CN107702829A - A kind of laser preparation method of copper-based flexible wearable formula pressure sensor - Google Patents
A kind of laser preparation method of copper-based flexible wearable formula pressure sensor Download PDFInfo
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- CN107702829A CN107702829A CN201710851343.2A CN201710851343A CN107702829A CN 107702829 A CN107702829 A CN 107702829A CN 201710851343 A CN201710851343 A CN 201710851343A CN 107702829 A CN107702829 A CN 107702829A
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- 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
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
- G01L1/2287—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges
- G01L1/2293—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges of the semi-conductor type
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- General Physics & Mathematics (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
A kind of laser preparation method of copper-based flexible wearable formula pressure sensor, belongs to laser micro/nano manufacturing field.The preparation of copper electrode in sensor, formed by infrared band laser device secondary process.The material for preparing of copper electrode is made up of cupric nitrate trihydrate, ethylene glycol, formic acid, water, first the film on glass, and then laser direct-writing, is transcribed using dimethyl silicone polymer；The flexible material of sensor is dimethyl silicone polymer.This kind of pliable pressure sensor as electrode material, greatly reduces the cost of raw material using copper.Using laser direct writing method, machining accuracy is high, and processing mode is flexible, and noncontact procession can be achieved.Dimethyl silicone polymer encapsulates copper electrode as flexible substrate so that electrode part has the characteristic such as anti-oxidant, corrosion-resistant.Generally speaking, manufacturing cost of the present invention is relatively low, features simple and practical process, the service life length of sensor.
Description
Technical field
The invention belongs to laser micro/nano manufacturing technology field, is related to laser direct-writing process equipment, specifically a kind of laser straight
Reduction mantoquita material is write to be used to prepare wearable voltage sensitive sensor.
Background technology
At present, wearable device is greatly enhanced in the production and living fields such as man-machine interaction, information identification, medical treatment ＆ health
The production work efficiency and living standard of people.Simultaneously because the wide application of wearable device and the use operation side of simplicity
Method, also it is increasingly subject to the favor of general public.
In general, flexible wearable equipment usually requires Sensitive Apparatus being worked into flexible substrate, the flexible substrate
Need that there is certain ductility, preferable recovery capability after bending property and deformation.When have outer signals (such as sound, light,
Electricity or external force etc.) when being loaded on device, the sensor of device inside will produce the signal generation corresponding with outer signals or
Change.Measured by the external receiver of sensor and be can be achieved by the signal of sensor to certain specific outer signals in real time
Dynamic instrumentation.
Especially because such a device architectures are on flexible substrates, when there is external force to put in equipment, it will be produced can
Restorative deformation.And deformation will bring the structure or change in shape to device inner sensor, and then sensing can be set up
Corresponding relation between device signal and external force.
In numerous materials for preparing wearable flexible sensor, metal_based material is wherein important one kind.Due to working as
When flexible substrate deforms upon, respective change also occurs for the structure of conductive material, thus resistance or electric capacity change rapidly, leads to
The size of external force can be detected by crossing the situation of change of test resistance or electric capacity.Gold, ag material due to its good electric conductivity with
Anticorrosive antioxygenic property turns into the first choice for preparing Metal Substrate flexible wearable sensor.Then due to precious metal materials such as gold and silver
With high costs, which results in the high enterprise of the price of product after commercialization.The copper-based material that thus electric conductivity can be comparable with silver
Become the alternative materials for preparing flexible sensing device.At present, the method for preparing copper-based flexible sensing device has a lot, such as：It is low
Warm sintering, the irradiation of high brightness xenon lamp, plane spraying process etc..Copper product used is generally copper particle, cupric oxide powdered granule
Deng.Can be interweaved copper particle using above-mentioned means the electrode part reticulated as sensor.But Metal Substrate is sensed at present
It is mainly still plane manufacture that device, which prepares common approach, and which results in the preparation technology of the sensor to 3-d modelling is non-
It is often complicated, therefore it is badly in need of a kind of simple, efficient, cost is cheap three-dimensional processing method.On the other hand, due to the copper used at present
Presoma be usually copper or cupric oxide powder, copper powders due to being easily oxidized into nonconducting cupric oxide in atmosphere,
Therefore autoxidation can occur for copper particle in process；And it is difficult all to go back cupric oxide if using cupric oxide powder
Original is into copper, and because the copper after cupric oxide is easy to and reduce in the fabrication process combines, therefore it is difficult to will be unnecessary
Cupric oxide removes.In a word, due to the presence of cupric oxide, the electric conductivity of electrode is greatly diminished in sensor.
It is an object of the invention to provide a kind of easy to operate, copper-based sensor processing method of the cheap practicality of cost.
The present invention provides copper using copper nitrate as precursor material, with reference to laser assisted direct writing technology in flexible material (poly dimethyl silicon
Oxygen alkane) on prepare pressure sensor.The senser element has high sensitivity, and stability is good, dependable performance, can measure in real time
Pressure change.Further, since the cellar area of this kind of sensor is small, pressure is enough measured simultaneously after multiple sensor combinations are encapsulated
Power position.
The content of the invention
The technical problem to be solved in the present invention is：Solve the Three-dimension process and Gao Ling of the existing copper-based sensor of presser sensor formula
The problem of sensitivity.A kind of preparation method for preparing low, good reliability the pressure sensor of cost is provided.
Technical scheme is as follows：
1) cupric nitrate trihydrate, ethylene glycol and deionized water are mixed evenly, until cupric nitrate trihydrate is complete
Portion dissolves, and obtains the precursor material of cupric；
2) ethylene glycol solution of copper nitrate is heated, needs to stir and to be aerated during heating；
3) after solution is cooled to room temperature, formic acid solution is instilled, and stir ultrasonic atomizatio；
4) reacted copper nitrate solution is spun in glass substrate；
5) by the laser of laser by focusing radiation after focusing objective len directly to the copper nitrate film scanning on glass；
6) after the completion of scanning, redundant nitric acid copper solution is cleaned up and dried with deionized water；
7) uncured dimethyl silicone polymer (before solidification) solution is covered on the copper film obtained by step 6)；
8) device is integrally heated so that polydimethyl siloxane material solidifies；
9) dimethyl silicone polymer is peeled off from glass；
Each component is preferably in the precursor material of step (1) cupric：40~50wt% of cupric nitrate trihydrate, ethylene glycol 30
~50wt%, solvent are water surplus, and preferably water is not 0.
Step (3) formic acid is preferably (10-100) with ethylene glycol volume ratio：1；Ultrasonic atomizatio, its supersonic frequency are 20 kilo hertzs
Hereby.
Step 5) laser wavelength is 808 nanometers, and laser type is semiconductor continuous laser, and focusing objective len multiplying power is 5-
20 times, laser power is 1-3W before focusing, and sweep speed is that 1-10 millimeters are per second；
Step 6) dimethyl silicone polymer solution includes dimethyl silicone polymer, curing agent.
Using automatically controlled Three-dimension process platform courses, the operating path in control can be individual layer plane, multi-layer three-dimension structure,
With straight line, netted, circular, spiral shape, the three-dimensional geometrical pattern to interweave.
The present invention principle be：When in laser irradiation to copper nitrate ethylene glycol solution, the area near laser facula
Domain is heated rapidly.When temperature rises to 200 DEG C or so, ethylene glycol is decomposed and generates the aldehydes with reproducibility
Matter.In a heated condition, due to the presence of reproducibility aldehyde radical, the cupric in copper nitrate can be reduced to copper simple substance.Change sentence
Talk about, by the copper for producing electric conductivity and adhered on a glass substrate by the copper nitrate ethylene glycol solution after laser scanning.Will
After dimethyl silicone polymer solidification, the adhesiveness and pliability that have due to itself, the copper electrode on glass substrate can be turned
Record on dimethyl silicone polymer.Thus there can be flexible pressure sensor to use as a kind of.
Compared with prior art, the invention has the advantages that：
(1) this method carries out in-situ reducing to the presoma of copper using semiconductor infrared laser device, laser use so that
Machining accuracy greatly increases, and the untouchable processing mode of laser is also easy to carry out the flexible processing of three dimensional constitution；
(2) this method use copper nitrate as copper electrode presoma, due to abandoning copper and copper oxide particle
Use so that the electric conductivity for the copper electrode prepared greatly increases.Preparation technology is simplified simultaneously, it is not necessary to first prepare copper
Nano-particle material, reach reduction with preparing the purpose of copper electrode using laser writing technology one step of energy.
(3) ultrasonic atomizatio has refining effect for the granular precursor of copper.This can greatly reduce the size of particle simultaneously
The fastness of copper electrode is lifted, the generation of numerous stomatas is effectively prevent, so as to improve the electric conductivity of electrode and stability.
(4) this method is packaged using dimethyl silicone polymer as flexible substrate material and to copper electrode, Neng Gouyou
Effect prevents the problem of oxidation of copper electrode under general condition.
Brief description of the drawings
Fig. 1 laser machines copper electrode schematic diagram
The copper-based sensor simple diagrams of Fig. 2
In figure：1 808 nano wave length semiconductor lasers；2 plane mirrors；3 focusing objective lens；4 copper nitrate ethylene glycol are thin
Film；5 glass substrates；6 Three-dimension process platforms；7 signals receive line；8 dimethyl silicone polymer flexible substrates；9 copper-based sensors；
The sensor of Fig. 3 embodiments 9 at various pressures, the situation of change of resistivity
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Thus
It is not intended that the limitation of the scope of the present invention.
Embodiment 1：
1) by cupric nitrate trihydrate, ethylene glycol, water in mass ratio 10:10:1 be mixed and stirred for it is thoroughly molten to copper nitrate
Solution；
2) solution is heated with stirring to 100 DEG C and is incubated 10 minutes, 300 revs/min of stir speed (S.S.), this process is needed logical
Carried out under wind environment；
3) solution is naturally cooled into room temperature after, formic acid is added dropwise and stirs, wherein formic acid and ethylene glycol volume ratio 100:
1；
4) solution is subjected to ultrasound 30 minutes, the KHz of supersonic frequency 20, stirred；
5) solution is spun in glass substrate, 1000 revs/min of spin speed；
6) copper nitrate ethylene glycol film is scanned using the semiconductor laser of 808 nano wavebands, using 10 times of things
Mirror is focused, and laser power is 3W before focusing, and sweep speed is 5 millimeters per second；
7) redundant nitric acid copper ethylene glycol is washed away with deionized water；
8) by polymethyl siloxane matrix and curing agent according to 10:1 ratio is well mixed, vacuum exhaust 30 minutes, flow coat
On the electrode prepared, solidify 6 hours at 100 DEG C；
9) polydimethylsiloxanefilm film after solidification is peeled off from glass substrate, and by electrode both ends and external signal
Receiving device connects；
Embodiment 2：
Present embodiment is as different from Example 1：Cupric nitrate trihydrate described in step 1), second two
Alcohol, water are 15 in mass ratio:10:1.Other are same as Example 1.
Embodiment 3：
Present embodiment is unlike embodiment 1 or 2：The volume ratio of formic acid described in step 3) and ethylene glycol is 20:
1.Other are identical with embodiment 1 or 2.
Embodiment 4：
Present embodiment is unlike embodiment 1 or 2：Described in step 5 by copper nitrate ethylene glycol spin coating after,
Preheated 1 minute under the conditions of 50 DEG C.Other are identical with embodiment 1 or 2.
Embodiment 5：
Present embodiment is unlike embodiment 1 or 2：20 zoom and focus object lens, laser power are used described in step 6)
For 1W.Other are identical with embodiment 1 or 2.
Embodiment 6：
Present embodiment is unlike embodiment 1 or 2：Use laser scanning speed every for 1 millimeter described in step 6)
Second.Other are identical with embodiment 1 or 2.
Embodiment 7：
Present embodiment is unlike embodiment 1 or 2：Four copper electrodes are prepared described in step 9, are coupled in parallel to
External signal receiving device.Other are identical with embodiment 1 or 2.
It is pointed out that on the premise of design concept of the present invention is not departed from, technology of the those skilled in the art to the present invention
The all variations and modifications that method is made, all should drop into protection scope of the present invention, and the scope of the present invention will by appended right
Ask rather than described above limits, it is intended that all changes in the implication and scope of the equivalency of claim will be fallen
Include in the present invention, any reference in claim should not be considered as to the involved claim of limitation.
Using the effect of following verification experimental verifications present invention：
Embodiment 8：Copper-based pressure sensor method is prepared using laser assisted, prepares the pressure switch of electronic device.
Specifically complete according to the following steps：
1) by cupric nitrate trihydrate, ethylene glycol, water in mass ratio 10:10:1 be mixed and stirred for it is thoroughly molten to copper nitrate
Solution；
2) solution is heated with stirring to 100 DEG C and is incubated 10 minutes, 300 revs/min of stir speed (S.S.), this process is needed logical
Carried out under wind environment；
3) solution is naturally cooled into room temperature after, methanol is added dropwise and stirs, wherein methanol and ethylene glycol volume ratio 100:
1；
4) solution is subjected to ultrasound 30 minutes, the KHz of supersonic frequency 20, stirred；
5) solution is spun in glass substrate, 1000 revs/min of spin speed, spin-coating time is 30 seconds；
6) copper nitrate ethylene glycol film is scanned using the semiconductor laser of 808 nano wavebands, using 10 times of things
Mirror is focused, and laser power is 3W before focusing, and sweep speed is 5 millimeters per second；
7) redundant nitric acid copper ethylene glycol is washed away with deionized water；
8) by polymethyl siloxane matrix and curing agent according to 10:1 ratio is well mixed, vacuum exhaust 30 minutes, flow coat
On the electrode prepared, solidify 6 hours at 100 DEG C；
9) polydimethylsiloxanefilm film after solidification is peeled off from glass substrate, and by electrode both ends and required control
Circuit connects；
10) by touching sensor surface, it is possible to achieve by the switch of control device.
Embodiment 9：Copper-based pressure sensor method is prepared using laser assisted, the pressure for preparing foot force analysis passes
Inductor component.Specifically complete according to the following steps：
1) by cupric nitrate trihydrate, ethylene glycol, water in mass ratio 10:10:1 be mixed and stirred for it is thoroughly molten to copper nitrate
Solution；
2) solution is heated with stirring to 100 DEG C and is incubated 10 minutes, 300 revs/min of stir speed (S.S.), this process is needed logical
Carried out under wind environment；
3) solution is naturally cooled into room temperature after, methanol is added dropwise and stirs, wherein methanol and ethylene glycol volume ratio 100:
1；
4) solution is subjected to ultrasound 30 minutes, the KHz of supersonic frequency 20, stirred；
5) solution is spun in glass substrate, 1000 revs/min of spin speed；
6) copper nitrate ethylene glycol film is scanned using the semiconductor laser of 808 nano wavebands, using 10 times of things
Mirror is focused, and laser power is 3W before focusing, and sweep speed is 5 millimeters per second；
7) redundant nitric acid copper ethylene glycol is washed away with deionized water；
8) by polymethyl siloxane matrix and curing agent according to 10:1 ratio is well mixed, vacuum exhaust 30 minutes, flow coat
On the electrode prepared, solidify 6 hours at 100 DEG C；
9) polydimethylsiloxanefilm film after solidification is peeled off from glass substrate；
10) repeat the above steps 1) to step 9) for several times, multiple sensor parallels are arranged in foot bottom or shoes
Lining, and connect the sensor to the signal receiver of outside, you can the pressure distribution at each position of measurement human foot.
Claims (8)
- A kind of 1. method for preparing copper-based pliable pressure sensor, it is characterised in that comprise the following steps：1) cupric nitrate trihydrate, ethylene glycol and deionized water are mixed evenly, until cupric nitrate trihydrate is all molten Solution, obtains the precursor material of cupric；2) ethylene glycol solution of copper nitrate is heated, needs to stir and to be aerated during heating；3) after solution is cooled to room temperature, formic acid solution is instilled, and stir ultrasonic atomizatio；4) reacted copper nitrate solution is spun in glass substrate；5) by the laser of laser by focusing radiation after focusing objective len directly to the copper nitrate film scanning on glass；6) after the completion of scanning, redundant nitric acid copper solution is cleaned up and dried with deionized water；7) uncured dimethyl silicone polymer solution is covered on the copper film obtained by step 6)；8) device is integrally heated so that polydimethyl siloxane material solidifies；9) dimethyl silicone polymer is peeled off from glass.
- 2. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that step (1) Each component is preferably in the precursor material of cupric：40~50wt% of cupric nitrate trihydrate, 30~50wt% of ethylene glycol, solvent are Water surplus, preferably water are not 0.
- 3. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that step (3) Formic acid is preferably (10-100) with ethylene glycol volume ratio：1.
- 4. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that ultrasound, its Supersonic frequency is 20 KHzs.
- 5. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that step 5) swashs Light device wavelength is 808 nanometers, and laser type is semiconductor continuous laser, and focusing objective len multiplying power is 5-20 times, laser before focusing Power is 1-3W, and sweep speed is that 1-10 millimeters are per second.
- 6. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that step 6) is poly- Dimethyl siloxane solution includes dimethyl silicone polymer, curing agent.
- 7. according to a kind of method for preparing copper-based pliable pressure sensor described in claim 1, it is characterised in that using automatically controlled Three-dimension process platform courses, the operating path in control are individual layer plane or multi-layer three-dimension structure, have straight line, it is netted, circular, One or more of geometrical patterns in spiral shape, three-dimensional intertexture.
- 8. according to the copper-based pliable pressure sensor described in claim any one of 1-7.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109489542A (en) * | 2018-11-15 | 2019-03-19 | 华东理工大学 | Strain transducer and its manufacturing method |
| CN110006334A (en) * | 2019-04-26 | 2019-07-12 | 华东理工大学 | A kind of flexible strain transducer and preparation method thereof based on laser direct-writing pomelo peel |
| CN110137183A (en) * | 2019-04-23 | 2019-08-16 | 深圳市华星光电技术有限公司 | Array substrate and its manufacturing method |
| CN113091970A (en) * | 2021-04-07 | 2021-07-09 | 西京学院 | Self-healing intelligent all-optical flexible diaphragm |
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