CN110256712A - Humidity driver and preparation method thereof - Google Patents
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- CN110256712A CN110256712A CN201910408289.3A CN201910408289A CN110256712A CN 110256712 A CN110256712 A CN 110256712A CN 201910408289 A CN201910408289 A CN 201910408289A CN 110256712 A CN110256712 A CN 110256712A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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Abstract
The present invention provides a kind of humidity drivers and preparation method thereof, comprising the following steps: conductive material suspension is diluted to after preset concentration and is spun in culture dish with pre-set velocity by S1；S2 prepares fibroin albumen/glycerol mixed solution；The fibroin albumen of predetermined amount/glycerol mixed solution is slowly injected into the culture dish of coated with conductive material by S3；The obtained culture dish of step S3 is placed in drying in draught cupboard, obtains humidity driver by S4.This method improves the flexibility of humidity driver by the way that glycerol is added in base material, and the technical process of the preparation method is simple, mild condition, environmental-friendly.The humidity driver prepared by the preparation method, structure is simple, has excellent electric conductivity, good mechanical performance sensitive to moisture signal.
Description
Technical field
The present invention relates to Drive technology fields more particularly to a kind of humidity driver and preparation method thereof.
Background technique
Production, the life of humidity and modern are closely bound up, and the selection of humidity-sensitive material is directly related to the spirit of humidity driving
The indexs such as sensitivity.Humidity brake is a kind of drying shrinkage bulking effect that can experience water vapour content and utilization material in gas
Brake is mainly used in mechanical engineering, sensor, gas and humidity driver etc..
Currently, the preparation method of humidity driver is broadly divided into two major classes: one kind is big using humidity expansion coefficient difference
Two kinds of materials be stacked.Such as, patent publication No. is disclosed in the Chinese invention patent of CN107297929, and one layer is carbon
Base cellulose composite material layer, another layer are polymer material layer, are binded between two layers by adhesives such as polyvinyl alcohol,
To obtain humidity driver；The humidity activation configuration of this method preparation is more single, and the structure that double layer material is stacked is curved
Qu Fangxiang is single, it is difficult to meet at present to the diversified demand of driver；Another kind of is to prepare humidity sensor using single material
Device also can be used as humidity driver.Such as, patent publication No. is disclosed in the Chinese invention patent of CN106290325；Party's legal system
Standby humidity driver driving dynamics is small, can only realize the conversion between power and power, application range is small.
The other methods of preparation humidity driver at present, that there are preparation process is cumbersome, toxic to environment, non-renewable,
The disadvantages of expensive, direction of motion and single application.
In view of this, it is necessary to a kind of improved humidity driver and preparation method thereof is designed, to solve the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of highly conductive, good biocompatibilities, the humidity driver of good mechanical performance
And the preparation method of the humidity driver.
For achieving the above object, it the present invention provides a kind of humidity driver, including flexible compound film and is spun on
Conductive coating on the flexible compound film；The flexible compound film is dry by the mixed solution of fibroin albumen and glycerol
It arrives.
As a further improvement of the present invention, when the two sides of the humidity driver are there are when psychrometric difference, the humidity is driven
The dynamic device curving low towards humidity.
As a further improvement of the present invention, the two sides of the humidity driver are driven by psychrometric difference, can compound bending.
As a further improvement of the present invention, the material of the conductive coating include but is not limited to be silver nanowires, oxidation
Graphene or carbon nanotube.
As a further improvement of the present invention, the material of the conductive coating is silver nanowires, the humidity driver
The minimum value range of square resistance is 5~15 Ω/sq.
As a further improvement of the present invention, the humidity driver can be used for electrochemical switch film.
For achieving the above object, the present invention also provides a kind of preparation methods of humidity driver, before being used to prepare
State humidity driver described in any technical solution in technical solution；The following steps are included:
Conductive material suspension is diluted to after preset concentration and is spun in culture dish with pre-set velocity by S1；
S2 prepares fibroin albumen/glycerol mixed solution；
The fibroin albumen/glycerol mixed solution of predetermined amount is slowly injected into the culture dish of coated with conductive material by S3；
The obtained culture dish of step S3 is placed in drying in draught cupboard, obtains humidity driver by S4.
As a further improvement of the present invention, the step S2 includes the following steps:
S21 carries out degumming process to silk with the sodium carbonate of predetermined amount or sodium bicarbonate, then is cleaned repeatedly with deionized water
Silk after degumming process；
S22 repeats step S21 at least three times, obtains fibroin fiber；
The fibroin fiber is placed in 60 DEG C of baking oven and dries for 24 hours by S23；
S24 dissolves the fibroin fiber with lithium-bromide solution or ternary solution, obtains fibroin albumen under preset temperature
Solution；
S25 dialyses to the silk fibroin protein solution, the silk fibroin protein solution purified；
S26, addition account for the glycerol of fibroin quality 5%~50% in the silk fibroin protein solution that step S25 is obtained, after blending
To fibroin albumen/glycerol mixed solution.
As a further improvement of the present invention, in the step S1, the value model of the preset concentration of the conductive material
It encloses for 0.5-20mg/mL, pre-set velocity is 1000-5000rpm in spin coating.
As a further improvement of the present invention, the conductive material is silver nanowires, the preset concentration of the silver nanowires
For 10mg/mL.
The beneficial effects of the present invention are: the preparation method of humidity driver of the invention, is mixed using fibroin albumen/glycerol
Solution forms humidity driver as base material, by the way that conductive material is spun on substrate material surface.By in substrate material
Glycerol is added in material, improves the flexibility of humidity driver, and the technical process of the preparation method is simple, mild condition, nontoxic
It is harmless, environmental-friendly；By spin coating mode, so that conductive material is uniformly distributed, the electric conductivity of humidity driver is improved.It is logical
The humidity driver of preparation method preparation is crossed, structure is simple, has ductility, toughness, flexibility and certain elasticity, bendable
Bent, stretching, good mechanical performance；It is sensitive to moisture signal with excellent electric conductivity；With excellent biocompatibility and non-
It is water-soluble.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of humidity driver of the present invention.
Fig. 2 is the flow diagram of step S2 in Fig. 1.
Fig. 3 is the structural schematic diagram of humidity driver of the present invention.
Fig. 4 is the sample drawing of humidity driver made from the embodiment one of the preparation method of humidity driver of the present invention.
Fig. 5 is the scanning electron microscope (SEM) photograph for being not added with the humidity driver of silver nanowires under 2000 amplification factors.
Fig. 6 is scanning electron microscope (SEM) photograph of the humidity driver under 2000 amplification factors added with silver nanowires.
Fig. 7 is the high-speed camera figure when humidity driver added with silver nanowires is not driven by humidity.
Fig. 8 is the high-speed camera figure when driving driver added with silver nanowires is driven by humidity.
Fig. 9 is the square resistance and the relational graph of the concentration of the silver nanowires used of humidity driver.
Figure 10 is the load-deformation curve of the humidity driver prepared using the silver nanowires of various concentration.
Appended drawing reference
100- humidity driver；10- flexible compound film；20- conductive coating.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, right in the following with reference to the drawings and specific embodiments
The present invention is described in detail.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show the structure and/or processing step closely related with the solution of the present invention, and be omitted with relationship of the present invention less its
His details.
In addition, it should also be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
It please refers to shown in Fig. 1 to Figure 10, the present invention provides a kind of preparation methods of humidity driver, including following step
It is rapid:
Conductive material suspension is diluted to after preset concentration and is spun in culture dish with pre-set velocity by S1；
S2 prepares fibroin albumen/glycerol mixed solution；
The fibroin albumen of predetermined amount/glycerol mixed solution is slowly injected into the culture dish of coated with conductive material by S3；
The obtained culture dish of step S3 is placed in drying in draught cupboard, obtains fibroin albumen/glycerol composite membrane i.e. humidity by S4
Driver.
Wherein, step S1 includes the following steps: 0.1-1mL being diluted to the conductive materials that concentration is 0.5-20mg/mL
It injects in flat culture dish, spin-coated instrument is uniformly sprawled.Spinning standard is to have dried in culture dish after spin coating stops.Spin coating it is pre-
If the value range of speed is 3000-7000rpm.Wherein, conductive material can be silver nanowires, graphene oxide or carbon nanometer
Other conductive materials such as pipe, it is specific not to limit.Preferably, conductive material is silver nanowires, and the preset concentration of silver nanowires is
5mg/mL。
Specifically, step S2 includes the following steps:
S21 carries out degumming process to silk with the sodium carbonate of predetermined amount or sodium bicarbonate, then is cleaned repeatedly with deionized water
Silk after degumming process；
S22 repeats step S21 at least three times, obtains fibroin fiber；
The fibroin fiber is placed in 60 DEG C of baking oven and dries for 24 hours by S23；
S24 dissolves the fibroin fiber with lithium-bromide solution or ternary solution, obtains fibroin albumen under preset temperature
Solution；
S25 dialyses to the silk fibroin protein solution, the silk fibroin protein solution purified；
S26, addition account for the glycerol of fibroin quality 5%~50% in the silk fibroin protein solution that step S25 is obtained, after blending
To fibroin albumen/glycerol mixed solution.
It should be noted that silk can be the silks such as mulberry silk, tussah silk, wild silk yarn or ricinus silk, it is specific to refuse
Limitation.
In the step s 21, generally the silk of 100g is put into the water of 5L and carries out degumming process；Certainly, operator can be with
It is specific not to limit according to the bath raio of actual set water and silk.It should be noted that the predetermined amount of sodium carbonate or sodium bicarbonate
(concentration of sodium carbonate or sodium bicarbonate) is specifically not limited with the corresponding adjustment of difference of silk type.
In step s 24, the preset temperature of use and the solvent soln of selection are related.Specifically, when using 9.3mol/
When the lithium-bromide solution of L dissolves fibroin fiber, preset temperature is 60 ± 2 DEG C；When using ternary solution dissolution fibroin fiber, in advance
If temperature is 72 ± 2 DEG C.
Step S25 includes the following steps: to be added in bag filter after the silk fibroin protein solution for obtaining step S24 is cooling, sets
It dialyses 3 days in 4 DEG C of refrigerator, the silk fibroin protein solution of purifying can be obtained.
In step s3, fibroin albumen/glycerol mixed solution predetermined amount is related with the specification of the culture dish of selection.Work as training
When feeding ware is the plastic culture dish that diameter is 6cm, the value range of predetermined amount is 2-7ml.
It please refers to shown in Fig. 3 to Fig. 4, according to humidity driver 100 prepared by the preparation method, including flexible compound film 10
And it is spun on the conductive coating 20 on flexible compound film.Wherein, flexible compound film 10 is the mixing by fibroin albumen and glycerol
Solution is dried to obtain.
The material of conductive coating 20 include but is not limited to be silver nanowires, graphene oxide or carbon nanotube.
Preferably, the material of conductive coating 20 is silver nanowires, the minimum value model of the square resistance of humidity driver 100
It encloses for 5-15 Ω/sq.
It should be noted that the structure in order to clearly illustrate humidity driver 100, in Fig. 3 by flexible compound film 10 with lead
The delamination of electrocoat 20 is exaggerated processing, in fact, the flexible compound film 10 in humidity driver 100 and conductive painting
Layer 20 is the composite membrane of composite integrated, as shown in Figure 4.
It is illustrated below with reference to the preparation method of embodiment one to three pairs of embodiment humidity drivers of the invention:
Embodiment one
The silver nanowires of the 5mg/mL of 0.5mL is injected in flat culture dish, spin-coated instrument is uniform with the speed of 2000rpm
It sprawls；
With sodium carbonate liquor 98-100 DEG C at a temperature of the degumming of 30min is carried out to mulberry silk, then be washed with deionized water
Only, this step is repeated three times, the mass fraction of sodium carbonate is 0.1%, 0.1%, 0.05% respectively in solution three times；Wherein silkworm
Silk and the ratio of deionized water are 1:50；
Fibroin fiber after degumming is dried for 24 hours at 60 DEG C；
It is dissolved into 1h in 60 DEG C of water-bath, in the lithium-bromide solution system of 9.3mol/L with the bath raio of 1:5；
Deionized water dialysis 3d is used after dissolution is cooling；The silk fibroin protein solution after centrifugation is filtered with gauze later,
The silk fibroin protein solution purified；
Silk fibroin protein solution is diluted to 4%, is then added and accounts for the glycerol of fibroin quality 30%, obtains fibroin albumen/sweet
Oily mixed solution；
The fibroin albumen of 4mL/glycerol mixed solution injection is coated in the flat culture dish of silver nanowires, draught cupboard is placed in
Humidity driver 100 can be obtained in middle dry 2-3d.
Fig. 4 is the sample drawing for the humidity driver 100 that the embodiment of the present invention 1 obtains, and is coated with silver nanoparticle as can be seen from Figure
The humidity driver 100 of line is translucent color, and it is flexible very well.
Fig. 5 and Fig. 6 is respectively to be not added with silver nanowires and be added to the humidity driver of silver nanowires in 2000 times magnifications
Scanning electron microscope (SEM) photograph under several.As can be seen from the figure silver nanowires is distributed very uniform on flexible compound film 10, and formed
Network structure is very complete, so that humidity driver 100 has high conductivity.
Fig. 7 and Fig. 8 is respectively that humidity driver 100 (fibroin albumen added with silver nanowires/glycerol composite membrane) is having
High-speed camera figure when humidity driving with without humidity driving.As can be seen from Figure 7 when 100 two sides of humidity driver are not deposited
In psychrometric difference, humidity driver 100 is simultaneously unchanged.As can be seen from Figure 8, when the palm of operator is close to humidity driver
When 100 side, since the natural humidity around operator's palm is different from the natural humidity around humidity driver 100, this
When, the humidity of humidity driver 100 towards the side of operator's palm is greater than the humidity away from the side of operator's palm, humidity
Driver 100 bends rapidly (curving small towards humidity), and will not generate slight crack；That is, working as humidity driver 100
There are when certain psychrometric difference, humidity driver 100 bends rapidly for two sides；When operator by palm close to humidity driver
When 100 other side, humidity driver 100 faces away from the curving (not shown) of operator's palm.It follows that humidity
The two sides of driver 100 are driven by humidity, can compound bending, and slight crack will not be generated；And humidity is responded fastly, humidity is believed
Number sensitivity, driving force is big and flexibility is good.
Fig. 9 is the square resistance situation for changing humidity driver 100 made from the concentration of silver nanowires in embodiment one.From
In figure it is clear that when the concentration of silver nanowires is 2-10mg/mL, the square resistance of humidity driver 100 is 10-35
The electric conductivity of Ω/sq, humidity driver 100 are fine.Particularly, when the concentration of silver nanowires is 10mg/mL, humidity driving
For the square resistance of device 100 in 10 Ω/sq or so, electric conductivity is excellent.
Figure 10 is the load-deformation curve of the humidity driver prepared using the silver nanowires of various concentration.Wherein, curve
The concentration of the corresponding silver nanowires of a-f be respectively 0mg/ml, 0.5mg/ml, 1.0mg/ml, 2.0mg/ml, 5.0mg/ml and
10.0mg/ml.As can be seen from the figure: the corresponding extension at break of curve b, c, d, e, f and breaking strength are substantially sequentially increased,
Illustrate the raising with silver nanowires concentration, the intensity of humidity driver (silver nanowires-fibroin albumen/glycerol composite membrane) with it is soft
Toughness is gradually increased；And the breaking strength of curve a is although minimum, but its extension at break is suitable with curve f's, illustrates only fibroin egg
The strength of white/glycerol composite membrane is generally less than normal than the composite membrane for being added to silver nanowires, but only fibroin albumen/glycerol composite membrane
Flexibility preferably, silver nanowires-fibroin albumen/glycerol composite membrane of ductility low concentration is more preferable, with 10.0mg/mL's
Silver nanowires-fibroin albumen/glycerol composite membrane is suitable.That is, the addition of glycerol, it is soft to improve fibroin albumen/glycerol composite membrane
Property；The addition of silver nanowires improves fibroin albumen/glycerol composite membrane breaking strength, and the silver nanowires of high concentration can be effective
Keep its excellent ductility.
Embodiment two
The graphene oxide of the 4mg/mL of 0.3mL is injected in flat culture dish, spin-coated instrument is equal with the speed of 4000rpm
It is even to sprawl；
Sodium carbonate is stirred evenly in 100 DEG C of water, tussah silk is added after dissolution and starts timing, is kept for 90 DEG C and boiled
30min；It is washed with deionized water again after degumming, repeats this step three times, the mass fraction of sodium carbonate is in solution three times
0.25%；Wherein, the ratio of tussah silk and water is 1:50；
Fibroin fiber after degumming is dried for 24 hours at 60 DEG C；
It is dissolved into 1h in 60 DEG C of water-bath, in the lithium-bromide solution system of 9.3mol/L with the bath raio of 1:5；
Deionized water dialysis 3d is used after dissolution is cooling；Again by obtained silk fibroin protein solution in the revolving speed of 5000rpm from
Heart 5min；The silk fibroin protein solution after centrifugation is filtered with gauze later, the silk fibroin protein solution purified；
Silk fibroin protein solution is diluted to 4%, the glycerol for accounting for fibroin quality 30% is then added, to obtain fibroin egg
White/glycerol mixed solution；
The fibroin albumen of 3mL/glycerol mixed solution injection is coated in the flat culture dish of graphene oxide, bubble removing is removed
Being placed in super-clean bench dry 2-3d can be obtained humidity driver 100.
Embodiment three
The silver nanowires of the 5mg/mL of 0.5mL is flowed into flat culture dish, spin-coated instrument is equal with the speed of 2000rpm
It is even to sprawl；
Sodium carbonate liquor is stirred evenly in 100 DEG C of water, tussah silk is added after dissolution and starts timing, is kept for 90 DEG C and boiled
30min is washed with deionized water again after degumming, repeats this step three times, the mass fraction of sodium carbonate is in solution three times
0.25%；Wherein the ratio of tussah silk and water is 1:50；
Fibroin fiber after degumming is dried for 24 hours at 60 DEG C；
By it with the bath raio of 1:10 in 72 DEG C of water-bath, molar ratio for 1:8:2 CaCl2-H2O-C2H5The ternary of OH
1h is dissolved in solution；
Deionized water dialysis 3d is used after dissolution is cooling；Again by obtained silk fibroin protein solution in the revolving speed of 5000rpm from
Heart 5min；The silk fibroin protein solution after centrifugation is filtered with gauze later, the silk fibroin protein solution purified；
Silk fibroin protein solution is diluted to 4%, is then added and accounts for the glycerol of fibroin quality 20%, obtains fibroin albumen/sweet
Oily mixed solution；
Fibroin albumen/glycerol mixed solution injection that 4mL is obtained is coated in the flat culture dish of silver nanowires, is placed in logical
Humidity driver 100 can be obtained in dry 2-3d in wind cupboard.
The humidity driver 100 has wide range of applications, for example, the humidity driver 100 is used for turning circuit.Initial
Under state, the small bulbs in circuit are in OFF state；When operator by palm close to humidity driver 100 when, humidity driving
Device 100 is lighted towards the lower curving of humidity, turning circuit, small bulbs, and effect is similar to switch, and operates more square
Just.
In conclusion the preparation method of humidity driver of the present invention, using fibroin albumen/glycerol mixed solution as substrate
Material forms humidity driver 100 by the way that conductive material is spun on substrate material surface.Wherein, fibroin albumen is from a wealth of sources,
Biocompatibility, reproducibility are high.By the way that glycerol is added in base material, the flexibility of humidity driver 100 is improved, and should
The technical process of preparation method is simple, mild condition, nontoxic, environmental-friendly；By spin coating mode, so that conductive material is equal
Even distribution improves the electric conductivity of humidity driver obtained.Silver nanowires has excellent electric conductivity, while to all kinds of thin
Bacterium has different degrees of inhibiting effect, the experiment proved that, have in terms of the driving of humidity to fibroin albumen/glycerol composite membrane
There is energetically booster action.The humidity driver 100 prepared by the preparation method, structure is simple, have ductility, toughness,
Flexible and certain elasticity, flexible, stretching, good mechanical performance；It is sensitive to moisture signal with excellent electric conductivity；Tool
There is excellent biocompatibility and water-insoluble.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferred embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that, it can modify to technical solution of the present invention
Or equivalent replacement, without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. a kind of humidity driver, including flexible compound film and the conductive coating being spun on the flexible compound film；Its feature
Be: the flexible compound film is dried to obtain by the mixed solution of fibroin albumen and glycerol.
2. humidity driver according to claim 1, it is characterised in that: when the two sides of the humidity driver, there are humidity
When poor, the humidity driver curving low towards humidity.
3. humidity driver according to claim 2, it is characterised in that: the two sides of the humidity driver are by psychrometric difference
Driving, can compound bending.
4. humidity driver according to claim 1, it is characterised in that: the material of the conductive coating includes but is not limited to
For silver nanowires, graphene oxide or carbon nanotube.
5. humidity driver according to claim 4, it is characterised in that: the material of the conductive coating is silver nanowires,
The minimum value range of the square resistance of the humidity driver is 5~15 Ω/sq.
6. humidity driver according to claim 1, it is characterised in that: the humidity driver can be used for electrochemical switch
Film.
7. a kind of preparation method of humidity driver is used to prepare humidity described in any claim in claim 1-6 and drives
Dynamic device；It is characterized by comprising following steps:
Conductive material suspension is diluted to after preset concentration and is spun in culture dish with pre-set velocity by S1；
S2 prepares fibroin albumen/glycerol mixed solution；
The fibroin albumen/glycerol mixed solution of predetermined amount is slowly injected into the culture dish of coated with conductive material by S3；
The obtained culture dish of step S3 is placed in drying in draught cupboard, obtains humidity driver by S4.
8. the preparation method of humidity driver according to claim 7, it is characterised in that: the step S2 includes following step
It is rapid:
S21 carries out degumming process to silk with the sodium carbonate of predetermined amount or sodium bicarbonate, then with deionized water cleaning and degumming repeatedly
Treated silk；
S22 repeats step S21 at least three times, obtains fibroin fiber；
The fibroin fiber is placed in 60 DEG C of baking oven and dries for 24 hours by S23；
S24 dissolves the fibroin fiber with lithium-bromide solution or ternary solution, obtains silk fibroin protein solution under preset temperature；
S25 dialyses to the silk fibroin protein solution, the silk fibroin protein solution purified；
S26, addition account for the glycerol of fibroin quality 5%~50% in the silk fibroin protein solution that step S25 is obtained, obtain silk after blending
Fibroin/glycerol mixed solution.
9. the preparation method of humidity driver according to claim 7, it is characterised in that: in the step S1, described
The value range of the preset concentration of conductive material is 0.5-20mg/mL, and pre-set velocity is 1000-5000rpm in spin coating.
10. the preparation method of humidity driver according to claim 9, it is characterised in that: the conductive material is received for silver
Rice noodles, the preset concentration of the silver nanowires are 10mg/mL.
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