CN114414107A - High-strength carbon fiber composite material with self-sensing function and preparation method thereof - Google Patents
High-strength carbon fiber composite material with self-sensing function and preparation method thereof Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 132
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 132
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010410 layer Substances 0.000 claims abstract description 153
- 239000013078 crystal Substances 0.000 claims abstract description 39
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- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 16
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 50
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
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- 238000001723 curing Methods 0.000 claims description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 20
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 10
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 5
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- G01L1/00—Measuring force or stress, in general
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- G—PHYSICS
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
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- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
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Abstract
The invention discloses a high-strength carbon fiber composite material with a self-sensing function and a preparation method thereof, belonging to the field of carbon fiber composite materials. According to the preparation method of the high-strength carbon fiber composite material with the self-sensing function, the piezoelectric nano layer is loaded on the carbon fiber woven layer, and the piezoelectric nano layer is made of the barium titanate nano material. The preparation of the piezoelectric nano layer is that a seed crystal layer grows on the surface of the carbon fiber woven layer by using an atomic layer deposition technology, the seed crystal layer has the function of enabling the piezoelectric nano layer to be uniformly and compactly attached to the carbon fiber woven layer, then the seed crystal layer is thickened by using a hydrothermal method, the thickened seed crystal layer is converted into the piezoelectric nano layer, and the carbon fiber woven layer loaded with the piezoelectric nano layer is used as a middle functional layer to construct the composite material with a sandwich structure; the atomic layer deposition technology is to plate the carbon fiber woven layer by layer in a single atomic film mode, so that the deposited seed crystal layer has extremely uniform thickness and excellent consistency, the shape and the array distribution of the subsequent piezoelectric nano layer can be accurately controlled through selective deposition of a mask, and the method becomes an important basis for finally detecting a considerable sensitive piezoelectric signal.
Description
Technical Field
The invention belongs to the field of carbon fiber composite materials, and particularly relates to a high-strength carbon fiber composite material with a self-sensing function and a preparation method thereof.
Background
The carbon fiber has the advantages of high specific strength and specific modulus, small density, strong designability, easy molding and the like, is the most important reinforcing material in advanced composite materials, and is widely applied to various fields in military and civil use. When carbon-fibre composite is used for large-scale structure spare such as aviation wing, can lead to the fact the damage to the material because fatigue and extreme environmental change in complicated service environment, these damage types are complicated various, disguise is strong, can not in time discover and restore, can bring serious potential safety hazard for whole equipment system, and traditional detection scheme is like infrared detection, acoustic emission detection etc. all need large-scalely, complicated outside check out test set, can't carry out real-time to the damage of material, online detection, consequently need to establish quick effectual structure health monitoring system urgently, in real time, the corresponding damage position of accurate acquisition and damage degree, thereby guarantee structure spare and complete machine system's safety in utilization.
Unlike traditional materials, smart materials have integrated sensing, feedback, and self-diagnostics functions, and thus have become important and focus of research in the field of materials. The intelligent material with the self-detection function at the present stage mainly comprises a strain gauge array, an optical fiber sensor, a piezoelectric composite material and the like, but the strain gauge array and the optical fiber sensor cannot meet the application requirement of a large strain scene due to the fragility of the materials, and the piezoelectric composite material is formed by laying a piezoelectric polymer layer between composite material layers, so that the piezoelectric composite material has high bendable deformation capability, but the introduced piezoelectric polymer layer is a heterogeneous material different from the original composite material, so that the mechanical strength and the physical performance of the whole material are inevitably reduced greatly.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-strength carbon fiber composite material with a self-sensing function and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a high-strength carbon fiber composite material with a self-sensing function comprises the following steps:
(1) depositing a titanium oxide seed crystal layer on the surface of the carbon fiber layer by using an atomic layer deposition technology, and thickening the titanium oxide seed crystal layer by adopting a hydrothermal reaction;
(2) adopting hydrothermal reaction to convert the thickened titanium oxide seed crystal into barium titanate to obtain a carbon fiber woven layer modified by the piezoelectric nano layer;
(3) coating epoxy resin on both sides of the carbon fiber woven layer modified by the piezoelectric nano layer, and heating and curing in a vacuum environment;
(4) coating electrodes on two sides of the cured piezoelectric nano-layer modified carbon fiber woven layer in a scraping mode, and then polarizing to obtain a piezoelectric functional layer;
(5) arranging the piezoelectric functional layers as a middle functional layer array, pasting carbon fiber cloth on two sides of the middle functional layer, adopting epoxy resin to carry out integral packaging, and carrying out vacuum heating and curing to obtain the carbon fiber composite material with a sandwich structure and a self-detection function.
Further, the process of depositing the titanium oxide seed layer on the surface of the carbon fiber layer by using the atomic layer deposition technology in the step (1) is as follows:
blowing a titanium source precursor in a steam mode by taking nitrogen as carrier gas for 0.1 second, blowing out redundant titanium source by the nitrogen, and chemically adsorbing the titanium source on the carbon fiber woven layer in 6 seconds; then introducing ozone for 0.5 second, introducing nitrogen to blow out redundant ozone, and reacting the ozone with a titanium source precursor adsorbed on the carbon fiber cloth to generate titanium oxide with a monoatomic layer in 6 seconds; blowing out reaction residues through nitrogen, wherein the reaction residues take 6 seconds to complete one period; the above cycle was repeated until a seed layer of titanium oxide having a thickness of 50nm was deposited on the carbon fiber woven layer.
Further, the step (1) of thickening the titanium oxide seed crystal layer by adopting a hydrothermal reaction is as follows:
measuring 10 parts of hydrochloric acid and 10 parts of deionized water in parts by volume, mixing, adding 2 parts of titanium isopropoxide and 1 part of titanium tetrachloride, and uniformly stirring to obtain a reaction solution;
and immersing the carbon fiber woven layer deposited with the titanium oxide seed crystal layer in the reaction liquid for hydrothermal reaction at the hydrothermal temperature of 180 ℃ for 20-60min to obtain the thickened titanium oxide seed crystal layer on the carbon fiber woven layer.
Further, the specific process of converting the thickened titanium oxide seed crystal into barium titanate in the step (2) is as follows:
0.02mol of Ba (NO)3)2And 0.08mol of NaOH is dissolved in 40ml of deionized water, the mixture is stirred uniformly, the carbon fiber woven layer loaded with the thickened titanium oxide seed crystal layer is immersed in the solution, hydrothermal reaction is carried out, the hydrothermal temperature is 230 ℃, the time is 36 hours, and after the reaction is finished, the titanium oxide seed crystal is converted into barium titanate.
Further, the specific operation of performing heating curing in the step (3) is as follows:
the curing temperature is 60-100 ℃, and the curing time is 2 h.
Further, the polarization conditions of step (4) are as follows:
the polarization electric field is a direct current electric field, the size of the electric field is 40-60V/um, the polarization temperature is 80-100 ℃, and the polarization time is 1-3 h.
Further, step (5) is followed by:
and connecting the upper electrode and the lower electrode of the middle functional layer with an oscilloscope, and synchronously reading data on a computer during testing to realize real-time monitoring on the high-strength carbon fiber composite material.
The invention discloses a high-strength carbon fiber composite material with a self-sensing function, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the high-strength carbon fiber composite material with the self-sensing function, the piezoelectric nano layer is loaded on the carbon fiber woven layer, and the piezoelectric nano layer is made of the barium titanate nano material. The preparation of the piezoelectric nano layer is that a seed crystal layer grows on the surface of the carbon fiber woven layer by using an atomic layer deposition technology, the seed crystal layer has the function of enabling the piezoelectric nano layer to be uniformly and compactly attached to the carbon fiber woven layer, then the seed crystal layer is thickened by using a hydrothermal method, the thickened seed crystal layer is converted into the piezoelectric nano layer, and the carbon fiber woven layer loaded with the piezoelectric nano layer is used as a middle functional layer to construct the composite material with a sandwich structure; the atomic layer deposition technology is to plate the carbon fiber woven layer by layer in a single atomic film mode, so that the deposited seed crystal layer has extremely uniform thickness and excellent consistency, the shape and the array distribution of the subsequent piezoelectric nano layer can be accurately controlled through selective deposition of a mask, and the method becomes an important basis for finally detecting a considerable sensitive piezoelectric signal.
According to the high-strength carbon fiber composite material with the self-sensing function, the light-weight high-strength carbon fiber is used as the substrate, due to the characteristics of corrosion resistance, high temperature resistance and the like of the carbon fiber, and the piezoelectric nano layers are uniformly and densely distributed on the substrate by the atomic layer deposition technology, tests of the interface strength of the carbon fiber show that the in-situ detection of the damage position and the damage degree is realized while the original high-strength performance advantage of the structural material is maintained, the early warning function is realized on serious damage of the material, and the use requirement of a complex scene can be met.
Drawings
Fig. 1 is an SEM scan of a single piezoelectric nanolayer-modified carbon fiber of example 1;
FIG. 2 is a comparison graph of the interfacial strength of a piezoelectric nanolayer modified carbon fiber and a blank carbon fiber measured using a bead debonding method;
FIG. 3 is a schematic view of an array of structural members of a carbon fiber composite material modified by piezoelectric nanolayers according to example 2;
fig. 4 is a graph showing the detection results of the self-sensing characteristics of the carbon fiber composite material structural member modified by the piezoelectric nanolayer in example 2 when the structural member is pressed at different positions, wherein fig. 4(a), 4(b), 4(c) and 4(d) correspond to the detection results of the self-sensing characteristics at the pressing position 1, the pressing position 2, the pressing position 3 and the pressing position 4, respectively.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1:
1) preparing a titanium oxide seed crystal layer on a carbon fiber woven layer
Firstly, the carbon fiber woven layer is cleaned by ultrasonic oscillation of acetone, ethanol and deionized water respectively, and then a titanium oxide seed crystal layer with the thickness of 50nm is deposited on the surface of the carbon fiber woven layer by using an Atomic Layer Deposition (ALD) technology. The process is as follows: blowing a titanium source precursor in a steam mode by taking nitrogen as carrier gas for 0.1 second, blowing out redundant titanium source by the nitrogen, and chemically adsorbing the titanium source on the carbon fiber woven layer in 6 seconds; then introducing ozone for 0.5 second, introducing nitrogen to blow out redundant ozone, and reacting the ozone with a titanium source precursor adsorbed on the carbon fiber cloth to generate titanium oxide with a monoatomic layer in 6 seconds; blowing out reaction residues through nitrogen, wherein the reaction residues take 6 seconds to complete one period; the above production cycle was repeated until a seed layer of titanium oxide having a thickness of 50nm was deposited on the carbon fiber woven layer.
2) Thickening a titanium oxide seed crystal layer by using a hydrothermal reaction
Measuring 17ml of hydrochloric acid and 17ml of deionized water, putting the hydrochloric acid and the deionized water into a 100ml beaker, continuously stirring the mixture by using a glass rod in the whole process, stirring the mixture for 5 minutes by using a magnetic stirrer, adding 3.4ml of titanium isopropoxide and 1.7ml of titanium tetrachloride, sealing the opening of the beaker by using a preservative film, magnetically stirring the mixture for 30 minutes, finally transferring the prepared solution into a lining of a reaction kettle, putting a carbon fiber woven layer on which a titanium peroxide seed layer is deposited, completely immersing the carbon fiber woven layer in the solution, carrying out water cooling after reacting for 20 minutes, taking out the carbon fiber woven layer, carrying out ultrasonic oscillation washing for a plurality of times by using pre-prepared dilute hydrochloric acid, distilled water and absolute ethyl alcohol in sequence, carrying out vacuum drying at 100 ℃, and obtaining titanium oxide with the thickness of about 150 microns through the reaction.
3) Conversion of thickened titanium oxide to barium titanate using hydrothermal reaction
0.02mol of Ba (NO)3)2Dissolving 0.08mol of NaOH in 40ml of deionized water, magnetically stirring for 30 minutes, transferring the prepared solution into a lining of a reaction kettle, putting the thickened titanium oxide layer carbon fiber woven layer into the solution, completely immersing the carbon fiber woven layer in the solution, cooling the reaction kettle by water at the hydrothermal temperature for 36 hours at the hydrothermal temperature, taking out the carbon fiber woven layer, and sequentially using the carbon fiber woven layerDiluted hydrochloric acid, distilled water and absolute ethyl alcohol which are prepared in advance are washed for a plurality of times by ultrasonic oscillation, vacuum drying is carried out at 100 ℃, and the thickness of barium titanate obtained by reaction is about 200 um.
4) Epoxy resin is respectively coated on the carbon fiber woven layer modified by the piezoelectric nano layer and the common carbon fiber woven layer, and is heated and cured in a vacuum environment, the curing temperature is 60 ℃, the curing time is 2 hours, and the thickness of the cured woven layer is about 0.4 mm.
5) And (3) coating electrodes on the upper surface and the lower surface of the cured piezoelectric nano-layer modified carbon fiber woven layer in a scraping mode, and then polarizing the carbon fiber woven layer, wherein the polarizing electric field is a direct current electric field with the size of 60V/um, the polarizing temperature is 100 ℃, and the polarizing time is 1 h.
6) And arranging the carbon fiber woven layers modified by the polarized piezoelectric nano layers as a middle functional layer array, pasting the blank carbon fiber woven layers up and down, using epoxy resin as a matrix, and performing vacuum curing for 2h to finally prepare the carbon fiber composite material modified by the piezoelectric nano layers with the sandwich structure.
7) And connecting the upper electrode and the lower electrode of the functional layer with an oscilloscope, performing mechanical tests such as stretching, three-point bending and the like on the composite material, and simultaneously reading data on a computer to realize real-time monitoring on the health state of the structural component.
Referring to fig. 1, fig. 1 is an SEM scan of a single piezoelectric nanolayer modified carbon fiber of example 1, and it can be seen from the SEM scan that a hydrothermally grown barium titanate nanolayer is densely and uniformly wrapped on the carbon fiber, which illustrates that a piezoelectric nanolayer is obtained on a carbon fiber substrate by an atomic layer deposition technique and a hydrothermal method, which also lays a foundation for obtaining a good piezoelectric signal in the following.
Referring to fig. 2, fig. 2 is a comparison graph of the interface strength of the carbon fiber modified by the piezoelectric nano layer and the blank carbon fiber measured by the bead debonding method, and it can be seen from the graph that the carbon fiber modified by the piezoelectric nano layer maintains the original high strength of the structural material and is reduced a little.
Example 2:
arranging 4 polarized piezoelectric nano-layer modified carbon fiber woven layers with the size of 1cm multiplied by 1cm as an intermediate functional layer array, pasting a blank carbon fiber woven layer up and down, bonding the blank carbon fiber woven layer by using epoxy resin, curing for about 2 hours at the temperature of 60-100 ℃ to prepare the piezoelectric nano-layer modified carbon fiber composite material structural member with a sandwich structure, connecting electrodes of 4 intermediate functional layers with 4 channels of an oscilloscope respectively, sequentially pressing the positions of the 4 intermediate functional layers by using the same force, and simultaneously collecting output signals of the 4 channels of the oscilloscope on a computer.
As shown in fig. 4, when the position 1 of the first intermediate functional layer is pressed, as shown in fig. 4(a), the voltage signal collected by the channel 1 is the largest, the voltage signals collected by the channels 2 and 3 corresponding to the positions 2 and 3 adjacent to the position 1 are obviously smaller, the voltage signal collected by the channel 4 corresponding to the position 4 farthest from the position 1 can hardly be collected, and the test results obtained when the rest positions 2, 3, and 4 are pressed, as shown in fig. 4(b), fig. 4(c), and fig. 4(d), are consistent corresponding conditions, so that the damage orientation and the damage degree of the structural component can be determined by comparing the magnitudes of the signals collected corresponding to the different positions, that is, the self-sensing characteristic of the composite material of the piezoelectric nanolayer modified carbon fiber is realized.
Example 3
1) Preparing a titanium oxide seed crystal layer on a carbon fiber woven layer
Firstly, the carbon fiber woven layer is cleaned by ultrasonic oscillation of acetone, ethanol and deionized water respectively, and then a titanium oxide seed crystal layer with the thickness of 50nm is deposited on the surface of the carbon fiber woven layer by using an Atomic Layer Deposition (ALD) technology. The process is as follows: blowing a titanium source precursor in a steam mode by taking nitrogen as carrier gas for 0.1 second, blowing out redundant titanium source by the nitrogen, and chemically adsorbing the titanium source on the carbon fiber woven layer in 6 seconds; then introducing ozone for 0.5 second, introducing nitrogen to blow out redundant ozone, and reacting the ozone with a titanium source precursor adsorbed on the carbon fiber cloth to generate titanium oxide with a monoatomic layer in 6 seconds; blowing out reaction residues through nitrogen, wherein the reaction residues take 6 seconds to complete one period; the above production cycle was repeated until a seed layer of titanium oxide having a thickness of 50nm was deposited on the carbon fiber woven layer.
2) Thickening a titanium oxide seed crystal layer by using a hydrothermal reaction
Measuring 17ml of hydrochloric acid and 17ml of deionized water, putting the hydrochloric acid and the deionized water into a 100ml beaker, continuously stirring the mixture by using a glass rod in the whole process, stirring the mixture for 5 minutes by using a magnetic stirrer, adding 3.4ml of titanium isopropoxide and 1.7ml of titanium tetrachloride, sealing the opening of the beaker by using a preservative film, magnetically stirring the mixture for 30 minutes, finally transferring the prepared solution into a lining of a reaction kettle, putting a carbon fiber woven layer on which a titanium peroxide seed crystal layer is deposited, completely immersing the carbon fiber woven layer in the solution, carrying out water cooling after reacting for 60 minutes, taking out the carbon fiber woven layer, carrying out ultrasonic oscillation washing for a plurality of times by using pre-prepared dilute hydrochloric acid, distilled water and absolute ethyl alcohol in sequence, carrying out vacuum drying at 80 ℃, and obtaining titanium oxide with the thickness of about 150 microns after the reaction.
3) Conversion of thickened titanium oxide to barium titanate using hydrothermal reaction
0.02mol of Ba (NO)3)2Dissolving 0.08mol of NaOH in 40ml of deionized water, magnetically stirring for 30 minutes, transferring the prepared solution into a lining of a reaction kettle, putting the thickened titanium oxide layer carbon fiber woven layer into the solution, completely immersing the carbon fiber woven layer in the solution, cooling the reaction kettle by water at the hydrothermal temperature and for 36 hours in sequence, taking out the carbon fiber woven layer after the reaction is finished, ultrasonically oscillating and washing the carbon fiber woven layer for a plurality of times by using pre-prepared dilute hydrochloric acid, distilled water and absolute ethyl alcohol in sequence, and drying the carbon fiber woven layer in vacuum at 80 ℃.
4) Respectively coating epoxy resin on the carbon fiber woven layer modified by the piezoelectric nano layer and the common carbon fiber woven layer, and heating and curing the carbon fiber woven layer and the common carbon fiber woven layer in a vacuum environment, wherein the curing temperature is 100 ℃, and the curing time is 2 hours.
5) And (3) coating electrodes on the upper and lower surfaces of the cured piezoelectric nano-layer modified carbon fiber woven layer in a scraping mode, and then polarizing the carbon fiber woven layer, wherein the polarizing electric field is a direct-current electric field with the size of 40V/um, the polarizing temperature is 80 ℃, and the polarizing time is 3 h.
6) And arranging the carbon fiber woven layers modified by the polarized piezoelectric nano layers as a middle functional layer array, pasting the blank carbon fiber woven layers up and down, using epoxy resin as a matrix, and performing vacuum curing for 2h to finally prepare the carbon fiber composite material modified by the piezoelectric nano layers with the sandwich structure.
Example 4
1) Preparing a titanium oxide seed crystal layer on a carbon fiber woven layer
Firstly, the carbon fiber woven layer is cleaned by ultrasonic oscillation of acetone, ethanol and deionized water respectively, and then a titanium oxide seed crystal layer with the thickness of 50nm is deposited on the surface of the carbon fiber woven layer by using an Atomic Layer Deposition (ALD) technology. The process is as follows: blowing a titanium source precursor in a steam mode by taking nitrogen as carrier gas for 0.1 second, blowing out redundant titanium source by the nitrogen, and chemically adsorbing the titanium source on the carbon fiber woven layer in 6 seconds; then introducing ozone for 0.5 second, introducing nitrogen to blow out redundant ozone, and reacting the ozone with a titanium source precursor adsorbed on the carbon fiber cloth to generate titanium oxide with a monoatomic layer in 6 seconds; blowing out reaction residues through nitrogen, wherein the reaction residues take 6 seconds to complete one period; the above production cycle was repeated until a seed layer of titanium oxide having a thickness of 50nm was deposited on the carbon fiber woven layer.
2) Thickening a titanium oxide seed crystal layer by using a hydrothermal reaction
Measuring 17ml of hydrochloric acid and 17ml of deionized water, putting the hydrochloric acid and the deionized water into a 100ml beaker, continuously stirring the mixture by using a glass rod in the whole process, stirring the mixture for 5 minutes by using a magnetic stirrer, then adding 3.4ml of titanium isopropoxide and 1.7ml of titanium tetrachloride, sealing the opening of the beaker by using a preservative film, magnetically stirring the mixture for 30 minutes, finally transferring the prepared solution into a lining of a reaction kettle, putting a carbon fiber woven layer on which a titanium peroxide seed crystal layer is deposited, completely immersing the carbon fiber woven layer in the solution, carrying out water cooling after reacting for 45 minutes, taking out the carbon fiber woven layer, carrying out ultrasonic oscillation washing on the carbon fiber woven layer for a plurality of times by using pre-prepared dilute hydrochloric acid, distilled water and absolute ethyl alcohol in sequence, and carrying out vacuum drying at 90 ℃.
3) Conversion of thickened titanium oxide to barium titanate using hydrothermal reaction
0.02mol of Ba (NO)3)2Dissolving 0.08mol of NaOH in 40ml of deionized water, magnetically stirring for 30 minutes, transferring the prepared solution into a reaction kettle lining, putting the carbon fiber woven layer with the thickened titanium oxide layer into the solution, and completely immersing the carbon fiber woven layer in the solutionThe hydrothermal temperature and the hydrothermal time are 230 ℃ and 36 hours in sequence, the reaction kettle is cooled by water after the reaction is finished, then the carbon fiber woven layer is taken out, ultrasonic oscillation washing is carried out for a plurality of times by using pre-prepared dilute hydrochloric acid, distilled water and absolute ethyl alcohol in sequence, and vacuum drying is carried out at 90 ℃.
4) Respectively coating epoxy resin on the carbon fiber woven layer modified by the piezoelectric nano layer and the common carbon fiber woven layer, and heating and curing the carbon fiber woven layer and the common carbon fiber woven layer in a vacuum environment, wherein the curing temperature is 80 ℃ and the curing time is 2 hours.
5) And (3) coating electrodes on the upper and lower surfaces of the cured piezoelectric nano-layer modified carbon fiber woven layer in a scraping mode, and then polarizing the carbon fiber woven layer, wherein the polarizing electric field is a direct-current electric field with the size of 50V/um, the polarizing temperature is 90 ℃, and the polarizing time is 2 hours.
6) And arranging the carbon fiber woven layers modified by the polarized piezoelectric nano layers as a middle functional layer array, pasting the blank carbon fiber woven layers up and down, using epoxy resin as a matrix, and performing vacuum curing for 2h to finally prepare the carbon fiber composite material modified by the piezoelectric nano layers with the sandwich structure.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. A preparation method of a high-strength carbon fiber composite material with a self-sensing function is characterized by comprising the following steps:
(1) depositing a titanium oxide seed crystal layer on the surface of the carbon fiber layer by using an atomic layer deposition technology, and thickening the titanium oxide seed crystal layer by adopting a hydrothermal reaction;
(2) adopting hydrothermal reaction to convert the thickened titanium oxide seed crystal into barium titanate to obtain a carbon fiber woven layer modified by the piezoelectric nano layer;
(3) coating epoxy resin on both sides of the carbon fiber woven layer modified by the piezoelectric nano layer, and heating and curing in a vacuum environment;
(4) coating electrodes on two sides of the cured piezoelectric nano-layer modified carbon fiber woven layer in a scraping mode, and then polarizing to obtain a piezoelectric functional layer;
(5) arranging the piezoelectric functional layers as a middle functional layer array, pasting carbon fiber cloth on two sides of the middle functional layer, adopting epoxy resin to carry out integral packaging, and carrying out vacuum heating and curing to obtain the carbon fiber composite material with a sandwich structure and a self-detection function.
2. The method for preparing a high-strength carbon fiber composite material with a self-sensing function according to claim 1, wherein the step (1) of depositing a titanium oxide seed layer on the surface of the carbon fiber layer by using an atomic layer deposition technology comprises the following steps:
blowing a titanium source precursor in a steam mode by taking nitrogen as carrier gas for 0.1 second, blowing out redundant titanium source by the nitrogen, and chemically adsorbing the titanium source on the carbon fiber woven layer in 6 seconds; then introducing ozone for 0.5 second, introducing nitrogen to blow out redundant ozone, and reacting the ozone with a titanium source precursor adsorbed on the carbon fiber cloth to generate titanium oxide with a monoatomic layer in 6 seconds; blowing out reaction residues through nitrogen, wherein the reaction residues take 6 seconds to complete one period; the above cycle was repeated until a seed layer of titanium oxide having a thickness of 50nm was deposited on the carbon fiber woven layer.
3. The method for preparing the high-strength carbon fiber composite material with the self-perception function according to claim 1, wherein the step (1) of thickening the titanium oxide seed crystal layer by using a hydrothermal reaction is specifically as follows:
measuring 10 parts of hydrochloric acid and 10 parts of deionized water in parts by volume, mixing, adding 2 parts of titanium isopropoxide and 1 part of titanium tetrachloride, and uniformly stirring to obtain a reaction solution;
and immersing the carbon fiber woven layer deposited with the titanium oxide seed crystal layer in the reaction liquid for hydrothermal reaction at the hydrothermal temperature of 180 ℃ for 20-60min to obtain the thickened titanium oxide seed crystal layer on the carbon fiber woven layer.
4. The method for preparing a high-strength carbon fiber composite material with a self-sensing function according to claim 1, wherein the step (2) of converting the thickened titanium oxide seed crystals into barium titanate comprises the following specific steps:
0.02mol of Ba (NO)3)2And 0.08mol of NaOH is dissolved in 40ml of deionized water, the mixture is stirred uniformly, the carbon fiber woven layer loaded with the thickened titanium oxide seed crystal layer is immersed in the solution, hydrothermal reaction is carried out, the hydrothermal temperature is 230 ℃, the time is 36 hours, and after the reaction is finished, the titanium oxide seed crystal is converted into barium titanate.
5. The method for preparing a high-strength carbon fiber composite material with a self-sensing function according to claim 1, wherein the specific operation of performing heat curing in the step (3) is as follows:
the curing temperature is 60-100 ℃, and the curing time is 2 h.
6. The method for preparing a high-strength carbon fiber composite material with a self-sensing function according to claim 1, wherein the polarization conditions of the step (4) are as follows:
the polarization electric field is a direct current electric field, the size of the electric field is 40-60V/um, the polarization temperature is 80-100 ℃, and the polarization time is 1-3 h.
7. The method for preparing a high-strength carbon fiber composite material with a self-sensing function according to claim 1, further comprising the following step (5):
and connecting the upper electrode and the lower electrode of the middle functional layer with an oscilloscope, and synchronously reading data on a computer during testing to realize real-time monitoring on the high-strength carbon fiber composite material.
8. A high-strength carbon fiber composite material having a self-sensing function, which is produced by the production method according to any one of claims 1 to 7.
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