CN105675182A - Preparation method of cellulose-based flexible stress-strain sensitive material - Google Patents
Preparation method of cellulose-based flexible stress-strain sensitive material Download PDFInfo
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Abstract
The invention provides a preparation method of a cellulose-based flexible stress-strain sensitive material. The preparation method comprises the steps of: 1) adding cellulose into water and mixing uniformly to form a 0.2-5wt% aqueous solution, and freeze-drying the aqueous solution to prepare a cellulose aerogel; 2) subjecting the cellulose aerogel prepared in the step 1) to pyrolysis processing at high temperature of 600-1000 DEG C for 0.5 to 5 hours under the protection of vacuum or inert atmosphere to prepare a carbon gel; 3) and pouring PDMS resin in the carbon gel, and carrying out vacuum defoamation, thereby the flexible stress-strain sensitive material with high sensitivity is obtained after resin is solidified. The preparation method has the advantages of rich, chip and renewable raw materials, simple and controllable preparation process, and wide strain range and high sensitivity of the prepared stress-strain sensitive material; and the preparation method has good application prospect in aspects of structural health monitoring, electronic skin, biological medicine, wearable electronic product and the like.
Description
Technical field
The preparation method that the present invention relates to a kind of stress-strain sensitive material, the present invention relates to a kind of preparation method based on cellulosic flexibility stress-Strain sensing material in particular, and this material can be used as the core parts of flexibility stress-strain transducer.
Background technology
Pressure transducer is a kind of sensor most commonly seen in each field, is widely used in the fields such as Aero-Space, military project, traffic, building, medical treatment & health. Traditional problem that strain gauge (such as resistance strain gage, semiconductor gauge etc.) exists pliability difference, range of strain is low, it is difficult to adapting to new generation sensor requirement in flexibility and convenience, its range of application is restricted. Novel flexibility stress sensor has the substrate of softness, it is suitable for the non-smooth surface of complexity, bears and significantly deform, greatly extend the range of application of sensor, have a good application prospect in monitoring structural health conditions, electronic skin, biological medicine, wearable electronic product etc. At present based on nano materials such as such as ZnO nano-wire, gold-silver nano-wire, CNT, Graphenes more than the research report of relevant flexibility stress sensor, but the problem such as these flexibility stress sensor ubiquity complicated process of preparation, cost be high.
It addition, developing rapidly recently as global economy, the non-renewable resources such as substantial amounts of coal, oil are constantly consumed, and cause the shortage of resource; Substantial amounts of CO simultaneously2、SO2Etc. the discharge of harmful gas, contaminated environment also causes " greenhouse effect ", the living environment of the serious threat mankind. Biomass, as a kind of Renewable resource, have that raw material is cheap, easily obtain, the feature such as sustainable and environmental friendliness, biomass prepare all kinds of carbon-based material and be increasingly subject to the attention of people. In recent years, people are based on biomass, multiple three-dimensional carbon material is have developed such as coconut husk, Cotton Gossypii, Citrullus vulgaris, Fructus Benincasae etc., this kind of material has the features such as high porosity, hydrophobic oleophilic oil, high conductivity and excellent in mechanical performance, presents good application prospect in fields such as solar energy conversion and storage, ultracapacitor, battery, electromagnetic wave shielding, water process.
Summary of the invention
The purpose of the present invention is for providing a kind of preparation method based on cellulosic flexibility stress-Strain sensing material, the method has abundant raw material, cheap, renewable, preparation technology is simple, controlled, the feature that obtained sensitive material range of strain is big, highly sensitive.
Preparation process based on cellulosic flexibility stress-Strain sensing material provided by the present invention is as follows:
1) preparation of cellulose aqueous solution
Cellulose is added to the water, utilizes stirring, the method such as ultrasonic to make its mix homogeneously, form the cellulose aqueous solution of 0.2～5wt%.
Described cellulose is natural biomass cellulose, Cellulose nanocrystal and the cellulose after chemical treatment.
Described natural biomass cellulose refers to paper cellulose and chitin fiber element.
Described through chemically treated cellulose be carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose.
2) preparation of cellulose aerogels
Above-mentioned cellulose aqueous solution freezing is become solid, carries out lyophilization, can be prepared by cellulose aerogels.
3) preparation of carbon gel
Cellulose aerosol as above, under vacuum or inert atmosphere protection, carries out cracking under the high temperature of 600～1000 DEG C and processes 0.5-5 hour, can be prepared by carbon gel.
4) preparation of flexibility stress-Strain sensing material
Above-mentioned carbon gel will be poured into a mould polymethyl siloxane (PDMS) resin of its volume 1～2 times, vacuum defoamation; After PDMS solidifies, namely prepare and there is highly sensitive flexibility stress-Strain sensing material.
The operation principle of the flexibility stress-Strain sensing material prepared by the present invention: there is good three-dimensional net structure based on the carbon sol prepared by Pintsch process cellulose, this network structure gives the good electric conductivity of carbon sol; PDMS then has good pliability and insulating properties. Composite by carbon gel and PDMS compound gained, not only maintain the pliability of PDMS but also have the electric conductivity of carbon gel concurrently, as shown in Figure 1, when there being extraneous stress to act on composite, soft silicones is easy to deform, thus causing that interior three-dimensional network structure is destroyed, network connection point reduces, thus causing resistance to increase, external force is cancelled rear network structure and is restPosed, and resistance also recovers initial value.
Accompanying drawing explanation
Fig. 1. the fundamental diagram of flexibility stress-Strain sensing material prepared by the present invention
Fig. 2. the SEM photograph of the cellulose carbon gel prepared by the present invention;
Fig. 3. the optical photograph of the flexibility stress-Strain sensing material prepared by the present invention;
Fig. 4. the relative resistance-stress changing curve of flexibility stress-Strain sensing material prepared by the present invention;
Fig. 5. the flexibility stress-Strain sensing material response to cyclic stress prepared by the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
1. 10g paper cellulose is added in 1000g water, utilize blender stirring 1h to form homogeneous solution, prepare the paper cellulose aqueous solution of 1wt%.
2. by step 1. in prepared paper cellulose aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under nitrogen protection, crack 2 hours at 800 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in the PDMS resin of prepared its volume of carbon gel rubber material upper 1.2 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Scanning electron microscope (TEM) photo of prepared cellulose carbon sol is as in figure 2 it is shown, as can be seen from the figure: cellulose carbon sol prepared by the present invention has a large amount of space, has a large amount of contact point, belong to three-dimensional network-like structure between fiber; Prepared carbon gel conductivity is 3.4Sm-1.The optical photograph of prepared stress-strain sensitive material, as it is shown on figure 3, material prepared by as can be seen from the figure has good flexibility, can do 180 ° and fold. Fig. 4 is the relative resistance-stress changing curve of prepared stress-strain sensitive material, it can be seen that the resistance counter stress of material is very sensitive, sensitivity is up to 2.2kPa-1. Fig. 5 is the response to cyclic stress of the prepared stress-strain sensitive material, it can be seen that cyclic stress is had good response by prepared material, more than circulating up to 1000 times service life.
Embodiment 2
1. 2g Cellulose nanocrystal is added in 1000g water, utilize Ultrasound Instrument to form homogeneous solution in ultrasonic 30 minutes, prepare the Cellulose nanocrystal aqueous solution of 0.2wt%.
2. by step 1. in prepared Cellulose nanocrystal aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under argon shield, crack 0.5 hour at 1000 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in the methyl silicone resins (Sylgard184, DowCorning) of prepared its volume of carbon gel rubber material upper 1 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Using method provided by the invention to prepare cellulose carbon sol and have three-dimensional network-like structure, conductivity is 0.82Sm-1. Prepared stress-strain sensitive material has good flexibility, and the resistance counter stress of material is very sensitive, and sensitivity is up to 1.5kPa-1, more than circulating up to 1000 times service life.
Embodiment 3
1. 50g chitin fiber element is added in 1000g water, utilize blender stirring 5h to form homogeneous solution, prepare the chitin fiber element aqueous solution of 5wt%.
2. by step 1. in prepared chitin fiber element aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under vacuo, crack 5 hours at 600 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in the PDMS resin of prepared its volume of carbon gel rubber material upper 2 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Using method provided by the invention to prepare cellulose carbon sol and have three-dimensional network-like structure, conductivity is 0.0012Sm-1. Prepared stress-strain sensitive material has good flexibility, and the resistance counter stress of material is sensitive, and sensitivity is up to 0.8kPa-1, more than circulating up to 1000 times service life.
Embodiment 4
1. 10g carboxymethyl cellulose is added in 1000g water, utilize blender stirring 1h to form homogeneous solution, prepare the carboxymethyl cellulose aqueous solution of 1wt%.
2. by step 1. in prepared carboxymethyl cellulose aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under nitrogen protection, crack 2 hours at 800 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in the PDMS resin of prepared its volume of carbon gel rubber material upper 1.5 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Using method provided by the invention to prepare the density of cellulose carbon sol medium, have three-dimensional network-like structure, prepared carbon gel conductivity is 4.2Sm-1.Prepared stress-strain sensitive material has good flexibility, and the resistance counter stress of material is sensitive, and sensitivity is up to 2.1kPa-1, more than circulating up to 1000 times service life.
Embodiment 5
1. 10g hydroxypropyl methyl cellulose is added in 1000g water, utilize blender stirring 1h to form homogeneous solution, prepare the hydroxypropyl methyl cellulose aqueous solution of 1wt%.
2. by step 1. in prepared hydroxypropyl methyl cellulose aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under nitrogen protection, crack 2 hours at 800 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in the PDMS resin of prepared its volume of carbon gel rubber material upper 1.4 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Using method provided by the invention to prepare the density of cellulose carbon sol medium, have three-dimensional network-like structure, prepared carbon gel conductivity is 2.8Sm-1. Prepared stress-strain sensitive material has good flexibility, and the resistance counter stress of material is sensitive, and sensitivity is up to 1.8kPa-1, more than circulating up to 1000 times service life.
Embodiment 6
1. 10g hydroxyethyl cellulose is added in 1000g water, utilize blender stirring 1h to form homogeneous solution, prepare the hydroxyethyl cellulose aqueous solution of 1wt%.
2. by step 1. in prepared hydroxyethyl cellulose aqueous solution freezing become solid, then utilize freeze drier to dry, prepare cellulose aerogels.
3. by step 2. in prepared cellulose aerogels under nitrogen protection, crack 2 hours at 800 DEG C, prepare based on cellulosic carbon gel rubber material.
4. by step 3. in prepared carbon gel rubber material waters the PDMS resin of its volume 1.4 times, vacuum defoamation, then 80 DEG C solidify 1h, namely prepare based on cellulosic flexibility stress-Strain sensing material.
Using method provided by the invention to prepare the density of cellulose carbon sol medium, have three-dimensional network-like structure, prepared carbon gel conductivity is 3.5Sm-1. Prepared stress-strain sensitive material has good flexibility, and the resistance counter stress of material is sensitive, and sensitivity is up to 1.9kPa-1, more than circulating up to 1000 times service life.
Claims (5)
1. the preparation method based on cellulosic flexibility stress-Strain sensing material, it is characterised in that comprise the following steps:
1) configuration of cellulose aqueous solution, is added to the water cellulose, utilizes stirring or ultrasonic method to make its mix homogeneously, forms the cellulose aqueous solution of 0.2～5wt%.
2) the aerocolloidal preparation of cellulose, by step 1) the cellulose aqueous solution freezing that configures becomes solid, and then carry out lyophilization, can be prepared by cellulose aerogels.
3) preparation of carbon gel, such as step 2) prepared by cellulose aerosol under vacuum or inert atmosphere protection, carry out under the high temperature of 600～1000 DEG C cracking process 0.5-5 hour, can be prepared by carbon gel.
4) preparation of flexibility stress-Strain sensing material, by step 3) prepared by carbon gel in pour into a mould 1～2 times of polymethyl siloxane (PDMS) of its volume, vacuum defoamation; After resin solidifies, namely prepare and there is highly sensitive flexibility stress-Strain sensing material.
2. the preparation method based on cellulosic flexibility stress-Strain sensing material according to claim 1, it is characterised in that: step 1) described in cellulose be natural biomass cellulose, Cellulose nanocrystal and chemically treated after cellulose in one.
3. natural biomass cellulose according to claim 2, it is characterised in that: described natural biomass cellulose is the one in paper cellulose and chitin fiber element.
4. according to claim 2 through chemically treated cellulose, it is characterised in that: described through chemically treated cellulose be the one in carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose.
5. the preparation method based on cellulosic flexibility stress-Strain sensing material according to claim 1, it is characterised in that: step 3) described in noble gas be the one in nitrogen, argon, helium.
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| CN108225621A (en) * | 2018-01-03 | 2018-06-29 | 电子科技大学 | One kind is based on organic field-effect tube pressure sensor and preparation method thereof |
| CN108332888A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院物理研究所 | A kind of full carbon aerogels pressure sensor |
| CN109082930A (en) * | 2018-08-09 | 2018-12-25 | 陕西科技大学 | A kind of sensor Strain sensing material and preparation method thereof |
| CN109612610A (en) * | 2018-11-06 | 2019-04-12 | 重庆大学 | A kind of color variable electronic skin and preparation method thereof based on hydrogel |
| CN109781316A (en) * | 2019-03-05 | 2019-05-21 | 齐鲁工业大学 | A kind of preparation method of cellulose base pliable pressure sensory device |
| CN109799012A (en) * | 2019-01-23 | 2019-05-24 | 河南工程学院 | A kind of class sandwich structure pressure sensor and preparation method thereof based on cellulose |
| CN110551308A (en) * | 2019-09-09 | 2019-12-10 | 西南石油大学 | Method for preparing flexible strain sensor by using biomass material |
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| CN109799012B (en) * | 2019-01-23 | 2021-01-22 | 河南工程学院 | Cellulose-based sandwich-like structure pressure sensor and preparation method thereof |
| CN109799012A (en) * | 2019-01-23 | 2019-05-24 | 河南工程学院 | A kind of class sandwich structure pressure sensor and preparation method thereof based on cellulose |
| CN109781316A (en) * | 2019-03-05 | 2019-05-21 | 齐鲁工业大学 | A kind of preparation method of cellulose base pliable pressure sensory device |
| CN110551308A (en) * | 2019-09-09 | 2019-12-10 | 西南石油大学 | Method for preparing flexible strain sensor by using biomass material |
| CN110551308B (en) * | 2019-09-09 | 2022-03-18 | 西南石油大学 | Method for preparing flexible strain sensor by using biomass material |
| CN112763106A (en) * | 2019-11-05 | 2021-05-07 | 武汉纺织大学 | High-sensitivity and wide-range composite conductive nanofiber aerogel sensor and preparation method thereof |
| CN114551117A (en) * | 2022-02-21 | 2022-05-27 | 浙江理工大学 | Preparation method of flexible antibacterial fiber type supercapacitor for electronic skin |
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Application publication date: 20160615 |