CN114773094A - Lead-free piezoelectric ceramic atomizing sheet for respirator and preparation method and application thereof - Google Patents
Lead-free piezoelectric ceramic atomizing sheet for respirator and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000010410 layer Substances 0.000 claims abstract description 95
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052709 silver Inorganic materials 0.000 claims abstract description 74
- 239000004332 silver Substances 0.000 claims abstract description 74
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
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- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
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- 238000000576 coating method Methods 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 15
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 12
- 235000019353 potassium silicate Nutrition 0.000 claims description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
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- 239000003595 mist Substances 0.000 claims description 8
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- 238000005507 spraying Methods 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 229910001940 europium oxide Inorganic materials 0.000 claims description 6
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 5
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 5
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- 238000009777 vacuum freeze-drying Methods 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
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- 239000000463 material Substances 0.000 claims description 4
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- 238000000465 moulding Methods 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000006199 nebulizer Substances 0.000 claims 1
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 238000000889 atomisation Methods 0.000 description 18
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- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 2
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a lead-free piezoelectric ceramic atomizing sheet for a respirator, a preparation method and an application thereof, wherein the lead-free piezoelectric ceramic atomizing sheet for the respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, and a carbon nanotube layer and a protective layer are sequentially coated outside the silver electrode layer; the protective layer comprises the following raw materials in parts by weight: 20-28 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 5-8 parts of LDHs nano particles, 6-11 parts of diatomite, 1-1.5 parts of nano titanium dioxide, 10-15 parts of binder, 0.5-0.8 part of auxiliary agent and 20-50 parts of water. According to the lead-free piezoelectric ceramic atomizing sheet, the carbon nanotube layer and the protective layer are arranged outside the silver electrode layer of the lead-free piezoelectric ceramic sheet, so that the service life of the lead-free piezoelectric ceramic atomizing sheet can be obviously prolonged, and the lead-free piezoelectric ceramic atomizing sheet is excellent in comprehensive performance.
Description
Technical Field
The invention relates to the technical field of atomization sheets, in particular to a lead-free piezoelectric ceramic atomization sheet for a respirator and a preparation method and application thereof.
Background
The aerosol inhalation is a direct administration method taking respiratory tract and lung as target organs, has the advantages of quick response, high local drug concentration, small dosage, convenient application, less systemic adverse reaction and the like, and has been used as an important treatment means for diseases related to the respiratory system. At present, in some ventilators, an aerosol inhalation device is used for realizing aerosol inhalation of a patient, converting a medicine into an aerosol form, and inhaling the medicine through an oral cavity or a nasal cavity. The atomization inhalation device contains a piezoelectric ceramic atomization sheet.
The piezoelectric ceramic is a functional ceramic material for realizing the interconversion of mechanical energy and electric energy, and has the common performance of ferroelectric ceramic and unique piezoelectric performance. The piezoelectric ceramic material has the characteristics of unique piezoelectric property, excellent electromechanical coupling property, dielectric property and elastic property, simple preparation process, small volume, no electromagnetic interference, low cost and the like, so the piezoelectric ceramic material is widely applied to the high and new technical fields of spaceflight, information, biology, precision instruments and the like and industrial production.
The piezoelectric atomization sheet used at present is made of lead zirconate titanate based piezoelectric material. In the lead zirconate titanate material, lead element accounts for about 70 percent of the total weight of the material, and the ceramic material can cause serious damage to human health and ecological environment in the processes of production, use and waste treatment. Especially when the air purifier is applied to a breathing machine, the damage to the human health is more easily caused. Therefore, lead-free piezoelectric ceramic atomizing sheets are increasingly used in most devices.
However, in the existing lead-free piezoelectric ceramic atomizing sheet, silver is coated by adopting a high-temperature silver-firing process, but the obtained silver layer is easy to generate silver ion migration and oxidation under the environments of long-time high humidity, direct-current electric field and the like, and after the lead-free piezoelectric ceramic atomizing sheet is used for a period of time, the performance of the lead-free piezoelectric ceramic atomizing sheet is increasingly poor, so that the service life of the atomizing sheet is obviously reduced.
Disclosure of Invention
The invention aims to provide a lead-free piezoelectric ceramic atomization sheet for a respirator as well as a preparation method and application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a lead-free piezoelectric ceramic atomizing sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, wherein a carbon nanotube layer and a protective layer are sequentially covered outside the silver electrode layer;
the protective layer comprises the following raw materials in parts by weight: 20-28 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 5-8 parts of LDHs nano particles, 6-11 parts of diatomite, 1-1.5 parts of nano titanium dioxide, 10-15 parts of binder, 0.5-0.8 part of auxiliary agent and 20-50 parts of water.
Preferably, the neodymium oxide/Mg/Al (CO)3) The LDHs nano-particles are prepared by the following method: adding nano neodymium oxide into water, stirring uniformly, then adding ethanol, and stirring to obtain a mixed solution; then adding Mg/Al (CO) into the mixed solution3) Grinding LDHs nano particles in a grinding machine, performing vacuum freeze drying on the ground mixture, and then grinding and sieving to obtain neodymium oxide/Mg/Al (CO)3) -LDHs nanoparticles.
Preferably, the nano neodymium oxide, water, ethanol, Mg/Al (CO)3) The mass ratio of the-LDHs nano particles is 1:5-8:3-5: 35-55. Mg/Al (CO) in the invention3) Use of LDHs document Mg/Al (CO)3) The preparation method in the research on mechanical properties of LDHs/cellulose aerogel.
Preferably, the particle size D50 of the silicon dioxide is 1-10 μm; the binder is water glass, the modulus of the water glass is 2.7-2.9, and the concentration of the water glass is 20-25 Baume degrees; the auxiliary agent comprises a dispersant which is an aqueous sodium polyacrylate dispersant.
As a general inventive concept, the present invention also provides a method for preparing a lead-free piezoelectric ceramic atomizing sheet for a respirator, comprising the steps of:
(1) preparing a leadless piezoelectric ceramic plate;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the leadless piezoelectric ceramic chip treated in the step (2), preserving heat for 10-20min at 700-750 ℃, and then cooling to room temperature to obtain the leadless piezoelectric ceramic chip coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in an oven with the temperature of 80-90 ℃ for baking for 40-60min to form a carbon nanotube layer outside the silver electrode layer;
(5) coating a protective layer coating outside the carbon nano tube layer to form a protective layer, and placing the protective layer in an oven at 100-105 ℃ for 8-15 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Preferably, in the step (1), the lead-free piezoelectric ceramic sheet comprises the following raw materials by weight: 10-15 parts of bismuth oxide, 4-6 parts of titanium dioxide, 1.5-2.5 parts of strontium carbonate, 1-2 parts of vanadium pentoxide, 0.8-1.1 parts of europium oxide and 0.5-0.8 part of lanthanum oxide;
preferably, the lead-free piezoelectric ceramic sheet is prepared by the following method: weighing the raw materials according to the proportion, ball-milling by adopting a wet method, uniformly mixing, drying, and presintering at 820-880 ℃ for 1.5-2h to obtain presintering powder; and grinding and sieving the pre-sintered powder, adding an adhesive for granulation, pressing and molding the obtained granules, removing the adhesive from the obtained blank, sintering at the high temperature of 1200-1250 ℃ for 2-3.5h, and cooling to room temperature to obtain the lead-free piezoelectric ceramic plate.
Preferably, the protective layer coating is prepared by the following method: weighing the raw materials according to the formula; mixing neodymium oxide/Mg/Al (CO)3) Putting the LDHs nano particles and the nano titanium dioxide into water, then carrying out ultrasonic dispersion for 15-30min while stirring, adding the rest raw materials, and carrying out ultrasonic dispersion for 30-45min while continuously stirring to obtain the protective layer coating.
Preferably, in the step (4), the concentration of the carbon nanotube solution is 1-1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m.
As a general inventive concept, the invention also provides an application, in particular to an application of the lead-free piezoelectric ceramic atomizing sheet for the respirator in a transducer and a transformer.
The invention has the technical effects that:
1. according to the invention, the carbon nanotube layer is arranged outside the silver electrode layer of the lead-free piezoelectric ceramic sheet, the carbon nanotube layer has excellent conductivity, and the carbon nanotubes can fill the pores among the metal silver layer particles and enhance the compactness of the metal silver layer particles, so that the conductivity of the conductive layer can be enhanced, and meanwhile, the carbon nanotubes can form a protective layer on the silver electrode layer to reduce silver ion migration and oxidation, thereby effectively prolonging the service life of the conductive layer and further prolonging the service life of the lead-free piezoelectric ceramic atomizing sheet.
2. The invention arranges a protective layer on the carbon nano tube layer, adopts silicon dioxide as a main substrate, and adds neodymium oxide/Mg/Al (CO)3) the-LDHs nano particles have good reinforcing effect on the protective layer and improve the corrosion resistance of the protective layer. Adopts nano neodymium oxide and Mg/Al (CO)3) The LDHs nano particles are compounded, so that the two particles have good dispersion performance in the protective layer and are not easy to agglomerate, and the reinforcing effect is optimal.
The protective layer provided by the invention has the advantages that the raw materials are reasonably matched, a stable protective layer coating can be formed without high-temperature treatment, the overall strength is high, the corrosion resistance is good, and the adhesive force is strong. The carbon nano tube layer can be further well protected, and the service life of the lead-free piezoelectric ceramic atomizing sheet is further prolonged.
3. When the lead-free piezoelectric ceramic sheet is prepared, europium oxide and lanthanum oxide are added into the raw materials, so that the growth of crystal grains can be promoted, the internal structure of the ceramic sheet is uniform, and the prepared piezoelectric ceramic has excellent high piezoelectric constant, electromechanical coupling coefficient and dielectric constant and excellent performance by matching with other raw materials, so that the quality of an atomizing sheet is improved.
4. The lead-free piezoelectric ceramic atomizing sheet prepared by the invention not only has good application effect in a respirator, but also can be applied to various transducers and transformers.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1:
the protective layer coating comprises the following raw materials in parts by weight: 25 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 8 parts of LDHs nano particles, 7 parts of diatomite, 1.2 parts of nano titanium dioxide, 12 parts of water glass, 0.5 part of water-based polyacrylic acid sodium salt dispersing agent and 30 parts of water.
The above-mentioned neodymium oxide/Mg/Al (CO)3) The LDHs nano-particles are prepared by the following method: adding nano neodymium oxide into water, stirring uniformly, then adding ethanol, and stirring to obtain a mixed solution; then adding Mg/Al (CO) into the mixed solution3) Grinding LDHs nano particles in a grinding machine, performing vacuum freeze drying on the ground mixture, and then grinding and sieving to obtain neodymium oxide/Mg/Al (CO)3) -LDHs nanoparticles.
Wherein, the nanometer neodymium oxide, water, ethanol, Mg/Al (CO)3) The mass ratio of the-LDHs nanoparticles is 1:8:3: 45. The particle size D50 of the silicon dioxide is 6 μm; the modulus of the water glass is 2.9, and the concentration is 25 Baume degrees.
The protective layer coating is prepared by the following method: weighing the raw materials according to a formula; mixing neodymium oxide/Mg/Al (CO)3) Putting the LDHs nano particles and the nano titanium dioxide into water, then carrying out ultrasonic dispersion for 30min while stirring, adding the rest raw materials, and carrying out ultrasonic dispersion for 45min while continuously stirring to obtain the protective layer coating.
Example 2:
the protective layer coating comprises the following raw materials in parts by weight: 28 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 7 parts of LDHs nano particles, 11 parts of diatomite, 1 part of nano titanium dioxide, 10 parts of water glass and water-based polypropylene0.5 part of acid sodium salt dispersant and 50 parts of water.
The above-mentioned neodymium oxide/Mg/Al (CO)3) The LDHs nano-particles are prepared by the following method: adding nano neodymium oxide into water, stirring uniformly, then adding ethanol, and stirring to obtain a mixed solution; then adding Mg/Al (CO) into the mixed solution3) The LDHs nano particles are ground in a grinding machine, the mixture obtained by grinding is subjected to vacuum freeze drying, and then grinding and sieving are carried out, thus obtaining the neodymium oxide/Mg/Al (CO)3) -LDHs nanoparticles.
Wherein, the nanometer neodymium oxide, water, ethanol,/Mg/Al (CO)3) The mass ratio of the-LDHs nanoparticles is 1:5:5: 35. The particle size D50 of the silicon dioxide is 10 μm; the modulus of the water glass is 2.7, and the concentration is 20 Baume degrees.
The protective layer coating is prepared by the following method: weighing the raw materials according to a formula; mixing neodymium oxide/Mg/Al (CO)3) Putting LDHs nano particles and nano titanium dioxide into water, stirring and ultrasonically dispersing for 15min, adding the rest raw materials, and continuously stirring and ultrasonically dispersing for 40min to obtain the protective layer coating.
Example 3:
the protective layer coating comprises the following raw materials in parts by weight: 20 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 5 parts of LDHs nano particles, 6 parts of diatomite, 1.5 parts of nano titanium dioxide, 15 parts of water glass, 0.8 part of water-based polyacrylic acid sodium salt dispersing agent and 20 parts of water.
The above-mentioned neodymium oxide/Mg/Al (CO)3) The LDHs nano-particles are prepared by the following method: adding nano neodymium oxide into water, stirring uniformly, then adding ethanol, and stirring to obtain a mixed solution; then adding Mg/Al (CO) into the mixed solution3) Grinding LDHs nano particles in a grinding machine, performing vacuum freeze drying on the ground mixture, and then grinding and sieving to obtain neodymium oxide/Mg/Al (CO)3) -LDHs nanoparticles.
Wherein, the nanometer neodymium oxide, water, ethanol, Mg/Al (CO)3) The mass ratio of the-LDHs nanoparticles is 1:6:4: 55. The particle size D50 of the silicon dioxide is 1 μm; the modulus of the water glass is 2.8, and the concentration is 23 Baume degrees.
The protective layer coating is prepared by the following method: weighing the raw materials according to a formula; mixing neodymium oxide/Mg/Al (CO)3) Putting the LDHs nano particles and the nano titanium dioxide into water, then carrying out ultrasonic dispersion for 20min while stirring, adding the rest raw materials, and carrying out ultrasonic dispersion for 30min while continuously stirring to obtain the protective layer coating.
Example 4:
the lead-free piezoelectric ceramic sheet comprises the following raw materials in parts by weight: 13 parts of bismuth oxide, 6 parts of titanium dioxide, 2.5 parts of strontium carbonate, 1.5 parts of vanadium pentoxide, 1 part of europium oxide and 0.6 part of lanthanum oxide.
The lead-free piezoelectric ceramic sheet is prepared by the following method: weighing the raw materials according to the proportion, ball-milling by adopting a wet method, uniformly mixing, drying, and presintering at 850 ℃ for 2h to obtain presintering powder; and grinding and sieving the pre-sintered powder, adding a proper amount of 7 mass percent polyvinyl alcohol solution for granulation, performing compression molding on the obtained granules, performing degumming treatment on the obtained blank, performing high-temperature sintering at 1230 ℃ for 3.5 hours, and cooling to room temperature to obtain the lead-free piezoelectric ceramic wafer.
Example 5:
the lead-free piezoelectric ceramic sheet comprises the following raw materials in parts by weight: 10 parts of bismuth oxide, 4 parts of titanium dioxide, 2 parts of strontium carbonate, 2 parts of vanadium pentoxide, 0.8 part of europium oxide and 0.5 part of lanthanum oxide.
The lead-free piezoelectric ceramic sheet is prepared by the following method: weighing the raw materials according to the proportion, ball-milling by adopting a wet method, uniformly mixing, drying, and presintering at 820 ℃ for 2h to obtain presintering powder; and grinding and sieving the pre-sintered powder, adding a proper amount of 7 mass percent polyvinyl alcohol solution for granulation, pressing and forming the obtained granules, removing the glue from the obtained blank, sintering at a high temperature of 1200 ℃ for 2 hours, and cooling to room temperature to obtain the lead-free piezoelectric ceramic chip.
Example 6:
the lead-free piezoelectric ceramic sheet comprises the following raw materials in parts by weight: 15 parts of bismuth oxide, 5.5 parts of titanium dioxide, 1.5 parts of strontium carbonate, 1 part of vanadium pentoxide, 1.1 parts of europium oxide and 0.8 part of lanthanum oxide.
The lead-free piezoelectric ceramic sheet is prepared by the following method: weighing the raw materials according to the proportion, ball-milling by adopting a wet method, uniformly mixing, drying, and presintering at 880 ℃ for 1.5 hours to obtain presintering powder; and grinding and sieving the pre-sintered powder, adding a proper amount of 7 mass percent polyvinyl alcohol solution for granulation, pressing and forming the obtained granules, removing the glue from the obtained blank, sintering at a high temperature of 1250 ℃ for 2-3 hours, and cooling to room temperature to obtain the lead-free piezoelectric ceramic chip.
Example 7:
a lead-free piezoelectric ceramic atomizing sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, wherein a carbon nanotube layer and a protective layer are sequentially covered outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 5;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surfaces (upper and lower surfaces) of the lead-free piezoelectric ceramic chip treated in the step (2), preserving heat for 16min at 730 ℃, and cooling to room temperature to obtain the lead-free piezoelectric ceramic chip with the surface coated with the silver electrode layer;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a baking oven at 90 ℃ for baking for 45min to form a carbon nanotube layer outside the silver electrode layer;
wherein, the concentration of the carbon nano tube solution is 1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m;
(5) coating the protective layer coating prepared by the method in the embodiment 1 outside the carbon nano tube layer to form a protective layer, and placing the protective layer in a drying oven at 105 ℃ for 8 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Example 8:
a leadless piezoelectric ceramic atomization piece for a respirator comprises a leadless piezoelectric ceramic piece and a silver electrode layer arranged on the surface of the leadless piezoelectric ceramic piece, wherein a carbon nanotube layer and a protective layer are sequentially coated outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in the embodiment 4;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic chip treated in the step (2), preserving heat for 20min at 700 ℃, and cooling to room temperature to obtain the lead-free piezoelectric ceramic chip with the surface coated with the silver electrode layer;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in an oven at 80 ℃ for baking for 60min to form a carbon nanotube layer outside the silver electrode layer;
wherein, the concentration of the carbon nano tube solution is 1mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m;
(5) coating the protective layer coating prepared by the method in the embodiment 2 outside the carbon nano tube layer to form a protective layer, and placing the protective layer in a drying oven at 100 ℃ for 15 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Example 9:
a leadless piezoelectric ceramic atomization piece for a respirator comprises a leadless piezoelectric ceramic piece and a silver electrode layer arranged on the surface of the leadless piezoelectric ceramic piece, wherein a carbon nanotube layer and a protective layer are sequentially coated outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 6;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), preserving heat for 10min at 750 ℃, and then cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a baking oven at 90 ℃ for baking for 40min to form a carbon nanotube layer outside the silver electrode layer;
wherein the concentration of the carbon nano tube solution is 1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m;
(5) coating the protective layer coating prepared by the method in the embodiment 3 outside the carbon nano tube layer to form a protective layer, and placing the protective layer in a drying oven at 105 ℃ for 10 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet with a stainless steel diaphragm with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Example 10:
a lead-free piezoelectric ceramic atomizing sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, wherein a carbon nanotube layer and a protective layer are sequentially covered outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 6;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), then preserving heat for 10min at 700 ℃, and then cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a baking oven at 90 ℃ for baking for 40min to form a carbon nanotube layer outside the silver electrode layer;
wherein the concentration of the carbon nano tube solution is 1.3mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m.
(5) Coating the protective layer coating prepared by the method in the embodiment 2 outside the carbon nano tube layer to form a protective layer, and placing the protective layer in a drying oven at 100 ℃ for 13 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Example 11:
a lead-free piezoelectric ceramic atomizing sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, wherein a carbon nanotube layer and a protective layer are sequentially covered outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in embodiment 4;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), then preserving heat for 20min at 700 ℃, and then cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a baking oven at 90 ℃ for baking for 45min to form a carbon nanotube layer outside the silver electrode layer;
wherein, the concentration of the carbon nano tube solution is 1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m.
(5) Coating the protective layer coating prepared by the method in the embodiment 1 outside the carbon nano tube layer to form a protective layer, and placing the protective layer in a drying oven at 105 ℃ for 10 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Comparative example 1:
a leadless piezoelectric ceramic atomization piece for a respirator comprises a leadless piezoelectric ceramic piece and a silver electrode layer arranged on the surface of the leadless piezoelectric ceramic piece, wherein a protective layer is coated outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 6;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), preserving heat at 750 ℃ for 10min, and cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) coating the protective layer coating prepared by the method in the embodiment 3 outside the silver electrode layer to form a protective layer, and placing the protective layer in a drying oven at 105 ℃ for 10 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(5) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet with a stainless steel diaphragm with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
Comparative example 2:
a leadless piezoelectric ceramic atomization piece for a respirator comprises a leadless piezoelectric ceramic piece and a silver electrode layer arranged on the surface of the leadless piezoelectric ceramic piece, wherein a carbon nanotube layer is sequentially coated outside the silver electrode layer.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 6;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), preserving heat at 750 ℃ for 10min, and cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a baking oven at 90 ℃ for baking for 40min to form a carbon nanotube layer outside the silver electrode layer;
wherein, the concentration of the carbon nano tube solution is 1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m;
(5) and (3) carrying out electrode treatment, and then bonding the bottom surface of the electrode with a stainless steel membrane with a fog outlet hole to prepare the lead-free piezoelectric ceramic atomization sheet.
Comparative example 3:
a lead-free piezoelectric ceramic atomization sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet.
The preparation method comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet by the method in example 6;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), preserving heat at 750 ℃ for 10min, and cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) and (3) carrying out electrode treatment, and then bonding the bottom surface of the electrode with a stainless steel membrane with a fog outlet hole to prepare the lead-free piezoelectric ceramic atomization sheet.
And (3) performance testing:
(1) by the production methods in examples 7 to 11 and comparative examples 1 to 2, a lead-free piezoelectric ceramic atomizing sheet having a ring-shaped diameter was produced, the lead-free piezoelectric ceramic sheet having an outer diameter of 15mm and an inner diameter of 6 mm. And carrying out a salt spray test on the piezoelectric ceramic atomization sheet, and detecting the service life. The results of the tests and experiments are shown in table 1.
Table 1:
as can be seen from Table 2, the carbon nanotube layer and the protective layer are arranged outside the silver electrode layer of the lead-free piezoelectric ceramic plate, so that the service life of the lead-free piezoelectric ceramic atomization plate can be obviously prolonged, and the protective layer is arranged, so that the lead-free piezoelectric ceramic atomization plate has a more obvious effect on improving the corrosion resistance of the piezoelectric ceramic atomization plate.
(2) The lead-free piezoelectric ceramics prepared by the methods in the embodiments 4 to 6 are tested for the piezoelectric constant, the electromechanical coupling coefficient and the dielectric constant, and the detection standard of the piezoelectric constant is GB/T11309-1989; the detection standard of the electromechanical coupling coefficient is GB/T11312-1989; the detection standard of the dielectric constant is GB/T3389-2008. Specific detection results are shown in table 2.
Table 2:
| piezoelectric constant d33(Pc/N) | Coefficient of electromechanical coupling | Dielectric constant | |
| Example 4 | 406 | 0.81 | 2790 |
| Example 5 | 412 | 0.83 | 2680 |
| Example 6 | 399 | 0.75 | 2730 |
As can be seen from Table 2, the lead-free piezoelectric ceramic prepared by the invention has high values of high piezoelectric constant, electromechanical coupling coefficient and dielectric constant, and excellent performance.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A lead-free piezoelectric ceramic atomizing sheet for a respirator comprises a lead-free piezoelectric ceramic sheet and a silver electrode layer arranged on the surface of the lead-free piezoelectric ceramic sheet, and is characterized in that a carbon nanotube layer and a protective layer are sequentially covered outside the silver electrode layer;
the protective layer comprises the following raw materials in parts by weight: 20-28 parts of silicon dioxide, neodymium oxide/Mg/Al (CO)3) 5-8 parts of LDHs nano particles, 6-11 parts of diatomite, 1-1.5 parts of nano titanium dioxide, 10-15 parts of binder, 0.5-0.8 part of auxiliary agent and 20-50 parts of water.
2. The lead-free piezoelectric ceramic atomizing sheet for respirators according to claim 1, wherein the neodymium oxide/Mg/Al (CO)3) The LDHs nano particles are prepared by the following method: adding nano neodymium oxide into water, stirring uniformly, then adding ethanol, and stirring to obtain a mixed solution; then adding Mg/Al (CO) into the mixed solution3) The LDHs nano particles are ground in a grinding machine, the mixture obtained by grinding is subjected to vacuum freeze drying, and then grinding and sieving are carried out, thus obtaining the neodymium oxide/Mg/Al (CO)3) -nanoparticles of LDHs.
3. The lead-free piezoelectric ceramic atomizing sheet for respirator as set forth in claim 2, wherein the atomizing sheet is made of a material having a specific compositionThe nano neodymium oxide, water, ethanol, Mg/Al (CO)3) The mass ratio of the-LDHs nano particles is 1:5-8:3-5: 35-55.
4. The lead-free piezoelectric ceramic atomizing sheet for a respirator according to claim 2, characterized in that the particle diameter D50 of the silicon dioxide is 1 to 10 μm; the binder is water glass, the modulus of the water glass is 2.7-2.9, and the concentration is 20-25 Baume degrees; the auxiliary agent comprises a dispersant which is an aqueous sodium polyacrylate dispersant.
5. A method for preparing the lead-free piezoelectric ceramic atomizing sheet for the respirator according to any one of claims 1 to 4, which comprises the following steps:
(1) preparing a lead-free piezoelectric ceramic sheet;
(2) cleaning and drying the lead-free piezoelectric ceramic plate;
(3) coating silver paste on the surface of the lead-free piezoelectric ceramic piece treated in the step (2), then preserving heat for 10-20min at the temperature of 700-750 ℃, and then cooling to room temperature to obtain the lead-free piezoelectric ceramic piece coated with the silver electrode layer on the surface;
(4) spraying a carbon nanotube solution on the silver electrode layer, and then placing the silver electrode layer in a drying oven at 80-90 ℃ to bake for 40-60min to form a carbon nanotube layer outside the silver electrode layer;
(5) coating a protective layer coating outside the carbon nano tube layer to form a protective layer, and placing the protective layer in an oven at 100-105 ℃ for 8-15 hours to obtain a lead-free piezoelectric ceramic atomizing sheet primary product;
(6) and (3) treating the primary lead-free piezoelectric ceramic atomizing sheet product by using an electrode, and then bonding the bottom surface of the primary lead-free piezoelectric ceramic atomizing sheet product with a stainless steel membrane with a mist outlet hole to prepare the lead-free piezoelectric ceramic atomizing sheet.
6. The manufacturing method according to claim 5, wherein in the step (1), the lead-free piezoelectric ceramic sheet comprises the following raw materials in parts by weight: 10-15 parts of bismuth oxide, 4-6 parts of titanium dioxide, 1.5-2.5 parts of strontium carbonate, 1-2 parts of vanadium pentoxide, 0.8-1.1 parts of europium oxide and 0.5-0.8 part of lanthanum oxide.
7. The manufacturing method according to claim 6, wherein the lead-free piezoelectric ceramic sheet is manufactured by the following method: weighing the raw materials according to the proportion, ball-milling by adopting a wet method, uniformly mixing, drying, and presintering at 820-880 ℃ for 1.5-2h to obtain presintering powder; grinding and sieving the pre-sintered powder, adding an adhesive for granulation, pressing and molding the obtained granules, carrying out glue removal treatment on the obtained blank, then carrying out high-temperature sintering at the high-temperature sintering temperature of 1200-1250 ℃ for 2-3.5h, and cooling to room temperature to obtain the lead-free piezoelectric ceramic plate.
8. The production method according to any one of claims 5 to 7, wherein the protective layer coating is produced by: weighing the raw materials according to a formula; mixing neodymium oxide/Mg/Al (CO)3) Putting LDHs nano particles and nano titanium dioxide into water, stirring and ultrasonically dispersing for 15-30min, adding the rest raw materials, and continuously stirring and ultrasonically dispersing for 30-45min to obtain the protective layer coating.
9. The method for preparing the lead-free piezoelectric ceramic atomizing sheet for the respirator according to any one of claims 5 to 7, characterized in that in the step (4), the concentration of the carbon nanotube solution is 1 to 1.5mg/ml, and the used solvent is water; the diameter of the carbon nano tube is 5-50nm, and the length of the carbon nano tube is 2-50 mu m.
10. Use of a lead-free piezoceramic nebulizer of any one of claims 1-4 in a transducer, transformer or the like.
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Denomination of invention: A lead-free piezoelectric ceramic nebulizer for ventilators and its preparation method and application Effective date of registration: 20231212 Granted publication date: 20221213 Pledgee: Industrial and Commercial Bank of China Limited Xinhua Branch Pledgor: HUNAN MEICHENG CERAMIC TECHNOLOGY Co.,Ltd. Registration number: Y2023980071037 |