CN109100055B - A kind of preparation method of sulphide-oxide composite Nano pressure sensor - Google Patents
A kind of preparation method of sulphide-oxide composite Nano pressure sensor Download PDFInfo
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- CN109100055B CN109100055B CN201810982411.3A CN201810982411A CN109100055B CN 109100055 B CN109100055 B CN 109100055B CN 201810982411 A CN201810982411 A CN 201810982411A CN 109100055 B CN109100055 B CN 109100055B
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 32
- 239000004744 fabric Substances 0.000 claims abstract description 32
- 229910005949 NiCo2O4 Inorganic materials 0.000 claims abstract description 26
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 20
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 20
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010276 construction Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 230000036571 hydration Effects 0.000 claims description 8
- 238000006703 hydration reaction Methods 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 238000004073 vulcanization Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 claims description 4
- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- VRRFSFYSLSPWQY-UHFFFAOYSA-N sulfanylidenecobalt Chemical class [Co]=S VRRFSFYSLSPWQY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 14
- 238000009940 knitting Methods 0.000 abstract description 8
- 238000005538 encapsulation Methods 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 description 26
- 238000010586 diagram Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 3
- -1 Transition-metal sulphides Chemical class 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 210000001145 finger joint Anatomy 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000011165 3D composite Substances 0.000 description 1
- 229910018298 Cu2Mo6S8 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- PGWMQVQLSMAHHO-UHFFFAOYSA-N sulfanylidenesilver Chemical compound [Ag]=S PGWMQVQLSMAHHO-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/14—Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Measuring Fluid Pressure (AREA)
- Force Measurement Appropriate To Specific Purposes (AREA)
Abstract
A kind of preparation method of sulphide-oxide composite Nano pressure sensor, is related to pressure sensor.Prepare three-dimensional Co9S8Nano whiskers array；Prepare Co9S8‑NiCo2O4Three-dimensional manometer composite construction；Prepare sulphide-oxide composite Nano pressure sensor.The pliable pressure sensor prepared tests the variation of capacitance parameter when being pressurized with small tensiometer.Preparation is simple, is quick on the draw, and Co is prepared on carbon cloth for pliable pressure sensor9S8‑NiCo2O4Three-dimensional large knitting needle structure, then will be with Co9S8‑NiCo2O4The carbon cloth of three-dimensional large knitting needle structure prepares pressure sensor with PDMS encapsulation, and pressure sensor preparation is simple, is quick on the draw, and provides a kind of novel method for the preparation of pliable pressure sensor.
Description
Technical field
The present invention relates to pressure sensors, more particularly, to a kind of sulphide-oxide composite Nano pressure sensor
Preparation method.
Background technique
In recent years, pliable pressure sensor was widely used in terms of flexible electronic device, for example electronic skin, can wear
Wear measuring of human health instrument, robot skin.But the microcosmic upper major part of material used in pressure sensor is planar junction at present
Structure, sensitivity is not high, and complex process limits its scope of application, therefore the pressure sensor with three-dimensional manometer composite construction
Building would be possible to provide new approaches for the preparation of the wearable pressure sensor of high-performance.
Transition-metal sulphides are mostly used for energy storage and catalysis aspect because its crystal structure enriches, has excellent performance
(Hong X,Liu Q,Iocozzi J,et al.Needle‐Leaf‐Like Cu2Mo6S8 Films for Highly
Efficient Visible‐Light Photocatalysis[J].Particle&Particle Systems
Characterization, 2018,35 (1)), it is not applied to capacitance type sensor field also at present.But metal sulfide
Stereochemical structure, such as Co can be grown9S8-NiCo2O4Three-dimensional large knitting needle structure reacts sensitive to pressure, is applied to sensor,
Relative to planar structure, there is very big structure and performance advantage.
Dimethyl siloxane (PDMS) has excellent flexibility, and in encapsulation process, the solid-state PDMS film of bottom is length
There is the carbon cloth of composite construction to provide substrate；The PDMS of upper layer liquid in the curing process, is coated on sulphide-oxide solid
Structure periphery provides bracket for sulfide, makes it while not influencing capacitance variations, non-breakable；Meanwhile PDMS is transparent
Film also strengthens the combination of silver wire and sulphide-oxide, improves sensitivity.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of sulphide-oxide composite Nano pressure sensor.
The present invention the following steps are included:
1) three-dimensional Co is prepared9S8Nano whiskers array；
In step 1), the preparation three-dimensional Co9S8The specific method of nano whiskers array can are as follows: carbon cloth is used third respectively
Ketone, ethyl alcohol, deionized water ultrasonic cleaning, are put into reaction kettle, will pour into reaction kettle containing urea and cobalt chloride hexahydrate solution,
Ultrasound, drying are cooled to room temperature after hydro-thermal reaction, then by the carbon cloth with cobalt hydrate array after hydro-thermal vulcanization reaction is complete again,
It is cleaned and dried to get three-dimensional Co9S8Nano whiskers array；1cm × 1cm carbon cloth can be used in the carbon cloth；Volume can be used in the urea
Mass ratio is 6.25%, and the molar concentration of the cobalt chloride hexahydrate solution can be 0.15M；The time of the ultrasound can be
30min；The temperature of the drying can be 90 DEG C, and the time of the hydro-thermal reaction can be 3h；It is described with cobalt hydrate array
Hydro-thermal vulcanization reaction can hydro-thermal vulcanization reaction 1h, solution used be the hydration of molar concentration 0.01M nine under the conditions of 180 DEG C to carbon cloth again
Sodium sulfide solution；Deionized water and washes of absolute alcohol can be used in the cleaning.
2) Co is prepared9S8-NiCo2O4Three-dimensional manometer composite construction；
In step 2), the preparation Co9S8-NiCo2O4The specific method of three-dimensional manometer composite construction can are as follows: by step
1) with three-dimensional Co in9S8The carbon cloth of nano whiskers array, which is put into reaction kettle, carries out hydro-thermal reaction, and the hydro-thermal reaction uses six
The mixed solution of hydrated nickel chloride and six hydration cobalt sulfides, rinses drying, obtains Co9S8-NiCo2O4Three-dimensional manometer composite construction；
The Nickel dichloride hexahydrate can be used molar concentration 0.005M Nickel dichloride hexahydrate, and the six hydrations cobalt sulfide can be used mole dense
Spend the six hydration cobalt sulfides of 0.01M；The temperature of the hydro-thermal reaction can be 180 DEG C, and the time of hydro-thermal reaction can be 12h.
3) sulphide-oxide composite Nano pressure sensor is prepared.
In step 3), the specific method for preparing sulphide-oxide composite Nano pressure sensor can are as follows: preparation
PDMS film, by prepared PDMS solution, stirring is applied on silicon wafer, then be placed in baking oven and keep the temperature with the method for blade coating,
It then, will be with Co9S8-NiCo2O4Carbon cloth be laid on PDMS film, two silver wires are fixed with silver paste in carbon cloth both sides, then
PDMS solution is coated in carbon cloth surfaces, the 2nd placement baking oven heat preservation obtains sulphide-oxide composite Nano pressure sensing
Device；The thickness of the smearing can be 1mm；The condition kept the temperature in baking oven that is placed in can be to be placed in 80 DEG C of baking ovens to keep the temperature
2h；Described 2nd time the condition for placing baking oven heat preservation can be to be placed in 80 DEG C of baking ovens to keep the temperature 2h.
The pliable pressure sensor that the present invention prepares tests the variation of capacitance parameter when being pressurized with small tensiometer.
Present invention preparation is simple, is quick on the draw, and Co is prepared on carbon cloth for pliable pressure sensor9S8-NiCo2O4It is three-dimensional
Large knitting needle structure, then will be with Co9S8-NiCo2O4The carbon cloth of three-dimensional large knitting needle structure prepares pressure sensor with PDMS encapsulation, should
Pressure sensor preparation is simple, is quick on the draw, and provides a kind of novel method for the preparation of pliable pressure sensor.
The present invention prepares Co on carbon cloth9S8-NiCo2O4Three-dimensional manometer composite construction, then will be this multiple with PDMS
Construction packages are closed, two end electrodes are drawn with filamentary silver, prepare the pressure sensor based on sulphide-oxide composite material.This
Kind pressure sensor has microscopic three-dimensional fine structure, flexible to pressure-sensitivity height, the property with the response of excellent capacitor
Energy.Furthermore this method repeatability is high, and preparation process is simple, provides new method for the preparation of pressure sensor.
Detailed description of the invention
Fig. 1 is the Co prepared in embodiment 19S8SEM (scanning electron microscope) front elevation (amplification factor 2 of nano whiskers array
Ten thousand times).In Fig. 1, scale 200nm.
Fig. 2 is the Co prepared in embodiment 29S8-NiCo2O4SEM (scanning electron microscope) front elevation of nano whiskers array (is put
Big multiple is 3000 times).In Fig. 2, scale is 2 μm.
Fig. 3 is the Co prepared in embodiment 29S8-NiCo2O4SEM (scanning electron microscope) front elevation of nano whiskers array (is put
Big multiple is 1.5 ten thousand times).In Fig. 3, scale is 1 μm.
Fig. 4 is the Co grown in embodiment 2 by hydro-thermal reaction9S8-NiCo2O4Three-dimensional manometer composite construction XRD diagram.?
In Fig. 4, abscissa is 2 times of angle of diffraction (°), and ordinate is the relative intensity (a.u.) of diffraction maximum；◆ sign flag is carbon cloth
The diffraction maximum of substrate, △ sign flag are Co9S8The diffraction maximum of nano needle arrays, ◇ sign flag are NiCo2O4Diffraction
Peak, -- sign flag is Co9S8-NiCo2O4XRD spectrum.
Fig. 5 is the pictorial diagram (1cm × 1cm) in embodiment 3 before sample encapsulation.This sample is with Co9S8-NiCo2O4Three
The carbon cloth for tieing up large knitting needle structure is obtained by embodiment 1 and embodiment 2.
Fig. 6 is will be with Co in embodiment 39S8-NiCo2O4After the carbon cloth of three-dimensional large knitting needle structure is encapsulated with PDMS, acquisition
Sulphide-oxide composite Nano pressure sensor pictorial diagram (1cm × 1cm).
Fig. 7 is the variation of pressure sensor capacitor at 80Pa in embodiment 3, testing time 200s.In Fig. 7,
Abscissa is the time (s), and ordinate is capacitor (pF).
Fig. 8 is the variation of pressure sensor capacitor at 140Pa in embodiment 3, testing time 200s.In fig. 8,
Abscissa is the time (s), and ordinate is capacitor (pF).
Fig. 9 is the variation of pressure sensor capacitor at 180Pa in embodiment 3, testing time 170s.In Fig. 9,
Abscissa is the time (s), and ordinate is capacitor (pF).
Figure 10 is the variation of pressure sensor capacitor at 230Pa in embodiment 3, testing time 200s.In Figure 10
In, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 11 is the variation of pressure sensor capacitor at 400Pa in embodiment 3, testing time 200s.In Figure 11
In, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 12 is the variation of pressure sensor capacitor at 900Pa in embodiment 3, testing time 200s.In Figure 12
In, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 13 is the variation of pressure sensor capacitor at 3000Pa in embodiment 3, testing time 200s.In Figure 13
In, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 14 is the variation of the pressure sensor circle of loop test 20 capacitor at 700Pa in embodiment 3.Testing time is
400s, in Figure 14, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 15 be embodiment 3 in pressure sensor continuously at 80Pa, 180Pa, 230Pa, 900Pa capacitor variation,
In Figure 15, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 16 is that the pressure sensor in embodiment 3 is pasted onto the pictorial diagram at finger-joint.It is curved in finger for testing
It is bent and when loosening, the variation of pressure sensor capacitor.
For Figure 17 for the pressure sensor in embodiment 3 as shown in figure 16 with digital flexion and when loosening, pressure sensor is electric
The variation of appearance.In Figure 17, abscissa is the time (s), and ordinate is capacitor (pF).
Figure 18 is the pressure sensor in embodiment 3 when loosening with finger, and capacitor is restored to the time used in stationary value.?
In Figure 18, abscissa is the time (s), and ordinate is capacitor (pF).
Specific embodiment
Embodiment 1
The urea of 6.25wt% and the cobalt chloride hexahydrate of 0.15M are weighed, is poured into 60mL deionized water, 30min is stirred, it will
It cleans up carbon cloth and is completely soaked ultrasound 30min, the reaction kettle for being then equipped with carbon cloth and reaction solution in the above solution and be put into
3h is reacted at 90 DEG C in baking oven, is cooled to room temperature, rinsed well, dried with deionized water, obtains cobalt sulfide nano whiskers sample
Product.
Hydro-thermal vulcanization is carried out to the cobalt sulfide nano whiskers array of above-mentioned growth, hydro-thermal reaction solution is 60mL 0.01M's
Sodium Sulphate Nine Hydroxide aqueous solution, reaction condition are to react 10h at 180 DEG C.It is then cooled to room temperature, is rinsed with deionized water dry
Only, dry, obtain Co9S8Nano whiskers array.As shown in Figure 1, obtaining Co by two step hydro-thermal reactions9S8Nanoneedle is equably
It is distributed in carbon cloth surfaces.
Embodiment 2
0.005M Nickel dichloride hexahydrate and the six hydration cobalt sulfides of 0.01M are weighed, pours into 60mL deionized water, stirs
30min obtains reaction solution.By above-mentioned reaction solution and with Co9S8The carbon cloth of nano needle arrays is put into 100mL reaction kettle,
Reaction kettle is put into baking oven, 180 DEG C of reaction 2h are then cooled to room temperature, are rinsed well, dried with deionized water, obtained
NiCo2O4Nanometer sheet modifies Co9S8The three dimensional composite structure of nano whiskers, as shown in Fig. 2, NiCo2O4It is coated on Co9S8Nanoneedle
Around.The Co prepared in embodiment 29S8-NiCo2O4(amplification factor is SEM (scanning electron microscope) front elevation of nano whiskers array
1.5 ten thousand times) as shown in Figure 3.As shown in figure 4, further XRD characterization it can also be seen that sample diffraction maximum and NiCo2O4Standard
The matching of PDF card.
Embodiment 3
1) sulphide-oxide composite Nano pressure sensor is prepared
PDMS solution A and solution B are uniformly mixed, and are formed the film of 1mm on silicon wafer by scratching, are put into 80 DEG C of baking ovens
Keep the temperature 2h.After PDMS curing molding, it is removed with silicon wafer, is cut into the square of 1.5cm × 1.5cm, the sample that will be prepared
It is placed on above PDMS film, two silver wires are placed on sample both ends, are fixed with silver paste.It, will after being completely fixed to conducting wire
PDMS is coated in above sample, is smeared uniformly, is placed 80 DEG C of baking oven 2h, and (Fig. 5 is the pictorial diagram in embodiment 3 before sample encapsulation
1cm × 1cm), this sample is with Co9S8-NiCo2O4The carbon cloth of three-dimensional large knitting needle structure, is obtained by embodiment 1 and embodiment 2
?.As shown in fig. 6, can be obtained sulphide-oxide composite Nano pressure sensor.
2) pressure sensor of preparation pressure-capacitor response performance is carried out to test
It is tested with small tension tester, pressure sensor is placed on instrument and is born at pressure, with TH2829 electric bridge
Instrument is separately connected the both ends of pressure sensor electrode,
Be respectively set 80Pa, 140Pa, 180Pa, 230Pa, 400Pa, 900Pa, 3000Pa tested (referring to Fig. 7~
13), in 3000Pa, capacitance variations are maximum.In 700Pa, loop test 20 is enclosed, and as shown in figure 14, pressure sensor is being surveyed
Variation is stablized during examination.Continuous setting 80Pa, 180Pa, 230Pa, 900Pa are tested, as shown in figure 15, pressure sensor
Under different pressure, capacitance variations are obvious.As shown in figure 16, the pressure sensor of preparation is pasted at finger-joint, is carried out
The movement for being bent and loosening.As shown in figure 17, the capacitor of pressure sensor has significant change with the movement of finger.Figure 18 is real
The pressure sensor in example 3 is applied when loosening with finger, capacitor is restored to the time used in stationary value.
Claims (7)
1. a kind of preparation method of sulphide-oxide composite Nano pressure sensor, it is characterised in that the following steps are included:
1) three-dimensional Co is prepared9S8Nano whiskers array, method particularly includes: carbon cloth is used to acetone, ethyl alcohol, deionized water ultrasound respectively
Cleaning, is put into reaction kettle, will pour into reaction kettle containing urea and cobalt chloride hexahydrate solution, ultrasound, drying, after hydro-thermal reaction
It is cooled to room temperature, then by the carbon cloth with cobalt hydrate array after hydro-thermal vulcanization reaction is complete again, is cleaned and dried to get three-dimensional Co9S8
Nano whiskers array；
2) Co is prepared9S8-NiCo2O4Three-dimensional manometer composite construction, method particularly includes: by step 1) with three-dimensional Co9S8Nanometer
The carbon cloth of needle-shaped array, which is put into reaction kettle, carries out hydro-thermal reaction, and the hydro-thermal reaction is using Nickel dichloride hexahydrate and six hydration sulphur
Change the mixed solution of cobalt, rinses drying, obtain Co9S8-NiCo2O4Three-dimensional manometer composite construction；
3) sulphide-oxide composite Nano pressure sensor is prepared, method particularly includes: PDMS film is prepared, it will be prepared
PDMS solution, stirring, is applied on silicon wafer, then be placed in baking oven and keep the temperature with the method for blade coating, then, will be with Co9S8-
NiCo2O4Carbon cloth be laid on PDMS film, two silver wires are fixed with silver paste in carbon cloth both sides, then PDMS solution is coated in
Carbon cloth surfaces, the 2nd placement baking oven heat preservation, obtain sulphide-oxide composite Nano pressure sensor.
2. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
The carbon cloth uses 1cm × 1cm carbon cloth；The urea uses volume mass ratio for 6.25%, the cobalt chloride hexahydrate solution
Molar concentration is 0.15M.
3. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
The time of the ultrasound is 30min；The temperature of the drying is 90 DEG C, and the time of the hydro-thermal reaction is 3h.
4. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
Hydro-thermal vulcanization reaction is hydro-thermal vulcanization reaction 1h under the conditions of 180 DEG C to the carbon cloth with cobalt hydrate array again, used molten
Liquid is molar concentration 0.01M Sodium Sulphate Nine Hydroxide solution；The cleaning uses deionized water and washes of absolute alcohol.
5. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
The Nickel dichloride hexahydrate uses molar concentration 0.005M Nickel dichloride hexahydrate, and the six hydrations cobalt sulfide uses molar concentration
The six hydration cobalt sulfides of 0.01M.
6. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
The temperature of the hydro-thermal reaction is 180 DEG C, and the time of hydro-thermal reaction is 12h.
7. a kind of preparation method of sulphide-oxide composite Nano pressure sensor as described in claim 1, it is characterised in that
The smearing with a thickness of 1mm；The condition kept the temperature in baking oven that is placed in is to be placed in 80 DEG C of baking ovens to keep the temperature 2h；Described
2 times the condition for placing baking oven heat preservation is to be placed in 80 DEG C of baking ovens to keep the temperature 2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810982411.3A CN109100055B (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of sulphide-oxide composite Nano pressure sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810982411.3A CN109100055B (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of sulphide-oxide composite Nano pressure sensor |
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| Publication Number | Publication Date |
|---|---|
| CN109100055A CN109100055A (en) | 2018-12-28 |
| CN109100055B true CN109100055B (en) | 2019-10-18 |
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