CN114380593A - Piezoelectric ceramic material for tumor electric field therapeutic apparatus and preparation method thereof - Google Patents

Piezoelectric ceramic material for tumor electric field therapeutic apparatus and preparation method thereof Download PDF

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CN114380593A
CN114380593A CN202210085451.4A CN202210085451A CN114380593A CN 114380593 A CN114380593 A CN 114380593A CN 202210085451 A CN202210085451 A CN 202210085451A CN 114380593 A CN114380593 A CN 114380593A
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treatment
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electric field
sintering
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田德辉
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Haitao Huzhou New Material Technology Co ltd
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Wuxi Huifeng Piezoeletric Co ltd
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Abstract

The invention belongs to the technical field of piezoelectric ceramics, and particularly relates to a piezoelectric ceramic material for a tumor electric field therapeutic apparatus and a preparation method thereof, wherein the piezoelectric ceramic material is obtained by the steps of mixing, presintering, mixing, granulating, molding, plastic removing, sintering, size processing, electrode feeding, measuring and the like, and the piezoelectric ceramic material does not need a polarization step, is adjusted by controlling the proportion of lead oxide and zirconium oxide, and is added with barium carbonate, so that the dielectric constant of the piezoelectric ceramic prepared by the invention is as high as 8500, and the dielectric loss is as low as 0.8% under the condition of no polarization.

Description

Piezoelectric ceramic material for tumor electric field therapeutic apparatus and preparation method thereof
Technical Field
The invention belongs to the technical field of piezoelectric ceramics, and particularly relates to a piezoelectric ceramic material for a tumor electric field therapeutic apparatus and a preparation method thereof.
Background
With the development of human medicine, more and more difficult miscellaneous diseases are overcome, wherein the difficult problems of brain tumor which has long plagued the medical field are also overcome. The brain tumor electric field therapeutic apparatus adopts low-field strength, medium-low frequency and alternating electric field which can affect the rapidly divided and proliferated tumor cells, thereby inhibiting the rapid growth of the tumor cells and improving the killing rate of tumor tissues, and the electric field and chemotherapy can play a synergistic effect in inhibiting the rapid growth of the tumor. The core component used in the tumor electric field therapeutic apparatus is piezoelectric ceramic with high dielectric constant, high compressive strength and low dielectric loss. The existing piezoceramic material has low dielectric constant, cannot meet the application of the tumor electric field therapeutic apparatus, and is replaced by other expensive imported materials, so that the cost burden of the tumor electric field therapeutic apparatus is undoubtedly increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a piezoceramic material for a tumor electric field therapeutic apparatus and a preparation method thereof, aiming at solving the technical problems that the conventional piezoceramic material has low dielectric constant, cannot meet the application of the tumor electric field therapeutic apparatus, is replaced by other imported materials with high price, and undoubtedly increases the cost burden of the tumor electric field therapeutic apparatus.
The invention provides a preparation method of a piezoceramic material for a tumor electric field therapeutic apparatus, which has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
s1, weighing the following raw materials in percentage by weight: 57-60% of lead tetraoxide, 8-10% of titanium dioxide, 13-16% of zirconium dioxide, 9-12% of barium carbonate, 3-5% of niobium pentoxide and 1-3% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing treatment in sequence to obtain a crushed material block;
s2, sieving the crushed blocks in the step S1, and then performing pre-sintering, ball milling, spray granulation and molding treatment to obtain molded blanks;
s3, performing plastic removal and sintering treatment on the molded blank in the step S2 to obtain a ceramic blank sheet;
s4, processing the ceramic blank sheet in the step S3 by size processing and silver electrode processing to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus.
In some embodiments, in step S1, the mixing process includes the following specific steps: adding deionized water, and grinding the raw materials into slurry with the particle size of 1-3 mu m by using a ball mill; the filter pressing treatment comprises the following specific steps: filtering and dehydrating the mixed slurry by using a filter press; the drying specifically comprises the following steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
Further, in the mixing treatment, the weight of the deionized water is 50-70% of the weight of the conveyed raw materials, the diameter of the zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials.
In some embodiments, in step S2, the specific steps of the burn-in process are as follows: pre-burning sealing powder in an alumina crucible;
the ball milling treatment comprises the following specific steps: adding deionized water into the pre-sintered material by using a ball mill, grinding into slurry with the particle size of 1-3 mu m, and then putting the obtained slurry into a sand mill, and grinding into slurry with the particle size of 0.5-0.7 mu m to obtain slurry;
the spray granulation treatment comprises the following steps: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation at 240-260 ℃ and the outlet temperature at 100-120 ℃ for spray granulation;
the molding treatment comprises the following steps: and (3) molding by using a die pressing process, and pressing the slurry subjected to spray granulation treatment into a blank.
Further, in the pre-sintering treatment, the pre-sintering temperature is 1000 ℃, and the heat preservation time is 3-5 h;
in the ball milling treatment, the weight of the deionized water is 50-70% of the weight of the conveyed raw materials, the diameter of the zirconium dioxide balls in the ball mill is 1-15%, the weight of the zirconium dioxide balls is 200% of the weight of the raw materials, and the sanding frequency is 10 times;
in the spray granulation treatment, the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials;
in the molding step, the dry pressure is 1.8 tons/cm2。
In some embodiments, in step S3, the plastic discharge processing comprises the following specific steps: heating the blank at high temperature, and discharging the binder out of the blank;
the sintering treatment comprises the following specific steps: and placing the formed blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering.
Further, in the plastic removal treatment, the plastic removal temperature is 700-900 ℃, and the time is 3-5 h;
in the sintering treatment, the sintering temperature is 1200-1300 ℃, and the sintering time is 4-6 h.
In some embodiments, in step S4, the specific steps of the silver electrode treatment are as follows: and (4) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing.
Further, the silver impregnation temperature is 750-.
The invention provides a second technical scheme, namely a piezoelectric ceramic material for a tumor electric field therapeutic apparatus, and the piezoelectric ceramic material for the tumor electric field therapeutic apparatus prepared by the method.
The invention has the following beneficial effects: the dielectric constant is generally improved by 20 to 40 percent compared with that of unpolarized silicon under the polarized condition. The piezoelectric ceramic material obtained by the steps of mixing, presintering, mixing, granulating, forming, plastic removing, sintering, size processing, electrode feeding, measuring and the like does not need a polarization step, is adjusted by controlling the proportion of lead oxide and zirconium oxide, and is added with barium carbonate, so that the dielectric constant of the piezoelectric ceramic material prepared by the invention is as high as 8500 and the dielectric loss is as low as 0.8 percent under the condition of no polarization.
Drawings
FIG. 1 is a flow chart of the preparation method of the piezoceramic material for tumor electric field therapeutic apparatus provided by the invention;
FIG. 2 is SEM image of ceramic crystal fracture of the piezoceramic material for tumor electric field therapy apparatus provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings 1-2 in conjunction with specific embodiments.
Example 1
The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus provided by the embodiment has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
weighing the following raw materials in percentage by weight: 60% of lead tetraoxide, 10% of titanium dioxide, 15% of zirconium dioxide, 11% of barium carbonate, 3% of niobium pentoxide and 1% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing in sequence to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 70% of the weight of the conveyed raw materials, the diameter of the zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: and pre-burning the sealing powder in an alumina crucible at 1000 ℃ for 5 h. The ball milling treatment comprises the following specific steps: grinding the presintered material into slurry with the particle size of 1-3 μm by adding deionized water into a ball mill, and grinding the obtained slurry into slurry with the particle size of 0.5-0.7 μm in a sand mill to obtain the slurry, wherein the weight of the deionized water is 70% of the weight of the conveyed raw material, the diameter of a zirconium dioxide ball in the ball mill is 1-15mm, the weight of the zirconium dioxide ball is 200% of the weight of the raw material, and the number of times of sand milling is 10. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by using a die pressing process, pressing the slurry subjected to spray granulation into a blank, wherein the dry pressing pressure is 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, wherein the plastic discharge temperature is 900 ℃, and the time is 3 hours. The sintering treatment comprises the following specific steps: and (3) placing the molded blank subjected to plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1300 ℃, and the sintering time is 4 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and performing silver impregnation at 850 ℃.
Example 2
The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus provided by the embodiment has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
weighing the following raw materials in percentage by weight: 57% lead tetraoxide, 8% titanium dioxide, 16% zirconium dioxide, 12% barium carbonate, 4% niobium pentoxide and 3% rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing in sequence to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 50% of the weight of the conveyed raw materials, and the diameter of zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: pre-sintering the sealing powder in an alumina crucibleThe burning temperature is 1000 ℃, and the heat preservation time is 3 h. The ball milling treatment comprises the following specific steps: grinding the presintered material into slurry with the particle size of 1-3 μm by adding deionized water into a ball mill, and grinding the obtained slurry into slurry with the particle size of 0.5-0.7 μm in a sand mill to obtain the slurry, wherein the weight of the deionized water is 50% of the weight of the conveyed raw material, the diameter of a zirconium dioxide ball in the ball mill is 1-15mm, the weight of the zirconium dioxide ball is 200% of the weight of the raw material, and the number of times of sand milling is 10. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by using a die pressing process, pressing the slurry subjected to spray granulation into a blank, wherein the dry pressing pressure is 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, wherein the plastic discharge temperature is 700 ℃, and the time is 5 hours. The sintering treatment comprises the following specific steps: and (3) placing the molded blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1200 ℃, and the sintering time is 6 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and carrying out silver impregnation at 750 ℃.
Example 3
The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus provided by the embodiment has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
weighing the following raw materials in percentage by weight: 60% of lead tetraoxide, 9% of titanium dioxide, 15% of zirconium dioxide, 9% of barium carbonate, 5% of niobium pentoxide and 2% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing in sequence to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 60% of the weight of the conveyed raw materials, and the diameter of zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: and pre-burning the sealing powder in an alumina crucible at 1000 ℃ for 4 h. The ball milling treatment comprises the following specific steps: grinding the presintered material into slurry with the particle size of 1-3 μm by adding deionized water into a ball mill, and grinding the obtained slurry into slurry with the particle size of 0.5-0.7 μm in a sand mill to obtain the slurry, wherein the weight of the deionized water is 60% of the weight of the conveyed raw material, the diameter of a zirconium dioxide ball in the ball mill is 1-15mm, the weight of the zirconium dioxide ball is 200% of the weight of the raw material, and the number of times of sand milling is 10. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by using a die pressing process, pressing the slurry subjected to spray granulation into a blank, wherein the dry pressing pressure is 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, and performing plastic discharge at the temperature of 800 ℃ for 4 hours. The sintering treatment comprises the following specific steps: and placing the molded blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1250 ℃, and the sintering time is 5 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and performing silver impregnation at 800 ℃.
Example 4
The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus provided by the embodiment has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
weighing the following raw materials in percentage by weight: 59% of lead tetraoxide, 10% of titanium dioxide, 13% of zirconium dioxide, 11% of barium carbonate, 5% of niobium pentoxide and 2% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing in sequence to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 60% of the weight of the conveyed raw materials, and the diameter of zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: and pre-burning the sealing powder in an alumina crucible at 1000 ℃ for 4 h. The ball milling treatment comprises the following specific steps: grinding the pre-sintered material into slurry with particle size of 1-3 μm by adding deionized water in a ball mill, and grinding the slurry into slurry with particle size of 0.5-0.7 μm in a sand mill to obtain slurry, wherein the weight of the deionized water is the weight of the transported raw material60% of the amount, the diameter of the zirconia balls in the ball mill is 1-15mm, the weight is 200% of the weight of the raw materials, and the sanding time is 10 times. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by using a die pressing process, pressing the slurry subjected to spray granulation into a blank, wherein the dry pressing pressure is 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, and performing plastic discharge at the temperature of 800 ℃ for 4 hours. The sintering treatment comprises the following specific steps: and placing the molded blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1250 ℃, and the sintering time is 5 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and performing silver impregnation at 800 ℃.
Example 5
The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus provided by the embodiment has the following specific technical scheme:
the preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus comprises the following steps:
weighing the following raw materials in percentage by weight: 59% of lead tetraoxide, 9% of titanium dioxide, 14.5% of zirconium dioxide, 11% of barium carbonate, 4% of niobium pentoxide and 2.5% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing in sequence to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 60% of the weight of the conveyed raw materials, and the diameter of zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: and pre-burning the sealing powder in an alumina crucible at 1000 ℃ for 4 h. The ball milling treatment comprises the following specific steps: grinding the presintered material into slurry with the particle size of 1-3 μm by adding deionized water into a ball mill, and grinding the obtained slurry into slurry with the particle size of 0.5-0.7 μm in a sand mill to obtain the slurry, wherein the weight of the deionized water is 60% of the weight of the conveyed raw material, the diameter of a zirconium dioxide ball in the ball mill is 1-15mm, the weight of the zirconium dioxide ball is 200% of the weight of the raw material, and the number of times of sand milling is 10. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by using a die pressing process, pressing the slurry subjected to spray granulation into a blank, wherein the dry pressing pressure is 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, and performing plastic discharge at the temperature of 800 ℃ for 4 hours. The sintering treatment comprises the following specific steps: and placing the molded blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1250 ℃, and the sintering time is 5 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and performing silver impregnation at 800 ℃.
Comparative example
The preparation method of the piezoelectric ceramic material provided by the comparative example comprises the following steps:
weighing the following raw materials in percentage by weight: 62 percent of lead tetraoxide, 12 percent of titanium dioxide, 16 percent of zirconium dioxide, 7 percent of niobium pentoxide and 3 percent of rare earth, and the raw materials are sequentially subjected to mixing, filter pressing, drying and crushing treatment to obtain a crushed material block. The mixing treatment comprises the following specific steps: adding deionized water, grinding the raw materials into slurry with the particle size of 1-3 μm by using a ball mill, wherein the weight of the deionized water is 60% of the weight of the conveyed raw materials, and the diameter of zirconium dioxide balls in the ball mill is 1-15mm, and the weight of the zirconium dioxide balls is 200% of the weight of the raw materials. The filter pressing treatment comprises the following specific steps: and filtering and dehydrating the mixed slurry by using a filter press. The drying method comprises the following specific steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
And sieving the crushed material blocks, and then performing pre-sintering, ball-milling, spray granulation and molding treatment to obtain molded blanks. The pre-burning treatment comprises the following specific steps: and pre-burning the sealing powder in an alumina crucible at 1000 ℃ for 4 h. The ball milling treatment comprises the following specific steps: grinding the presintered material into slurry with the particle size of 1-3 μm by adding deionized water into a ball mill, and grinding the obtained slurry into slurry with the particle size of 0.5-0.7 μm in a sand mill to obtain the slurry, wherein the weight of the deionized water is 60% of the weight of the conveyed raw material, the diameter of a zirconium dioxide ball in the ball mill is 1-15mm, the weight of the zirconium dioxide ball is 200% of the weight of the raw material, and the number of times of sand milling is 10. The spray granulation treatment steps are as follows: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation to be 240-260 ℃ and the outlet temperature to be 100-120 ℃ for spray granulation, wherein the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials. The molding treatment steps are as follows: molding by a molding processPressing the pulp after the particle treatment into a blank with a dry pressing pressure of 1.8 tons/cm2。
And performing plastic removal and sintering treatment on the molded blank to obtain a ceramic blank sheet. The plastic removing treatment comprises the following specific steps: and (3) heating the blank at a high temperature, discharging the binder out of the blank, and performing plastic discharge at the temperature of 800 ℃ for 4 hours. The sintering treatment comprises the following specific steps: and placing the molded blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering, wherein the sintering temperature is 1250 ℃, and the sintering time is 5 hours.
And (3) processing the ceramic blank sheet in the step by size and processing the ceramic blank sheet by a silver electrode to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus. The size processing comprises the following specific steps: the ceramic green sheet is processed to a suitable size and ultrasonically cleaned. The specific steps of silver electrode treatment are as follows: and (3) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing, and performing silver impregnation at 800 ℃.
15 samples of the piezoceramic material (ceramic crystal fracture is shown in fig. 1) for the tumor electric field therapy apparatus prepared in the embodiment are tested, and the piezoceramic material has higher dielectric constant and lower dielectric loss compared with the piezoceramic material (shown in table 2) of the comparative example through the performance test (shown in table 1), so that the requirements of the brain tumor electric field therapy apparatus are met.
TABLE 1 Performance testing of piezoceramic materials prepared according to the present invention for tumor E-field therapy
Figure BDA0003487640620000071
Figure BDA0003487640620000081
TABLE 2 Performance testing of the piezoceramic materials of the comparative examples
Figure BDA0003487640620000082
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.

Claims (10)

1. The preparation method of the piezoceramic material for the tumor electric field therapeutic apparatus is characterized by comprising the following steps:
s1, weighing the following raw materials in percentage by weight: 57-60% of lead tetraoxide, 8-10% of titanium dioxide, 13-16% of zirconium dioxide, 9-12% of barium carbonate, 3-5% of niobium pentoxide and 1-3% of rare earth, and the raw materials are subjected to mixing, filter pressing, drying and crushing treatment in sequence to obtain a crushed material block;
s2, sieving the crushed blocks in the step S1, and then performing pre-sintering, ball milling, spray granulation and molding treatment to obtain molded blanks;
s3, performing plastic removal and sintering treatment on the molded blank in the step S2 to obtain a ceramic blank sheet;
s4, processing the ceramic blank sheet in the step S3 by size processing and silver electrode processing to obtain the piezoelectric ceramic material for the tumor electric field therapeutic apparatus.
2. The preparation method of the piezoceramic material for electric field tumor therapy apparatus according to claim 1, wherein in step S1, the mixing treatment comprises the following specific steps: adding deionized water, and grinding the raw materials into slurry with the particle size of 1-3 mu m by using a ball mill; the filter pressing treatment comprises the following specific steps: filtering and dehydrating the mixed slurry by using a filter press; the drying specifically comprises the following steps: putting the filter-pressed slurry into a constant-temperature circulating oven to evaporate water; in the crushing treatment, the crushing degree needs to be sieved by a 20-mesh sieve.
3. The method for preparing a piezoceramic material for electric field tumor therapy apparatus according to claim 2, wherein in the mixing treatment, the weight of the deionized water is 50-70% of the weight of the raw materials, the diameter of the zirconia balls in the ball mill is 1-15mm, and the weight of the zirconia balls is 200% of the weight of the raw materials.
4. The method for preparing a piezoceramic material for tumor electric field therapy apparatus according to claim 1, wherein in step S2, the pre-firing treatment comprises the following specific steps: pre-burning sealing powder in an alumina crucible;
the ball milling treatment comprises the following specific steps: adding deionized water into the pre-sintered material by using a ball mill, grinding into slurry with the particle size of 1-3 mu m, and then putting the obtained slurry into a sand mill, and grinding into slurry with the particle size of 0.5-0.7 mu m to obtain slurry;
the spray granulation treatment comprises the following steps: adding an adhesive into the ball-milled materials and stirring, controlling the inlet temperature of granulation at 240-260 ℃ and the outlet temperature at 100-120 ℃ for spray granulation;
the molding treatment comprises the following steps: and (3) molding by using a die pressing process, and pressing the slurry subjected to spray granulation treatment into a blank.
5. The preparation method of the piezoceramic material for tumor electric field therapeutic instrument according to claim 4, wherein in the pre-sintering treatment, the pre-sintering temperature is 1000 ℃, and the heat preservation time is 3-5 h;
in the ball milling treatment, the weight of the deionized water is 50-70% of the weight of the conveyed raw materials, the diameter of the zirconium dioxide balls in the ball mill is 1-15%, the weight of the zirconium dioxide balls is 200% of the weight of the raw materials, and the sanding frequency is 10 times;
in the spray granulation treatment, the adhesive is polyvinyl alcohol, and the weight of the polyvinyl alcohol is 9% of the weight of the raw materials;
in the molding step, the dry pressure is 1.8 tons/cm2。
6. The method for preparing the piezoceramic material for tumor electric field therapy apparatus according to claim 1, wherein in step S3, the plastic discharge treatment comprises the following specific steps: heating the blank at high temperature, and discharging the binder out of the blank;
the sintering treatment comprises the following specific steps: and placing the formed blank subjected to the plastic removal treatment into an alumina crucible, sealing, and placing the alumina crucible into a sintering furnace for sintering.
7. The method for preparing a piezoceramic material for tumor electric field therapeutic apparatus according to claim 6, wherein in the plastic removal treatment, the plastic removal temperature is 700-900 ℃ and the time is 3-5 h;
in the sintering treatment, the sintering temperature is 1200-1300 ℃, and the sintering time is 4-6 h.
8. The method for preparing a piezoceramic material for electric field tumor therapy apparatus according to claim 1, wherein in step S4, the silver electrode treatment comprises the following specific steps: and (4) coating silver on the upper surface and the lower surface of the ceramic blank sheet subjected to size processing.
9. The method for preparing piezoelectric ceramic material for electric field therapeutic apparatus of tumor as claimed in claim 8, wherein the silver-infiltrated temperature in the treatment with silver electrode is 750-850 ℃.
10. Piezoceramic material for electric field therapy of tumors, characterized in that it is prepared by the method according to any one of claims 1-9.
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