CN115819106B - Preparation method of composite PZT porous ceramic with functionally gradient structure - Google Patents
Preparation method of composite PZT porous ceramic with functionally gradient structure Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 46
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- 238000007639 printing Methods 0.000 claims abstract description 15
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- 238000005245 sintering Methods 0.000 claims abstract description 10
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- 239000002356 single layer Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
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- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 4
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011540 sensing material Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 claims description 2
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 claims description 2
- 229930006739 camphene Natural products 0.000 claims description 2
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 claims description 2
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a preparation method of a composite PZT porous ceramic with a functional gradient structure, and relates to the technical field of functional material preparation. The method comprises the following steps: (1) preparation of PZT slurry: uniformly dispersing PZT powder, a dispersing agent and a binder in a solvent to obtain a PZT slurry suspension, and adjusting the pH to 6-8 to form PZT slurry; (2) preparation of a green body with a three-dimensional structure: the ceramic model with the gradient structure is designed by drawing software, and a three-dimensional structure blank is obtained in a directional temperature field through a 3D direct writing technology; (3) preparation of PZT porous ceramics: and freeze-drying and sintering the three-dimensional structure obtained by printing to obtain the PZT porous ceramic with macroscopic and microscopic composite porous structures. According to the invention, by setting the directional temperature field, liquid medium water in the slurry grows along the temperature gradient crystal, so that the sensor has excellent sensing characteristics.
Description
Technical Field
The invention relates to the technical field of functional material preparation, in particular to a preparation method of a composite PZT porous ceramic with a functional gradient structure.
Background
With the increasing maturity of 3D technology, the technology of realizing device preparation with complex structure by combining additive manufacturing with functional ceramics through 3D technology has been rapidly developed, which makes many structures which cannot be realized by traditional preparation methods possible.
For example, in patent application document CN112028628B, a method for preparing PZT ferroelectric ceramic with periodic pore structure by 3D printing, a method for forming ceramic blank with periodic pore structure by layer-by-layer printing and drying by 3D printing is disclosed, the material can realize periodic uniform distribution of pore structure and controllable porosity, and can significantly improve the detection rate figure of merit of PZT piezoelectric ceramic applied in terms of water sound, or significantly regulate and control the shock resistance of PZT ferroelectric ceramic, and better meet application requirements.
In the patent application document CN111747775B, a gradient functional ceramic material based on photo-curing 3D printing and an additive manufacturing method thereof, a preparation technology for preparing a porous ceramic material with a functional gradient structure by adopting a 3D printing technology is disclosed, and the prepared porous ceramic material has the performance advantages of higher bending strength, higher density, uniform tissue, better overall oxidation resistance, gradient change of the characteristics and functions of the material, and can be used for shell materials of hot end parts such as engine blades, nose cones and the like in the aerospace field and hypersonic aircrafts.
The patent application document No. CN109400200B, namely hydroxyapatite porous ceramic with controllable macroscopic and microscopic structures, and a preparation method and application thereof, is applied to biological ceramics.
However, for preparing the sensor material, the above-mentioned periodic uniform distribution of the pore structure, controllable porosity, shock resistance and the like are considered, and the most important point is that the sensing sensitivity is controlled, and the composite porous sensing material prepared by the existing 3D printing technology is further required to be enhanced in the sensing sensitivity.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of composite PZT porous ceramic with a functional gradient structure, which aims to solve the technical problem that the sensing sensitivity of the composite porous sensing material prepared by the prior art is not ideal.
The technical scheme adopted by the invention is as follows:
a preparation method of a composite PZT porous ceramic with a functionally gradient structure comprises the following steps:
(1) Preparing PZT slurry: uniformly dispersing PZT powder, a dispersing agent and a binder in a solvent to obtain a PZT slurry suspension, and adjusting the pH to 6-8 to form PZT slurry, wherein the solid content of the PZT slurry is 30 vol%;
(2) Preparing a blank with a three-dimensional structure: the ceramic model with the gradient structure is designed by utilizing drawing software, a multilayer three-dimensional structure blank is obtained in a directional temperature field through a 3D direct writing technology, the single-layer volume fraction of the three-dimensional structure blank is set to be a structure with a small middle layer and a large two-end layer, the ceramic model specifically comprises 6 layers, the volume fraction of the upper two layers and the lower two layers is 48.8%, and the volume fraction of the middle two layers is 43.2%;
(3) Preparation of PZT porous ceramics: and freeze-drying and sintering the three-dimensional structure obtained by printing to obtain the PZT porous ceramic with macroscopic and microscopic composite porous structures.
Preferably, in the step (1), the solvent is one or more of tert-butanol, camphene and water.
Preferably, in the step (2), the diameter of the printing needle head of the 3D direct writing technology is 0.16-0.61 mm, the printing speed is 50-100 mm/s, and the paste extrusion speed is 0.8-3.2 ml/h.
Preferably, in the step (2), the specific operation of obtaining the three-dimensional structure blank in the directional temperature field is as follows: and extruding PZT slurry on a cold and hot flat plate, wherein the surface of the cold and hot flat plate is a cold end of a directional temperature field, the temperature of the cold end is-50 to-10 ℃, the cold and hot flat plate is placed in room temperature, the hot end is room temperature, a directional temperature field is formed between the cold end and the hot end, and a set three-dimensional structure is directly obtained through layer-by-layer printing in the direction Wen Changxia.
Preferably, in the step (2), the specific operation of obtaining the three-dimensional structure blank in the directional temperature field is as follows: the PZT slurry was extruded at room temperature and then placed in a directional temperature field for a freezing process.
Preferably, in the step (3), the freeze-drying temperature is-50 to-20 ℃ and the drying time is 48 hours; the sintering temperature is 1200-1250 ℃, and the heating rate is 4-5 ℃/min.
The composite PZT porous ceramic prepared by any one of the above preparation methods.
The application of the composite PZT porous ceramic in sensing materials.
In summary, compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, by setting the directional temperature field, liquid medium water in the slurry is crystallized and grown along a temperature gradient, ice crystals push ceramic particles to rearrange in the process of directional growth, and after solidification, the ice crystals are sublimated and removed under the condition of low temperature and low pressure, so that directional pore channels taking the ice crystals as templates are left. After the sample sintering was completed, corona polarization was performed for 30min under a direct voltage of 15kV with heating at 80 ℃. The polarization direction is along the freezing direction, i.e. the direction of the directional temperature field during printing. In the polarization direction, the ceramic has good connectivity, higher polarization efficiency and excellent sensing characteristic, and the highest sensitivity can reach 8.98V/kPa under the action of 0.1-1N external force.
Drawings
FIG. 1 is a process flow diagram of a preparation method provided by the invention;
FIG. 2 is a schematic diagram of a single layer PZT porous ceramic structure with different volume fractions;
FIG. 3 is a diagram of the composite PZT porous ceramic material prepared in example 1;
FIG. 4 is a microscopic topography of a composite PZT porous ceramic;
FIG. 5 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with the composite porous structure prepared in example 1 is electrically polarized;
FIG. 6 is a graph showing response time corresponding to external force after the PZT porous ceramic with composite porous structure prepared in example 1 is electrically polarized;
FIG. 7 is a graph showing the sensitivity analysis of the external force output voltage after the PZT porous ceramic with the composite porous structure prepared in example 1 is electrically polarized;
FIG. 8 is a diagram of the composite PZT porous ceramic material prepared in example 2;
FIG. 9 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with composite porous structure prepared in example 2 is electrically polarized;
FIG. 10 is a graph showing the sensitivity analysis of the external force output voltage after the PZT porous ceramic with the composite porous structure prepared in example 2 is electrically polarized;
FIG. 11 is a diagram of a composite PZT porous ceramic material prepared in example 3;
FIG. 12 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with composite porous structure prepared in example 3 is electrically polarized;
FIG. 13 is a graph showing the sensitivity analysis of the external force output voltage after the PZT porous ceramic with the composite porous structure prepared in example 3 is electrically polarized;
FIG. 14 is a diagram of the composite PZT porous ceramic material prepared in example 4;
FIG. 15 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with composite porous structure prepared in example 4 is electrically polarized;
FIG. 16 is a graph showing the sensitivity analysis of the external force output voltage after the electrical polarization of the PZT porous ceramic with the composite porous structure prepared in example 4;
FIG. 17 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with composite porous structure prepared in example 5 is electrically polarized;
FIG. 18 is a graph showing the sensitivity analysis of the external force output voltage after the electrical polarization of the PZT porous ceramic with the composite porous structure prepared in example 5;
FIG. 19 is a bar graph showing the output voltage corresponding to different external forces after the PZT porous ceramic with composite porous structure prepared in example 6 is electrically polarized;
FIG. 20 is a graph showing the sensitivity analysis of the external force output voltage after the electrical polarization of the PZT porous ceramic with the composite porous structure prepared in example 6.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and embodiments. It should be understood that the particular embodiments described herein are illustrative only and are not intended to limit the invention, i.e., the embodiments described are merely some, but not all, of the embodiments of the invention.
The word "embodiment" as used herein does not necessarily mean that any embodiment described as "exemplary" is preferred or advantageous over other embodiments. Performance index testing in this method example unless otherwise specified, conventional testing methods in the art were employed. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure.
Unless otherwise defined, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; other raw materials, reagents, test methods and technical means not specifically mentioned in the present invention refer to raw materials and reagents commonly used by those skilled in the art, and experimental methods and technical means commonly employed.
The process flow chart of the invention is shown in figure 1, and comprises the following steps:
(1) Preparing PZT slurry: uniformly dispersing PZT powder, a dispersing agent and a binder in a solvent to obtain a PZT slurry suspension, and adjusting the pH to 6-8 to form PZT slurry;
(2) Preparing a blank with a three-dimensional structure: the ceramic model with the gradient structure is designed by drawing software, and a multilayer three-dimensional structure blank is obtained in a directional temperature field through a 3D direct writing technology;
(3) Preparation of PZT porous ceramics: and freeze-drying and sintering the three-dimensional structure obtained by printing to obtain the PZT porous ceramic with macroscopic and microscopic composite porous structures.
Wherein, each single layer of the multi-layer three-dimensional structure blank controls the macroscopic structure by adjusting the volume fraction, as shown in figure 2, is a single layer PZT porous ceramic structure with different volume fractions, the volume fraction on the left is 48.8%, and the invention is named as a layer A structure; the volume fraction on the right is 43.2%, and the invention is named as a B layer structure.
Example 1
The embodiment provides a specific preparation scheme of a composite PZT porous ceramic with a functionally gradient structure, which comprises the following steps:
step one, preparing slurry: uniformly dispersing PZT powder, a dispersing agent and a binder in deionized water to obtain a PZT slurry suspension. 5wt.% of dilute nitric acid is added to adjust the pH to about 6, and the rheological property of the slurry is changed, so that the slurry is suitable for direct writing forming. Wherein the dispersant is polyacrylate (BYK-154); the binder is polyvinyl alcohol (PVA-124, chemical engineering Co., ltd.), and the actual operation shows that the pH is too high, the slurry viscosity is low, and the molding can not be performed; the pH is too low, the fluidity of the slurry is poor, the growth of ice crystals is hindered, and the pH can achieve a better balance at about 6. The solid content of the PZT slurry prepared in the embodiment is 30 vol%, when the solid content is too low, the slurry has good fluidity, the storage modulus of the extruded lines is low, the support is poor, and the PZT slurry cannot be molded; when the solid content is too high, the shape of the micro-holes is not obvious, and the density tends to be high.
Step two, preparing a blank with a three-dimensional structure: and (3) designing a ceramic model with a gradient structure by using drawing software, extruding slurry on a cold and hot flat plate by using a 3D direct writing technology, and printing layer by layer in an orientation Wen Changxia to obtain a set three-dimensional structure. Wherein, print head diameter is 0.26mm. The cold end temperature of the cold and hot flat plate is-25 ℃. Too low a temperature at the cold end will cause the slurry in the syringe to solidify and not be able to extrude. The cold end temperature is too high, and the temperature gradient is not obvious, so that the microscopic pore morphology orientation is poor. The printing speed was 75mm/s. The slurry extrusion speed is 1.2ml/h; the glue discharging temperature is 600 ℃, and the heating rate is 1 ℃/min; the single-layer volume fraction of the multi-layer three-dimensional structure blank is set to be a structure with a small middle layer and a large two-end layer, and the three-dimensional structure blank specifically comprises 6 layers, wherein the volume fraction of the upper two layers and the lower two layers is 48.8%, the volume fraction of the middle two layers is 43.2%, and the three-dimensional structure blank obtained by the embodiment is of an A-A-B-B-A-A structure according to the naming shorthand.
Step three, preparing PZT porous ceramics: and freeze-drying and sintering the three-dimensional structure obtained by printing to obtain the PZT porous ceramic with macroscopic and microscopic composite porous structures, wherein the obtained material object is shown in figure 3, and the microscopic morphology is shown in figure 4. Wherein the freeze drying temperature is between 50 ℃ below zero and 20 ℃ below zero for 48 hours; the sintering temperature is 1250 ℃, and the heating rate is 5 ℃/min.
The sensing performance test was performed on the PZT porous ceramic of the composite porous structure obtained in the present example: the porous ceramic obtained by sintering is uniformly coated with electrodes on the upper and lower surfaces, polarization is carried out along the freezing direction of a directional temperature field, and the sensing performance test is carried out by carrying out periodic or random external force stimulation on the three-dimensional ceramic structure, wherein the conditions of output voltage, response time and sensitivity are as shown in figures 5-7, the sensitivity is 8.98V/kPa, and the output voltage is 191V under the action of 1N external force.
Example 2
On the basis of the embodiment 1, other steps are kept unchanged, only the single-layer volume fraction of the multi-layer three-dimensional structure blank is set to be B-B-B-B, the sensing performance test is carried out on the PZT porous ceramic with the composite porous structure obtained in the embodiment, as shown in fig. 8, the result is that the sensitivity is 7.02V/kPa, and the output voltage is 150V under the action of 1N external force, as shown in fig. 9/10.
Example 3
Based on the embodiment 1, other steps are kept unchanged, only the single-layer volume fraction of the multi-layer three-dimensional structure blank is set to be A-A-A-B-B, the actual sensing performance test is carried out on the PZT porous ceramic with the composite porous structure obtained in the embodiment as shown in FIG. 11, the result is that the sensitivity is 7.83V/kPa, and the output voltage is 165V under the action of 1N external force as shown in FIG. 12/13.
Example 4
Based on the embodiment 1, other steps are kept unchanged, only the single-layer volume fraction of the multi-layer three-dimensional structure blank is set to be A-B-A-B, the actual sensing performance test is carried out on the PZT porous ceramic with the composite porous structure obtained in the embodiment as shown in fig. 14, the result is that the sensitivity is 7.33V/kPase:Sub>A, and the output voltage is 156V under the action of 1N external force as shown in fig. 15/16.
Example 5
On the basis of example 1, the other steps remain unchanged, only step two is changed: the PZT slurry is extruded at room temperature, then placed in a directional temperature field (cold end-25 ℃ and hot end room temperature), and frozen to obtain a multilayer three-dimensional structure green body A-A-B-B-A-A structure.
The sensing performance test was conducted on the PZT porous ceramic with the composite porous structure obtained in this example, and the result is shown in FIG. 17/18, the sensitivity is 8.78V/kPa, and the output voltage is 180V under the action of 1N external force.
Example 6
On the basis of example 1, the other steps remain unchanged, only step two is changed: the PZT slurry is extruded at room temperature, and then is placed in a non-directional temperature field, namely at the temperature of minus 25 ℃, and the multi-layer three-dimensional structure green body A-A-B-B-A-A structure is obtained through freezing treatment.
The composite porous structure PZT porous ceramic obtained in this example was subjected to a sensing performance test, and the result is shown in FIG. 19/20, the sensitivity was 8.27V/kPa, and the output voltage was 164V under the 1N external effect.
The foregoing examples merely represent specific embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, which fall within the protection scope of the present application.
Claims (6)
1. The preparation method of the composite PZT porous ceramic with the functional gradient structure is characterized by comprising the following steps:
(1) Preparing PZT slurry: uniformly dispersing PZT powder, a dispersing agent and a binder in a solvent to obtain a PZT slurry suspension, and adjusting the pH to 6-8 to form PZT slurry, wherein the solid content of the PZT slurry is 30 vol%;
(2) Preparing a blank with a three-dimensional structure: the ceramic model with the gradient structure is designed and obtained by drawing software, a multilayer three-dimensional structure blank is obtained in a directional temperature field by a 3D direct writing technology, and the specific operation of obtaining the three-dimensional structure blank in the directional temperature field is as follows: extruding PZT slurry on a cold and hot flat plate, wherein the surface of the cold and hot flat plate is a cold end of a directional temperature field, the temperature of the cold end is between-50 ℃ and-10 ℃, the cold and hot flat plate is placed in room temperature, the hot end is room temperature, a directional temperature field is formed between the cold end and the hot end, a set three-dimensional structure blank body is directly obtained through layer-by-layer printing in the direction Wen Changxia, the single-layer volume fraction of the three-dimensional structure blank body is set to be in a structure with a small middle layer and a large two-end layer, the three-dimensional structure blank body specifically comprises 6 layers, the volume fraction of an upper two layer and a lower two layer is 48.8%, and the volume fraction of the middle two layers is 43.2%;
(3) Preparation of PZT porous ceramics: and freeze-drying and sintering the three-dimensional structure obtained by printing to obtain the PZT porous ceramic with macroscopic and microscopic composite porous structures.
2. The method for preparing a functionally graded structured composite PZT porous ceramic according to claim 1, wherein in step (1), the solvent is one or more of t-butanol, camphene and water.
3. The method for preparing a composite PZT porous ceramic with a functionally graded structure according to claim 1, wherein in the step (2), the diameter of the printing tip of the 3D direct writing technique is 0.16 to 0.61mm, the printing speed is 50 to 100mm/s, and the paste extrusion speed is 0.8 to 3.2ml/h.
4. The method for preparing a composite PZT porous ceramic having a functionally graded structure according to claim 1, wherein in the step (3), the freeze-drying temperature is-50 to-20 ℃ and the drying time is 48 hours; the sintering temperature is 1200-1250 ℃, and the heating rate is 4-5 ℃/min.
5. A composite PZT porous ceramic prepared by the method of any one of claims 1 to 4.
6. Use of the composite PZT porous ceramic according to claim 5 in a sensing material.
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