CN115254610B

CN115254610B - Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof

Info

Publication number: CN115254610B
Application number: CN202210921811.XA
Authority: CN
Inventors: 章海燕; 高绍兵; 刘传兵; 郭道九; 何梦瑜
Original assignee: Zhejiang Yuanji New Material Co ltd
Current assignee: Zhejiang Yuanji New Material Co ltd
Priority date: 2022-08-02
Filing date: 2022-08-02
Publication date: 2023-09-15
Anticipated expiration: 2042-08-02
Also published as: CN115254610A

Abstract

The application relates to the technical field of impeller back manufacturing of micro-graders, in particular to a micro-grader impeller for processing ceramic powder for copper-clad plates and a manufacturing method thereof. A micro classifier impeller for processing ceramic powder for copper-clad plates is prepared from the following raw materials in parts by weight: 100 parts of piezoelectric ceramic particles and 20-40 parts of first binder; the piezoelectric ceramic particles are mainly prepared by granulating piezoelectric ceramic powder and a second binder; the particle size of the piezoelectric ceramic particles is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by adopting a hydrothermal synthesis method, the expression is Pb (1-x) SmxZryTi (1-y) O3, x=0-0.05, and y=0.46-0.48; the piezoelectric ceramic powder D50 is controlled to be 0.2-16 microns. The impeller prepared by the application is applied to a micro classifier, and is not easy to cause powder blocking and sticking during classification of the material powder, thereby improving the classification and screening effects of the material.

Description

Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof

Technical Field

The application relates to the technical field of impeller back manufacturing of micro-graders, in particular to a micro-grader impeller for processing ceramic powder for copper-clad plates and a manufacturing method thereof.

Background

In the industrial production process, the particle size of various fine powder materials is strictly limited, such as the fineness, purity and passing rate of the fine powder materials. The superfine classifier can classify materials with different granularity and is widely applied to industries such as cement, mine, chemical industry, filler, food and the like. In the production process of the high-frequency high-speed copper-clad plate, a micro classifier is required to carry out classification screening on ceramic powder for the special copper-clad plate, and the quality of classification screening quality directly influences the quality of the prepared high-frequency high-speed copper-clad plate.

Grading principle of micro grader: let the circle S represent the outer contour of the classifying impeller, the airflow is represented by a dotted line, P is a point of intersection on the impeller surface, and the particles are acted on by two opposite forces at the point P, namely centrifugal inertia force F generated by the rotation of the impeller and resistance R from the airflow. F= (pi/6) d ³ (ρs-ρ)(u _θ ² /r)，R＝3πμdu _r Wherein d is the particle diameter of the material; r-average radius of impeller; ρs is the material powder density; ρ—air density; u (u) _θ- Average peripheral velocity of impeller (tangential velocity of particles); mu is the air viscosity, u _r Radial velocity of the gas flow (radial velocity of the particles). When the centrifugal force exerted on the particles is greater than the air flow resistance (F>And R) the particles fly to the inner wall of the classifying chamber along the direction of the impeller and then fall down along the chamber wall under the action of gravity to the outside of the coarse grain discharge port to be discharged out of the machine to become coarse powder. When the centrifugal force exerted on the particles is smaller than the air flow resistance (F <And R) enabling particles to pass through the gaps of the blades of the classifying impeller along with the air flow, and discharging the particles out of the machine through a fine powder discharge port to form fine powder. When the force f=r to which the particles are subjected, the particle diameter at this time is referred to as a critical particle diameter.

The vertical classifying device in the related art consists of a classifying impeller, a bearing box, a bearing cover, a belt pulley and a motor. The general materials of the classifying impeller comprise stainless steel, carbon steel, manganese steel alloy and 99 alumina wear-resistant ceramic. The applicant has found that, with respect to the impeller of the micro classifier in the related art described above, the technical solution has the following drawbacks: the impeller of the micro classifier in the related art is liable to be clogged or stuck at the impeller when pulverizing ceramic powder.

Disclosure of Invention

The application provides a micro classifier impeller for processing ceramic powder for a copper-clad plate and a manufacturing method thereof, aiming at solving the problem that the impeller of the micro classifier is easy to be blocked or stuck at the impeller when ceramic powder is crushed.

In a first aspect, the application provides a micro classifier impeller for processing ceramic powder for copper-clad plates, which is realized by the following technical scheme:

a micro classifier impeller for processing ceramic powder for copper-clad plates is prepared from the following raw materials in parts by weight: 100 parts of piezoelectric ceramic particles and 20-40 parts of first binder; the piezoelectric ceramic particles are mainly prepared by granulating piezoelectric ceramic powder and a second binder; the particle size of the piezoelectric ceramic particles is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by adopting a hydrothermal synthesis method, and the expression is Pb _(1－x) Sm _x Zr _y Ti _(1-y) O ₃ X=0 to 0.05, y=0.46 to 0.48; the grain diameter D50 of the piezoelectric ceramic powder is controlled to be 0.2-16 mu m.

Pb with tetragonal perovskite structure prepared by hydrothermal synthesis method _1－x Sm _x Zr _0.52 Ti _0.48 O ₃ The impeller of the micro classifier is prepared by taking the piezoelectric ceramic powder as a raw material, and vibration with a certain amplitude is generated in the use process of the impeller, so that the impeller is applied to the micro classifier, and the situation of powder blocking and powder sticking is not easy to occur when the material powder classification is carried out, and the material classification and screening effects are improved.

Preferably, the expression of the piezoelectric ceramic powder is Pb _(1－x) Sm _x Zr _0.52 Ti _0.48 O ₃ X= 0,0.01,0.02,0.03,0.04,0.05; the piezoelectric ceramic powder D50 is controlled to be 0.5-4.8 mu m.

By adopting the technical scheme, the Sm infiltration amount and Zr are reduced ₀ Limiting the ratio of Ti to Pb _1－ _x Sm _x Zr _0.52 Ti _0.48 O ₃ The crystal phase structure of the impeller of the prepared micro classifier can improve the piezoelectric constant, the relative dielectric constant and the dielectric loss, thereby improving the whole powder classifying and screening effect.

Preferably, the preparation method of the piezoelectric ceramic particles comprises the following steps:

s1, preparing piezoelectric ceramic powder;

s1.1, preparing a titanium tetrachloride aqueous solution, a zirconium oxychloride aqueous solution and a lead nitrate aqueous solution, wherein the molar concentration of the titanium tetrachloride aqueous solution is 0.5mol/L, the molar concentration of the zirconium oxychloride aqueous solution is 1mol/L, and the molar concentration of the lead nitrate aqueous solution is 2mol/L;

S1.2, according to the expression of the PZT powder, the method comprises the following steps: pb _(1－x) Sm _x Zr _0.52 Ti _0.48 O ₃ Respectively measuring the stoichiometric ratio of the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution prepared in the step S1.1, adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating for 5-10min in a water bath at 50-70 ℃, dropwise adding the lead nitrate aqueous solution at 0.1-0.2g/min under the stirring condition of 1200-1500r/min, stirring for 10-20min, and then adding ammonia water with the concentration of 25% to adjust the pH value of the solution to 8-10 to obtain a mixed solution;

s1.3, preserving heat for 20-40min, centrifuging, washing the obtained filter cake with a mixed solvent for 2-3 times, placing the filter cake in the mixed solvent again, adding a mineralizer, wherein the concentration of the mineralizer in the mixed liquid is 0.5-4mol/L, and dispersing for 25-35min by magnetic stirring to obtain precursor slurry;

s1.4, putting the precursor slurry obtained in the step S1.3 into a reaction kettle, carrying out solvothermal reaction for 2-20h in a baking oven at 130-190 ℃ to obtain suspension, centrifuging the obtained suspension, washing with deionized water, 10% acetic acid solution, deionized water and absolute ethyl alcohol respectively, drying filter cakes at 80-85 ℃, sealing bags, placing into a dryer for storage, and ball-milling for 10-15min to obtain PZT piezoelectric ceramic powder;

S1.5, mixing and calcining, grinding and sieving the PZT piezoelectric ceramic powder with the concentration of 99.5-100% and the samarium carbonate with the concentration of 0-0.05% to obtain Pb _1－x Sm _x Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder;

s2, ball milling and screening to obtain piezoelectric ceramic powder with D50 of 0.3-16 mu m;

s3, granulating, wherein a second binder PVA solution with the concentration of 3-5wt% is added into the piezoelectric ceramic powder in the S2, the dosage of the second binder PVA solution is 8-10wt% of the total mass of the piezoelectric ceramic powder, granulating, grinding the obtained granules for 30-40min, pressing the obtained granules into large blocks, standing for 24h, crushing the large blocks into powder, granulating for the second time, and sieving to obtain ceramic particles with good fluidity.

By adopting the technical scheme, pb with tetragonal perovskite structure prepared by adopting hydrothermal synthesis method _1－ _x Sm _x Zr _0.52 Ti _0.48 O ₃ The piezoelectric ceramic powder has excellent piezoelectric performance. The preparation method of the piezoelectric ceramic powder provided by the application has relatively mature process technology and is convenient for industrial production.

Preferably, the expression of the piezoelectric ceramic powder is Pb _(1－x) Sm _x Zr _0.52 Ti _0.48 O ₃ ，x＝0.02。

By adopting the technical scheme, pb with tetragonal perovskite structure prepared by adopting hydrothermal synthesis method _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x ZT ceramics have optimal overall electrical properties: piezoelectric constant d ₃₃ =232 pC/N, relative dielectric constant ε _r The dielectric loss tan delta=0.22 is taken as the piezoelectric vibrating element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller can not occur.

Preferably, the piezoelectric ceramic particles are mainly prepared from piezoelectric ceramic powder, a second binder, functional powder, functional short fibers and functional whiskers; the mass of the functional powder is 0.003-0.015 times of that of the piezoelectric ceramic powder; the mass of the functional short fiber is 0.002-0.01 times of the mass of the piezoelectric ceramic powder; the mass of the functional whisker is 0.001-0.004 times of that of the piezoelectric ceramic powder; the second binder is prepared from organic silicon resin, modified siloxane, diethylenetriamine and a diluting solvent, and the solid content is 40-50%; the modified siloxane is one or a combination of more of fluorine-containing siloxane, FM-3311 siloxane, FM-4411 siloxane, FM-7711 siloxane, FM-0411 siloxane, FM-DA11 siloxane, FM-0711 siloxane and TM-0701T siloxane; the preparation method of the second binder comprises the steps of firstly preparing raw materials, uniformly stirring the organic silicon resin and the modified siloxane, preheating to 70-75 ℃, reacting for 2-3min in advance, cooling to below 10 ℃, adding a diluting solvent, uniformly stirring, finally adding diethylenetriamine, and uniformly stirring to obtain the finished second binder.

By adopting the technical scheme, the piezoelectric ceramic particles with good fluidity and good storage stability can be prepared, and the subsequent preparation of the piezoelectric ceramic impeller is facilitated. In addition, the addition of the functional powder, the functional short fibers and the functional whiskers can effectively improve the mechanical property, the toughness, the heat resistance and the corrosion resistance of the piezoelectric ceramic impeller on the premise of ensuring the overall piezoelectric property.

Preferably, the functional powder is one or a combination of more of silicon nitride powder, cubic boron nitride powder, zirconium oxide, calcium oxide, cerium oxide, magnesium oxide and yttrium oxide; the functional powder D50 is 1-5 microns; the functional short fiber is one or a combination of more of silicon nitride fiber, aluminum oxide fiber and boron nitride fiber; the length of the functional short fiber is 1-10 micrometers; the functional whisker is one or a combination of more of silicon nitride whisker, potassium titanate whisker and zinc oxide whisker.

By optimizing the selection and combination of the functional powder, the functional short fiber and the functional whisker, the mechanical property, the toughness, the heat resistance and the corrosion resistance of the piezoelectric ceramic impeller can be effectively improved on the premise of ensuring the overall piezoelectric property.

Preferably, the piezoelectric ceramic particles are prepared from the following raw materials in parts by weight: 100 parts of piezoelectric ceramic powder, 10-15 parts of second binder, 1-1.2 parts of functional powder, 0.4-0.6 part of functional short fiber and 0.2-0.25 part of functional whisker; the functional powder consists of cubic boron nitride powder, zirconia and cerium oxide; the mass ratio of the cubic boron nitride powder to the zirconia to the cerium oxide is (80-200): 100: (1-3); the functional short fiber is prepared from silicon nitride fiber and boron nitride fiber according to the mass ratio of 1:1, the composition is as follows; the functional whisker is prepared from silicon nitride whisker, potassium titanate whisker and zinc oxide whisker according to the mass ratio of 1: (0.2-0.8): 1.

By adopting the technical scheme, the piezoelectric ceramic impeller with better piezoelectric performance and better mechanical property, toughness, heat resistance and corrosion resistance can be obtained by optimizing the components and the consumption of the piezoelectric ceramic particles, so that the overall powder classifying and screening effect is improved.

Preferably, the first binder is mainly prepared from main components, injection molding grade polyolefin PP, compatilizer EVA, lubricant, dispersing agent and antioxidant; the main component is copolyformaldehyde POM, and the number average molecular weight is 2-4 ten thousand; the lubricant is a CBT resin polymer with a hyperbranched structure; the preparation method of the first adhesive comprises the steps of mixing main components, polyolefin PP, compatilizer EVA, lubricant, dispersing agent and antioxidant at 0-4 ℃ for 10-15min at 300-400rpm to obtain the finished first adhesive.

By adopting the technical scheme, the mixing granulation and the rubber discharging and degreasing operation of the subsequent working section are facilitated, the overall production efficiency of the piezoelectric ceramic impeller can be optimized, and the quality stability of the piezoelectric ceramic impeller can be ensured.

In a second aspect, the application provides a method for manufacturing a micro classifier impeller for processing ceramic powder for a copper-clad plate, which is realized by the following technical scheme:

a manufacturing method of a micro classifier impeller for processing ceramic powder for a copper-clad plate comprises the following steps:

s1, preparing piezoelectric ceramic powder;

s3, granulating, namely adding a second binder into the piezoelectric ceramic powder in the step S2, granulating, grinding the obtained granules for 30-40min, pressing into large blocks, standing for 24h, crushing into powder, granulating for the second time, and sieving to obtain piezoelectric ceramic particles with good fluidity;

s4, press forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to be 150-180Mpa, and the compression time is set to be 300-360s, so as to obtain a green body impeller;

s5, discharging glue and sintering: heating the green body impeller to 520-550 ℃ at 0.2-0.4 ℃/min, preserving heat for 3-3.2h, removing the binder, sealing the crucible, burying powder, sintering, heating to 1200-1320 ℃ at 0.5-0.6 ℃/min, preserving heat for 2-2.5h, and obtaining the piezoelectric ceramic impeller;

S6, carrying out polarization treatment on the piezoelectric ceramic impeller, then manufacturing two electrodes at the front end and the rear end of the piezoelectric ceramic impeller, respectively connecting electrode leads to the electrodes at the front end and the rear end of the piezoelectric ceramic impeller, pouring insulating impregnating resin around the connection of the electrodes and the electrode leads, and curing to obtain the finished micro classifier impeller.

By adopting the technical scheme, the preparation method is relatively simple, the preparation process is relatively mature, the product quality control difficulty is relatively low, the production investment cost is easy to reduce for a production enterprise, and the industrial mass production is convenient.

Preferably, the step S4 of press forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to 180Mpa, and the compression time is set to 360s, so as to obtain a green body impeller; the rubber discharging and sintering are carried out: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1280 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.0-2.5 ℃/min, and opening a furnace for natural cooling to obtain the piezoelectric ceramic impeller.

By adopting the technical scheme, the technological parameters are limited and controlled, so that the quality of products in the same batch can be stabilized, and the piezoelectric performance of the prepared piezoelectric ceramic impeller can be ensured.

In summary, the application has the following advantages:

1. the impeller prepared by the application generates vibration with a certain amplitude in the use process, and is not easy to cause powder blocking and sticking when crushing ceramic powder, and the powder classifying and screening effect is good.

2. The preparation method is relatively simple, the preparation process is relatively mature, the product quality control difficulty is relatively low, the production investment cost is easy to reduce for production enterprises, and the industrialized mass production is facilitated.

3. Pb with tetragonal perovskite structure prepared by hydrothermal synthesis method _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x ZT ceramics have optimal overall electrical properties: piezoelectric constant d ₃₃ =232 pC/N, relative dielectric constant ε _r The dielectric loss tan delta=0.22 is taken as the piezoelectric vibrating element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller can not occur.

Detailed Description

The present application will be described in further detail with reference to comparative examples and examples.

Preparation example

Preparation example 1

The first binder was prepared from 842g of POM (M90-44, injection grade), 86g of PP (brand AW 564) injection grade polyolefin, 34g of EVA (DuPont 30E783, maleic anhydride grafted EVA) as a molding grade compatibilizer, 16g of PETS plastic lubricant, 4g of microcrystalline wax, 18g of stearic acid dispersant (CAS: 57-11-4), and 15g of antioxidant B900.

The preparation method of the first adhesive comprises the steps of adding 833g of main component-Baoli copolyformaldehyde POM (M90-44, injection molding grade), 88g of injection molding grade polyolefin PP (brand AW 564), 38g of molding grade compatilizer EVA (DuPont 30E783, maleic anhydride grafted EVA), 16g of PETS plastic lubricant, 6g of microcrystalline wax, 18g of stearic acid dispersing agent (CAS: 57-11-4) and 16g of antioxidant B900 into a reaction kettle, introducing nitrogen to control the temperature between 0 ℃ and 4 ℃, starting stirring, mixing for 12min at 360rpm, vacuumizing and defoaming to obtain the finished first adhesive.

Preparation example 2

The second binder was prepared from 36% KR-242A silicone resin, 4% fluorosilicone, 0.1% diethylenetriamine, 59.9% methanol.

A method of preparing a second binder comprising the steps of:

step one, preparation of fluorine-containing siloxane: 19.01g of perfluorohexyl ethanethiol and 250g of TM-0701T siloxane are placed in a three-necked flask, heated to 45 ℃ in a water bath, added with 0.1g of azodiisobutyronitrile, stirred at 320rpm and subjected to hydrosulfide reaction for 1.0h to obtain fluorine-containing siloxane;

step two, mixing 40g of the fluorine-containing siloxane prepared in the step one with 360g of KR-242A silicone resin at 240rpm, stirring for 5min, heating to 72-75 ℃, and pre-reacting for 150s;

And thirdly, adopting an ice salt bath to cool, controlling the temperature to be 0-4 ℃, adding 599g of methanol, stirring for 10min at 250rpm, adding 1.0g of diethylenetriamine, and stirring for 100s at 80rpm to obtain the finished second binder.

Preparation example 3

The second binder was prepared from 36% KR-242A silicone resin, 4% TM-0701T siloxane, 0.1% diethylenetriamine, 59.9% methanol.

The preparation method of the second binder comprises the following steps: 40g of TM-0701T siloxane and 360g of KR-242A silicone resin are mixed and stirred at 240rpm for 5min, then the temperature is raised to 72-75 ℃ and the pre-reaction is carried out for 150s; cooling with ice salt bath, controlling the temperature at 0-4deg.C, adding 599g of methanol, stirring at 250rpm for 10min, adding 1.0g of diethylenetriamine, and stirring at 80rpm for 100s to obtain the final product.

Preparation example 4

The functional powder consists of cubic boron nitride powder, zirconia and cerium oxide. The mass ratio of the cubic boron nitride powder to the zirconia to the cerium oxide is 198:100:2. preparing functional powder, namely mixing cubic boron nitride powder, zirconia and cerium oxide according to the mass ratio of 198:100:2, weighing, adding into a planetary ball mill, wherein the inner container is polytetrafluoroethylene, the grinding balls are 95 zirconia beads, ball milling for 30min at 120rpm, screening to obtain functional powder with the granularity of 1-5 microns, placing into a KH570 coupling agent with the granularity of 3g/L, performing ultrasonic dispersion for 10min, transferring into an oven, and drying at 40 ℃ for 8h to obtain the functional powder.

Preparation example 5

The functional short fiber is prepared from silicon nitride fiber and boron nitride fiber according to the mass ratio of 1: 1.

Preparing functional short fibers: capatiue 4g/L ^TM Preparing organic functional silane aqueous solution, soaking silicon nitride fiber and boron nitride fiber in Capatiue ^TM Ultrasonic wave in organic functional silane aqueous solutionDispersing for 10min, taking out, and drying at 40 ℃ for 8h, wherein the mass ratio of the silicon nitride fiber to the boron nitride fiber is 1:1 to obtain the functional short fiber.

Preparation example 6

The functional whisker is prepared from silicon nitride whisker, potassium titanate whisker and zinc oxide whisker according to the mass ratio of 1:0.2: 1. The preparation method of the functional whisker comprises the following steps: step one, preparing an organofluorine modified acrylic acid polymerization emulsion: preparation of pre-emulsion A: taking 375g of total amount of water, 5.0g of emulsifier AES, 75.2g of methyl methacrylate and 340.2g of butyl methacrylate, placing the mixture in a high-speed shear at 3200rpm for pre-emulsifying for 10min, and taking 1/3 of pre-emulsion for later use; simultaneously preparing an initiating liquid, and dissolving 1.25g of initiating agent-azodiisobutyronitrile into 250g of water for later use; meanwhile, preparing a pre-emulsion B: 84.6g of the side chain is C ₈ F ₁₇ (CH ₂ ) ₃ Adding the fluorosilicone polymer into the residual 2/3 of the pre-emulsion A, placing the mixture in high-speed shear at 3200rpm, and continuing to emulsify for 15min for later use; heating 125g of deionized water to 80 ℃, adding the pre-emulsion A in the first step, stirring at 100rpm, simultaneously dripping the initiating liquid prepared in the second step at 6mL/min, stopping heating and dripping the initiating agent after dripping for 22min, continuously stirring at 100rpm for 5min, dripping the pre-emulsion B at 24mL/min, controlling the rotating speed at 160rpm, simultaneously dripping the initiating liquid, controlling the dripping speed to be 1.0mL/min, controlling the reaction at 85 ℃ for 2.0h, and cooling to normal temperature to obtain the organofluorine modified acrylic acid polymerization emulsion; step two, taking 10mL of organic fluorine modified acrylic acid polymerization emulsion and 1000mL of deionized water, dispersing and mixing uniformly, adding silicon nitride whisker, potassium titanate whisker and zinc oxide whisker, dispersing for 10min by ultrasonic, draining, transferring into a baking oven, and baking for 8h at 40 ℃; step three, silicon nitride whisker, potassium titanate whisker and zinc oxide whisker in mass ratio of 1:0.2:1, mixing to obtain the functional whisker.

Preparation example 7

The preparation of the piezoelectric ceramic powder comprises the following steps:

the preparation method of the titanium tetrachloride aqueous solution comprises the following steps: adding ice cubes solidified by deionized water into a beaker, adding 50ml of hydrochloric acid, accurately measuring 14ml of titanium tetrachloride liquid by a pipette, slowly adding titanium tetrachloride under a magnetic stirring state, and finally obtaining a clear and transparent solution, wherein the titanium tetrachloride solution is a solution cooled in a refrigerator, the whole preparation process is carried out in an ice-water mixture state, and finally 250ml of 0.5mol/L titanium tetrachloride aqueous solution is obtained, and then the solution is put into a dryer for storage for standby;

s1.2, according to the expression of the PZT powder, the method comprises the following steps: pbZr (PbZr) _0.52 Ti _0.48 O ₃ Respectively measuring the stoichiometric ratio of the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution prepared in the step S1.1, adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating for 10min in a water bath at 65 ℃, dropwise adding the lead nitrate aqueous solution at 0.2g/min under the stirring condition of 1400r/min, stirring for 15min, and then adding 25% ammonia water to adjust the pH value of the solution to 9 to obtain a mixed solution;

S1.3, preserving the heat of the mixed solution prepared in the step S1.2 for 30min, centrifuging, washing the obtained filter cake for 3 times by using a mixed solvent (ethanol water solution prepared in a volume ratio of 1:1), then placing the filter cake in the mixed solvent again, adding a mineralizer CaO, wherein the concentration of the mineralizer in the mixed solution is 2mol/L, and then magnetically stirring and dispersing the filter cake for 25min to obtain precursor slurry;

s1.4, putting the precursor slurry obtained in the step S1.3 into a reaction kettle, carrying out solvothermal reaction for 8 hours in a baking oven at 150 ℃ to obtain a suspension, centrifuging the obtained suspension, washing with deionized water, 10% acetic acid solution, deionized water and absolute ethyl alcohol respectively, drying a filter cake at 80 ℃, sealing a bag, placing in a dryer for storage, and carrying out ball milling for 10-15 minutes to obtain PZT piezoelectric ceramic powder with the particle size of 0.3 mu m.

Preparation 8 (comparative)

Preparation 8 differs from preparation 7 in that: s1.2, according to the expression of PZT powderThe method comprises the following steps: pbZr (PbZr) _0.55 Ti _0.45 O ₃ Respectively measuring the stoichiometric ratio of the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution prepared in the step S1.1, adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating for 10min in a water bath at 65 ℃, dropwise adding the lead nitrate aqueous solution at 0.2g/min under the stirring condition of 1400r/min, stirring for 15min, and then adding 25% ammonia water to adjust the pH value of the solution to 9 to obtain a mixed solution.

Preparation example 9

Preparation 9 differs from preparation 7 in that:

s1.2, according to the expression of the PZT powder, the method comprises the following steps: pb _0.99 Sm _0.01 Zr _0.52 Ti _0.48 O ₃ Respectively measuring the stoichiometric ratio of the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution prepared in the step S1.1, adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating for 10min in a water bath at 65 ℃, dropwise adding the lead nitrate aqueous solution at 0.2g/min under the stirring condition of 1400r/min, stirring for 15min, and then adding 25% ammonia water to adjust the pH value of the solution to 9 to obtain a mixed solution;

s1.4, putting the precursor slurry obtained in the step S1.3 into a reaction kettle, carrying out solvothermal reaction for 8 hours in a baking oven at 150 ℃ to obtain a suspension, centrifuging the obtained suspension, washing with deionized water, 10% acetic acid solution, deionized water and absolute ethyl alcohol respectively, drying a filter cake at 80 ℃, sealing a bag, placing in a dryer for storage, and ball-milling for 10-15 minutes to obtain PZT piezoelectric ceramic powder with the particle size of 0.3 mu m;

s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.99 Sm _0.01 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.99 Sm _0.01 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation example 10

Preparation 10 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

PREPARATION EXAMPLE 11

Preparation 11 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.97 Sm _0.03 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.97 Sm _0.03 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation example 12

Preparation 12 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.96 Sm _0.04 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.96 Sm _0.04 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation example 13

Preparation 13 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.95 Sm _0.05 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.95 Sm _0.05 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation 14 (comparative)

Preparation 14 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder, the method comprises the following steps: pb _0.94 Sm _0.06 Zr _0.52 Ti _0.48 O ₃ The stoichiometric ratio of the PZT piezoelectric ceramic powder in S1.4 and samarium carbonate are respectively measured, the mixture is placed in a muffle furnace for calcination after being uniformly mixed, the calcination temperature is 900 ℃ for 3 hours, the mixture is ground for 10 minutes and then is transferred into a planetary ball mill, ball milling is carried out for 12 hours at 200rpm, and Pb with the granularity of 0.5 μm is obtained by screening _0.94 Sm _0.06 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Examples

Example 1

A micro classifier impeller for processing ceramic powder for copper-clad plates is prepared from the following raw materials in parts by weight: 100 parts of piezoelectric ceramic particles and 26.8 parts of the first binder in preparation example 1. The particle size of the piezoelectric ceramic particles is controlled to be 40-60 meshes. The piezoelectric ceramic particles are mainly prepared by granulating piezoelectric ceramic powder and a second binder. The piezoelectric ceramic powder in preparation example 7 was used as the piezoelectric ceramic powder. The second binder is a 5wt% strength PVA solution.

s1, a preparation method of piezoelectric ceramic particles comprises the following steps:

s1.1, preparing piezoelectric ceramic powder, see preparation example 7;

s1.2, placing the piezoelectric ceramic powder in S1.1 into a planetary ball mill for ball milling, wherein the inner container of the planetary ball mill is made of polytetrafluoroethylene, the grinding balls are 95 zirconia beads, the ball milling speed is 200rpm, and the piezoelectric ceramic powder with the D50 of 0.3-1 mu m is obtained after ball milling for 8 hours;

s1.3, granulating, wherein a second binder PVA solution with the concentration of 5wt% accounting for 10wt% of the total mass of the piezoelectric ceramic powder is added into the piezoelectric ceramic powder in S1.2, the mixture is placed into a granulator for granulating, the obtained granules are transported to a grinder for grinding for 30min, the obtained grinding powder is pressed into large blocks by a pressing machine, the large blocks are 6cm x 1cm and placed for 24h, the large blocks are crushed into powder, the powder is placed into a planetary ball mill for ball milling at the speed of 200rpm for 2h, the obtained ball milling powder is placed into the granulator for secondary granulating, and the obtained ball milling powder is screened to obtain ceramic particles with good fluidity, and the granularity is controlled between 40 and 60 meshes;

s2, press forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to 180Mpa, and the compression time is set to 360s, so as to obtain a green body impeller;

S3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing the crucible, burying powder, sintering, heating to 1280 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and naturally cooling in a furnace to obtain the piezoelectric ceramic impeller;

s4, polarization treatment of the piezoelectric ceramic impeller, and polarization environment: and (3) silicon oil, wherein the polarization voltage is 4.5kV, the polarization temperature is 120 ℃, the polarization time is 30min, the leakage current is 0.04mA-0.38mA in the polarization process, two electrodes are manufactured at the front end and the rear end of the piezoelectric ceramic impeller after the polarization is completed, electrode leads are respectively connected with the electrodes at the front end and the rear end of the piezoelectric ceramic impeller, insulating impregnating resin is poured around the connection of the electrodes and the electrode leads, the electrodes are solidified, and 500# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper are sequentially adopted to polish the electrodes to the surface to be smooth, so that the finished micro classifier impeller is obtained. The insulating impregnating resin is commercially available epoxy resin pouring sealant, and has an insulating safety effect.

Example 2

Example 2 differs from example 1 in that: the piezoelectric ceramic particles are mainly prepared by granulating 100 parts of piezoelectric ceramic powder and 12.8 parts of second binder. The piezoelectric ceramic powder in preparation example 7 was used as the piezoelectric ceramic powder. The second binder was the second binder prepared in preparation example 2.

S1.3, granulating, wherein 1000g of piezoelectric ceramic powder in S1.2 is granulated by using 128g of the second binder prepared in preparation example 2, the obtained granules are transported to a grinder for grinding for 30min, the obtained ground powder is pressed into large blocks by a pressing machine, the large blocks have the specification of 6cm x 1cm, the large blocks are placed for 24 hours, the large blocks are crushed into powder, the powder is placed in a planetary ball mill for ball milling at the speed of 200rpm for 2 hours, the obtained ball milling powder is placed in the granulator for secondary granulation, and the obtained ball milling powder is screened to obtain ceramic particles with good fluidity, and the granularity is controlled between 40 and 60 meshes.

Example 3

Example 3 differs from example 2 in that: the piezoelectric ceramic particles are mainly prepared by granulating piezoelectric ceramic powder and a second binder. The piezoelectric ceramic powder in preparation example 7 was used as the piezoelectric ceramic powder. The second binder was the second binder prepared in preparation example 3.

Example 4

Example 4 differs from example 2 in that: the piezoelectric ceramic powder in preparation example 9 was used as the piezoelectric ceramic powder.

Example 5

Example 5 differs from example 2 in that: the piezoelectric ceramic powder in preparation example 10 was used as the piezoelectric ceramic powder.

Example 6

Example 6 differs from example 2 in that: the piezoelectric ceramic powder in preparation example 11 was used as the piezoelectric ceramic powder.

Example 7

Example 7 differs from example 2 in that: the piezoelectric ceramic powder in preparation example 12 was used as the piezoelectric ceramic powder.

Example 8

Example 8 differs from example 2 in that: the piezoelectric ceramic powder in preparation example 13 was used as the piezoelectric ceramic powder.

Example 9

Example 9 differs from example 5 in that: the piezoelectric ceramic particles are prepared from the following raw materials in parts by weight: 100 parts of Pb of 0.5 μm in preparation example 10 _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ 12.8 parts of the second binder in preparation example 2, 1.2 parts of the functional powder in preparation example 4, 0.6 part of the functional short fiber in preparation example 5 and 0.25 part of the functional whisker in preparation example 6.

s1.1, preparing piezoelectric ceramic powder, see preparation example 10;

s1.2, placing the piezoelectric ceramic powder in S1.1 into a planetary ball mill for ball milling, wherein the inner container of the planetary ball mill is made of polytetrafluoroethylene, the grinding balls are 95 zirconia balls, the ball milling speed is 200rpm, screening is carried out after ball milling for 8 hours to obtain piezoelectric ceramic powder with the D50 of 0.3-1 mu m, weighing 1000g of the piezoelectric ceramic powder in S1.1 after ball milling, adding into a high-speed dispersion kettle, dispersing for 100S at 300rpm in advance, then adding 12g of the functional powder in preparation example 4, 6g of the functional short fiber in preparation example 5 and 2.5g of the functional whisker in preparation example 6, adjusting the ball milling speed to 120rpm, and dispersing for 5min to obtain a mixture;

S1.3, granulating, wherein 128g of the second binder prepared in the preparation example 2 is adopted in the mixture in S1.2 for granulation, the obtained granules are transported to a grinder for grinding for 30min, the obtained ground powder is pressed into large blocks by a pressing machine, the large blocks have the specification of 6cm x 1cm, the large blocks are placed for 24h, the large blocks are crushed into powder, the powder is placed in a planetary ball mill for ball milling at 200rpm, the ball milling speed is 2h, the obtained ball milling powder is placed in the granulator for secondary granulation, ceramic particles with good fluidity are obtained through sieving, and the granularity is controlled between 40 and 60 meshes;

s3, discharging glue and sintering: heating the green body impeller to 550 ℃ at 0.25 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1280 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and naturally cooling in a furnace to obtain the piezoelectric ceramic impeller.

Example 10

Example 10 differs from example 1 in that: s3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1200 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and opening a furnace for natural cooling to obtain the piezoelectric ceramic impeller.

Example 11

Example 11 differs from example 1 in that:

s3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing the crucible, burying powder, sintering, heating to 1240 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and opening the furnace for natural cooling to obtain the piezoelectric ceramic impeller.

Example 12

Example 12 differs from example 1 in that:

s3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1320 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and opening a furnace for natural cooling to obtain the piezoelectric ceramic impeller.

Example 13

Example 13 differs from example 9 in that: the outer surface of the piezoelectric ceramic impeller is vapor deposited with a silicon oxide coating of 1+/-0.005 microns by a PVD physical vapor deposition process. And connecting areas between the electrodes and the wires are reserved at two ends of the piezoelectric ceramic impeller, the connecting areas are protected, and a silicon oxide coating is not plated. The Mohs hardness of the implementation is 8 and the friction coefficient is 0.35 under the improvement of the silicon oxide coating, so that the requirements of the impeller of the micro classifier can be better met.

Comparative example

Comparative example 1

Comparative example 1 differs from example 1 in that: the piezoelectric ceramic powder in preparation example 8 was used as the piezoelectric ceramic powder.

Comparative example 2

Comparative example 2 differs from example 1 in that: the piezoelectric ceramic powder in preparation example 14 was used as the piezoelectric ceramic powder.

Comparative example 3

Comparative example 3 differs from example 1 in that:

s3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1360 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and opening the furnace for natural cooling to obtain the piezoelectric ceramic impeller.

Comparative example 4

Comparative example 4 differs from example 1 in that:

s3, discharging glue and sintering: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1150 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and opening a furnace for natural cooling to obtain the piezoelectric ceramic impeller.

Performance test

Detection method/test method

1. Dielectric property test: analysis of the internal polarization of a material may use a dielectric constant that reflects the dielectric properties of the material, generally denoted epsilon. The relative dielectric constant is typically used. Measuring the thickness D of a sample, measuring the diameter D, testing the capacitance value C and the dielectric loss value of the sample at 1KHz by using an Agilent4284A precise impedance analyzer, and calculating the relative dielectric constant according to a formula:

Wherein A is the surface area, ε, of the sample ₀ ≈8.85×10 ^-12 F/m is the vacuum dielectric constant value.

2. Piezoelectric performance test: by Sinocera brand YE2730 type d ₃₃ The tester tests the piezoelectric constant.

Testing the parallel resonance frequency fp and the series resonance frequency fs, and calculating an electromechanical coupling coefficient according to a formula:

3. dielectric loss tan delta test: dielectric losses occur due to the polarization relaxation of the medium under an alternating electric field, resulting in the formation of an electric displacement density always lagging by a phase angle delta. It reflects the energy loss of a material due to heat generation per unit time under the action of an electric field, and is generally expressed by the loss tangent tan delta.

The test conditions were 1KHz. Test equipment: dielectric constant and dielectric loss tester STD-C.

4. Mohs hardness test: the surface of the tested mineral was scored with a pyramid-shaped diamond pin by scoring and the depth of the score, the depth of the score being the mohs hardness, indicated by the symbol HM. The application adopts a Mohs hardness tester to test the Mohs hardness of the impeller. In addition, the application uses HV-1000 automatic turret microhardness tester for testing. Friction coefficient test: the test was performed using an MXD-02 coefficient of friction meter.

5. Mechanical strength test:

Test subjects test specimens were prepared for blue books using the preparation methods provided in examples 1-12 and comparative examples 1-4. The test specimens differ from examples 1-12 and comparative examples 1-4 in the use of a mold. Examples 1-12 and comparative examples 1-4 were prepared in the shape of impellers and test samples were prepared as 80mm by 60mm by 3mm test piezoelectric ceramic wafers.

The preparation of the test sample, the specific preparation method is different from the preparation method of the impeller of the application in that:

s2, press forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to 180Mpa, the compression time is set to 360s, and the test green ceramic sheet with the specification of 80mm 60mm 3mm is obtained; s3, discharging glue and sintering: heating the test green ceramic sheet to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing the crucible, burying powder, sintering, heating to 1280 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.5 ℃/min, and naturally cooling in a furnace to obtain the test ceramic sheet; s4, testing the polarization treatment and polarization environment of the ceramic plate: and (3) silicon oil with a polarization voltage of 4.5kV, a polarization temperature of 120 ℃ and a polarization time of 30min, wherein leakage current in the polarization process is 0.04mA-0.38mA, and a finished product test ceramic wafer is obtained.

The testing method is tested according to the static bending strength of the piezoelectric ceramic material performance testing method of national standard GB/T1 1387-2008 of the people's republic of China.

6. Actual measurement: test subjects the impellers in examples 1, 9, 13 and impellers made with mill steel (consistent with the impeller shapes in examples 1, 9, 13). In the test method, the impellers in examples 1, 9 and 13 and the impellers prepared from the grinding tool steel are loaded in a micro classifier, the blocky calcium carbonate is respectively ground for 3.0h, and whether blocking and sticky powder occur at the impellers or not is observed.

Data analysis

Table 1 shows the detection parameters of examples 1 to 12 and comparative examples 1 to 4

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Table 3 shows the parameters measured for examples 1, 9, and 13 and for the grinding wheel made of steel

	Observation conditions
		Example 1	Non-blocking adhesive powder
Example 9	Non-blocking adhesive powder
		Example 13	Non-blocking adhesive powder
Grinding tool steel impeller	Non-blocking but surface-sticky small amount of powder

It can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and the combination of table 1 that the dielectric properties and piezoelectric properties of example 3 are slightly better than those of example 2 and example 1, and therefore, the use of the second binder in preparation examples 2 to 3 positively contributes to the improvement of the dielectric properties and piezoelectric properties of the whole impeller of the micro classifier.

As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and Table 1, the dielectric properties and piezoelectric properties of example 1 are superior to those of comparative example 1, and therefore PbZr _y Ti _(1-y) O ₃ When y=0.48, the impeller of the micro classifier has excellent dielectric and piezoelectric properties and small dielectric loss.

As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and Table 1, the dielectric properties and piezoelectric properties of examples 4 to 8 are superior to those of comparative example 2, and the dielectric loss of examples 4 to 8 is smaller than that of comparative example 2, pb _(1－x) Sm _x Zr _y Ti _(1-y) O ₃ When x=0 to 0.05 and y=0.48, the dielectric performance and piezoelectric performance of the whole impeller of the micro classifier are excellent, and the dielectric loss is small.

As can be seen in combination with examples 1-12 and comparative examples 1-4 and in combination with table 1, the dielectric properties and piezoelectric properties of example 1 are better than those of examples 10-12, and the dielectric loss of example 1 is smaller than that of examples 10-12; the dielectric properties and piezoelectric properties of examples 1, 10-12 are superior to those of comparative examples 3-4, and the dielectric losses of examples 1, 10-12 are smaller than those of comparative examples 3-4, so that the sintering temperature is controlled at 1280 ℃, and the dielectric properties and piezoelectric properties of the whole impeller of the prepared micro classifier are superior and the dielectric losses are smaller.

As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and the combination of Table 1, pb of tetragonal perovskite structure was prepared by hydrothermal synthesis _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x ZT ceramics have optimal overall electrical properties: piezoelectric constant d ₃₃ =232 pC/N, relative dielectric constant ε _r The dielectric loss tan delta=0.22 is taken as the piezoelectric vibrating element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller can not occur.

As can be seen in combination with examples 1-12 and comparative examples 1-4 and in combination with table 1,pb with tetragonal perovskite structure prepared by hydrothermal synthesis method _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x ZT ceramics have optimal overall electrical properties: piezoelectric constant d ₃₃ =229 pC/N, relative permittivity ε _r The dielectric loss tan delta=0.16 is taken as the piezoelectric vibrating element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller can not occur.

As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and the combination of Table 1, pb of tetragonal perovskite structure was prepared by hydrothermal synthesis _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ Impeller of micro classifier prepared by combining functional powder in preparation example 4, functional short fiber in preparation example 5 and functional whisker in preparation example 6, when sintering temperature is 1280 ℃, PSm _x ZT ceramics have optimal overall electrical properties: piezoelectric constant d ₃₃ Relative permittivity ε =243 pC/N _r The dielectric loss tan delta=0.18 is used as a piezoelectric vibrating element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller is avoided.

As can be seen by combining examples 1-12 and comparative examples 1-4 and combining tables 1-3, the application not only has better piezoelectric performance, but also generates vibration with certain amplitude in the use process, so that the phenomenon of blocking or sticking of materials at the impeller can not occur; in addition, the application has relatively long mechanical property and service life.

The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims

1. A fine classifier impeller for processing ceramic powder for copper-clad plate which characterized in that: is composed of the following components by weightThe raw materials are prepared as follows: 100 parts of piezoelectric ceramic particles and 20-40 parts of first binder; the piezoelectric ceramic particles are mainly prepared by granulating piezoelectric ceramic powder and a second binder; the particle size of the piezoelectric ceramic particles is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by adopting a hydrothermal synthesis method, and the expression of the piezoelectric ceramic powder is Pb _（1－x） Sm _x Zr _0.52 Ti _0.48 O ₃ X=0.02; the grain diameter D50 of the piezoelectric ceramic powder is controlled to be 0.3-0.5 mu m;

the preparation method of the piezoelectric ceramic particles comprises the following steps:

s1, preparing piezoelectric ceramic powder;

s1.2, according to the expression of the PZT powder, the method comprises the following steps: pb _（1－x） Sm _x Zr _0.52 Ti _0.48 O ₃ Respectively measuring the stoichiometric ratio of the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution prepared in the step S1.1, adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating for 5-10min in a water bath at 50-70 ℃, dropwise adding the lead nitrate aqueous solution at 0.1-0.2g/min under the stirring condition of 1200-1500r/min, stirring for 10-20min, and then adding ammonia water with the concentration of 25% to adjust the pH value of the solution to 8-10 to obtain a mixed solution;

s1.5, mixing and calcining, grinding and sieving the PZT piezoelectric ceramic powder with the concentration of 99.5-100% and the samarium carbonate with the concentration of 0-0.05% to obtain Pb _（1－x） Sm _x Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder;

s2, ball milling and screening to obtain piezoelectric ceramic powder with D50 of 0.3-0.5 mu m;

2. The micro classifier impeller for processing ceramic powder for copper-clad plate according to claim 1, wherein: the piezoelectric ceramic particles are mainly prepared from piezoelectric ceramic powder, a second binder, functional powder, functional short fibers and functional whiskers; the mass of the functional powder is 0.003-0.015 times of that of the piezoelectric ceramic powder; the mass of the functional short fiber is 0.002-0.01 times of the mass of the piezoelectric ceramic powder; the mass of the functional whisker is 0.001-0.004 times of that of the piezoelectric ceramic powder; the second binder is prepared from organic silicon resin, modified siloxane, diethylenetriamine and a diluting solvent, and the solid content is 40-50%; the modified siloxane is one or a combination of more of fluorine-containing siloxane, FM-3311 siloxane, FM-4411 siloxane, FM-7711 siloxane, FM-0411 siloxane, FM-DA11 siloxane, FM-0711 siloxane and TM-0701T siloxane; the preparation method of the second binder comprises the steps of firstly preparing raw materials, uniformly stirring the organic silicon resin and the modified siloxane, preheating to 70-75 ℃, reacting for 2-3min in advance, cooling to below 10 ℃, adding a diluting solvent, uniformly stirring, finally adding diethylenetriamine, and uniformly stirring to obtain the finished second binder.

3. The micro classifier impeller for processing ceramic powder for copper-clad plate according to claim 2, wherein: the functional powder is one or a combination of more of silicon nitride powder, cubic boron nitride powder, zirconium oxide, calcium oxide, cerium oxide, magnesium oxide and yttrium oxide; the functional powder D50 is 1-5 microns; the functional short fiber is one or a combination of more of silicon nitride fiber, aluminum oxide fiber and boron nitride fiber; the length of the functional short fiber is 1-10 micrometers; the functional whisker is one or a combination of more of silicon nitride whisker, potassium titanate whisker and zinc oxide whisker.

4. The micro classifier impeller for processing ceramic powder for copper-clad plate according to claim 2, wherein: the piezoelectric ceramic particles are prepared from the following raw materials in parts by weight: 100 parts of piezoelectric ceramic powder, 10-15 parts of second binder, 1-1.2 parts of functional powder, 0.4-0.6 part of functional short fiber and 0.2-0.25 part of functional whisker; the functional powder consists of cubic boron nitride powder, zirconia and cerium oxide; the mass ratio of the cubic boron nitride powder to the zirconia to the cerium oxide is (80-200): 100: (1-3); the functional short fiber is prepared from silicon nitride fiber and boron nitride fiber according to the mass ratio of 1:1, the composition is as follows; the functional whisker is prepared from silicon nitride whisker, potassium titanate whisker and zinc oxide whisker according to the mass ratio of 1: (0.2-0.8): 1.

5. The micro classifier impeller for processing ceramic powder for copper-clad plate according to claim 1, wherein: the first binder is mainly prepared from main components, injection molding grade polyolefin PP, compatilizer EVA, lubricant, dispersing agent and antioxidant; the main component is copolyformaldehyde POM, and the number average molecular weight is 2-4 ten thousand; the lubricant is a CBT resin polymer with a hyperbranched structure; the preparation method of the first adhesive comprises the steps of mixing main components, polyolefin PP, compatilizer EVA, lubricant, dispersing agent and antioxidant at 0-4 ℃ for 10-15min at 300-400rpm to obtain the finished first adhesive.

6. A method for manufacturing an impeller of a micro-classifier according to any one of claims 1 to 5, characterized in that: the method comprises the following steps:

s1, preparing piezoelectric ceramic powder;

7. The method for manufacturing a micro classifier impeller for processing ceramic powder for copper-clad plate according to claim 6, wherein: s4, pressing and forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to 180Mpa, and the compression time is set to 360s, so as to obtain a green body impeller; the rubber discharging and sintering are carried out: heating the green body impeller to 540 ℃ at 0.2 ℃/min, preserving heat for 3 hours, removing the binder, sealing and embedding powder by a crucible, sintering, heating to 1280 ℃ at 0.5 ℃/min, preserving heat for 125 minutes, cooling to 650 ℃ at 2.0-2.5 ℃/min, and opening a furnace for natural cooling to obtain the piezoelectric ceramic impeller.