materials (200 mesh) in etching solution at 36 deg.C for 24 hr, washing with deionized waterWashing the reaction solution, centrifuging at 3500rpm to pH value of about 5, collecting precipitate, re-dispersing in deionized water, freezing at-20 deg.C for 12 hr, thawing in refrigerator, performing five cycles of freeze thawing, ultrasonically dispersing the obtained dispersion in nitrogen atmosphere for 30 min, centrifuging at 7000rpm for 0.5 hr, and collecting upper layer dispersion phase to obtain Ti3C2TXA dispersion, the concentration of the dispersion being 5 mg/mL;
3) preparation of TOCN/Ti3C2TXComposite aerogel: taking 19g of the TOCN dispersion prepared in the step 1) and 1mL of Ti prepared in the step 2)3C2TXDispersing the mixture, mixing and stirring for 6 hours to obtain a uniform mixed solution, wherein the TOCN and the Ti in the mixed solution3C2TXThe total mass of (A) is 100mg, and the mass ratio of TOCN: ti3C2TX90: 10, density of-5 mg/cm3Pouring the mixed solution into a plastic mold of 3cm multiplied by 3cm, placing the mold on a bidirectional freezing device for bidirectional freezing, placing the mold on a wedge-shaped block, wherein the upper end of the wedge-shaped block is an inclined plane with an inclination angle of 15 degrees, the lower end of the wedge-shaped block is contacted with a round copper block, placing the round copper block in liquid nitrogen for freezing for 1h, and finally, freezing and drying the frozen material for 24h under the conditions of-60 ℃ and 30Pa vacuum degree to obtain the bidirectional freeze-dried B-TOCN/Ti3C2TXCompounding aerogel, and freeze drying B-TOCN/Ti in two directions3C2TXPlacing the composite aerogel and 2mL of MTMS in a vacuum drying oven at the same time, and performing reaction and deposition at 75 ℃ for 12 hours to obtain hydrophobic M-TOCN/Ti3C2TX-10 composite aerogels.
This example, Ti prepared in step 2)3C2TXThe TEM image of the dispersion is shown in FIG. 1, in which Ti is seen3C2TXIs a few-layer or single-layer structure, the thickness of a single layer is about 1nm, and the transverse dimension is about 600 nm.
FIG. 3 shows M-TOCN/Ti prepared in this example3C2TXSEM image of-10 composite aerogel, which can be seen to have orderly stacked wavy lamellar nodulesThe thickness of each layer is about 1 μm, and the distance between each layer is less than 200 μm.
M-TOCN/Ti was measured at room temperature using MTS excepted E44 (China) electromechanical universal tester3C2TX-10 mechanical and compression properties of the composite aerogel. The aerogel shows good compression elasticity and can recover the original shape after being stressed and deformed, because of the uniform composite of the TOCN/Ti3C2TXThe microstructure shows a wave-shaped lamellar structure, so that the composite aerogel has excellent compression elasticity, and the compression elasticity cannot be lost when the composite aerogel is placed in the air after hydrophobic modification. FIG. 4 shows M-TOCN/Ti prepared in this example3C2TX-10 composite aerogel stress-strain curve, from which it can be seen that the aerogel has a high compressive strength of 4.5 KPa.
FIG. 5 shows the M-TOCN/Ti prepared in this example3C2TX-10 static contact angle photo of the surface of composite aerogel against water, the hydrophobic angle of the aerogel is 120 ° as seen from fig. 5.
The M-TOCN/Ti prepared in this example was added3C2TX-10 composite aerogel composition sensor main element, M-TOCN/Ti3C2TXAnd (3) respectively arranging copper foil electrodes on the upper surface and the lower surface of the-10 composite aerogel, connecting the electrodes with copper wires, and finally packaging to prepare the high-compression-elasticity flexible pressure sensor. The current (I) -time (t) curve of the sensor was measured in real time at a direct voltage of 1V using an electrochemical workstation model CHI 660E, as shown in FIG. 6, based on M-TOCN/Ti3C2TX-10 sensors prepared from composite aerogels exhibit 1.01kPa-1The sensitivity of (2).
The sensor prepared in this example was attached to the finger, and the current (I) -time (t) curve of the sensor was measured in real time at a dc voltage of 1V using a CHI 660E electrochemical workstation, as shown in fig. 9, the current signal increased with the increase of the finger bending angle, indicating that the sensor can be used to detect the finger bending movement.
Example 2
Preparation of TOCN/Ti3C2TXThe composite aerogel comprises the following steps:
1) preparation of TOCN dispersion: a0.5 wt% dispersion of the TOCN was prepared using the method of example 1;
2) preparation of Ti3C2TX: ti was prepared in a concentration of 5mg/mL by the method of example 13C2TXA dispersion liquid;
3) preparation of TOCN/Ti3C2TXComposite aerogel: taking 14g of the TOCN dispersion prepared in the step 1) and 6mL of Ti prepared in the step 2)3C2TXDispersing the mixture, mixing and stirring for 6 hours to obtain a uniform mixed solution, wherein the TOCN and the Ti in the mixed solution3C2TXThe total mass of (2) is 100mg, the mass ratio of TOCN: ti3C2TX70: 30, density of-5 mg/cm3Pouring the mixed solution into a plastic mold of 3cm multiplied by 3cm, placing the mold on a bidirectional freezing device for bidirectional freezing, placing the mold on a wedge-shaped block, wherein the upper end of the wedge-shaped block is an inclined plane with an inclination angle of 15 degrees, the lower end of the wedge-shaped block is contacted with a round copper block, placing the round copper block in liquid nitrogen for freezing for 1h, and finally, freezing and drying the frozen material for 24h under the conditions of-60 ℃ and 30Pa vacuum degree to obtain the bidirectional freeze-dried B-TOCN/Ti3C2TXCompounding aerogel, and freeze drying B-TOCN/Ti in two directions3C2TXPlacing the composite aerogel and 2mL of MTMS in a vacuum drying oven at the same time, and performing reaction and deposition at 75 ℃ for 12 hours to obtain M-TOCN/Ti3C2TX-30 composite aerogels.
B-TOCN/Ti prepared in this example3C2TXThe composite aerogel can be placed on green bristlegrass and does not fall off, and the photo is shown in figure 8, which shows that the composite aerogel has the advantage of light weight, and the density is about 5mg/cm3。
M-TOCN/Ti prepared in this example was measured at room temperature using an MTS Exended E44 (China) electromechanical Universal tester3C2TX-30 mechanical and compression properties of the composite aerogel. The M-TOCN/Ti3C2TXThe-30 composite aerogel shows good compression elasticity, can recover the original shape after being subjected to force deformation, has excellent compression elasticity, and cannot cause loss of the compression elasticity when placed in air. FIG. 7 shows M-TOCN/Ti prepared in this example3C2TX-30 stress-strain curve of composite aerogel under 10% compressive strain, the composite aerogel being compressed 300 times and the compressive strength remaining 92%.
The M-TOCN/Ti prepared in this example was added3C2TX-30 composite aerogel composition sensor main element, M-TOCN/Ti3C2TXAnd (3) respectively arranging copper foil electrodes on the upper surface and the lower surface of the-30 composite aerogel, connecting the electrodes with copper wires, and finally packaging to prepare the high-compression-elasticity flexible pressure sensor. The current (I) -time (t) curve of the sensor was measured in real time at a direct voltage of 1V using an electrochemical workstation model CHI 660E, and the sensor exhibited 4.05kPa as shown in FIG. 6-1Sensitivity of 50ms, response time of 50ms and detection limit of 1 Pa.
The sensor prepared in the embodiment is tightly attached to the pulse of the arm, and the current (I) -time (t) curve of the sensor is measured in real time at a direct current voltage of 1V by using a CHI 660E type electrochemical workstation, as shown in fig. 10, the sensor can generate an obvious signal peak, which indicates that the sensor can be used for detecting pulse beat.
Claims (10)
1. Nano cellulose/Ti3C2TXThe composite aerogel is characterized by being obtained by orderly and densely stacking a plurality of layers of wavy layered materials, wherein the layered materials are nano cellulose and Ti3C2TXUniformly mixing the components, and coating a layer of methyltrimethoxysilane on the surface of each layer of the layered material.
2. The nanocellulose/Ti of claim 13C2TXThe composite aerogel is characterized in that the thickness of the wavy layered material is 0.1-1 mu m, and the distance between the layered materials of all layers is less than 200 mu m; the nano-cellulose/Ti3C2TXTi in composite aerogel3C2TXThe mass percentage of the component (A) is 10-70%.
3. A nanocellulose/Ti as claimed in claim 1 or 23C2TXThe preparation method of the composite aerogel is characterized by comprising the following specific steps of:
1) preparation of TEMPO oxidized cellulose nanofibers: adding TEMPO, natural fiber, NaBr and NaClO into deionized water, stirring uniformly, then dropwise adding NaOH solution to keep the pH value of the system at 9, carrying out oxidation reaction under the condition of stirring at room temperature, and then adding NaBH4Reducing incompletely oxidized aldehyde groups, performing suction filtration to neutrality after the reaction is finished, washing the obtained solid to neutrality, and dispersing the solid in deionized water to obtain dispersion liquid of TEMPO oxidized cellulose nanofibers;
2) preparation of Ti3C2TX: adding sodium fluoride into concentrated hydrochloric acid, stirring until the sodium fluoride is completely dissolved to obtain an etching solution, and then adding Ti3AlC2Adding into etching solution for etching reaction, centrifugally washing reaction solution with deionized water after reaction, collecting precipitate, re-dispersing in deionized water, freezing in refrigerator, thawing in refrigerator, ultrasonically dispersing the obtained dispersion liquid in nitrogen atmosphere for several times, centrifuging the obtained suspension, and collecting upper dispersion phase to obtain Ti3C2TXA dispersion liquid;
3) nano cellulose/Ti3C2TXPreparing the composite aerogel: mixing the dispersion of TEMPO oxidized cellulose nano-fiber obtained in the step 1) and the Ti obtained in the step 2)3C2TXMixing the dispersion liquid and stirring uniformly, then performing bidirectional freezing on the obtained mixed liquid, and freeze-drying the frozen sample to obtain the TOCN/Ti3C2TXComposite aerogel, and the obtained TOCN/Ti3C2TXPlacing the composite aerogel and methyltrimethoxysilane in a vacuum drying oven, and heating to deposit the methyltrimethoxysilane to the TOCN/Ti3C2TXThe surface of the composite aerogel obtains the nano-cellulose/Ti with hydrophobic surface3C2TXAnd (3) compounding the aerogel.
4. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that the natural cellulose in the step 1) is one or more of cotton cellulose, wood pulp cellulose, ramie cellulose, bagasse cellulose, bacterial cellulose and ascidian cellulose; step 1) the TEMPO, natural fiber, NaBr, NaClO and NaBH4The mass ratio of (1): 5-100: 5-100: 5-100: 5 to 100; the concentration of the dispersion liquid of the TEMPO oxidized cellulose nano-fibers in the step 1) is 0.1-2 wt%.
5. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that in the step 2), the concentration of the concentrated hydrochloric acid is 5-12 mol/L, and the molar ratio of hydrochloric acid to sodium fluoride in the etching solution is 1-4: 1; step 2) the Ti3AlC2The mass ratio of the sodium fluoride to the sodium fluoride in the etching solution is 0.2-5: 1; and 2) etching reaction temperature is 25-36 ℃, and etching reaction time is 2-24 h.
6. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that the Ti in the step 2) is3AlC2The particle size is 100-600 meshes; step 2), the number of times of cyclic freezing and thawing is 1-5; step 2) the Ti3C2TXThe concentration of the dispersion is 1-20 mg/mL.
7. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that Ti in the mixed solution in the step 3)3C2TXThe mass of (a) is 10-70% of the total mass of the solid.
8. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that the bidirectional freezing method in the step 3) comprises the following steps: and injecting the mixed solution into a bidirectional freezing mould, placing the bidirectional freezing mould on a wedge-shaped block, wherein the upper end of the wedge-shaped block is an inclined plane with an inclination angle of 15-30 degrees, the lower end of the wedge-shaped block is in contact with a round copper block, and placing the round copper block in liquid nitrogen to completely freeze the mixed solution for 1-4 hours.
9. The nanocellulose/Ti of claim 33C2TXThe preparation method of the composite aerogel is characterized in that the methyltrimethoxysilane is deposited to the TOCN/Ti in the step 3)3C2TXThe specific process conditions of the composite aerogel surface are as follows: reacting and depositing for 2-24 hours at 25-100 ℃ under vacuum condition.
10. nanocellulose/Ti according to claim 1 or 23C2TXThe application of the composite aerogel in the field of sensors.
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