WO2020029530A1 - Procédé de préparation de céramique de zircone et de matériau composite - Google Patents

Procédé de préparation de céramique de zircone et de matériau composite Download PDF

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WO2020029530A1
WO2020029530A1 PCT/CN2018/124712 CN2018124712W WO2020029530A1 WO 2020029530 A1 WO2020029530 A1 WO 2020029530A1 CN 2018124712 W CN2018124712 W CN 2018124712W WO 2020029530 A1 WO2020029530 A1 WO 2020029530A1
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powder
ceramic
zirconia
hole structure
preparation
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PCT/CN2018/124712
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Chinese (zh)
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夏庆路
孔德洲
张子会
俞胜平
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歌尔股份有限公司
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Definitions

  • the invention relates to the technical field of material preparation, and more particularly, to a method for preparing a zirconia ceramic and a composite material.
  • Zirconia ceramic is a modern ceramic material with high hardness, high strength, good appearance effect, good biocompatibility, and certain toughness.
  • the molding methods of zirconia ceramics include, but are not limited to, dry pressing, isostatic pressing, injection molding, cast molding, and gel injection molding. The good performance of zirconia ceramics makes it widely used in many industries.
  • the surface of the zirconia ceramics is relatively smooth, and the surface properties of the zirconia ceramics are relatively stable, which makes the bonding effect worse when bonding with other types of materials.
  • the shear strength of the bonding surface usually does not exceed 30Mpa, and there are higher requirements for the adhesive.
  • the chemical etching method usually uses an etchant to corrode the zirconia ceramic surface.
  • the etchant can destroy the integrity of the grain structure of the zirconia ceramic surface and form a surface with a certain roughness.
  • the chemical properties of zirconia ceramics are very stable and there are very few types of caustic agents available.
  • the pores produced on the surface of the zirconia ceramic after etching are small and the pore depth is small, and the morphology of the pores is not conducive to bonding with other materials.
  • An object of the present invention is to provide a new technical solution for a method for preparing a zirconia ceramic.
  • a method for preparing a zirconia ceramic comprises: mixing a first powder and a second powder, and preparing a ceramic green body with a set shape, the first powder includes yttria-stabilized zirconia powder and yttrium oxide and other At least one of a composite stabilized zirconia powder having an oxide component, the second powder includes at least one of a yttrium oxide stabilized zirconia powder and a composite stabilized zirconia powder containing yttria and other oxide components
  • One type wherein the molar percentage content of yttrium oxide in the first powder is x 1 , and the molar percentage content of yttrium oxide in the second powder is x 2 , x 1 ⁇ x 2 ;
  • the green body is sintered to form a ceramic green body, and the yttrium oxide is not diffused uniformly in the ceramic green body; the ceramic green body is etched to form a hole structure
  • the mass ratio of the first powder and the second powder is y 1 : y 2 , where 2 ⁇ (x 1 * y 1 + x 2 * y 2 ) / (y 1 + y 2 ) ⁇ 4.
  • an average particle diameter of at least one of the first powder and the second powder is 0.2-2 ⁇ m.
  • the sintering temperature is 1300-1500 ° C, and the time is 1-6 hours.
  • the temperature of the heat treatment is 1200-1400 ° C, and the time is 2-10 hours.
  • the ceramic rough body is placed in a mixed solution of a fluoride and an acidic solution for corrosion treatment.
  • the fluoride includes at least one of sodium fluoride, potassium fluoride, and ammonium fluoride; and the acidic solution includes at least one of an oxalic acid solution, a nitric acid solution, and a sulfuric acid solution.
  • the hole structure includes a uniformly distributed first hole structure and a second hole structure, and the first hole structure has a pore diameter of 0.2-0.5 ⁇ m and a depth of 0.2-0.5 ⁇ m;
  • the pore diameter is 0.5-2 ⁇ m, and the depth is 0.1-0.3 ⁇ m.
  • a composite material includes a zirconia ceramic and a polymer material formed by injection molding or melting on a porous surface of the zirconia ceramic, and the zirconia ceramic is prepared according to the preparation method provided by the present invention.
  • the ceramic component with a lower yttrium oxide content has poor corrosion resistance, and the solution is pitted.
  • This part will be corroded to form a small and deep hole structure, that is, the first hole structure.
  • the component with a higher yttrium oxide content has better corrosion resistance and is prone to surface corrosion.
  • the surface layer is poor in corrosion resistance.
  • This part is corroded and peeled off, exposing the part with high yttrium oxide content that is not easily corroded, and becomes a hole The bottom, thereby forming a large and shallow hole structure, that is, a second hole structure.
  • the first hole structure and the second hole structure are evenly distributed on the surface of the ceramic rough, which effectively improves the specific surface area of the ceramic rough and the diversity of the hole structure, and improves the binding force of the zirconia ceramic and the polymer material.
  • FIG. 1 is a flowchart of a method for preparing a zirconia ceramic according to an embodiment of the present invention.
  • FIG. 2 is a surface structure diagram of a zirconia ceramic according to an embodiment of the present invention.
  • any specific value should be construed as exemplary only and not as a limitation. Therefore, other examples of the exemplary embodiments may have different values.
  • FIG. 1 is a flowchart of a method for preparing a zirconia ceramic according to an embodiment of the present invention.
  • FIG. 2 is a surface structure diagram of a zirconia ceramic according to an embodiment of the present invention.
  • the preparation method includes:
  • the first powder and the second powder are mixed and prepared into a ceramic green body of a set shape.
  • the first powder includes yttria-stabilized zirconia powder and a compound containing yttrium oxide and other oxide components.
  • At least one of stabilized zirconia powder, and the second powder includes at least one of yttria-stabilized zirconia powder and composite stabilized zirconia powder containing yttrium oxide and other oxide components, wherein the first The molar percentage content of yttrium oxide in the powder is x 1 , and the molar percentage content of yttrium oxide in the second powder is x 2 , x 1 ⁇ x 2 ;
  • the ceramic green body is sintered to form a ceramic green body, and yttrium oxide is not diffused uniformly in the ceramic green body;
  • the rough ceramic body is etched to form a hole structure on the surface of the rough ceramic body
  • the ceramic rough body after the corrosion treatment is heat-treated to form a ceramic product.
  • the first powder and the second powder may be mixed by means of mechanical stirring, roller ball milling, planetary ball milling, etc. to form a uniform mixed powder.
  • the average particle diameter of at least one of the first powder and the second powder is 0.2-2 ⁇ m.
  • the formed zirconia ceramic has a good sintering effect, high structural strength, and a more delicate ceramic surface.
  • a dispersant can also be added to the two powders.
  • the binder Before preparing the ceramic green body, an aqueous or alcoholic solution of a binder is added to the mixed powder.
  • the binder may be, but is not limited to, at least one of PVA (polyvinyl alcohol), PVB (polyvinyl butyral), and PEG (polyethylene glycol), where PVA and PEG are easily soluble in water, PVB is easily soluble in alcohol.
  • the mass concentration of the binder is 1-3%.
  • Yttrium oxide stabilized zirconia refers to the addition of yttrium oxide to change the phase transition temperature range of zirconia to produce cubic and tetragonal zirconia that are stable at room temperature.
  • Composite stabilized zirconia containing yttrium oxide and other oxide components refers to the addition of yttrium oxide and other oxides to change the phase transition temperature range of zirconia, thereby producing cubic and tetragonal zirconia that are stable at room temperature.
  • the other oxides include at least one of calcium oxide, aluminum oxide, magnesium oxide, and cerium oxide.
  • the molding of the ceramic green body is performed in a molding apparatus.
  • molding is performed by injection molding, extrusion, or the like.
  • Those skilled in the art can prepare the blank into a set shape according to actual needs. Understandably, during the molding process, if glue is added to the billet, the glue should be removed before sintering to prevent the glue from adversely affecting sintering.
  • the ceramic green body is placed in a sintering furnace for sintering. During the sintering process, the ceramic green body becomes dense and obtains preliminary structural strength, thereby forming a ceramic green body.
  • yttrium oxide is doped into the crystal structure of zirconia to change the crystal phase.
  • the process of physical mixing can form a uniformly mixed powder, however, it does not change the crystal structure, that is, components with high yttrium oxide content (for example, concentration x 2 ) and components with low yttrium oxide content (for example, concentration X 1 ).
  • a mass transfer process occurs. With the progress of mass transfer, yttrium oxide gradually becomes uniform in the ceramic body.
  • the ceramic component includes a component with a high yttrium oxide content and a component with a low yttrium oxide content.
  • the sintering temperature is 1300-1500 ° C, and the time is 1-6 hours. Under this condition, the ceramic rough body becomes dense, so that sufficient structural strength is obtained, and sufficient diffusion of yttrium oxide can be effectively avoided.
  • the ceramic rough body is placed in an etching solution to be etched.
  • the ceramic rough body is placed in a mixed solution of a fluoride and an acidic solution for corrosion treatment.
  • Fluoride has a good penetration effect, and can quickly corrode the ceramic rough under the acid environment.
  • the fluoride includes at least one of sodium fluoride, potassium fluoride, and ammonium fluoride.
  • the acidic solution includes at least one of an oxalic acid solution, a nitric acid solution, and a sulfuric acid solution. The stability of the above solution is good, and the fluoride can be quickly dissolved.
  • the total concentration of the fluoride is 50-200 g / L, and the total concentration of the acid is 20-60 g / L.
  • the immersion temperature in the corrosion solution is 50-100 ° C, and the immersion time is 5-30 minutes. Under these reaction conditions, a uniform pore structure can be formed on the surface of the ceramic rough body.
  • the fluoride and the acidic solution are not limited to the above embodiments.
  • the etching solution is not limited to the above embodiments, and those skilled in the art can select according to actual needs.
  • the ceramic component with a lower yttrium oxide content has poor corrosion resistance, and is prone to pitting corrosion.
  • This part will be corroded to form a small and deep hole structure, that is, the first hole structure 11.
  • the component with a higher yttrium oxide content has better corrosion resistance and is prone to surface corrosion.
  • the surface layer is poor in corrosion resistance.
  • This part is corroded and peeled off, exposing the part with high yttrium oxide content that is not easily corroded, and becomes a hole The bottom, thereby forming a large and shallow hole structure, that is, the second hole structure 12.
  • the first hole structure 11 and the second hole structure 12 are evenly distributed on the surface of the ceramic rough, which effectively improves the specific surface area of the ceramic rough and the diversity of the hole structure, as shown in FIG. 2.
  • the yttrium oxide continues to diffuse at a set temperature, so that the yttrium oxide in the ceramic product becomes uniform, and the compactness of the ceramic product is further improved, and the mechanical properties and structural strength are further improved.
  • the temperature of the heat treatment is 1200-1400 ° C, and the time is 2-10 hours.
  • yttrium oxide can be sufficiently diffused, thereby being uniformly dispersed in the zirconia product, and improving the structural strength and mechanical properties of the zirconia ceramic.
  • the concentration range makes the sizes of the first hole structure 11 and the second hole structure 12 more uniform, and forms a micron-sized hole structure.
  • the pore diameter of the first hole structure 11 is 0.2-0.5 ⁇ m and the depth is 0.2-0.5 ⁇ m; the pore diameter of the second hole structure 12 is 0.5-2 ⁇ m and the depth is 0.1-0.3 ⁇ m.
  • This size range makes the binding force of polymer materials and zirconia ceramics stronger.
  • the mass ratio of the first powder and the second powder is y 1 : y 2 , where 2 ⁇ (x 1 * y 1 + x 2 * y 2 ) / (y 1 + y 2 ) ⁇ 4, That is, the arithmetic mean of the yttrium oxide content of the mixed powder is 2-4 mol%. Within this range, micron-sized hole structures can be formed.
  • a composite material includes a zirconia ceramic and a polymer material formed on the porous surface of the zirconia ceramic by injection molding or melting.
  • the zirconia ceramic is prepared according to the preparation method of the present invention.
  • the polymer material can be directly injection-molded onto the surface of the zirconia ceramic by means of insert injection molding, wherein the zirconia ceramic is used as the insert.
  • the polymer material after molding may be partially melted and then adhered to the surface of the zirconia ceramic.
  • the polymer material may be, but is not limited to, plastic, silicone, rubber, and the like.
  • the plastic is one or more of polybutylene terephthalate, polybutylene terephthalate, polyphenylene sulfide or polyamide with good fluidity. The plastic can be quickly filled into the first hole structure 11 and the second hole structure 12 in a molten state.
  • glass fiber can improve the structural strength of plastics, making the bonding force between plastics and ceramic products stronger.

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  • Compositions Of Oxide Ceramics (AREA)

Abstract

La présente invention concerne un procédé de préparation de céramique de zircone et d'un matériau composite. Le procédé de préparation consiste à : mélanger une première poudre et une deuxième poudre et préparer un corps cru en céramique dans une forme définie, la première poudre et la deuxième poudre comprenant au moins l'une parmi une poudre de zircone stabilisée par de l'oxyde d'yttrium et une poudre de zircone composite stabilisée comprenant de l'oxyde d'yttrium et d'autres constituants d'oxyde, la teneur en pourcentage molaire en oxyde d'yttrium dans la première poudre est de x1, la teneur en pourcentage molaire en oxyde d'yttrium dans la deuxième poudre est de x2, x1＜x2 ; fritter le corps cru en céramique pour former une ébauche brute en céramique, l'oxyde d'yttrium n'étant pas diffusé uniformément dans l'ébauche brute en céramique ; soumettre l'ébauche brute en céramique à un traitement de corrosion pour former une structure poreuse dans la surface de l'ébauche brute en céramique ; et soumettre l'ébauche brute en céramique après le traitement de corrosion à un traitement thermique, de façon à former un article en céramique.
PCT/CN2018/124712 2018-08-10 2018-12-28 Procédé de préparation de céramique de zircone et de matériau composite WO2020029530A1 (fr)

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CN201810911063.0 2018-08-10
CN201810911063.0A CN108911744B (zh) 2018-08-10 2018-08-10 氧化锆陶瓷的制备方法以及复合材料

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CN113105234B (zh) * 2021-04-16 2022-08-16 深圳陶陶科技有限公司 氧化锆复合材料、陶瓷产品、制备方法、及其应用

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