CN115109358A - Preparation method of piezoelectric material and three-dimensional film of drill rod fatigue wear monitoring equipment - Google Patents
Preparation method of piezoelectric material and three-dimensional film of drill rod fatigue wear monitoring equipment Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2327/00—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 a halogen; Derivatives of such polymers
- C08J2327/02—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
The invention discloses a method for preparing a piezoelectric material and a three-dimensional film of a drill rod fatigue wear monitoring device, which comprises the following steps: ag @ PZT ceramic powder is prepared through a photoreduction reaction, and a PVDF-based piezoelectric composite film is prepared. The method solves the technical problems that in the prior art, the precision and/or the efficiency of a method for detecting the fatigue flaw detection of the drill rod mill are low, and piezoelectric ceramics serving as piezoelectric materials are difficult to adapt to detection equipment for detecting the fatigue flaw detection of the drill rod mill due to the fact that the piezoelectric ceramics are hard in physical properties and poor in toughness and ductility.
Description
Technical Field
The invention relates to the technical field of ultra-deep wells, large-displacement directional wells and horizontal wells, in particular to a method for preparing a piezoelectric material and a three-dimensional film of a drill rod fatigue wear monitoring device.
Background
The geological drill rod is poor in working environment, easy to wear, corrode and fatigue, the drill rod is often subjected to strong tensile force and torsion force in the guiding and directional drilling process, and is also subjected to the action of bending force, when the drill rod rotates through a curve section, the rod body is subjected to tensile and compressive alternating stress, and the smaller the curvature radius of an arc line, the larger the alternating stress is. After the alternating stress reaches a certain value, the drill rod is easy to generate fatigue cracks.
The fatigue cracks that initially develop in the drill rod are very small and difficult to detect by the naked eye, but the fatigue cracks develop at a very rapid rate and eventually appear as sudden brittle fractures. In addition, the stress of the drill rod is complex under the well, the drill rod is often under the action of composite load, and meanwhile, the drill rod in the well has 3 modes of rotation, revolution, rotation and revolution, the rotation causes the drill rod to be uniformly worn, the revolution causes the drill rod to be eccentrically worn, and the strength of the drill rod is reduced after the drill rod is worn. Stratum constitution is different, and the inhomogeneity is strong, also is different to the coupling grinding degree of drilling rod, takes place to hold back, jump the phenomenon at the drilling in-process, aggravates drilling rod longitudinal vibration, makes the drilling rod take place fatigue wear, when the stratum is softer, takes place the jam accident easily. In addition, in the drilling process, rock chips, clean water, mud, foam and other complex environments exist, and some stratums have serious corrosivity, so that the corrosivity of the drilling fluid can enter micro cracks when fatigue wear occurs, the cracks can be accelerated to pierce through the drill rod, the effective section of the drill rod is continuously reduced as a result of the piercing development, and the drill rod is broken when the total length of the pierced holes and the cracks exceeds the critical crack size.
At present, eddy current detection, magnetic flux measurement and ultrasonic methods are mainly adopted for detecting fatigue defects of drill rods. The eddy current detection method is insensitive to damage detection of the inner wall of the drill rod, and particularly when the wall thickness of the drill rod is more than 6mm, the eddy current detection method cannot be selected for flaw detection of the drill rod body; the detection precision of the magnetic flux method is very low, and when the drill rod is eccentrically ground, the detection result has larger error, mainly because the average wall thickness is measured by the magnetic flux, and the local wall thickness is reduced by eccentric grinding; although the ultrasonic method is reasonable in precision, the drill rod body belongs to a pipe material and is large in surface area, the whole full-process full-section measurement of the drill rod body is needed for identifying the eccentric wear of the drill rod, and a multi-channel ultrasonic automatic thickness measuring system is needed, so that the overall detection efficiency is low.
Magnetic powder inspection and ultrasonic inspection can be used for the inspection of both ends of the drill rod and joints. The former is generally used for detecting the flaw of the outer surface and the thread part of the screw thread or the joint of the drill rod in a detection center, and is characterized in that the flaw detection speed of the screw thread is high and visual; the disadvantage is that only superficial or near-superficial lesions can be detected. The latter is mainly used for the on-site flaw detection of screw threads and joints, and has the advantages that the detector is portable and can simultaneously detect internal and external defects; the disadvantage is that ultrasonic inspection threads do not have uniform standards and ready-made inspection devices available.
The piezoelectric ceramic has high piezoelectric performance when being used as a material of equipment for detecting the flaw of the fatigue mill of the drill rod, but the physical performance of the piezoelectric ceramic is hard, and the development of the piezoelectric ceramic in some aspects is limited due to poor toughness and ductility. Thus, ceramic materials that are hard and brittle in texture are clearly inadequate. However, the flexible integrated circuit, the flexible intelligent robot and the like are more and more emphasized in daily life or national development.
Disclosure of Invention
Therefore, the invention provides a preparation method of a piezoelectric material and a three-dimensional film of a drill rod fatigue wear monitoring device, and aims to solve the technical problems that in the prior art, the precision and/or efficiency of a method for detecting the flaw detection of the drill rod fatigue wear is low, and piezoelectric ceramics serving as the piezoelectric material are difficult to adapt to the detection device for detecting the flaw detection of the drill rod fatigue wear due to the fact that the piezoelectric material has hard physical properties and poor toughness and ductility.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of a piezoelectric material of a drill pipe fatigue wear monitoring device comprises the following steps:
s100: preparing Ag @ PZT ceramic powder through a photoreduction reaction;
s101: putting ceramic powder and absolute ethyl alcohol into a three-neck flask, uniformly stirring by a magnetic stirrer, and then adding AgNO into the three-neck flask 3 Introducing nitrogen for 20min to remove air in the solution, preventing the temperature of the solution irradiated by a xenon lamp from rising to oxidize Ag nano particles into AgO, and irradiating the solution under the xenon lamp in the nitrogen atmosphere and continuously stirring to obtain an Ag @ PZT solution;
s102: washing off redundant silver ions in the Ag @ PZT solution, placing the Ag @ PZT solution after the photoreduction reaction in a centrifugal machine to quickly separate a solvent from a solute, and placing the solution in a vacuum drying oven after the solvent is removed until the Ag @ PZT solution is completely dried;
s103: putting the dried Ag @ PZT into an agate mortar, grinding into powder, pouring the powder into a glass bottle, and marking the powder as Ag @ PZT by using label paper to prepare the PVDF-based piezoelectric composite film;
s200: preparing a PVDF-based piezoelectric composite film;
s201: firstly, weighing PVDF (polyvinylidene fluoride) and placing the PVDF in N, N-Dimethylformamide (DMF) solution, sequentially carrying out ultrasonic oscillation, uniformly stirring by using a magnetic stirrer, and stirring until the PVDF is completely dissolved;
s202: weighing a certain amount of PZT powder, adding the PZT powder into a DMF solution for dissolving PVDF, and continuously stirring until the solution is uniformly mixed so as to avoid ceramic agglomeration;
s203: pouring the uniform solution onto a glass plate which is adjusted to be horizontal by a level meter in a vacuum drying oven, setting the temperature at a certain value, keeping the temperature, drying to form a film, and taking out the film to obtain a PVDF-based composite film sample, namely the PVDF-based piezoelectric composite film.
Further, in the step S101, the ceramic powder and the absolute ethyl alcohol are matched according to the proportion of 1:1, the working time of the magnetic stirrer ranges from 0.5 to 3 hours, and AgNO with the mass of 5 to 10 percent of the ceramic powder is added 3 And irradiating the solution under a xenon lamp under the protection of nitrogen for 0.5-2 h.
Further, in the step S102, redundant silver ions are removed to rapidly separate the solvent from the solute, the separation is repeated for 4-6 times, and then the obtained product is placed in a vacuum drying oven at 50-70 ℃.
Further, in the step S201, 1g of PVDF is weighed and placed in 10ml of N, N-Dimethylformamide (DMF) solution, the duration of ultrasonic oscillation is 5-10 min, and the PVDF is stirred by a magnetic stirrer until being completely dissolved.
Further, in step S202, 10g of PZT powder is then weighed and added to the DMF solution dissolving PVDF, and stirring is continued for 24h until the solution is mixed uniformly.
Further, in step S203, the uniform solution is poured into a vacuum drying oven, the temperature is set to be 70-90 ℃, the uniform solution is kept warm and dried to form a film, and the film is taken out after 2-3 hours to obtain the PVDF-based piezoelectric composite film.
Further, 100g of ceramic powder is firstly put into a three-neck flask, 100ml of absolute ethyl alcohol is added, the mixture is uniformly stirred for 1 hour by a magnetic stirrer, and then 5g of AgNO is continuously put into the three-neck flask 3 Introducing nitrogen, irradiating the solution under a xenon lamp in the nitrogen atmosphere, and continuously stirring by a magnetic stirrer, wherein the xenon lamp irradiates for 1 hour to obtain an Ag @ PZT solution;
washing off redundant silver ions in the Ag @ PZT solution, centrifuging the collected Ag @ PZT solution for 4 times at 2000 revolutions by using a centrifugal machine, and then putting the solution into a vacuum box at 60 ℃ for drying for 24 hours until the Ag @ PZT solution is completely dried;
putting all the dried Ag @ PZT into an agate mortar, performing ball milling at the ball milling rotation speed of 100 revolutions per minute for 2 hours to obtain dried Ag @ PZT, pouring the dried Ag @ PZT into a glass bottle, and marking the dried Ag @ PZT as Ag @ PZT by using label paper;
putting 10g of PVDF into a beaker, adding 100ml of N, N-Dimethylformamide (DMF), ultrasonically vibrating for 15min, and then uniformly stirring for 30min by a magnetic stirrer until the PVDF is completely dissolved;
adding 5g of Ag @ PZT powder into a DMF solution in which PVDF is dissolved, and continuing magnetically stirring for 12 hours by using a magnetic stirrer until the solution is uniformly mixed so as to avoid ceramic agglomeration;
flatly paving the uniformly stirred solution on a release film, pressing the release film into a 1mm rear film through a three-roller machine, and drying the rear film in a drying and heat-preserving box at the temperature of 80 ℃ for 3 hours to obtain a PVDF-based ceramic piezoelectric film;
the resulting PVDF-based piezoelectric ceramic film was attached to a given monitoring device as shown in fig. 1. The fatigue wear degree of the drill rod is judged through the piezoelectric signal of the piezoelectric ceramic film, and the slight fatigue wear of the drill rod in the drilling process is reflected in real time through the monitoring equipment.
A preparation method of a three-dimensional film for monitoring fatigue wear of a drill rod is provided, wherein the drill rod fatigue wear monitoring device is used for adapting to a piezoelectric material of the drill rod fatigue wear monitoring device, and comprises the following steps:
s1: weighing PVDF and PZT (50-100 nm, disposable pre-sintered powder), mixing, dissolving in DMF, placing the mixed solution in a planetary ball mill, adding zirconia balls for ball milling, and stirring at a high rotating speed to obtain a mixed solution;
s2: placing the mixed solution in a drying oven for 24 hours, and removing DMF to obtain a dried PZT composite material;
s3: ultrasonically oscillating DMF (dimethyl formamide), acetone and DMSO (dimethyl sulfoxide) solvents, and magnetically stirring until the DMF solvents, the acetone and the DMSO solvents are completely dissolved to obtain 3D printing slurry;
s4: 3D printing slurry is filled into a 20cc dispensing tube, a dispensing head with the inner diameter of 0.51mm is adopted in the dispensing tube, an air compressor is used for modulating the dispensing head to 6-10 MPa, a printing program is set, and a three-dimensional film with the length, width and height corresponding to 600mm, 400mm and 200mm is printed.
Further, in the step S1, the mass ratio of PVDF to Ag @ PZT is 10:1, the ball milling time is 2-6 h (the time is in proportion according to the total amount of the added materials), and the rotating speed is 800-1500;
placing the mixed solution in a drying oven at the temperature of 60-80 ℃ in step S2;
in the step S3, the volume ratio of DMF, acetone and DNSO is 6:10:1, and ultrasonic oscillation is carried out for 3-5 h;
in step S4, the printing speed Z is greater than 80 to 100 layers/h, the power consumption is less than 200W, and the structure is free of support (length, width, height, 600mm, 400mm, 200 mm).
Further, weighing PVDF100g and PZT10g, putting the weighed materials into a ball milling tank, adding 200ml of DMF solution and 2mm zirconia balls into the ball milling tank, carrying out ball milling for 3 hours, and stirring at the rotating speed of 1200 to obtain a mixed solution;
carrying out vacuum drying on the ball-milled solution at 60 ℃ for 8h, carrying out ultrasonic oscillation on 10g of the nano composite material, 40ml of DMF (dimethyl formamide), 60ml of acetone and 6ml of DMSO (dimethyl sulfoxide) for 4h after drying, and then carrying out magnetic stirring for 2h by using a magnetic stirrer until the nano composite material is completely dissolved to obtain 3D printing slurry;
and injecting the obtained 3D printing slurry into a 30cc rubber outlet pipe, selecting a rubber outlet head with the thickness of 0.51mm and the pressure of 6MPa, and printing a hollow cuboid piezoelectric module with the length, width and height of 300mm, 200mm and 100mm by using 3D printing.
The invention has the following beneficial effects:
1. the invention adopts the polymer-based flexible piezoelectric material, monitors the occurrence of unfavorable conditions such as fatigue wear, puncture and the like in the using process of the drill rod in real time in the using process, and timely adjusts the conditions to avoid accidents.
2. The Pb (Zr, Ti) O3 (PZT)/polyvinylidene fluoride (PVDF) -based piezoelectric composite film is prepared by a solution casting method, the process is simpler than the steps of a casting method, and compared with a hot pressing method, the thickness of the prepared film is thinner. The thickness of the prepared film is about 10-100 mu m, and the mass fraction of the PZT ceramic powder is 5-15%. The piezoelectric composite film with low piezoelectric ceramic content has the advantages that as the ceramic is compounded in the PVDF in a 0-3 structure, the ceramic particles exist in the composite film in a non-communicated mode, the partial pressure applied to the piezoelectric particles during polarization is small, and the degree of consistent dipole orientation is low. Therefore, the method for introducing the conductive particles, such as forming a drastic heterostructure on the surface of the PZT ceramic through the photoreduction reaction of Ag nano particles, doping multi-wall carbon nano tubes and the like, increases a conductive channel and promotes the partial pressure of inorganic particles. Thereby realizing the improvement of the piezoelectric property of the piezoelectric composite film prepared when the quality of the doped piezoelectric ceramic is low in time sharing. The PVDF composite exists in the form of a film. Therefore, PDMS and Pb (NiNb) O3-Pb (Zr, Ti) O3 (PNN-PZT) ceramics are prepared into paste suitable for 3D printing according to a certain proportion, and the Polydimethylsiloxane (PDMS) has certain designability in a forming structure and combines the advantages of a 3D printing technology to prepare a flexible piezoelectric transducer similar to a classic multilayer ceramic capacitor, so that the combination of 3D printing of an electrode layer and a paste layer is realized. The piezoelectric property, the temperature adaptability, the mechanical property and the like of the structure are tested, the function of integration of structure and self-sensing is realized, the structure and the self-sensing are combined with corresponding monitoring equipment, the fatigue wear and the puncture of the drill rod can be effectively monitored in real time in the drilling process, and the functional practicability is improved.
Drawings
In order to clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly introduced, and the structures, the proportions, the sizes, and the like shown in the specification are only used for matching with the contents disclosed in the specification, so that those skilled in the art can understand and read the modifications of any structures, the changes of the proportion relationships, or the adjustments of the sizes, without affecting the functions and the achievable purposes of the present invention, and still fall within the scope of the technical contents disclosed in the present invention.
Fig. 1 is a schematic structural diagram of an external shape of a piezoelectric device based on monitoring fatigue wear and puncture of a drill rod according to an embodiment of the present invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. 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.
In the present specification, the terms "upper", "lower", "left", "right" and "middle" are used for clarity of description only, and are not used to limit the scope of the present invention, and the relative relationship between the terms and the relative positions may be changed or adjusted without substantial technical change.
Example 1
In embodiment 1, an embodiment of the present invention provides a method for preparing a piezoelectric material for a drill pipe fatigue wear monitoring device, including the following steps:
s100: and preparing the Ag @ PZT ceramic powder through a photoreduction reaction.
S101: putting ceramic powder and absolute ethyl alcohol into a three-neck flask, uniformly stirring by a magnetic stirrer, and then adding AgNO into the three-neck flask 3 And introducing nitrogen for 20min to remove air in the solution, preventing the Ag nanoparticles from being oxidized into AgO due to the temperature rise of the solution irradiated by a xenon lamp, and irradiating the solution under the xenon lamp in the nitrogen atmosphere and continuously stirring to obtain the Ag @ PZT solution.
S102: and (3) washing off redundant silver ions in the Ag @ PZT solution, putting the Ag @ PZT solution after the photoreduction reaction in a centrifugal machine to quickly separate a solvent from a solute, and putting the solution in a vacuum drying oven after the solvent is removed until the Ag @ PZT solution is completely dried.
S103: putting all the dried Ag @ PZT into an agate mortar, grinding into powder, pouring into a glass bottle, and marking as Ag @ PZT by using label paper to prepare the PVDF-based piezoelectric composite film.
S200: and preparing the PVDF-based piezoelectric composite film.
S201: firstly, weighing PVDF (polyvinylidene fluoride) and placing the PVDF in N, N-Dimethylformamide (DMF) solution, sequentially carrying out ultrasonic oscillation, uniformly stirring the PVDF by using a magnetic stirrer until the PVDF is completely dissolved.
S202: then weighing a certain amount of PZT powder, adding the PZT powder into a DMF solution for dissolving PVDF, and continuously stirring until the solution is uniformly mixed so as to prevent the ceramic from agglomerating.
S203: pouring the uniform solution on a glass plate which is adjusted to be horizontal by a level meter in a vacuum drying oven, setting the temperature at a certain value, preserving heat, drying to form a film, and taking out to obtain a PVDF-based composite film sample, namely the PVDF-based piezoelectric composite film.
According to one embodiment of the invention, in the step S101, the ceramic powder and the absolute ethyl alcohol are matched according to a ratio of 1:1, the working time of the magnetic stirrer ranges from 0.5 h to 3h, and AgNO with the mass of 5% -10% of the ceramic powder is added 3 And irradiating the solution under a xenon lamp under the protection of nitrogen for 0.5-2 h.
According to an embodiment of the invention, the excess silver ions are removed in step S102 to rapidly separate the solvent and the solute, the process is repeated 4-6 times, and then the obtained product is placed in a vacuum drying oven at 50-70 ℃.
According to one embodiment of the invention, 1g of PVDF weighed in step S201 is placed in 10ml of N, N-Dimethylformamide (DMF) solution, the duration of ultrasonic oscillation is 5-10 min, and the PVDF is stirred by a magnetic stirrer until the PVDF is completely dissolved.
According to one embodiment of the present invention, 10g of PZT powder is then weighed in step S202 and added to the DMF solution dissolving PVDF, and stirring is continued for 24h until the solution is mixed uniformly.
According to one embodiment of the invention, in step S203, the homogeneous solution is poured into a vacuum drying oven, the temperature is set to be 70-90 ℃, the solution is kept warm and dried to form a film, and the film is taken out after 2-3 hours to obtain the PVDF-based piezoelectric composite film.
The following is a preferred overall preparation method provided in example 1:
firstly, 100g of ceramic powder is put into a three-neck flask, 100ml of absolute ethyl alcohol is added, the mixture is uniformly stirred for 1 hour by a magnetic stirrer, and then 5g of AgNO is continuously put into the three-neck flask 3 And introducing nitrogen, irradiating the solution under a xenon lamp in the nitrogen atmosphere, and continuously stirring by a magnetic stirrer, wherein the xenon lamp irradiates for 1h to obtain the Ag @ PZT solution.
And (3) washing off redundant silver ions in the Ag @ PZT solution, centrifuging the collected Ag @ PZT solution for 4 times by using a centrifugal machine, and then putting the solution into a vacuum box at 60 ℃ for drying for 24 hours until the Ag @ PZT is completely dried.
And putting all the dried Ag @ PZT into an agate mortar for ball milling at the ball milling speed of 100 rpm for 2 hours to obtain dried Ag @ PZT, pouring the dried Ag @ PZT into a glass bottle, and marking the dried Ag @ PZT as Ag @ PZT by using label paper.
Putting 10g of PVDF into a beaker, adding 100ml of N, N-Dimethylformamide (DMF), ultrasonically vibrating for 15min, and then uniformly stirring for 30min by a magnetic stirrer until the PVDF is completely dissolved.
5g of Ag @ PZT powder is added into a DMF solution in which PVDF is dissolved, and magnetic stirring is continued for 12 hours by a magnetic stirrer until the solution is uniformly mixed so as to avoid ceramic agglomeration.
And flatly paving the uniformly stirred solution on a release film, pressing the release film into a 1mm rear film by a three-roller machine, and drying the rear film in a drying and heat-preserving box at the temperature of 80 ℃ for 3 hours to obtain the PVDF-based ceramic piezoelectric film.
The resulting PVDF-based piezoelectric ceramic film was attached to a given monitoring device as shown in fig. 1. The fatigue wear degree of the drill rod is judged through the piezoelectric signal of the piezoelectric ceramic film, and the slight fatigue wear of the drill rod in the drilling process is reflected in real time through the monitoring equipment.
Example 2
In embodiment 2, the embodiment of the invention further provides a preparation method of the drill rod fatigue wear monitoring three-dimensional film, which specifically comprises the following steps:
s1: weighing PVDF and PZT (50-100 nm, disposable pre-sintered powder), mixing, dissolving in DMF, placing the mixed solution in a planetary ball mill, adding zirconia balls for ball milling, and stirring at a high rotating speed to obtain the mixed solution.
S2: and (5) placing the mixed solution in a drying oven for 24 hours, and removing DMF to obtain the dried PZT composite material.
S3: and ultrasonically oscillating the DMF, acetone and DMSO solvents, and magnetically stirring until the DMF, acetone and DMSO solvents are completely dissolved to obtain the 3D printing slurry.
S4: 3D printing slurry is filled into a 20cc dispensing tube, a dispensing head with the inner diameter of 0.51mm is adopted in the dispensing tube, an air compressor is used for modulating the dispensing head to 6-10 MPa, a printing program is set, and a three-dimensional film with the length, width and height corresponding to 600mm, 400mm and 200mm is printed.
According to one embodiment of the invention, the mass ratio of PVDF to Ag @ PZT in the step S1 is 10:1, the ball milling time is 2-6 h (the time is proportional to the total amount of the added materials), and the rotating speed is 800-1500.
According to an embodiment of the invention, the mixed solution in the step S2 is placed in a drying oven at 60-80 ℃.
According to an embodiment of the invention, in the step S3, the volume ratio of DMF, acetone and DNSO is 6:10:1, and ultrasonic oscillation is performed for 3-5 hours.
According to one embodiment of the present invention, the printing speed Z direction in step S4 is greater than 80 to 100 layers/h, the power consumption is less than 200W, and the structure is free of support and upright (length, width, height, 600mm, 400mm, 200 mm).
The following is a preferred overall preparation method provided in example 2:
PVDF100g and PZT10g are weighed and placed into a ball milling tank, 200ml of DMF solution and 2mm zirconia balls are added into the ball milling tank, ball milling is carried out for 3 hours, and stirring is carried out at the rotating speed of 1200, so as to obtain a mixed solution.
And (3) drying the ball-milled solution at 60 ℃ for 8h in vacuum, ultrasonically oscillating 10g of the nano composite material with 40ml of DMF, 60ml of acetone and 6ml of DMSO for 4h after drying, and then magnetically stirring for 2h by using a magnetic stirrer until the nano composite material is completely dissolved to obtain the 3D printing slurry.
And injecting the obtained 3D printing slurry into a 30cc rubber outlet pipe, selecting a rubber outlet head with the thickness of 0.51mm and the pressure of 6MPa, and printing a hollow cuboid piezoelectric module with the length, width and height of 300mm, 200mm and 100mm by using 3D printing.
Although the invention has been described in detail with respect to the general description and the specific embodiments, it will be apparent to those skilled in the art that modifications and improvements may be made based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a piezoelectric material of a drill pipe fatigue wear monitoring device is characterized by comprising the following steps:
s100: preparing Ag @ PZT ceramic powder through a photoreduction reaction;
s101: putting ceramic powder and absolute ethyl alcohol into a three-neck flask, and uniformly stirring by a magnetic stirrerThen adding AgNO into the three-neck flask 3 Introducing nitrogen for 20min to remove air in the solution, preventing the temperature of the solution irradiated by a xenon lamp from rising to oxidize Ag nano particles into AgO, and irradiating the solution under the xenon lamp in the nitrogen atmosphere and continuously stirring to obtain an Ag @ PZT solution;
s102: washing off redundant silver ions in the Ag @ PZT solution, putting the Ag @ PZT solution after the photoreduction reaction in a centrifugal machine to quickly separate a solvent and a solute, and putting the solution in a vacuum drying oven after the solvent is removed until the Ag @ PZT solution is completely dried;
s103: putting the dried Ag @ PZT into an agate mortar, grinding into powder, pouring the powder into a glass bottle, and marking the powder as Ag @ PZT by using label paper to prepare the PVDF-based piezoelectric composite film;
s200: preparing a PVDF-based piezoelectric composite film;
s201: firstly, weighing PVDF (polyvinylidene fluoride) and placing the PVDF in N, N-Dimethylformamide (DMF) solution, sequentially carrying out ultrasonic oscillation, uniformly stirring by using a magnetic stirrer, and stirring until the PVDF is completely dissolved;
s202: weighing a certain amount of PZT powder, adding the PZT powder into a DMF solution for dissolving PVDF, and continuously stirring until the solution is uniformly mixed so as to avoid ceramic agglomeration;
s203: pouring the uniform solution onto a glass plate which is adjusted to be horizontal by a level meter in a vacuum drying oven, setting the temperature at a certain value, keeping the temperature, drying to form a film, and taking out the film to obtain a PVDF-based composite film sample, namely the PVDF-based piezoelectric composite film.
2. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 1,
in the step S101, the ceramic powder and the absolute ethyl alcohol are matched according to the proportion of 1:1, the working time of the magnetic stirrer ranges from 0.5 to 3 hours, and AgNO with the mass of 5 to 10 percent of the ceramic powder is added 3 And irradiating the solution under a xenon lamp under the protection of nitrogen for 0.5-2 h.
3. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 2,
and step S102, removing redundant silver ions to quickly separate the solvent from the solute, repeating for 4-6 times, and then placing in a vacuum drying oven at 50-70 ℃.
4. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 1,
step S201, weighing 1g of PVDF, placing the PVDF in 10ml of N, N-Dimethylformamide (DMF) solution, carrying out ultrasonic oscillation for 5-10 min, and stirring the PVDF by a magnetic stirrer until the PVDF is completely dissolved.
5. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 4,
in step S202, 10g of PZT powder is then weighed and added to the DMF solution dissolving PVDF, and stirring is continued for 24h until the solution is uniformly mixed.
6. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 5,
and step S203, pouring the uniform solution into a vacuum drying oven, setting the temperature at 70-90 ℃, preserving the heat, drying and forming a film, and taking out the film after 2-3 hours to obtain the PVDF-based piezoelectric composite film.
7. The method for preparing the piezoelectric material of the drill pipe fatigue wear monitoring device according to claim 1,
firstly, 100g of ceramic powder is put into a three-neck flask, 100ml of absolute ethyl alcohol is added, the mixture is uniformly stirred for 1 hour by a magnetic stirrer, and then 5g of AgNO is continuously put into the three-neck flask 3 Introducing nitrogen, irradiating the solution under a xenon lamp in the nitrogen atmosphere, and continuously stirring the solution by a magnetic stirrer, wherein the xenon lamp irradiates for 1 hour to obtain an Ag @ PZT solution;
washing off redundant silver ions in the Ag @ PZT solution, centrifuging the collected Ag @ PZT solution for 4 times at 2000 revolutions by using a centrifugal machine, and then putting the solution into a vacuum box at 60 ℃ for drying for 24 hours until the Ag @ PZT solution is completely dried;
putting all the dried Ag @ PZT into an agate mortar, performing ball milling at the ball milling rotation speed of 100 revolutions per minute for 2 hours to obtain dried Ag @ PZT, pouring the dried Ag @ PZT into a glass bottle, and marking the dried Ag @ PZT as Ag @ PZT by using label paper;
putting 10g of PVDF into a beaker, adding 100ml of N, N-Dimethylformamide (DMF), ultrasonically vibrating for 15min, and then uniformly stirring for 30min by a magnetic stirrer until the PVDF is completely dissolved;
adding 5g of Ag @ PZT powder into a DMF solution in which PVDF is dissolved, and continuing magnetically stirring for 12 hours by using a magnetic stirrer until the solution is uniformly mixed so as to avoid ceramic agglomeration;
flatly paving the uniformly stirred solution on a release film, pressing the release film into a 1mm rear film through a three-roller machine, and drying the rear film in a drying and heat-preserving box at the temperature of 80 ℃ for 3 hours to obtain a PVDF-based ceramic piezoelectric film;
the resulting PVDF-based piezoelectric ceramic film was attached to a given monitoring device as shown in fig. 1. The fatigue wear degree of the drill rod is judged through the piezoelectric signal of the piezoelectric ceramic film, and the slight fatigue wear of the drill rod in the drilling process is reflected in real time through the monitoring equipment.
8. A preparation method of a drill pipe fatigue wear monitoring three-dimensional film, wherein the drill pipe fatigue wear monitoring device is used for adapting the piezoelectric material of the drill pipe fatigue wear monitoring device according to any one of claims 1-7, and the method comprises the following steps:
s1: weighing PVDF and PZT (50-100 nm, disposable pre-sintered powder), mixing, dissolving in DMF, placing the mixed solution in a planetary ball mill, adding zirconia balls for ball milling, and stirring at a high rotating speed to obtain a mixed solution;
s2: placing the mixed solution in a drying oven for 24 hours, and removing DMF to obtain a dried PZT composite material;
s3: ultrasonically oscillating DMF (dimethyl formamide), acetone and DMSO (dimethyl sulfoxide) solvents, and magnetically stirring until the DMF solvents, the acetone and the DMSO solvents are completely dissolved to obtain 3D printing slurry;
s4: 3D printing slurry is filled into a 20cc dispensing tube, a dispensing head with the inner diameter of 0.51mm is adopted in the dispensing tube, an air compressor is used for modulating the dispensing head to 6-10 MPa, a printing program is set, and a three-dimensional film with the length, width and height corresponding to 600mm, 400mm and 200mm is printed.
9. The method for preparing the three-dimensional film for monitoring the fatigue and wear of the drill rod according to claim 8,
in the step S1, the mass ratio of PVDF to Ag @ PZT is 10:1, the ball milling time is 2-6 h (the time corresponds to the proportion of the total amount of the added materials), and the rotating speed is 800-1500;
placing the mixed solution in a drying oven at 60-80 ℃ in step S2;
in the step S3, the volume ratio of DMF, acetone and DNSO is 6:10:1, and ultrasonic oscillation is carried out for 3-5 h;
in step S4, the printing speed Z direction is greater than 80-100 layers/h, the power consumption is less than 200W, and the structure is free of support (length, width, height, 600mm, 400mm, 200 mm).
10. The method for preparing the three-dimensional film for monitoring the fatigue and wear of the drill rod according to claim 8,
weighing PVDF100g and PZT10g, putting into a ball milling tank, adding 200ml of DMF solution and 2mm zirconia balls into the ball milling tank, carrying out ball milling for 3h, and stirring at the rotating speed of 1200 to obtain a mixed solution;
carrying out vacuum drying on the ball-milled solution at 60 ℃ for 8h, carrying out ultrasonic oscillation on 10g of the nano composite material, 40ml of DMF (dimethyl formamide), 60ml of acetone and 6ml of DMSO (dimethyl sulfoxide) for 4h after drying, and then carrying out magnetic stirring for 2h by using a magnetic stirrer until the nano composite material is completely dissolved to obtain 3D printing slurry;
and injecting the obtained 3D printing slurry into a 30cc rubber outlet pipe, selecting a rubber outlet head with the thickness of 0.51mm and the pressure of 6MPa, and printing a hollow cuboid piezoelectric module with the length, width and height of 300mm, 200mm and 100mm by using 3D printing.
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