CN107383845A - A kind of water sensing conductive shapes memory polymer composite of adjustable type and its preparation method and application - Google Patents
A kind of water sensing conductive shapes memory polymer composite of adjustable type and its preparation method and application Download PDFInfo
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- CN107383845A CN107383845A CN201710400402.4A CN201710400402A CN107383845A CN 107383845 A CN107383845 A CN 107383845A CN 201710400402 A CN201710400402 A CN 201710400402A CN 107383845 A CN107383845 A CN 107383845A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
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Abstract
The invention belongs to shape memory high molecule material and electrical-conductive nanometer Material Field, discloses water sensing conductive shapes memory polymer composite of a kind of adjustable type and its preparation method and application.This method comprises the following steps：Nanometer conductive material is embedded into shape high polymer material substrate surface by transfer method, forms the conductive shapes memory polymer composite of stratiform；The mass percent of the nanometer conductive material and shape high polymer material is respectively 5% 10% and 90% 95%.Resulting composite has the function of conduction and the sensing of reply water on the basis of shape-memory properties, the utilization in terms of this conduction and sensing are applied in terms of intellectual material is greatly improved and particular surroundings is tackled in increase.
Description
Technical field
The invention belongs to shape memory high molecule material and electrical-conductive nanometer Material Field, and in particular to a kind of water of adjustable type
Sense conductive shapes memory polymer composite and its preparation method and application.
Background technology
Intellectual material has started mankind's design and the New Times using material.So-called intellectual material is that itself can perceive it
Residing external environment is changed, and a kind of material of corresponding instantaneous active reaction is made to the change.In brief,
It is a kind of material with a series of specific functions such as OBD, self-adaptation, self-regeneration.Conventional intellectual material has certainly
Cleaning and self-repair material, magnetostriction materials, piezoelectric, marmem and shape-memory polymer etc..Therefore, base
In the preparation of the functionalization of shape-memory polymer, cause extensive concern and pay attention to.And shape-memory polymer (Shape
Memory Polymer) be it is a kind of there is original shape, deformed under the effect of certain external condition it is fixed after, by heat, it is electric,
The outside stimulus such as magnetic, light, the polymer of its original shapes can be replied.Shape memory polyurethane (SMPU) have weatherability it is strong,
Shock resistance is good, repeats the features such as deformation effects are good, light refraction and moisture vapor permeability are excellent, is defended in engineering construction, clothes, medical treatment
The application potential of raw and daily life etc. is huge.
Compound-type conducting high polymer is using high polymer material as matrix, adulterates a number of conductive materials (carbon modified
Nanotube (diameter 0.4nm or so), graphene (individual layer, double-deck, based on multilayer), carbon dust (mesh of 40 mesh -80, the mesh of 80 mesh -100) and
Compounding substances more than both or both etc.) combine.Conductive polymeric composite is high polymer material with leading
Isoelectric substance by it is scattered it is compound, lamination is compound and forms a kind of functional high molecule material that the modes such as surface conductance film form.
Often it is used as flexible sensing, conductive electrode material etc..
Due to its unique surface texture of CNT, being a kind of hollow structure with unique nanoscale, knot
The features such as high, the larger specific surface area of brilliant degree, good electric conductivity, certain limit internal orifice dimension size be controllable, and these features are all
It is the advantage of carbon nanotube used as electrode materials.Its unique structure provides good condition for water sensing.Based on carbon
The application of nanotube water sensing, someone make use of cellulose aerogels to be prepared for conducing composite material, so as to enter water-filling sensing, but
Operating process is more complicated, and can not be regulated and controled and be stretched.
The content of the invention
The shortcomings that in order to overcome prior art and deficiency, primary and foremost purpose of the invention are that the water for providing a kind of adjustable type passes
Feel the preparation method of conductive shapes memory polymer composite.Utilize the CNT after the graphene oxide of synthesis and acidifying
By the way that one layer of conductive network structure is formed the methods of drop coating and spin coating on matrix, then shape memory polyurethane (SMPU) is high
Molecular solution drop coating is on the surface of conducting film, by being heated under vacuum drier and vacuum obtains the film of conduction.
A kind of water sensing for the adjustable type being prepared another object of the present invention is to provide above-mentioned preparation method is conductive
Shape memory macromolecule composite material.The material regulates and controls the sensing of water by following two modes：Conductive layer provides electronics path
Ratio with regulation to water sensing, shape memory matrix provide flexible extensible and adjustable fixed performance.
It is still another object of the present invention to provide the water of above-mentioned adjustable type sensing conductive shapes memory polymer composite
Application.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of the water sensing conductive shapes memory polymer composite of adjustable type, comprises the following steps：
Nanometer conductive material is embedded into shape high polymer material substrate surface by transfer method, the conductive shapes memory for forming stratiform is high
Molecular composite material；The mass percent of the nanometer conductive material and shape high polymer material be respectively 5%-10% and
90%-95%.
Above-mentioned preparation method, specifically includes following steps：First by shape on the liquid deposition of nanometer conductive material to substrate
Into conducting film, then by the solution of shape high polymer material composite curing therewith, finally the composite membrane of formation is peeled off in substrate,
Obtain the water sensing conductive shapes memory polymer composite of adjustable type.
The solution of the nanometer conductive material is that graphene oxide first is dissolved in into the scattered 0.5-1h of solvent supersonic and then added
Enter CNT, be again stirring for and ultrasonic 1-3h；The liquid deposition by nanometer conductive material is to forming conducting film in substrate
Comprise the concrete steps that nanometer conductive material drop coating or be spin-coated on matrix, and dry, then at 200 DEG C -500 in Muffle furnace
High temperature reduction 1-12h at DEG C.
The mass ratio of the graphene oxide and CNT is 0:10、1:9、2:8、3:7、5:5、7:3、9:1 or 10:
0；The solvent is ethanol, methanol or water, preferably ethanol.
The solution of the shape high polymer material is that shape memory polyurethane (SMPU) is dissolved in solvent, stirring condition
Under be heated to 60-80 DEG C, ultrasound, forms solution of the concentration for 100mg/ml；The solution by shape high polymer material is therewith
Composite curing comprises the concrete steps that the solution drop coating by shape high polymer material after conducting film, and it is small that 6-12 is heated in drying box
When, then in vacuum drying chamber 60~80 DEG C vacuum drying 12-24 hours.
The solvent is N, N dimethyl acetamide, dimethyl sulfoxide (DMSO), DMF or tetrahydrofuran, is preferably
N, N dimethyl acetamide.
The water sensing conductive shapes memory polymer composite for the adjustable type that above-mentioned preparation method is prepared.
Application of the water sensing conductive shapes memory polymer composite of above-mentioned adjustable type in water sensing.
The shape high polymer material refers to that one kind has original shape, deforms and fixes under the effect of certain external condition
Afterwards, by outside stimulus, the polymer of its original shapes can be replied.
The high polymer material that the present invention uses is with shape memory function, and it can be polyester or polyether-type high score
Son, there is transition temperature, in shape memory function, what is showed is to stretch at high temperature, after the fixed interim shape of cooling at low temperature
Shape.
The sensing refers to that the change of external environment can be changed into electricity by material by the conductive layer in composite construction
The change of signal, it is that the sensing of water will be come out by resistivity, or the reacting condition of electrical conductivity.
The regulatable water sensing, that is, referring to including can be square to the reaction time of water and resistance change rate size
Just regulation and control.
Controllable mode of the present invention has 2 kinds of method regulation and control：First, the component regulation and control for the conductive path for passing through hydridization are
Refer to carrying out the hydridization of different proportion by two kinds and two or more conductive materials.Second, the ratio of stretching fixation utilizes shape
The stretchable and adjustable fixed performance of shape memory polyurethane.
For the present invention creatively using graphene oxide as one of control measures, graphene oxide is a kind of good disperses
Agent acts on CNT, and its cooperative effect not only increases its electric conductivity, while also changes the pattern of conductive network.It is different
The conducting film of ratio has different water sensings.Therefore, the invention has the characteristics that：One, conductive material aspect is applied, and is passed through
The combination of single or both conductive material obtains the conductive network of different performance.Two, the application of shape memory polyurethane, it
Fixation, it is stretchable, and flexible the characteristics of provide good matrix.Three, both combinations provide leading for multiple functions
Electric polymer composite.The ratio mixing of conductive material provides different water sensing functions, is the resistance variations to water
Different effects is presented；And the shape memory function of polyurethane provides stretching and fixed, conduction is set to carry out different stretch ratio, from
And change its water effect function.The present invention on this basis, is obtained by adding graphene oxide and shape memory high molecule
The means of a variety of regulation water sensings.
The present invention is had the following advantages relative to prior art and effect：
The present invention is prepared for a kind of conductive materials/high molecular composite wood for having special microscopic appearance and having certain conduction
Material, its preparation method is relatively simple, and resulting composite has conductive and reply on the basis of shape-memory properties
The function of the sensing of water, reply particular surroundings is applied and increased to this conductive and sensing in terms of intellectual material is greatly improved in terms of
Utilize.
Brief description of the drawings
Fig. 1 is that the water of adjustable type of the present invention senses the making schematic diagram that conductive shapes remember polymer composite.
Fig. 2 is that the water of adjustable type of the present invention senses the electron microscope pattern that conductive shapes remember polymer composite
Figure, wherein a are CNT, and b is graphene oxide, and c is hybrid films after high temperature reduction.
Fig. 3 is that water senses schematic diagram.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1 (manufacturing process is as shown in Figure 1)
1st, by the graphene oxide and CNT of different quality ratio (as listed in table 1), gross mass 10mg, it is dissolved in second
In alcoholic solution, stirring and ultrasonic 2h, the solution of nanometer conductive material is obtained；By the solution drop coating of gained nanometer conductive material or rotation
Be coated on matrix, and dry, then in Muffle furnace at 200 DEG C high temperature reduction 12 hours, formed conducting film；
2nd, shape memory polyurethane SMPU (quality 190mg) is dissolved in N, in N dimethyl acetamide (DMAC), stirring
Under the conditions of be heated to 60-80 DEG C, ultrasound, obtain the solution for the shape high polymer material that concentration is 100mg/ml；
3rd, by the solution drop coating of gained shape high polymer material in step 2 after step 1 gained conducting film, in drying box
Heat 12 hours, vacuum 24 hours in rear vacuum drying chamber, the water sensing conductive shapes memory macromolecule for obtaining adjustable type is compound
Material；The electron microscope pattern of gained composite is as shown in Figure 2；
4th, the wide * of * one long are cut from the water sensing conductive shapes memory polymer composite of above-mentioned gained adjustable type
Thickness=35mm*4*0.05mm film, in soaking water, the change of electric conductivity of its conducting film in water is surveyed at both ends, from data
Reach balance in 10min or so to electric conductivity, the resistance variations situation of its conducting film is as shown in table 1.
5th, this water sensing conductive shapes memory polymer composite applies such as Fig. 3, and its a is that conducting film starts 0s in water
State, the brightness of lamp is very strong；B figures are the brightness changes of lamp of the conducting film in water after 2min, and lamp starts to die down；C figures are to lead
Change of the electrolemma in water after 5min, now lamp extinguished.D, e, f figure are to remove conducting film from water, pass through the thorn in the external world
Goad 0s after water removes, the change of 10s, 100s lamp into action.The advantages of demonstrating conductive film water sensing and reusable edible.
The resistance variations situation of the conducting film of table 1
| Graphene oxide/carbon nanotube mass ratio | Starting resistivity | Resistivity after balance | Rate of change |
| 0:10 | 0.35559 | 0.407 | 14.5% |
| 1:9 | 0.14321 | 0.17767 | 24.1% |
| 5:5 | 0.05669 | 0.12117 | 64.5% |
| 9:1 | 0.27565 | 0.30186 | 9.5% |
| 10:0 | 0.30759 | 0.3159 | 2.7% |
Embodiment 2
1st, it is 5 by mass ratio:5 graphene oxide and CNT, gross mass 10mg, is dissolved in ethanol solution,
Stirring and ultrasonic 2h, obtain the solution of nanometer conductive material；By the solution drop coating of gained nanometer conductive material or it is spin-coated on matrix
On.And dry；After high temperature reduction in Muffle furnace 200 DEG C, conducting film is formed；
2nd, shape memory polyurethane SMPU (quality 190mg) is dissolved in N, in N dimethyl acetamide (DMAC), heating
To 60-80 DEG C, ultrasound, make solution uniform, obtain the solution for the shape high polymer material that concentration is 100mg/ml；
3rd, by Polymer Solution drop coating in step 2 after step 1 gained conducting film, heated 12 hours in drying box, after
Vacuum 24 hours in vacuum drying chamber, obtain the water sensing conductive polymer composite of adjustable type；
4th, a same wide * thickness=35mm*4*0.05mm of long * film is cut；
5th, conducting film heating is stretched, stretch ratio 5%, in rear soaking water, its conducting film leading in water is surveyed at both ends
Electrical change, see that electric conductivity reaches balance, the resistance variations 80% of its conducting film in 10min or so from data.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of adjustable type water sensing conductive shapes memory polymer composite preparation method, it is characterised in that including with
Lower step：Nanometer conductive material is embedded into shape high polymer material substrate surface by transfer method, forms the conductive shape of stratiform
Shape remembers polymer composite；The mass percent of the nanometer conductive material and shape high polymer material is respectively 5%-
10% and 90%-95%.
2. preparation method according to claim 1, it is characterised in that specifically include following steps：First by nanometer conductive material
Liquid deposition to conducting film is formed in substrate, then by the solution of shape high polymer material composite curing therewith, finally by shape
Into composite membrane peel off in substrate, obtain adjustable type water sensing conductive shapes memory polymer composite.
3. preparation method according to claim 2, it is characterised in that：The solution of the nanometer conductive material is first will oxidation
Graphene, which is dissolved in solvent supersonic, to be disperseed 0.5-1h and then to add CNT, is again stirring for and ultrasonic 1-3h；It is described by nanometer
The liquid deposition of conductive material is to forming comprising the concrete steps that nanometer conductive material drop coating or being spin-coated on base for conducting film in substrate
On body, and dry, then in Muffle furnace at 200 DEG C -500 DEG C high temperature reduction 1-12h.
4. preparation method according to claim 3, it is characterised in that：The mass ratio of the graphene oxide and CNT
Example is 0:10、1:9、2:8、3:7、5:5、7:3、9:1 or 10:0；The solvent is ethanol, methanol or water.
5. preparation method according to claim 3, it is characterised in that：The solvent is ethanol.
6. preparation method according to claim 2, it is characterised in that：The solution of the shape high polymer material is by shape
Memory polyurethane is dissolved in solvent, and 60-80 DEG C is heated under stirring condition, ultrasound, forms the solution that concentration is 100mg/ml；
Composite curing comprises the concrete steps that the solution drop coating of shape high polymer material the solution by shape high polymer material therewith
After conducting film, 6-12 hours are heated in drying box, then 60~80 DEG C of vacuum drying 12-24 are small in vacuum drying chamber
When.
7. preparation method according to claim 6, it is characterised in that：The solvent is N, N dimethyl acetamide, dimethyl
Sulfoxide, N, N-dimethylformamide or tetrahydrofuran.
8. preparation method according to claim 7, it is characterised in that：The solvent is N, N dimethyl acetamide.
9. the water sensing conductive shapes memory for the adjustable type that the preparation method according to claim any one of 1-8 is prepared
Polymer composite.
10. the water sensing conductive shapes memory polymer composite of adjustable type according to claim 9 is in water sensing
Application.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974072A (en) * | 2017-12-01 | 2018-05-01 | 中国科学院深圳先进技术研究院 | A kind of selfreparing dielectric composite material and preparation method thereof |
| WO2019206167A1 (en) * | 2018-04-26 | 2019-10-31 | 京东方科技集团股份有限公司 | Humidity sensor and manufacturing method therefor, and electronic device |
| CN112239593A (en) * | 2019-07-19 | 2021-01-19 | 深圳市行远科技发展有限公司 | Multi-response shape memory polyurethane material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674998A (en) * | 2017-01-05 | 2017-05-17 | 广东工业大学 | Shape memory-based multi-stimulated sensing conductive polymer material and preparation method and application thereof |
-
2017
- 2017-05-31 CN CN201710400402.4A patent/CN107383845A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674998A (en) * | 2017-01-05 | 2017-05-17 | 广东工业大学 | Shape memory-based multi-stimulated sensing conductive polymer material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| HONGSHENG LUO等: "Shape memory-enhanced water sensing of conductive polymer composites", 《MATERIALS LETTERS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974072A (en) * | 2017-12-01 | 2018-05-01 | 中国科学院深圳先进技术研究院 | A kind of selfreparing dielectric composite material and preparation method thereof |
| WO2019206167A1 (en) * | 2018-04-26 | 2019-10-31 | 京东方科技集团股份有限公司 | Humidity sensor and manufacturing method therefor, and electronic device |
| CN112239593A (en) * | 2019-07-19 | 2021-01-19 | 深圳市行远科技发展有限公司 | Multi-response shape memory polyurethane material and preparation method and application thereof |
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