CN111635556A - Method for preparing flexible mechanical sensing element by sponge metallization - Google Patents
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
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- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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Abstract
The invention relates to a method for preparing a flexible mechanical sensing element by sponge metallization, belonging to the fields of material science, engineering technology and flexible electronics. The flexible mechanical sensing element prepared by the method is mainly used in an active sensing matrix array. The flexible sensing element is formed by compounding a flexible material with high porosity and a metal nanowire with high conductivity, wherein the flexible material can be melamine sponge (MF), polyurethane sponge, polyether foam sponge, rubber sponge and the like, and the metal nanowire can be selected from gold nanowire (AuNWs), silver nanowire (AgNWs), copper nanowire (CuNWs), nickel nanowire (NiNWs), copper-nickel alloy nanowire (Cu-NiNWs) and the like. The invention has the advantages of simple and easy operation, high efficiency, strong applicability and the like.
Description
(2) Field of the invention
The invention relates to a method for preparing a flexible mechanical sensing element by sponge metallization, belonging to the fields of material science, engineering technology and flexible electronics.
(3) Background of the invention
The emerging development track of electronics has focused on portable and flexible devices, and electronic circuits integrating pressure sensors have been widely studied as key components of emerging electronic applications, involving applications integrated with the human body, such as machine learning, artificial muscle skin, sensor networks, and health monitoring devices. In the field of machine learning, a pressure sensing device is crucial to the learning of various functions of grabbing, touching, transferring external things and the like by a machine, and electroencephalogram signals containing a large amount of real-time brain information are collected and analyzed.
Various types of pressure sensing devices have been developed based on piezoresistive, capacitive, piezoelectric, and Field Effect Transistor (FET) sensing mechanisms. Piezoresistive devices are simple in structure, high in sensitivity and fast in response time, but when the sensor is integrated in an array, the pixel density may be low. The capacitance type has a simple device structure and operation principle, but is easily affected by proximity interference. The piezoelectric type has high sensitivity and fast response time, but the sensing characteristic may be unreliable because a general piezoelectric material also has a pyroelectric characteristic. Sensor arrays using these three types of switching mechanisms are electrically controlled by passive matrix addressing, which does not prevent low contrast and cross-talk effects. In contrast, FET-type pressure sensors can take advantage of active matrix sensor arrays that can achieve high array uniformity, high spatial contrast and convenient integration with circuitry, can also provide high quality sensing signals, and reduce cross-talk between individual pixels.
The metal nano-wire has good conductive performance, and the signal loss is small in the transmission process. The metal nanowires have a larger length-diameter ratio, can be attached to the flexible material framework in a winding or lapping mode, and are connected tightly and stably. While the sensor must have some flexibility and toughness to overcome the mechanical mismatch between rigid and flexible components, strain-dependent flexible materials that transmit electrical signals are extremely potential. We can optimize strain sensitivity by controlling the incorporation quality of the metal nanowires, which is highly correlated with the effective charge transport during compression and release of the local distance between the structures.
(4) Summary of the invention
1. Objects of the invention
The invention aims to provide a method for preparing a flexible mechanical sensing element by sponge metallization, which is characterized in that metal nanowires and a flexible material are simply and effectively compounded by utilizing a vacuum environment, so that the flexible material has the function of reacting a stress state and has the capability of transmitting signals.
2. The invention of the technology
The key points of the invention are as follows:
1. a method for preparing a flexible mechanical sensing element by sponge metallization is characterized by comprising the following steps:
(1) selecting proper flexible materials with high porosity, such as melamine sponge (MF), polyurethane sponge, polyether foam sponge and rubber sponge, wherein the flexible materials have various densities and are different from different kinds of sponges and sponges with different densities, and the physical properties of the flexible materials are directly reflected by Young modulus.
(2) Polylactic acid (PLA) is used as a raw material, and a specification mould (mould A) with the thickness of 0.7cm multiplied by 0.5cm is printed by a 3D printing technology.
(3) Cutting sponge in the step (1) into a plurality of parts according to the die A in the step (2), and obtaining melamine sponge with the specification of 0.7cm multiplied by 0.5cm, namely raw material A, polyurethane sponge, polyether foaming sponge and rubber sponge, namely raw material B, raw material C and rubber sponge.
(4) In order to prevent oxidation and multi-storage of the metal nanowires in the alcohol solution, ultrasonic treatment is carried out for 30s to 1min by an ultrasonic machine under the condition that the power is less than 400W, so that the metal nanowires obtain better dispersibility and are not cracked. Measuring a certain amount of metal nanowires in a beaker, adding a polyvinyl butyral (PVB) solution with a certain concentration according to a proportion, uniformly stirring, and then putting a plurality of raw materials A in the step (3). The ratio of the PVB solution to the alcohol solution of the metal nanowires can be selected from 1: 2 and 1: 3 (volume ratio), the concentration of the PVB solution can be selected from 1 wt% and 2 wt% of PVB, and the metal nanowires can be selected from gold nanowires (AuNWs), silver nanowires (AgNWs), copper nanowires (CuNWs), nickel nanowires (NiNWs), copper-nickel alloy nanowires (Cu-NiNWs) and the like.
(5) And vacuumizing the whole body, stopping and ventilating when the pressure is reduced to 1000Pa, taking out the sponge when the pressure is recovered to the atmospheric pressure, putting the sponge into a culture dish, drying the sponge in a 25 ℃ oven, and taking out the sponge after the sponge is completely dried to obtain the novel flexible mechanical sensing element.
(5) Description of the drawings
Fig. 1 is a scanning transmission electron microscope (SEM) image of the flexible mechanical sensing element compounded by the melamine sponge and the nickel nanowire prepared by the method of the present invention.
(6) Examples of the invention
The following describes embodiments of the method of the invention:
example 1
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the silver nanowires.
Firstly, after dispersing the alcohol solution of the silver nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and silver nanowire composite flexible mechanical sensing element.
Example 2
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the silver nanowires.
Firstly, after dispersing the alcohol solution of the silver nanowires, measuring 10ml of the alcohol solution, adding 30ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and silver nanowire composite flexible mechanical sensing element.
Example 3
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowire.
Firstly, after dispersing the alcohol solution of the copper nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and copper nanowire composite flexible mechanical sensing element.
Example 4
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowire.
Firstly, after dispersing the alcohol solution of the copper nanowires, measuring 10ml of the alcohol solution of the copper nanowires, adding 30ml of PVB solution with the concentration of 1 wt%, uniformly stirring, then adding the raw material A, vacuumizing the beaker to be below 1000Pa, then taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at the temperature of 25 ℃, thus obtaining the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowires.
Example 5
Preparing a flexible mechanical sensing element compounded by melamine sponge and gold nanowires.
Firstly, after dispersing the alcohol solution of the gold nanowires, measuring 10ml of the alcohol solution of the gold nanowires in a beaker, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the culture dish in an oven at the temperature of 25 ℃, thus obtaining the flexible mechanical sensing element compounded by the melamine sponge and the gold nanowires.
Example 6
And preparing the melamine sponge and nickel nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing the alcohol solution of the nickel nanowires, measuring 10ml of the alcohol solution of the nickel nanowires, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, then adding the raw material A, vacuumizing the beaker to be below 1000Pa, then taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at the temperature of 25 ℃, thus obtaining the melamine sponge and nickel nanowire composite flexible mechanical sensing element.
Example 7
And preparing the melamine sponge and nickel nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing the alcohol solution of the nickel nanowires, measuring 10ml of the alcohol solution of the nickel nanowires, adding 30ml of PVB solution with the concentration of 1 wt%, uniformly stirring, then adding the raw material A, vacuumizing the beaker to below 1000Pa, then taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃, thus obtaining the melamine sponge and nickel nanowire composite flexible mechanical sensing element.
Example 8
And preparing the melamine sponge and copper-nickel alloy nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing alcohol solution of the copper-nickel alloy nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the beaker in an oven at the temperature of 25 ℃, thus obtaining the melamine sponge and copper-nickel alloy nanowire composite flexible mechanical sensing element.
Example 9
And preparing the melamine sponge and copper-nickel alloy nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing alcohol solution of the copper-nickel alloy nanowires, measuring 10ml of the alcohol solution, adding 30ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the beaker in an oven at the temperature of 25 ℃, thus obtaining the melamine sponge and copper-nickel alloy nanowire composite flexible mechanical sensing element.
Example 10
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the silver nanowires.
Firstly, after dispersing the alcohol solution of the silver nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 2 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and silver nanowire composite flexible mechanical sensing element.
Example 11
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowire.
Firstly, after dispersing the alcohol solution of the copper nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 2 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and copper nanowire composite flexible mechanical sensing element.
Example 12
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowire.
Firstly, after dispersing the alcohol solution of the copper nanowires, measuring 10ml of the alcohol solution, adding 30ml of PVB solution with the concentration of 2 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the melamine sponge and copper nanowire composite flexible mechanical sensing element.
Example 13
Preparing a flexible mechanical sensing element compounded by melamine sponge and gold nanowires.
Firstly, after dispersing the alcohol solution of the gold nanowires, measuring 10ml of the alcohol solution of the gold nanowires, adding 30ml of PVB solution with the concentration of 2 wt%, uniformly stirring, then adding the raw material A, vacuumizing the beaker to below 1000Pa, then taking out the sponge, placing the sponge in a culture dish, and drying the culture dish in an oven at the temperature of 25 ℃, thus obtaining the flexible mechanical sensing element compounded by the melamine sponge and the gold nanowires.
Example 14
And preparing the melamine sponge and nickel nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing the alcohol solution of the nickel nanowires, measuring 10ml of the alcohol solution of the nickel nanowires, adding 20ml of PVB solution with the concentration of 2 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to be below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at the temperature of 25 ℃ to obtain the melamine sponge and nickel nanowire composite flexible mechanical sensing element.
Example 15
And preparing the melamine sponge and copper-nickel alloy nanowire compounded flexible mechanical sensing element.
Firstly, after dispersing alcohol solution of the copper-nickel alloy nanowires, measuring 10ml of the alcohol solution, adding 20ml of PVB solution with the concentration of 2 wt%, uniformly stirring, adding the raw material A, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the beaker in an oven at the temperature of 25 ℃, thus obtaining the melamine sponge and copper-nickel alloy nanowire composite flexible mechanical sensing element.
Example 16
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the silver nanowires.
Firstly, 10ml of alcohol solution of dispersed silver nanowires is measured and placed in a beaker, the raw material A is directly placed in the beaker without adding PVB solution, the beaker is vacuumized to be below 1000Pa, then the sponge is taken out and placed in a culture dish, and the culture dish is sent to a baking oven at 25 ℃ for drying, so that the melamine sponge and silver nanowire composite flexible mechanical sensing element can be obtained.
Example 17
And (3) preparing the flexible mechanical sensing element compounded by the melamine sponge and the copper nanowire.
Firstly, 10ml of alcohol solution of dispersed copper nanowires is measured and placed in a beaker, the raw material A is directly placed in the beaker without adding PVB solution, the beaker is vacuumized to be below 1000Pa, then the sponge is taken out and placed in a culture dish, and the culture dish is sent to a baking oven at 25 ℃ for drying, so that the melamine sponge and copper nanowire composite flexible mechanical sensing element can be obtained.
Example 18
And preparing the melamine sponge and nickel nanowire compounded flexible mechanical sensing element.
Firstly, 10ml of alcohol solution of the nickel nanowires is measured and placed in a beaker, the raw material A is directly placed in the beaker without adding PVB solution, the beaker is vacuumized to be below 1000Pa, then the sponge is taken out and placed in a culture dish, and the culture dish is sent to a baking oven at 25 ℃ for drying, so that the melamine sponge and nickel nanowire composite flexible mechanical sensing element can be obtained.
Example 19
And preparing the melamine sponge and copper-nickel alloy nanowire compounded flexible mechanical sensing element.
Firstly, 10ml of alcohol solution of the copper-nickel alloy nanowires is measured and placed in a beaker, the raw material A is directly placed in the beaker without adding PVB solution, the beaker is vacuumized to be below 1000Pa, then the sponge is taken out and placed in a culture dish, and the culture dish is conveyed to a baking oven at 25 ℃ for drying, so that the melamine sponge and copper-nickel alloy nanowire composite flexible mechanical sensing element can be obtained.
Example 20
And preparing the flexible mechanical sensing element compounded by the polyurethane sponge and the silver nanowires.
Firstly, measuring 10ml of alcohol solution of dispersed silver nanowires in a beaker, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding a raw material B, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the flexible mechanical sensing element compounded by the polyurethane sponge and the silver nanowires.
Example 21
And preparing the flexible mechanical sensing element compounded by the polyether foaming sponge and the silver nanowires.
Firstly, measuring 10ml of alcohol solution of dispersed silver nanowires in a beaker, adding 30ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding the raw material C, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the flexible mechanical sensing element compounded by the polyether foaming sponge and the silver nanowires.
Example 22
And preparing the flexible mechanical sensing element compounded by the rubber sponge and the copper nanowire.
Firstly, measuring 10ml of alcohol solution of dispersed copper nanowires in a beaker, adding 20ml of PVB solution with the concentration of 1 wt%, uniformly stirring, adding a raw material D, vacuumizing the beaker to below 1000Pa, taking out the sponge, placing the sponge in a culture dish, and drying the sponge in an oven at 25 ℃ to obtain the flexible mechanical sensing element compounded by the rubber sponge and the copper nanowires.
Claims (1)
1. A method for preparing a flexible mechanical sensing element by sponge metallization is characterized by comprising the following steps:
(1) selecting proper flexible materials with high porosity, such as melamine sponge (MF), polyurethane sponge, polyether foam sponge and rubber sponge, wherein the flexible materials have various densities and are different from different kinds of sponges and sponges with different densities, and the physical properties of the flexible materials are directly reflected by Young modulus.
(2) Polylactic acid (PLA) is used as a raw material, and a specification mould (mould A) with the thickness of 0.7cm multiplied by 0.5cm is printed by a 3D printing technology.
(3) Cutting sponge in the step (1) into a plurality of parts according to the die A in the step (2), and obtaining melamine sponge with the specification of 0.7cm multiplied by 0.5cm, namely raw material A, polyurethane sponge, polyether foaming sponge and rubber sponge, namely raw material B, raw material C and rubber sponge.
(4) The metal nanowires are mostly stored in alcohol solution for preventing oxidation, and ultrasonic treatment is carried out for 30s to 1min by an ultrasonic machine under the condition that the power is less than 400W, so that the metal nanowires obtain better dispersibility and are not cracked. Measuring a certain amount of metal nanowires in a beaker, adding a polyvinyl butyral (PVB) solution with a certain concentration according to a proportion, uniformly stirring, and then putting a plurality of raw materials A in the step (3). The ratio of the PVB solution to the alcohol solution of the metal nanowires can be selected from 1: 2 and 1: 3 (volume ratio), the concentration of the PVB solution can be selected from 1 wt% and 2 wt% of PVB, and the metal nanowires can be selected from gold nanowires (AuNWs), silver nanowires (AgNWs), copper nanowires (CuNWs), nickel nanowires (NiNWs), copper-nickel alloy nanowires (Cu-NiNWs) and the like.
(5) And vacuumizing the whole body, stopping and ventilating when the pressure is reduced to 1000Pa, taking out the sponge when the pressure is recovered to the atmospheric pressure, putting the sponge into a culture dish, drying the sponge in a 25 ℃ oven, and taking out the sponge after the sponge is completely dried to obtain the novel flexible mechanical sensing element.
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