CN115254610A

CN115254610A - Fine classifier impeller for processing ceramic powder for copper-clad plate and manufacturing method thereof

Info

Publication number: CN115254610A
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: 2022-11-01
Anticipated expiration: 2042-08-02
Also published as: CN115254610B

Abstract

The application relates to the technical field of impeller back manufacturing of a fine grader, in particular to a fine grader impeller for processing ceramic powder for a copper-clad plate and a manufacturing method thereof. A fine grader impeller for processing ceramic powder for copper clad laminate 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 grain size of the piezoelectric ceramic grains is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by a hydrothermal synthesis method, and the expression is Pb (1-x) SmxZryTi (1-y) O3, wherein x = 0-0.05, y = 0.46-0.48; the D50 of the piezoelectric ceramic powder is controlled to be 0.2-16 microns. The impeller of this application preparation is applied to fine grader, when carrying out the material powder and grading, is difficult for appearing stifled powder, glutinous powder condition, improves material grading, screening effect.

Description

Fine grader 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 a fine grader, in particular to a fine grader impeller for processing ceramic powder for a copper-clad plate and a manufacturing method thereof.

Background

In the industrial production process, the grain diameter of various fine powder materials is strictly limited, such as the fineness, the purity and the passing rate of the fine powder materials. The ultrafine classifier can be used for classifying materials with different particle sizes, and is widely applied to the industries of cement, mines, chemical industry, fillers, food and the like. In the production process of the high-frequency and high-speed copper-clad plate, a micro classifier is required to carry out classified screening on the special copper-clad plate ceramic powder, and the quality of the classified screening quality directly influences the quality of the prepared high-frequency and high-speed copper-clad plate.

Classification principle of a fine classifier: the circle S represents the outer contour line of the classifying impeller, the air flow is represented by a dotted line, P is a point intersecting the surface of the impeller, and the particles are subjected to two opposite forces at the point P, namely, centrifugal inertia force F generated by the rotation of the impeller and resistance R from the air flow. F = (pi/6) d ³ (ρs-ρ)(u _θ ² /r)，R＝3πμdu _r Wherein d is the diameter of the material powder particles; r-mean radius of impeller; ρ s is the density of the material particles; ρ -air density; u. u _θ- Impeller mean peripheral velocity (tangential velocity of the particles); μ is the air viscosity, u _r Radial velocity of the gas flow (radial velocity of the particles). When the particles are subjected to a centrifugal force greater than the resistance to the air flow (F)>R) the particles fly to the inner wall of the grading chamber along the direction of the impeller, then fall along the chamber wall due to the action of gravity, and are discharged out of the machine to form coarse powder at a coarse particle discharge port. When the particles are subjected to a centrifugal force less than the resistance to the air flow (F)<R) the particles pass through the gaps of the grading impeller blades along with the airflow and are discharged out of the machine from a fine powder discharge port to form fine powder. When the force F = R applied to the particle, the particle diameter at this time is referred to as a critical particle diameter.

The vertical grading device in the related technology is composed of a grading impeller, a bearing box, a bearing cover, a belt pulley and a motor. The grading impeller is generally made of stainless steel, carbon steel, manganese steel alloy and 99-alumina anti-wear ceramic. In view of the impeller of the fine classifier in the above-mentioned related art, the applicant has found that the following drawbacks exist in the technical solution: the impeller of the fine classifier in the related art is likely to be clogged or stuck at the impeller when the ceramic powder is pulverized.

Disclosure of Invention

In order to solve the problem that the impeller of the micro-fine grader is easy to block or be sticky at the impeller when ceramic powder is crushed, the application provides the micro-fine grader impeller for processing the ceramic powder for the copper-clad plate and the manufacturing method thereof.

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

a fine grader impeller for processing ceramic powder for copper clad laminate 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 grain size of the piezoelectric ceramic grains is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by 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 Piezoelectric ceramic powder is the impeller that fine grader was obtained in raw materials preparation, and the impeller that this application was prepared produces the vibration of certain amplitude in the use, is applied to fine grader, when carrying out the material powder and grading, is difficult for appearing stifled powder, glutinous powder condition, improves material grading, screening effect.

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 D50 of the piezoelectric ceramic powder is controlled to be 0.5-4.8 mu m.

By adopting the technical scheme, the Sm infiltration amount and the Zr are reduced ₀ The ratio of/Ti is defined, varying Pb _1－ _x Sm _x Zr _0.52 Ti _0.48 O ₃ The crystal phase structure of the crystal can be improvedThe piezoelectric constant, the relative dielectric constant and the dielectric loss of the impeller of the prepared micro-classifier further improve 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: pb _(1－x) Sm _x Zr _0.52 Ti _0.48 O ₃ Respectively measuring the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution which are prepared in S1.1 according to the stoichiometric ratio, then 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 kettle at 50-70 ℃, dropwise adding the lead nitrate aqueous solution at 0.1-0.2g/min under the stirring condition of 1200-1500r/min, then 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 the heat of the mixed liquid prepared in the step S1.2 for 20-40min, centrifuging, washing the obtained filter cake for 2-3 times by using the mixed solvent, then 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 then magnetically stirring and dispersing for 25-35min to obtain precursor slurry;

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

s1.5, mixing 99.5-100% of PZT piezoelectric ceramic powder and 0-0.05% of samarium carbonate, calcining, grinding and screening 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;

and S3, granulating, namely adding a second binder PVA solution with the concentration of 3-5wt% into the piezoelectric ceramic powder in the S2, wherein the using amount 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 granules into large blocks, standing the large blocks for 24h, crushing the large blocks into powder, granulating the powder for the second time, and sieving the powder to obtain the ceramic granules with good fluidity.

By adopting the technical scheme, the Pb with the tetragonal phase perovskite structure is prepared by adopting a hydrothermal synthesis method _1－ _x Sm _x Zr _0.52 Ti _0.48 O ₃ A piezoelectric ceramic powder having excellent piezoelectric properties. The preparation method of the piezoelectric ceramic powder provided by the application has a 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, the Pb with the tetragonal phase perovskite structure is prepared by adopting a hydrothermal synthesis method _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x The ZT ceramic has the optimal comprehensive electrical property: piezoelectric constant d ₃₃ =232pC/N, relative dielectric constant ε _r The impeller generates vibration with certain amplitude in the use process as a piezoelectric vibrator of the ultrasonic transducer, so that the phenomenon of blockage or adhesion 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 time of that of the piezoelectric ceramic powder; the mass of the functional short fiber is 0.002-0.01 times of that of the piezoelectric ceramic powder; the functional crystal whisker is 0.001-0.004 times of the piezoelectric ceramic powder in mass; 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 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 the diluent solvent, uniformly stirring, finally adding the diethylenetriamine, and uniformly stirring to obtain the finished product of the second binder.

By adopting the technical scheme, the piezoelectric ceramic particles with good fluidity and good storage stability can be prepared, so that 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, toughness, heat resistance and 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, zirconia, and any one of calcium oxide, cerium oxide, magnesium oxide and yttrium oxide; the D50 of the functional powder is 1-5 microns; the functional short fiber is one or a combination of more of silicon nitride fiber, alumina fiber and boron nitride fiber; the length of the functional short fiber is 1-10 microns; 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 fibers and the functional whiskers, the mechanical property, toughness, heat resistance and 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, preparing a composition; the functional crystal whisker is prepared from silicon nitride crystal whisker, potassium titanate crystal whisker and zinc oxide crystal whisker in a mass ratio of 1: (0.2-0.8): 1.

By adopting the technical scheme, the components and the using amount of the piezoelectric ceramic particles are optimized, so that the piezoelectric ceramic impeller with better piezoelectric property and better part spacing and excellent mechanical property, toughness, heat resistance and corrosion resistance can be obtained, and the integral powder grading and screening effect is further improved.

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

Through adopting above-mentioned technical scheme, be convenient for carry out mixing granulation and the binder removal of follow-up workshop section, degrease operation, can optimize the holistic production efficiency of this application and guarantee the piezoceramics impeller stability of quality of this application simultaneously.

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

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

s1, preparing piezoelectric ceramic powder;

s3, granulating, namely adding a second binder into the piezoelectric ceramic powder in the S2, granulating, grinding the obtained granules for 30-40min, pressing the granules into large blocks, standing the large blocks for 24h, crushing the large blocks into powder, performing secondary granulation, and sieving the powder 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, removing glue and sintering: heating the green impeller to 520-550 ℃ at a speed of 0.2-0.4 ℃/min, preserving heat for 3-3.2h, removing the binder, sealing and embedding the powder in a crucible for sintering, heating to 1200-1320 ℃ at a speed of 0.5-0.6 ℃/min, preserving heat for 2-2.5h, and obtaining the piezoelectric ceramic impeller;

and 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 product of the fine grader impeller.

By adopting the technical scheme, the preparation method is relatively simple, the preparation process is relatively mature, the difficulty of controlling the product quality is relatively low, the production investment cost of production enterprises is easily reduced, and the industrial batch production is facilitated.

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

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

In summary, the present application has the following advantages:

1. the impeller of this application preparation produces the vibration of certain amplitude in the use, when smashing ceramic powder, is difficult for appearing stifled powder, glutinous powder condition, and the powder is sieved in grades effectually.

2. The preparation method is relatively simple, the preparation process is relatively mature, the difficulty in controlling the product quality is relatively low, production enterprises can reduce the production input cost easily, and industrial batch 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 The ZT ceramic has the optimal comprehensive electrical property: piezoelectric constant d ₃₃ =232pC/N, relative dielectric constant ε _r The impeller generates vibration with certain amplitude in the use process as a piezoelectric vibrator of the ultrasonic transducer, so that the phenomenon of blockage or adhesion 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 examples

Preparation example 1

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

The preparation method of the first binder comprises the steps of adding 833g of main component-physical copolyformaldehyde POM (M90-44, injection molding grade), 88g of injection molding grade polyolefin PP (trade mark 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 dispersant (CAS: 57-11-4) and 16g of antioxidant B900 into a reaction kettle, introducing nitrogen to control the temperature to be 0-4 ℃, starting stirring, mixing for 12min at 360rpm, vacuumizing and defoaming to obtain the finished product first binder.

Preparation example 2

The second adhesive is prepared from 36% of KR-242A silicone resin, 4% of fluorine-containing siloxane, 0.1% of diethylenetriamine and 59.9% of methanol.

The preparation method of the second adhesive comprises the following steps:

step one, preparing fluorine-containing siloxane: 19.01g perfluorohexylethanethiol and 250g TM-0701T siloxane are put in a three-neck flask, heated to 45 ℃ in water bath, added with 0.1g azodiisobutyronitrile, stirred at 320rpm, and subjected to a hydrosulfurization reaction for 1.0h to obtain the fluorine-containing siloxane;

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

and step three, cooling by using an ice salt bath, controlling the temperature to be 0-4 ℃, adding 599g of methanol, stirring at 250rpm for 10min, adding 1.0g of diethylenetriamine, and stirring at 80rpm for 100s to obtain the finished product of the second binder.

Preparation example 3

The second adhesive is prepared from 36% of KR-242A organic silicon resin, 4% of TM-0701T siloxane, 0.1% of diethylenetriamine and 59.9% of methanol.

The preparation method of the second adhesive comprises the following steps: mixing 40g of TM-0701T siloxane with 360g of KR-242A silicon resin at 240rpm, stirring for 5min, heating to 72-75 ℃, and pre-reacting for 150s; and cooling by using a ice salt bath, controlling the temperature to be 0-4 ℃, adding 599g of methanol, stirring at 250rpm for 10min, adding 1.0g of diethylenetriamine, and stirring at 80rpm for 100s to obtain the finished product of the second binder.

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 ceria is 198:100:2. preparing functional powder, namely preparing cubic boron nitride powder, zirconia and cerium oxide according to a mass ratio of 198:100:2, adding the mixture into a planetary ball mill after weighing, wherein the inner container is made of polytetrafluoroethylene, the grinding ball is made of 95 zirconium oxide beads, carrying out ball milling for 30min at 120rpm, screening to obtain functional powder with the granularity of 1-5 microns, placing the functional powder into a KH570 coupling agent with the granularity of 3g/L for ultrasonic dispersion for 10min, transferring the powder into an oven, and drying for 8h at the temperature of 40 ℃ 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: 4g/L of Capatue ^TM Preparing organic functional silane water solution by soaking silicon nitride fiber and boron nitride fiber in Capatue ^TM Ultrasonically dispersing in an organic functional silane aqueous solution for 10min, taking out, drying at 40 ℃ for 8h, wherein the mass ratio of silicon nitride fibers to boron nitride fibers is 1:1 mixing to obtain the functional short fiber.

Preparation example 6

The functional crystal whisker is prepared from silicon nitride crystal whisker, potassium titanate crystal whisker and zinc oxide crystal whisker in a mass ratio of 1:0.2: 1. The preparation method of the functional whisker comprises the following steps: step one, preparing organic fluorine modified acrylic acid polymerization emulsion: preparation of pre-emulsion A: taking 375g of water, 5.0g of emulsifier AES, 75.2g of methyl methacrylate and 340.2g of butyl methacrylate in total, pre-emulsifying for 10min in high-speed shears at 3200rpm, and taking 1/3 of pre-emulsion for later use; preparing an initiating solution, and dissolving 1.25g of azodiisobutyronitrile serving as an initiator into 250g of water for later use; and simultaneously preparing a pre-emulsion B: 84.6g of side chain being C ₈ F ₁₇ (CH ₂ ) ₃ Adding the fluorosilicone polymer into the rest 2/3 of the pre-emulsion A, placing the pre-emulsion A 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 dropwise adding the initiation liquid prepared in the second step at 6mL/min, stopping heating and dropwise adding the initiator after 22min, continuously stirring at 100rpm for 5min, dropwise adding the pre-emulsion B at 24mL/min, controlling the rotating speed at 160rpm, dropwise adding the initiation liquid at the same time, controlling the dropwise adding speed to be 1.0mL/min, controlling the temperature to be 85 ℃ for reacting for 2.0h, and cooling to normal temperature to obtain the organic fluorine 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 whiskers, potassium titanate whiskers and zinc oxide whiskers, dispersing for 10min by ultrasonic, draining, transferring to a drying oven, and drying for 8h at 40 ℃; step three, silicon nitride whisker, potassium titanate whisker and zinc oxide whisker in a mass ratio of 1:0.2:1, mixing to obtain the functional crystal 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 blocks formed by solidifying deionized water into a beaker, adding 50ml of hydrochloric acid, accurately measuring 14ml of titanium tetrachloride liquid by using a pipette, slowly adding titanium tetrachloride under a magnetic stirring state to finally obtain 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 to finally obtain 250ml of 0.5mol/L titanium tetrachloride aqueous solution, and then placing the titanium tetrachloride aqueous solution into a dryer for storage;

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

s1.3, preserving the temperature of the mixed liquid prepared in the step S1.2 for 30min, then carrying out centrifugal treatment, washing the obtained filter cake for 3 times by using a mixed solvent (ethanol water solution prepared by 1:1 in volume ratio), then placing the washed filter cake into the mixed solvent again, adding a mineralizer CaO, wherein the concentration of the mineralizer in the mixed liquid is 2mol/L, and then carrying out magnetic stirring and dispersion for 25min to obtain precursor slurry;

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

Preparation example 8 (comparative)

Preparation 8 differs from preparation 7 in that: s1.2, according to the expression of the PZT powder: pbZr _0.55 Ti _0.45 O ₃ Respectively measuring the titanium tetrachloride aqueous solution, the zirconium oxychloride aqueous solution and the lead nitrate aqueous solution which are prepared in the step S1.1 according to the stoichiometric ratio, then adding the titanium tetrachloride aqueous solution and the zirconium oxychloride aqueous solution into a three-necked bottle, preheating the three-necked bottle in a 65 ℃ water bath kettle for 10min, dropwise adding the lead nitrate aqueous solution at the speed of 0.2g/min under the stirring condition of 1400r/min, stirring the mixture for 15min, and then adding ammonia water with the concentration of 25% 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:

the preparation method of the titanium tetrachloride aqueous solution comprises the following steps: adding ice blocks formed by solidifying deionized water into a beaker, adding 50ml of hydrochloric acid, accurately measuring 14ml of titanium tetrachloride liquid by using a pipette, slowly adding titanium tetrachloride under a magnetic stirring state to obtain 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 to obtain 250ml of 0.5mol/L titanium tetrachloride aqueous solution, and then putting the titanium tetrachloride aqueous solution into a dryer for storage;

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

s1.4, putting the precursor slurry obtained in the S1.3 into a reaction kettle, carrying out solvothermal reaction for 8 hours in a drying oven at 150 ℃ to obtain a suspension, centrifuging the obtained suspension, washing the suspension with deionized water, a 10% acetic acid solution, deionized water and absolute ethyl alcohol respectively, drying a filter cake at 80 ℃, sealing a bag, placing the bag in a dryer for storage, and carrying out ball milling for 10-15min 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: pb _0.99 Sm _0.01 Zr _0.52 Ti _0.48 O ₃ Respectively measuring PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio, uniformly mixing, calcining in a muffle furnace at 900 ℃ for 3h, grinding for 10min, transferring to a planetary ball mill, ball-milling at 200rpm for 12h, and sieving to obtain Pb with the particle size of 0.5 mu m _0.99 Sm _0.01 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation example 10

The preparation 10 differs from the preparation 9 in that: s1.5, according to the expression of the PZT powder: pb _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ Respectively measuring PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio, uniformly mixing, calcining in a muffle furnace at 900 ℃ for 3h, grinding for 10min, transferring to a planetary ball mill, ball-milling at 200rpm for 12h, and sieving to obtain Pb with the particle size of 0.5 mu m _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: pb _0.97 Sm _0.03 Zr _0.52 Ti _0.48 O ₃ Respectively measuring PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio, uniformly mixing, calcining in a muffle furnace at 900 ℃ for 3h, grinding for 10min, transferring to a planetary ball mill, ball-milling at 200rpm for 12h, and sieving to obtain Pb with the particle size of 0.5 mu m _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: pb _0.96 Sm _0.04 Zr _0.52 Ti _0.48 O ₃ Respectively measuring PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio, uniformly mixing, calcining in a muffle furnace at 900 ℃ for 3h, grinding for 10min, transferring to a planetary ball mill, ball-milling at 200rpm for 12h, and sieving to obtain Pb with the particle size of 0.5 mu m _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: pb _0.95 Sm _0.05 Zr _0.52 Ti _0.48 O ₃ Respectively measuring PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio, uniformly mixing, calcining in a muffle furnace at 900 ℃ for 3h, grinding for 10min, transferring to a planetary ball mill, ball-milling at 200rpm for 12h, and sieving to obtain Pb with the particle size of 0.5 mu m _0.95 Sm _0.05 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder.

Preparation example 14 (comparative)

Preparation 14 differs from preparation 9 in that: s1.5, according to the expression of the PZT powder: pb _0.94 Sm _0.06 Zr _0.52 Ti _0.48 O ₃ Respectively weighing PZT piezoelectric ceramic powder and samarium carbonate in S1.4 according to the stoichiometric ratio,mixing, calcining in muffle furnace at 900 deg.C for 3 hr, grinding for 10min, transferring to planetary ball mill, ball milling at 200rpm for 12 hr, and sieving to obtain Pb with particle size of 0.5 μm _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, 26.8 parts of the first binder in production example 1. The grain diameter of the piezoelectric ceramic grains 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 used in preparation example 7 was used. The second binder was a 5wt% concentration PVA solution.

A manufacturing method of a micro-fine grader impeller for processing ceramic powder for copper-clad plates comprises the following steps:

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

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

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

s1.3, granulating, adding a second binder PVA solution with the concentration of 5wt% accounting for 10wt% of the total mass of the piezoelectric ceramic powder into the piezoelectric ceramic powder in S1.2, placing the piezoelectric ceramic powder in a granulator for granulation treatment, transferring the obtained granules to a grinder for grinding for 30min, pressing the obtained ground powder into blocks with the specification of 6cm 1cm, placing the blocks for 24h, crushing the blocks into powder, placing the powder in a planetary ball mill for ball milling, ball milling at the ball milling speed of 200rpm for 2h, placing the obtained ball-milled powder in the granulator for secondary granulation, and sieving to obtain ceramic particles with good fluidity, wherein the particle size is controlled to be 40-60 meshes;

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

s3, removing glue and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible for sintering, heating to 1280 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.5 ℃/min, opening the furnace, and naturally cooling to obtain the piezoelectric ceramic impeller;

s4, piezoelectric ceramic impeller polarization treatment, wherein the polarization environment is as follows: the method comprises the following steps of preparing silicon oil, wherein the polarization voltage is 4.5kV, the polarization temperature is 120 ℃, the polarization time is 30min, the leakage current in the polarization process is 0.04mA-0.38mA, manufacturing two electrodes at the front end and the rear end of the piezoelectric ceramic impeller after polarization is completed, electrode leads are respectively connected with 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, curing, and sequentially polishing by 500#, 1000#, 1500#, and 2000# abrasive paper until the surface is smooth to obtain the finished product of the fine grader impeller. 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 used in preparation example 7 was used. The second binder was the second binder prepared in preparation example 2.

S1.3, granulating 1000g of the piezoelectric ceramic powder in S1.2 by using 128g of the second binder prepared in preparation example 2, transferring the obtained granules into a grinder to grind for 30min, pressing the obtained ground powder into blocks with the size of 6cm x 1cm by using a pressing machine, standing for 24h, crushing the blocks into powder, ball-milling the powder in a planetary ball mill at the ball-milling speed of 200rpm for 2h, carrying out secondary granulation on the obtained ball-milled powder in a granulator, and sieving to obtain ceramic particles with good fluidity, wherein the particle size is controlled to be 40-60 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 used in preparation example 7 was used. 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 used in preparation example 9 was used.

Example 5

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

Example 6

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

Example 7

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

Example 8

Example 8 differs from example 2 in that: the piezoelectric ceramic powder used in preparation example 13 was 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 0.5 μm Pb of production example 10 _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ Piezoelectric ceramic powder, 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, a preparation method of the piezoelectric ceramic particles comprises the following steps:

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

s1.2, ball-milling the piezoelectric ceramic powder in the S1.1 in a planetary ball mill, wherein an inner container of the planetary ball mill is made of polytetrafluoroethylene, a milling ball is made of 95 zirconia beads, the ball-milling speed is 200rpm, the piezoelectric ceramic powder with the D50 of 0.3-1 mu m is obtained by screening after ball-milling for 8 hours, 1000g of the piezoelectric ceramic powder in the S1.1 after ball-milling is weighed and added into a high-speed dispersion kettle, the powder is dispersed for 100S at 300rpm in advance, then 12g of the functional powder in the preparation example 4, 6g of the functional short fibers in the preparation example 5 and 2.5g of the functional whiskers in the preparation example 6 are added, the ball-milling speed is adjusted to 120rpm, and the mixture is obtained by dispersing for 5 minutes;

s1.3, granulating, namely granulating 128g of the second binder prepared in the preparation example 2 in the mixture in the S1.2, transferring the obtained granules into a grinder for grinding for 30min, pressing the obtained ground powder into large blocks with the specification of 6cm x 1cm by a pressing machine, standing for 24h, crushing the large blocks into powder, placing the powder into a planetary ball mill for ball milling at the ball milling speed of 200rpm for 2h, placing the obtained ball-milled powder into a granulator for secondary granulation, and sieving to obtain ceramic particles with good fluidity, wherein the granularity is controlled to be 40-60 meshes;

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

Example 10

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

Example 11

Example 11 differs from example 1 in that:

s3, removing glue and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible for sintering, heating to 1240 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.5 ℃/min, opening the furnace, and naturally cooling to obtain the piezoelectric ceramic impeller.

Example 12

Example 12 differs from example 1 in that:

s3, removing glue and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible, sintering, heating to 1320 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.5 ℃/min, opening the furnace, and naturally 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 evaporated with a silicon oxide coating of 1 +/-0.005 micron by a PVD physical vapor deposition process. The connection areas of the electrodes and the leads are reserved at the two ends of the piezoelectric ceramic impeller and are protected, and the silicon oxide coating is not plated. The implementation has the advantages that the Mohs hardness is 8 and the friction coefficient is 0.35 under the improvement of the silicon oxide coating, and the requirement 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 used in preparation example 8 was used.

Comparative example 2

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

Comparative example 3

Comparative example 3 differs from example 1 in that:

s3, removing glue and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible, sintering, heating to 1360 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.5 ℃/min, opening the furnace, and naturally cooling to obtain the piezoelectric ceramic impeller.

Comparative example 4

Comparative example 4 differs from example 1 in that:

s3, removing glue and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible for sintering, heating to 1150 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.5 ℃/min, opening the furnace, and naturally cooling to obtain the piezoelectric ceramic impeller.

Performance test

Detection method/test method

1. And (3) dielectric property test: analysis of the internal polarization of a material may use a dielectric constant, which reflects the dielectric properties of the material, generally denoted by ε. The relative dielectric constant is typically used. Firstly measuring the thickness D of a sample, then measuring the diameter D, then testing the capacitance C and the dielectric loss value of the sample under 1KHz by using an Agilent4284A precision impedance analyzer, and finally calculating the relative dielectric constant according to a formula:

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

2. And (3) testing the piezoelectric performance: using 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 the electromechanical coupling coefficient according to a formula:

3. dielectric loss tan δ test: dielectric losses occur due to the polarization relaxation of the medium under an alternating electric field, so that the formation of the electrical displacement density is always delayed by a phase angle δ. It reflects the energy loss of the material due to heating per unit time under the action of an electric field, usually expressed as loss tangent tan δ.

The test conditions were 1KHz. And (3) testing equipment: dielectric constant and dielectric loss tester STD-C.

4. Mohs hardness test: the surface of the mineral to be tested was scribed with a diamond pyramid-shaped diamond needle by the scoring method, and the depth of the scratch, which is the mohs hardness and is expressed by the symbol HM, was measured. This application adopts the mohs hardness tester to test the mohs hardness of impeller. In addition, the present application employs an HV-1000 automatic turret microhardness tester for testing. And (3) testing the friction coefficient: and testing by adopting an MXD-02 friction coefficient measuring instrument.

5. And (3) testing mechanical strength:

test subjects, test specimens were prepared for the blue pad by the preparation methods provided in examples 1 to 12 and comparative examples 1 to 4. The test specimens differ from examples 1 to 12 and comparative examples 1 to 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 60mm 3mm test piezoceramic wafers.

The preparation of the test sample, the specific preparation method and the preparation method of the impeller of the application are different in that:

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

The test method is carried out according to the static bending strength test of the piezoceramic material performance test method of the national standard GB/T1 1387-2008 of the people's republic of China.

6. Actually measuring: test objects the impellers of examples 1, 9, 13 and the impellers made with abrasive tool steel (conforming to the shape of the impellers of examples 1, 9, 13) were tested. The testing method comprises the steps of loading the impellers in the examples 1, 9 and 13 and the impeller prepared by the grinding tool steel into a micro-classifier, respectively grinding the massive calcium carbonate for 3.0 hours, and observing whether the impeller is blocked and adhered with powder.

Data analysis

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

Table 3 shows the measured parameters of the steel impellers of examples 1, 9 and 13 and the grinding tools

	Observation of conditions
		Example 1	Non-blocking and sticky powder
Example 9	Non-blocking and sticky powder
		Example 13	Non-blocking and sticky powder
Steel impeller of grinding tool	No blocking but small amount of powder adhered to the surface

It can be seen from the combination of examples 1 to 12 and comparative examples 1 to 4 and from table 1 that the dielectric properties and piezoelectric properties of example 3 are slightly superior to those of examples 2 and 1, and therefore, the use of the second binder of preparation examples 2 to 3 has a positive effect on the improvement of the dielectric properties and piezoelectric properties of the impeller of the fine classifier as a whole.

As can be seen by combining examples 1 to 12 and comparative examples 1 to 4 with Table 1, the dielectric properties and piezoelectric properties of example 1 are superior to those of comparative example 1, and thus, pbZr _y Ti _(1-y) O ₃ When y =0.48, the dielectric properties and piezoelectric properties of the entire impeller of the fine classifier are excellent, and the dielectric loss is small.

As can be seen by combining examples 1-12 and comparative examples 1-4 with Table 1, the dielectric and piezoelectric properties of examples 4-8 are superior to those of comparative example 2, and the dielectric loss of examples 4-8 is less 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 properties and piezoelectric properties of the entire impeller of the fine classifier are excellent, and the dielectric loss is small.

Combining examples 1-12 and comparative examples 1-4 with Table 1, it can be seen that the dielectric and piezoelectric properties of example 1 are superior to those of examples 10-12, and the dielectric loss of example 1 is less than that of examples 10-12; the dielectric properties and piezoelectric properties of examples 1 and 10-12 are superior to those of comparative examples 3-4, and the dielectric loss of examples 1 and 10-12 is less than that of comparative examples 3-4, so that the sintering temperature is controlled at 1280 ℃, and the prepared impeller of the fine classifier has better overall dielectric properties and piezoelectric properties and smaller dielectric loss.

As can be seen by combining examples 1 to 12 and comparative examples 1 to 4 with Table 1, pb having a 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 The ZT ceramic has the optimal comprehensive electrical property: piezoelectric constant d ₃₃ =232pC/N, relative dielectric constant ε _r The impeller generates vibration with certain amplitude in the use process as a piezoelectric vibrator of the ultrasonic transducer, so that the phenomenon of blockage or adhesion of materials at the impeller can not occur.

As can be seen by combining examples 1 to 12 and comparative examples 1 to 4 with Table 1, the catalyst was prepared by hydrothermal synthesisPrepared tetragonal phase perovskite structure Pb _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ When the sintering temperature is 1280 ℃, PSm _x The ZT ceramic has the optimal comprehensive electrical property: piezoelectric constant d ₃₃ =229pC/N, relative dielectric constant ε _r The piezoelectric vibration element is used as a piezoelectric vibration element of the ultrasonic transducer, and the impeller generates vibration with certain amplitude in the use process, so that the phenomenon of blockage or adhesion of materials at the impeller can be avoided.

As can be seen by combining examples 1 to 12 and comparative examples 1 to 4 with Table 1, pb having a tetragonal perovskite structure was prepared by hydrothermal synthesis _0.98 Sm _0.02 Zr _0.52 Ti _0.48 O ₃ Impeller of fine classifier prepared by combining the functional powder of preparation example 4, the functional short fiber of preparation example 5, and the functional whisker of preparation example 6, when sintering temperature is 1280 ℃, PSm _x The ZT ceramic has the optimal comprehensive electrical property: piezoelectric constant d ₃₃ =243pC/N, relative dielectric constant ε _r The impeller generates vibration with certain amplitude in the use process as a piezoelectric vibrator of the ultrasonic transducer, so that the phenomenon of blockage or adhesion of materials at the impeller can not occur.

By combining the examples 1-12 and the comparative examples 1-4 and the tables 1-3, the piezoelectric ceramic material has better piezoelectric performance, and generates vibration with certain amplitude in the using process, so that the material cannot be blocked or adhered at the impeller; in addition, the mechanical property of this application is comparatively, and life is comparatively lasting.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims

1. A fine grader impeller for processing ceramic powder for copper-clad plates is characterized in that: the feed 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 grain size of the piezoelectric ceramic grains is controlled to be 40-60 meshes; the piezoelectric ceramic powder is prepared by a hydrothermal synthesis method, and the expression is Pb (1-x) SmxZryTi (1-y) O3, wherein x = 0-0.05, y = 0.46-0.48; the D50 of the piezoelectric ceramic powder is controlled to be 0.2-16 mu m.

2. The impeller of the fine classifier for processing the ceramic powder for the copper-clad plate according to claim 1, which is characterized in that: the expression of the piezoelectric ceramic powder is Pb (1-x) SmxZr0.52Ti0.48O3, and x =0,0.01,0.02,0.03,0.04,0.05; the grain diameter D50 of the piezoelectric ceramic powder is controlled to be 0.5-4.8 mu m.

3. The impeller of the fine classifier for processing the ceramic powder for the copper-clad plate according to claim 2, which is characterized in that: 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: respectively measuring a titanium tetrachloride aqueous solution, a zirconium oxychloride aqueous solution and a lead nitrate aqueous solution which are prepared in S1.1 according to the stoichiometric ratio of Pb (1-x) SmxZr0.52Ti0.48O3, then 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 kettle at 50-70 ℃, dropwise adding a lead nitrate aqueous solution at 0.1-0.2g/min under the stirring condition of 1200-1500r/min, then stirring for 10-20min, adding ammonia water with the concentration of 25% to adjust the pH value of the solution to be 8-10, and obtaining a mixed solution;

s1.5, mixing 99.5-100% of PZT piezoelectric ceramic powder and 0-0.05% of samarium carbonate, calcining, grinding and screening to obtain Pb1-xSmxZr0.52Ti0.48O3 piezoelectric ceramic powder;

and S3, granulating, namely adding a second binder PVA solution with the concentration of 3-5wt% into the piezoelectric ceramic powder in the S2, wherein the using amount 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 granules into large blocks, standing the large blocks for 24h, crushing the large blocks into powder, granulating for the second time, and sieving to obtain the ceramic granules with good fluidity.

4. The impeller of the fine classifier for processing the ceramic powder for the copper-clad plate according to claim 1, which is characterized in that: the expression of the piezoelectric ceramic powder is Pb (1-x) SmxZr0.52Ti0.48O3, and x =0.02.

5. The impeller of the micro-classifier for processing the ceramic powder for copper-clad plates according to claim 4, which is characterized in that: 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 time of that of the piezoelectric ceramic powder; the mass of the functional short fiber is 0.002-0.01 times of that of the piezoelectric ceramic powder; the functional crystal whisker is 0.001-0.004 times of the piezoelectric ceramic powder by mass; 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 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 the diluent solvent, uniformly stirring, finally adding the diethylenetriamine, and uniformly stirring to obtain the finished product of the second binder.

6. The impeller of the micro-classifier for processing the ceramic powder for the copper-clad plate according to claim 5, wherein: the functional powder is one or a combination of more of silicon nitride powder, cubic boron nitride powder, zirconia and any one of mixed powder of calcium oxide, cerium oxide, magnesium oxide and yttrium oxide; the D50 of the functional powder is 1-5 microns; the functional short fiber is one or a combination of more of silicon nitride fiber, alumina 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.

7. The impeller of the micro-classifier for processing the ceramic powder for copper-clad plates according to claim 5, which is characterized in that: 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, preparing a composition; the functional crystal whisker is prepared from silicon nitride crystal whisker, potassium titanate crystal whisker and zinc oxide crystal whisker in a mass ratio of 1: (0.2-0.8): 1.

8. The impeller of the micro-classifier for processing the ceramic powder for copper-clad plates according to claim 1, which is characterized in that: the first binder is mainly prepared from main components, injection-molded polyolefin PP, a compatilizer EVA, a lubricant, a dispersant and an antioxidant; the main component is copolyformaldehyde POM with the number average molecular weight of 2-4 ten thousand; the lubricant is a CBT resin polymer with a hyperbranched structure; the preparation method of the first binder comprises the steps of mixing the main component, the polyolefin PP, the compatilizer EVA, the lubricant, the dispersant and the antioxidant at 0-4 ℃ and 300-400rpm for 10-15min to obtain the finished product of the first binder.

9. A method for manufacturing an impeller of a fine classifier according to any one of claims 1 to 8, characterized in that: the method comprises the following steps:

s1, preparing piezoelectric ceramic powder;

10. The manufacturing method of the impeller of the micro-classifier for processing the ceramic powder for the copper-clad plate according to claim 9, which is characterized in that: and S4, press forming: performing compression molding by a hydraulic powder molding machine, wherein the pressure is set to be 180Mpa, and the compression time is set to be 360s, so as to obtain a green body impeller; and (3) glue discharging and sintering: heating the green impeller to 540 ℃ at a speed of 0.2 ℃/min, preserving heat for 3h, removing the binder, sealing and embedding the powder in a crucible for sintering, heating to 1280 ℃ at a speed of 0.5 ℃/min, preserving heat for 125min, cooling to 650 ℃ at a speed of 2.0-2.5 ℃/min, opening the furnace, and naturally cooling to obtain the piezoelectric ceramic impeller.