WO2017133049A1 - 一种注射成型制备透明陶瓷部件的方法 - Google Patents

一种注射成型制备透明陶瓷部件的方法 Download PDF

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WO2017133049A1
WO2017133049A1 PCT/CN2016/075447 CN2016075447W WO2017133049A1 WO 2017133049 A1 WO2017133049 A1 WO 2017133049A1 CN 2016075447 W CN2016075447 W CN 2016075447W WO 2017133049 A1 WO2017133049 A1 WO 2017133049A1
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ceramic
powder
injection molding
degreasing
ceramic powder
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French (fr)
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刘伟
陈健
周茂鹏
伍海东
伍尚华
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Guangdong University of Technology
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Guangdong University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • 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
    • 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
    • C04B35/10—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 aluminium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina

Definitions

  • the invention relates to the technical field of transparent ceramics preparation, in particular to a method for preparing transparent ceramic parts by injection molding.
  • Transparent ceramic materials have the properties inherent in structural ceramics such as high temperature resistance, corrosion resistance, high strength, high hardness, chemical stability and biocompatibility. They also have functional properties such as light transmission, wave transmission and laser, which are already in energy and machinery. High-tech fields such as military, electronics, semiconductors, and medicine are becoming more and more widely used. Since the 1960s, ceramic materials scientists have done a lot of research and research on the synthesis, sintering, crystal structure, performance, light transmission mechanism and application of transparent ceramic materials. For example, oxide transparent ceramics such as alumina, yttrium aluminum garnet, yttrium oxide, magnesium oxide, magnesium aluminum spinel, and non-oxide transparent ceramics such as aluminum nitride and sialon are studied.
  • transparent ceramic properties such as transparent alumina ceramic discharge tubes in ceramic metal halide lamps, transparent alumina ceramic brackets, transparent zirconia ceramic lenses, Aluminum garnet laser transparent ceramic, transparent ceramic armor and magnesium aluminum spinel ceramic fairing.
  • transparent ceramics often use traditional molding methods, such as dry pressing, grouting, and isostatic pressing. These conventional molding methods are not suitable for preparing high-performance, high-reliability transparent ceramic materials with precise and complex shapes, as currently Oral correction has a good application prospects of transparent alumina brackets, ceramic metal halide lamp discharge tubes.
  • ceramic dry press molding has high efficiency, there is a phenomenon of density difference and uneven microstructure, and it is difficult to form a profiled part.
  • ceramic injection molding can form shaped products, the molded body is prone to problems such as uneven density and composition segregation, low dimensional accuracy and reduced product reliability.
  • Cold isostatic pressing can obtain a high-density and high-uniformity molded body, but it is difficult to form a ceramic component having a complicated shape, and the molding efficiency is low and manual operation is large.
  • An object of the present invention is to provide a method for preparing a transparent ceramic member by injection molding, which avoids the deficiencies of the prior art, and is capable of producing a transparent ceramic member of a net size, high performance, and complicated complex shape.
  • a method of preparing a transparent ceramic component by injection molding comprising the steps of:
  • the ceramic powder having a purity of more than 99.9% and a particle size of submicron is used as a raw material for surface modification.
  • the surface modifier used in the above step (1) is any one of stearic acid, oleic acid or lauryl stearic acid, and the content of the surface modifier is 1.5 to the weight of the ceramic powder. 3%.
  • the surface modifier is mixed with the ceramic powder, and the surface modifier is esterified with the ceramic powder by ball milling to obtain a surface-modified ceramic powder.
  • the ball milling medium is alcohol, and the ball milling time is 3 to 12 hours.
  • the surface-modified ceramic powder and the adhesive dosage system constitute an injection molding mixture
  • the weight percent of the surface-modified ceramic powder accounts for 58 to 65% by weight of the injection molding mixture
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer. In weight percent, polyethylene accounts for 8-20% of the binder system, and polypropylene accounts for 8 ⁇ of the binder system. 20%, paraffin accounted for 54 to 65% of the binder system, stearic acid accounted for 5 to 10% of the binder system, and plasticizers accounted for 4 to 8% of the binder system.
  • the step (2) ceramic injection feeding mixing process specifically comprises:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid are mixed for 30 to 45 minutes, and a plasticizer is added within 3 to 5 minutes before the end of the mixing.
  • the above (4) degreasing the ceramic body is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, specifically comprising:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, and heat preservation for 1.5 to 3 h; Within 3h from 80 ° C to 150 ° C, heat 1.5 ⁇ 3h; then in 4h from 150 ° C to 250 ° C, holding 1.5 ⁇ 3h; then in 4h from 250 ° C to 350 ° C, holding 2.5 ⁇ 3.5h; Then, it is raised from 250 °C to 350 °C in 4h, and it is kept for 2.5-3.5h; then it is raised from 350°C to 450°C in 4h, and it is kept for 2.5-3.5h; finally, it is raised from 450°C to 500°C within 4h, and it is kept at 2.5. ⁇ 3.5h; the entire thermal degreasing process is controlled within 44h.
  • the thermal degreasing process of the above step (4.2) is carried out by a burying method, and the powder used for embedding is any of ⁇ -Al 2 O 3 powder, zirconia powder, ⁇ -Al 2 O 3 powder, and activated carbon powder.
  • the powder used for embedding is any of ⁇ -Al 2 O 3 powder, zirconia powder, ⁇ -Al 2 O 3 powder, and activated carbon powder.
  • the above step (5) is carried out by any one of atmospheric sintering, hot press sintering, or normal pressure sintering, followed by hot isostatic pressing.
  • the method for preparing a transparent ceramic component by injection molding of the invention comprises the following steps: (1) surface modification of the ceramic powder, so that the surface modifier forms a nanometer organic acid coating layer on the surface of the ceramic powder, and the surface is modified. (2) Surface modified ceramic powder and adhesive system Ceramic injection and mixing; (3) injection molding to obtain a ceramic body; (4) degreasing the ceramic body; (5) sintering the degreased ceramic body to obtain a finished transparent ceramic part.
  • the method of the invention can prepare transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • Fig. 1 is a transmission electron micrograph of ceramic particles of a surface-modified alumina ceramic powder in Example 5 of the present invention.
  • Fig. 2 is a graph showing the results of powder Fourier infrared analysis of alumina ceramic powder, surface-modified alumina ceramic powder and hard acid in Example 5 of the present invention.
  • Fig. 3 is a view showing the surface morphology of a scanning electron microscope of the transparent alumina ceramic after sintering in Example 5 of the present invention.
  • Figure 4 is a schematic illustration of a partially complex shaped transparent ceramic component prepared by the method of the present invention in Example 5 of the present invention.
  • a method for preparing a transparent ceramic component by injection molding comprising the following steps:
  • the surface modification of the ceramic powder causes the surface modifier to form a nano-scale organic acid coating on the surface of the ceramic powder to obtain a surface-modified ceramic powder.
  • step (1) the ceramic powder having a purity greater than 99.9% and a particle size of submicron is used as a raw material for surface modification.
  • the surface modifier used in the step (1) is any one of stearic acid, oleic acid or dodecyl stearic acid, and the surface modifier is present in an amount of from 1.5 to 3% by weight based on the weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, and the surface modification agent and the ceramic powder are esterified by ball milling to obtain a surface-modified ceramic powder.
  • the ball milling medium is alcohol, and the ball milling time is 3 to 12 hours.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid coating is formed on the surface of the ceramic by esterification reaction between the surface modifier and the ceramic powder.
  • Floor Unlike the prior art introduction of a surface modifier in the mixing stage, the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 58 to 65% by weight of the injection molding mixture by weight percentage.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer.
  • polyethylene accounts for 8-20% of the binder system
  • polypropylene accounts for 8-20% of the binder system
  • paraffin accounts for 54-65% of the binder system
  • stearic acid accounts for the binder system.
  • 5 to 10% of the plasticizer accounts for 4 to 8% of the binder system.
  • the ceramic body is degreased, and the degreasing may be carried out by thermal degreasing or by a two-step degreasing method.
  • the method of the invention can prepare transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • a method for preparing a transparent ceramic component by injection molding comprising the following steps:
  • the surface modification of the ceramic powder causes the surface modifier to form a nano-scale organic acid coating on the surface of the ceramic powder to obtain a surface-modified ceramic powder.
  • step (1) the ceramic powder having a purity greater than 99.9% and a particle size of submicron is used as a raw material for surface modification.
  • the surface modifier used in the step (1) is any one of stearic acid, oleic acid or dodecyl stearic acid, and the surface modifier is present in an amount of 2% by weight based on the weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, and the surface modification agent and the ceramic powder are esterified by ball milling to obtain a surface-modified ceramic powder.
  • the ball milling medium is alcohol, and the ball milling time is 3 to 12 hours.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid coating is formed on the surface of the ceramic by esterification reaction between the surface modifier and the ceramic powder.
  • Floor Unlike the prior art introduction of a surface modifier in the mixing stage, the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 58 to 65% by weight of the injection molding mixture by weight percentage.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer. In weight percent, polyethylene accounts for 8-20% of the binder system, and polypropylene accounts for 8 ⁇ of the binder system. 20%, paraffin accounted for 54 to 65% of the binder system, stearic acid accounted for 5 to 10% of the binder system, and plasticizers accounted for 4 to 8% of the binder system.
  • the ceramic injection feeding mixing process specifically includes:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid are mixed for 30 to 45 minutes, and a plasticizer is added within 3 to 5 minutes before the end of the mixing.
  • Degreasing is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, including:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, and heat preservation for 1.5 to 3 h; Within 3h from 80 ° C to 150 ° C, heat 1.5 ⁇ 3h; then in 4h from 150 ° C to 250 ° C, holding 1.5 ⁇ 3h; then in 4h from 250 ° C to 350 ° C, holding 2.5 ⁇ 3.5h; Then, it is raised from 250 °C to 350 °C in 4h, and it is kept for 2.5-3.5h; then it is raised from 350°C to 450°C in 4h, and it is kept for 2.5-3.5h; finally, it is raised from 450°C to 500°C within 4h, and it is kept at 2.5. ⁇ 3.5h; the entire thermal degreasing process is controlled within 44h.
  • Step (4.2) The thermal degreasing process may be carried out by a buried powder method, and the powder used for the buried powder is any one of ⁇ -Al 2 O 3 powder, zirconia powder, ⁇ -Al 2 O 3 powder, and activated carbon powder.
  • the embedding method can support the green body, avoiding deformation of the green body under the action of self-weight when the binder softens, and capillary adsorption of the embedding powder on the other side can promote the elimination of the organic binder.
  • the sintering can be carried out by any one of atmospheric sintering, hot press sintering, or normal pressure sintering, followed by hot isostatic pressing.
  • the method for preparing transparent ceramic parts by injection molding according to the invention pre-treats the ceramic powder, then carries out the raw material mixing and injection molding, degreases by a two-step degreasing method, and finally obtains transparent ceramic parts with excellent performance by sintering.
  • the method of the invention is suitable for preparing transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • a method for preparing a transparent ceramic component by injection molding comprising the following steps:
  • the surface modification of the ceramic powder causes the surface modifier to form a nano-scale organic acid coating on the surface of the ceramic powder to obtain a surface-modified ceramic powder.
  • step (1) the ceramic powder having a purity greater than 99.9% and a particle size of submicron is used as a raw material for surface modification.
  • the surface modifier used in the step (1) is stearic acid, and the surface modifier is present in an amount of 2.3% by weight based on the weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, and use alcohol as the ball milling medium. After ball milling for 10 hours, the surface modifier and the ceramic powder are esterified to obtain the surface modified ceramic powder.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid coating layer is formed on the ceramic surface by esterification reaction between the surface modifier and the ceramic powder.
  • the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 60% by weight of the injection molding mixture by weight percent.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer.
  • polyethylene accounts for 10% of the binder system
  • polypropylene accounts for 10% of the binder system
  • Paraffin It accounts for 65% of the binder system
  • stearic acid accounts for 10% of the binder system
  • plasticizer accounts for 5% of the binder system.
  • the ceramic injection feeding mixing process specifically includes:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid were mixed for 30 minutes, and a plasticizer was added within 5 minutes before the end of the mixing.
  • Degreasing is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, including:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, heat preservation for 2 h; then within 3 h Increasing from 80 ° C to 150 ° C, holding for 2 h; then rising from 150 ° C to 250 ° C in 4 h, holding for 2 h; then rising from 250 ° C to 350 ° C in 4 h, holding for 3 h; then rising from 250 ° C in 4 h 350 ° C, holding 3h; then rising from 350 ° C to 450 ° C in 4h, holding 3h; finally in 4h from 450 ° C to 500 ° C, holding 3h; the entire thermal degreasing process is controlled within 44h.
  • Step (4.2) The thermal degreasing process can be carried out by means of burying powder, and the powder used for burying powder is ⁇ -Al 2 O 3 powder.
  • the embedding method can support the green body, avoiding deformation of the green body under the action of self-weight when the binder softens, and capillary adsorption of the embedding powder on the other side can promote the elimination of the organic binder.
  • the sintering can be carried out by any one of atmospheric sintering, hot press sintering, or normal pressure sintering, followed by hot isostatic pressing.
  • the method for preparing transparent ceramic parts by injection molding according to the invention pre-treats the ceramic powder, then carries out the raw material mixing and injection molding, degreases by a two-step degreasing method, and finally obtains transparent ceramic parts with excellent performance by sintering.
  • the method of the invention is suitable for preparing transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • a method for preparing a transparent ceramic component by injection molding comprising the following steps:
  • the surface modification of the ceramic powder causes the surface modifier to form a nano-scale organic acid coating on the surface of the ceramic powder to obtain a surface-modified ceramic powder.
  • step (1) the ceramic powder having a purity greater than 99.9% and a particle size of submicron is used as a raw material for surface modification.
  • the surface modifier used in the step (1) is any one of stearic acid, oleic acid or dodecyl stearic acid, and the surface modifier is present in an amount of 1.8% by weight based on the weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, and the surface modification agent and the ceramic powder are esterified by ball milling to obtain a surface-modified ceramic powder.
  • the ball milling medium is alcohol and the ball milling time is 6h.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid coating is formed on the surface of the ceramic by esterification reaction between the surface modifier and the ceramic powder.
  • Floor Unlike the prior art introduction of a surface modifier in the mixing stage, the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 62% by weight of the injection molding mixture by weight percent.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer.
  • polyethylene accounts for 15% of the binder system
  • polypropylene accounts for 15% of the binder system.
  • Paraffin It accounts for 60% of the binder system
  • stearic acid accounts for 6% of the binder system
  • plasticizer accounts for 4% of the binder system.
  • the ceramic injection feeding mixing process specifically includes:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid were mixed for 30 minutes, and a plasticizer was added within 3 minutes before the end of the mixing.
  • Degreasing is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, including:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, heat preservation for 3 h; then within 3 h Increasing from 80 ° C to 150 ° C, holding for 3 h; then rising from 150 ° C to 250 ° C in 4 h, holding for 1.5 h; then rising from 250 ° C to 350 ° C in 4 h, holding for 2.5 h; then from 250 ° C in 4 h It was raised to 350 ° C, kept for 3.5 h; then it was raised from 350 ° C to 450 ° C in 4 h, and kept for 3.5 h; finally, it was raised from 450 ° C to 500 ° C in 4 h, and kept for 2.5 h; the whole thermal degreasing process was controlled within 44 h.
  • Step (4.2) The thermal degreasing process can be carried out by means of burying powder, and the powder used for burying powder is zirconia powder.
  • the embedding method can support the green body, avoiding deformation of the green body under the action of self-weight when the binder softens, and capillary adsorption of the embedding powder on the other side can promote the elimination of the organic binder.
  • the sintering can be carried out by any one of atmospheric sintering, hot press sintering, or normal pressure sintering, followed by hot isostatic pressing.
  • the method for preparing transparent ceramic parts by injection molding according to the invention pre-treats the ceramic powder, then carries out the raw material mixing and injection molding, degreases by a two-step degreasing method, and finally obtains transparent ceramic parts with excellent performance by sintering.
  • the method of the invention is suitable for preparing transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • the preparation of the transparent alumina ceramic by the method for preparing a transparent ceramic component by injection molding according to the present invention comprises the following steps:
  • the surface modification was carried out using alumina ceramic powder having a purity of more than 99.9% and a submicron particle size as a raw material.
  • the surface modifier is stearic acid and the surface modifier is 2% by weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, using alcohol as the ball milling medium, and ball milling for 5 hours, so that the surface modifier reacts with the ceramic powder to form a surface modifier on the surface of the ceramic powder.
  • a layer of 1-3 nm thick stearic acid coating is applied to obtain a surface-modified alumina ceramic powder.
  • the transmission electron micrograph of the ceramic particles of the surface-modified alumina ceramic powder in this embodiment is shown in FIG.
  • the aluminum oxide ceramic powder, the surface-modified alumina ceramic powder and the hard acid in the present embodiment were respectively subjected to powder Fourier infrared analysis, and the results are shown in Fig. 2, as can be seen from Fig. 2,
  • the surface modified alumina ceramic powder has a different profile than pure alumina.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid package is formed on the surface of the ceramic by esterification reaction between the surface modifier and the ceramic powder. Cladding. Unlike the prior art introduction of a surface modifier in the mixing stage, the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 62% by weight of the injection molding mixture by weight percent.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer.
  • polyethylene accounts for 15% of the binder system
  • polypropylene accounts for 15% of the binder system.
  • Paraffin It accounts for 60% of the binder system
  • stearic acid accounts for 6% of the binder system
  • plasticizer accounts for 4% of the binder system.
  • the ceramic injection feeding mixing process specifically includes:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid were mixed for 30 minutes, and a plasticizer was added within 3 minutes before the end of the mixing.
  • Degreasing is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, including:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, heat preservation for 1.5 h; then at 3 h
  • the temperature is raised from 80 ° C to 150 ° C, held for 2.5 h; then raised from 150 ° C to 250 ° C in 4 h, kept for 2 h; then increased from 250 ° C to 350 ° C in 4 h, kept for 3 h; then from 250 ° C in 4 h It is raised to 350 ° C, kept for 3.5 h; then it is raised from 350 ° C to 450 ° C in 4 h, and kept for 3.5 h; finally, it is raised from 450 ° C to 500 ° C in 4 h, and kept for 2 h; the whole thermal degreasing process is controlled within 44 h.
  • Step (4.2) The thermal degreasing process is carried out by means of burying powder, and the powder used for burying powder is activated carbon powder.
  • the embedding method can support the green body, avoiding deformation of the green body under the action of self-weight when the binder softens, and capillary adsorption of the embedding powder on the other side can promote the elimination of the organic binder.
  • the sintering method of the ceramic body is not limited to the atmosphere sintering of the present embodiment, and may be carried out by any one of hot press sintering or normal pressure sintering followed by hot isostatic pressing.
  • FIG. 4 A picture of a complex shaped transparent ceramic component prepared by the method of the present invention is shown in Figure 4, which contains four transparent alumina brackets and a discharge tube such as a transparent alumina.
  • Figure 4 contains four transparent alumina brackets and a discharge tube such as a transparent alumina.
  • Other complex shapes of transparent alumina ceramic components can also be prepared by the method of the present invention, which will not be repeated herein.
  • the method for preparing transparent ceramic parts by injection molding according to the invention pre-treats the ceramic powder, then carries out the raw material mixing and injection molding, degreases by a two-step degreasing method, and finally obtains transparent ceramic parts with excellent performance by sintering.
  • the method of the invention is suitable for preparing transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.
  • the preparation of the cerium oxide transparent ceramic by the method for preparing a transparent ceramic component by injection molding of the present invention comprises the following steps:
  • the surface modification was carried out using a cerium oxide ceramic powder having a purity of more than 99.9% and a submicron particle size as a raw material.
  • the surface modifier is stearic acid and the surface modifier is 1.6% by weight of the ceramic powder.
  • the surface modification process is to mix the surface modifier with the ceramic powder, using alcohol as the ball milling medium, and ball milling for 3 hours, so that the surface modifier and the ceramic powder are esterified, so that the surface modifier forms on the surface of the ceramic powder.
  • a layer of 1-3 nm thick stearic acid coating is applied to obtain a surface-modified cerium oxide ceramic powder.
  • the surface modifier is introduced into the ceramic powder by ball milling to be surface-modified in advance, and a nano-scale organic acid package is formed on the surface of the ceramic by esterification reaction between the surface modifier and the ceramic powder. Cladding. Unlike the prior art introduction of a surface modifier in the mixing stage, the process of the present invention ensures that the entire preparation process is carried out efficiently, ultimately resulting in a high performance transparent ceramic part.
  • Step (2) The surface-modified ceramic powder and the binder system are subjected to ceramic injection feeding and kneading. Step (2) In the ceramic injection feeding mixing, the surface-modified ceramic powder and the bonding amount system constitute an injection molding mixture. The surface-modified ceramic powder accounts for 61% by weight of the injection molding mixture by weight percent.
  • the adhesive system consists of polyethylene, polypropylene, paraffin, stearic acid and plasticizer.
  • polyethylene accounts for 13% of the binder system
  • polypropylene accounts for 13% of the binder system
  • Paraffin It accounts for 64% of the binder system
  • stearic acid accounts for 5% of the binder system
  • plasticizer accounts for 5% of the binder system.
  • the ceramic injection feeding mixing process specifically includes:
  • the two-roll mill is preheated. After the temperature of the roll reaches 170 ° C, polyethylene and polypropylene are added to the gap between the two rolls. After the polyethylene and polypropylene are completely melted, the surface modification is added. The ceramic powder, paraffin and stearic acid were mixed for 33 minutes, and a plasticizer was added within 4 minutes before the end of the mixing.
  • Degreasing is a two-step degreasing method using solvent extraction degreasing combined with thermal degreasing to degrease the ceramic body, including:
  • thermal degreasing The ceramic body after solvent extraction and degreasing is placed in a muffle furnace for thermal degreasing.
  • the heating curve of thermal degreasing is: from room temperature to 80 ° C in 4 h, heat preservation for 1.5 h; then at 3 h
  • the temperature is raised from 80 ° C to 150 ° C, held for 2.5 h; then raised from 150 ° C to 250 ° C in 4 h, kept for 2 h; then increased from 250 ° C to 350 ° C in 4 h, kept for 3 h; then from 250 ° C in 4 h It is raised to 350 ° C, kept for 3.5 h; then it is raised from 350 ° C to 450 ° C in 4 h, and kept for 3.5 h; finally, it is raised from 450 ° C to 500 ° C in 4 h, and kept for 2 h; the whole thermal degreasing process is controlled within 44 h.
  • Step (4.2) The thermal degreasing process is carried out by means of burying powder, and the powder used for burying powder is activated carbon powder.
  • the embedding method can support the green body, avoiding deformation of the green body under the action of self-weight when the binder softens, and capillary adsorption of the embedding powder on the other side can promote the elimination of the organic binder.
  • the method of sintering the ceramic body is not limited to the hot press sintering of the present embodiment, and may be carried out by any one of atmospheric sintering or normal pressure sintering followed by hot isostatic pressing.
  • Complex shape transparent ceramic parts such as transparent yttria brackets, transparent yttria, etc., can be prepared by the method of the present invention.
  • the method for preparing transparent ceramic parts by injection molding according to the invention pre-treats the ceramic powder, then carries out the raw material mixing and injection molding, degreases by a two-step degreasing method, and finally obtains transparent ceramic parts with excellent performance by sintering.
  • the method of the invention is suitable for preparing transparent ceramic parts with high performance and complex shape, and the prepared transparent ceramic parts have fine microstructure, good compactness and excellent performance.

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Abstract

一种注射成型制备透明陶瓷部件的方法，包括如下步骤：(1)在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体；(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼；(3)注射成型得到陶瓷坯体；(4)对陶瓷坯体进行脱脂；(5)对脱脂后的陶瓷坯体进行烧结，获得透明陶瓷部件。该方法能够制备高性能、复杂形状的透明陶瓷部件。

Description

一种注射成型制备透明陶瓷部件的方法 技术领域
本发明涉及透明陶瓷制备技术领域，特别涉及一种注射成型制备透明陶瓷部件的方法。
背景技术
透明陶瓷材料具有耐高温、耐腐蚀、高强度、高硬度、化学稳定性和生物相容性等结构陶瓷所固有的属性，同时具备透光、透波、激光等功能特性，已在能源、机械、军工、电子、半导体、医学等高科技领域得到愈来愈广泛的应用。自上世纪60年代以来，陶瓷材料科学工作者对透明陶瓷材料的合成、烧结、晶体结构、性能、透光机理以及应用等方面做了许多探索和研究工作。如研究了氧化铝、钇铝石榴石、氧化钇、氧化镁、镁铝尖晶石等氧化物透明陶瓷以及氮化铝、塞隆等非氧化物透明陶瓷。然而，随着科技的发展，对透明陶瓷性能的制备也提出了更高的要求，例如陶瓷金卤灯中的透明氧化铝陶瓷放电管，透明氧化铝陶瓷托槽，透明氧化锆陶瓷镜头，钇铝石榴石激光透明陶瓷，透明陶瓷装甲以及镁铝尖晶石陶瓷整流罩。
目前透明陶瓷多采用传统的成型方法，如干压、注浆、等静压成型，这些传统成型方法并不适用于制备精密、复杂形状的高性能、高可靠性的透明陶瓷材料，如目前在牙齿矫正具有较好应用前景的透明氧化铝托槽、陶瓷金卤灯放电管。传统的成型方法中，陶瓷干压成型虽然效率较高，但存在密度差异、显微结构不均匀的现象，同时不易成型异形部件。陶瓷注浆成型虽可成型异形产品，但成型坯体易产生密度不均和成分偏析，成型尺寸精度低和产品可靠性下降等问题。冷等静压成型可得到高密度和高均匀性的成型坯体，但难以成型形状复杂的陶瓷零部件，且成型效率低和手工操作多。
因此，针对现有技术不足，提供一种具备净尺寸、高精度、高密度、高均匀性且适合制备高性能、复杂形状部件的成型方法以克服现有技术不足甚为必要。
发明内容
本发明的目的在于避免现有技术的不足之处而提供一种注射成型制备透明陶瓷部件的方法，能够制备净尺寸、高性能、复杂复杂形状的透明陶瓷部件。
本发明的上述目的通过如下技术手段实现。
提供一种注射成型制备透明陶瓷部件的方法，包括如下步骤：
(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体；
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼；
(3)注射成型得到陶瓷坯体；
(4)对陶瓷坯体进行脱脂；
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。
优选的，上述步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
优选的，上述步骤(1)中使用的表面改性剂为硬脂酸、油酸或者十二烷基硬脂酸中的任意一种，表面改性剂的含量占陶瓷粉体重量的1.5～3％。
优选的，上述步骤(1)具体是将表面改性剂与陶瓷粉体混合，通过球磨使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。
优选的，上述步骤(1)中，球磨介质为酒精，球磨时间为3～12h。
优选的，上述步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料；
以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为58～65％；
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的8～20％，聚丙烯占粘接剂体系的8～20％，石蜡占粘接剂体系的54～65％，硬脂酸占粘接剂体系的5～10％，增塑剂占粘接剂体系的4～8％。
优选的，上述步骤(2)陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30～45min，在混炼结束前3～5min内加入增塑剂。
优选的，上述(4)对陶瓷坯体进行脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为40～60℃下萃取4～12h，然后放入烘箱中在80～100℃的温度下干燥20-50分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温1.5～3h；然后在3h内从80℃升至150℃，保温1.5～3h；接着在4h内从150℃升至250℃，保温1.5～3h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从350℃升至450℃，保温2.5～3.5h；最后在4h内从450℃升至500℃，保温2.5～3.5h；整个热脱脂过程控制在44h内。
优选的，上述步骤(4.2)热脱脂过程采用埋粉方式进行，埋粉采用的粉体为α-Al2O3粉、氧化锆粉、γ-Al2O3粉、活性碳粉中的任意一种。
优选的，上述步骤(5)采用气氛烧结、热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
本发明的注射成型制备透明陶瓷部件的方法，包括如下步骤：(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体；(2)将表面改性化陶瓷粉体与粘接剂体系进 行陶瓷注射喂料混炼；(3)注射成型得到陶瓷坯体；(4)对陶瓷坯体进行脱脂；(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。本发明的方法能够制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
说明书附图
结合附图对本发明作进一步解释说明，但附图中的内容不构成对本发明的限制。
图1是本发明实施例5中表面改性化氧化铝陶瓷粉体的陶瓷颗粒透射电子显微镜图。
图2是本发明实施例5中氧化铝陶瓷粉体、表面改性化的氧化铝陶瓷粉体及硬质酸的粉体傅里叶红外分析结果图。
图3是本发明实施例5中烧结后的透明氧化铝陶瓷的扫描电镜表面形貌图。
图4是本发明实施例5中通过本发明的方法制备的部分复杂形状透明陶瓷部件的示意图。
具体实施方式
结合以下实施例对本发明作进一步描述。
实施例1。
一种注射成型制备透明陶瓷部件的方法，包括如下步骤：
(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体。
其中，步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
步骤(1)中使用的表面改性剂为硬脂酸、油酸或者十二烷基硬脂酸中的任意一种，表面改性剂的含量占陶瓷粉体重量的1.5～3％。
表面改性过程是将表面改性剂与陶瓷粉体混合，通过球磨使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。球磨介质为酒精，球磨时间为3～12h。
本实施例通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为58～65％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百 分比计，聚乙烯占粘接剂体系的8～20％，聚丙烯占粘接剂体系的8～20％，石蜡占粘接剂体系的54～65％，硬脂酸占粘接剂体系的5～10％，增塑剂占粘接剂体系的4～8％。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂，脱脂可以采用热脱脂，也可以采用二步脱脂法。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。
本发明的方法能够制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
实施例2。
一种注射成型制备透明陶瓷部件的方法，包括如下步骤：
(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体。
其中，步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
步骤(1)中使用的表面改性剂为硬脂酸、油酸或者十二烷基硬脂酸中的任意一种，表面改性剂的含量占陶瓷粉体重量的2％。
表面改性过程是将表面改性剂与陶瓷粉体混合，通过球磨使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。球磨介质为酒精，球磨时间为3～12h。
本实施例通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为58～65％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的8～20％，聚丙烯占粘接剂体系的8～20％，石蜡占粘接剂体系的54～65％，硬脂酸占粘接剂体系的5～10％，增塑剂占粘接剂体系的4～8％。
陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30～45min，在混炼结束前3～5min内加入增塑剂。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂。脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为40～60℃下萃取4～12h，然后放入烘箱中在80～100℃的温度下干燥20-50分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温1.5～3h；然后在3h内从80℃升至150℃，保温1.5～3h；接着在4h内从150℃升至250℃，保温1.5～3h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从350℃升至450℃，保温2.5～3.5h；最后在4h内从450℃升至500℃，保温2.5～3.5h；整个热脱脂过程控制在44h内。
步骤(4.2)热脱脂过程可以采用埋粉方式进行，埋粉采用的粉体为α-Al2O3粉、氧化锆粉、γ-Al2O3粉、活性碳粉中的任意一种。埋粉方式一方面可以对坯体起到支撑作用，避免粘结剂软化时坯体在自重作用下发生形变，另一面坯体埋粉的毛细吸附作用可以促进有机粘结剂的排除。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。烧结可以采用气氛烧结、热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
本发明注射成型制备透明陶瓷部件的方法，对陶瓷粉体预处理，然后进行原料混炼、注射成型，采用二步脱脂法进行脱脂，最后经过烧结制备出性能优良的透明陶瓷部件。本发明的方法适合制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
实施例3。
一种注射成型制备透明陶瓷部件的方法，包括如下步骤：
(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体。
其中，步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
步骤(1)中使用的表面改性剂为硬脂酸，表面改性剂的含量占陶瓷粉体重量的2.3％。
表面改性过程是将表面改性剂与陶瓷粉体混合，以酒精作为球磨介质，通过球磨10h，使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。
通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为60％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的10％，聚丙烯占粘接剂体系的10％，石蜡占粘接剂体系的65％，硬脂酸占粘接剂体系的10％，增塑剂占粘接剂体系的5％。
陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30min，在混炼结束前5min内加入增塑剂。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂。脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为50℃下萃取6h，然后放入烘箱中在90℃的温度下干燥30分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温2h；然后在3h内从80℃升至150℃，保温2h；接着在4h内从150℃升至250℃，保温2h；接着在4h内从250℃升至350℃，保温3h；接着在4h内从250℃升至350℃，保温3h；接着在4h内从350℃升至450℃，保温3h；最后在4h内从450℃升至500℃，保温3h；整个热脱脂过程控制在44h内。
步骤(4.2)热脱脂过程可以采用埋粉方式进行，埋粉采用的粉体为α-Al2O3粉。埋粉方式一方面可以对坯体起到支撑作用，避免粘结剂软化时坯体在自重作用下发生形变，另一面坯体埋粉的毛细吸附作用可以促进有机粘结剂的排除。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。烧结可以采用气氛烧结、热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
本发明注射成型制备透明陶瓷部件的方法，对陶瓷粉体预处理，然后进行原料混炼、注射成型，采用二步脱脂法进行脱脂，最后经过烧结制备出性能优良的透明陶瓷部件。本发明的方法适合制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
实施例4。
一种注射成型制备透明陶瓷部件的方法，包括如下步骤：
(1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体。
其中，步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
步骤(1)中使用的表面改性剂为硬脂酸、油酸或者十二烷基硬脂酸中的任意一种，表面改性剂的含量占陶瓷粉体重量的1.8％。
表面改性过程是将表面改性剂与陶瓷粉体混合，通过球磨使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。球磨介质为酒精，球磨时间为6h。
本实施例通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为62％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的15％，聚丙烯占粘接剂体系的15％，石蜡占粘接剂体系的60％，硬脂酸占粘接剂体系的6％，增塑剂占粘接剂体系的4％。
陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30min，在混炼结束前3min内加入增塑剂。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂。脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为40～60℃下萃取12h，然后放入烘箱中在80～100℃的温度下干燥45分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温3h；然后在3h内从80℃升至150℃，保温3h；接着在4h内从150℃升至250℃，保温1.5h；接着在4h内从250℃升至350℃，保温2.5h；接着在4h内从250℃升至350℃，保温3.5h；接着在4h内从350℃升至450℃，保温3.5h；最后在4h内从450℃升至500℃，保温2.5h；整个热脱脂过程控制在44h内。
步骤(4.2)热脱脂过程可以采用埋粉方式进行，埋粉采用的粉体为氧化锆粉。埋粉方式一方面可以对坯体起到支撑作用，避免粘结剂软化时坯体在自重作用下发生形变，另一面坯体埋粉的毛细吸附作用可以促进有机粘结剂的排除。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。烧结可以采用气氛烧结、热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
本发明注射成型制备透明陶瓷部件的方法，对陶瓷粉体预处理，然后进行原料混炼、注射成型，采用二步脱脂法进行脱脂，最后经过烧结制备出性能优良的透明陶瓷部件。本发明的方法适合制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
实施例5。
通过本发明一种注射成型制备透明陶瓷部件的方法进行氧化铝透明陶瓷的制备，包括如下步骤：
(1)陶瓷粉体表面改性
采用纯度大于99.9％、颗粒尺寸为亚微米级的氧化铝陶瓷粉体作为原料进行表面改性。表面改性剂为硬脂酸，表面改性剂的含量占陶瓷粉体重量的2％。
表面改性过程是将表面改性剂与陶瓷粉体混合，采用酒精作为球磨介质，球磨5h，使得表面改性剂与陶瓷粉体发生酯化反应，使表面改性剂在陶瓷粉末表面形成一层1-3纳米厚的硬脂酸酸包覆层，得到表面改性化的氧化铝陶瓷粉体。本实施例中表面改性化的氧化铝陶瓷粉体的陶瓷颗粒透射电子显微镜图片如图1所示。对本实施例中的氧化铝陶瓷粉体、表面改性化的氧化铝陶瓷粉体及硬质酸分别进行粉体傅里叶红外分析，结果如图2所示，从图2中可以看出，表面改性化的氧化铝陶瓷粉体的图谱与纯氧化铝不同。
本实施例中通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为62％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的15％，聚丙烯占粘接剂体系的15％，石蜡占粘接剂体系的60％，硬脂酸占粘接剂体系的6％，增塑剂占粘接剂体系的4％。
陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30min，在混炼结束前3min内加入增塑剂。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂。脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为55℃下萃取12h，然后放入烘箱中在1000℃的温度下干燥42分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温1.5h；然后在3h内从80℃升至150℃，保温2.5h；接着在4h内从150℃升至250℃，保温2h；接着在4h内从250℃升至350℃，保温3h；接着在4h内从250℃升至350℃，保温3.5h；接着在4h内从350℃升至450℃，保温3.5h；最后在4h内从450℃升至500℃，保温2h；整个热脱脂过程控制在44h内。
步骤(4.2)热脱脂过程采用埋粉方式进行，埋粉采用的粉体为活性炭粉。埋粉方式一方面可以对坯体起到支撑作用，避免粘结剂软化时坯体在自重作用下发生形变，另一面坯体埋粉的毛细吸附作用可以促进有机粘结剂的排除。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。烧结可以采用气氛烧结的方式进行。烧结后的透明氧化铝陶瓷的扫描电镜表面形貌图如图3所示。需要说明的是，氧化铝陶瓷部件的气氛烧结方式为本领域公知常识，在此不再赘述。
对陶瓷坯体的烧结方式不局限于本实施例的气氛烧结，也可以选择热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
通过本发明的方法制备的复杂形状透明陶瓷部件的图片如图4所示，图4中含有四个透明氧化铝托槽和一个透明氧化铝等放电管。通过本发明的方法还可以制备其它复杂形状的透明氧化铝陶瓷部件，在此不一一赘述。
本发明注射成型制备透明陶瓷部件的方法，对陶瓷粉体预处理，然后进行原料混炼、注射成型，采用二步脱脂法进行脱脂，最后经过烧结制备出性能优良的透明陶瓷部件。本发明的方法适合制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
实施例6。
通过本发明一种注射成型制备透明陶瓷部件的方法进行氧化钇透明陶瓷的制备，包括如下步骤：
(1)陶瓷粉体表面改性
采用纯度大于99.9％、颗粒尺寸为亚微米级的氧化钇陶瓷粉体作为原料进行表面改性。表面改性剂为硬脂酸，表面改性剂的含量占陶瓷粉体重量的1.6％。
表面改性过程是将表面改性剂与陶瓷粉体混合，采用酒精作为球磨介质，球磨3h，使得表面改性剂与陶瓷粉体发生酯化反应，使表面改性剂在陶瓷粉末表面形成一层1-3纳米厚的硬脂酸酸包覆层，得到表面改性化的氧化钇陶瓷粉体。
本实施例中通过球磨方式将表面改性剂引入陶瓷粉体预先进行表面改性，通过表面改性剂与陶瓷粉体之间发生的酯化反应在陶瓷表面形成一层纳米级的有机酸包覆层。与现有技术中在混炼阶段引入表面改性剂不同，本发明的工艺方法能够确保整个制备工艺有效进行，最终获得高性能的透明陶瓷部件。
陶瓷粉体表面改性后进入步骤(2)混炼。
(2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼。步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料。以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为61％。
粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的13％，聚丙烯占粘接剂体系的13％，石蜡占粘接剂体系的64％，硬脂酸占粘接剂体系的5％，增塑剂占粘接剂体系的5％。
陶瓷注射喂料混炼过程具体包括：
首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼33min，在混炼结束前4min内加入增塑剂。
(3)注射成型得到陶瓷坯体。
(4)对陶瓷坯体进行脱脂。脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
(4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为55℃下萃取12h，然后放入烘箱中在1000℃的温度下干燥42分钟；
(4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温1.5h；然后在3h内从80℃升至150℃，保温2.5h；接着在4h内从150℃升至250℃，保温2h；接着在4h内从250℃升至350℃，保温3h；接着在4h内从250℃升至350℃，保温3.5h；接着在4h内从350℃升至450℃，保温3.5h；最后在4h内从450℃升至500℃，保温2h；整个热脱脂过程控制在44h内。
步骤(4.2)热脱脂过程采用埋粉方式进行，埋粉采用的粉体为活性炭粉。埋粉方式一方面可以对坯体起到支撑作用，避免粘结剂软化时坯体在自重作用下发生形变，另一面坯体埋粉的毛细吸附作用可以促进有机粘结剂的排除。
(5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。烧结可以采用热压烧结的方式进行。需要说明的是，氧化钇陶瓷部件的气氛烧结方式为本领域公知常识，在此不再赘述。
对陶瓷坯体的烧结方式不局限于本实施例的热压烧结，也可以选择气氛烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
通过本发明的方法可以制备复杂形状透明陶瓷部件，如透明氧化钇托槽、透明氧化钇等放电管等等。
本发明注射成型制备透明陶瓷部件的方法，对陶瓷粉体预处理，然后进行原料混炼、注射成型，采用二步脱脂法进行脱脂，最后经过烧结制备出性能优良的透明陶瓷部件。本发明的方法适合制备高性能、复杂形状的透明陶瓷部件，所制备的透明陶瓷部件显微结构精细、致密性好、性能优良。
需要说明的是，本发明的方便不适用于所有透明透明陶瓷部件制备，不仅仅局限于氧化铝透明陶瓷部件和氧化钇透明陶瓷部件的制备，在此不一一赘述。
最后应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

  1. 一种注射成型制备透明陶瓷部件的方法，其特征在于，包括如下步骤：
    (1)陶瓷粉体表面改性，使表面改性剂在陶瓷粉末表面形成一层纳米级的有机酸包覆层，得到表面改性化陶瓷粉体；
    (2)将表面改性化陶瓷粉体与粘接剂体系进行陶瓷注射喂料混炼；
    (3)注射成型得到陶瓷坯体；
    (4)对陶瓷坯体进行脱脂；
    (5)对脱脂后的陶瓷坯体进行烧结，获得成品透明陶瓷部件。
  2. 根据权利要求1所述的注射成型制备透明陶瓷部件的方法，其特征在于，步骤(1)中采用纯度大于99.9％、颗粒尺寸为亚微米级的陶瓷粉体作为原料进行表面改性。
  3. 根据权利要求2所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(1)中使用的表面改性剂为硬脂酸、油酸或者十二烷基硬脂酸中的任意一种，表面改性剂的含量占陶瓷粉体重量的1.5～3％。
  4. 根据权利要求3所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(1)具体是将表面改性剂与陶瓷粉体混合，通过球磨使得表面改性剂与陶瓷粉体发生酯化反应得到表面改性化陶瓷粉体。
  5. 根据权利要求4所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(1)中，球磨介质为酒精，球磨时间为3～12h。
  6. 根据权利要求5所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(2)陶瓷注射喂料混炼中，由表面改性化陶瓷粉体和粘接剂量体系构成注射成型混合料；
    以重量百分比计，表面改性化陶瓷粉体占注射成型混合料的重量百分比为58～65％；
    粘接剂体系由聚乙烯、聚丙烯、石蜡、硬脂酸和增塑剂组成，以重量百分比计，聚乙烯占粘接剂体系的8～20％，聚丙烯占粘接剂体系的8～20％，石蜡占粘接剂体系的54～65％，硬脂酸占粘接剂体系的5～10％，增塑剂占粘接剂体系的4～8％。
  7. 根据权利要求6所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(2)陶瓷注射喂料混炼过程具体包括：
    首先预热双辊开炼机，待辊筒的温度达到170℃后，在两个辊筒之间的间隙中加入聚乙烯和聚丙烯，待聚乙烯、聚丙烯完全熔融后，加入表面改性化陶瓷粉末、石蜡和硬脂酸，混炼30～45min，在混炼结束前3～5min内加入增塑剂。
  8. 根据权利要求7所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述(4)对陶瓷坯体进行脱脂是采用溶剂萃取脱脂结合热脱脂的二步脱脂法对陶瓷坯体进行脱脂，具体包括：
    (4.1)溶剂萃取脱脂：采用煤油作为有机溶剂，在萃取温度为40～60℃ 下萃取4～12h，然后放入烘箱中在80～100℃的温度下干燥20-50分钟；
    (4.2)热脱脂：将溶剂萃取脱脂后的陶瓷坯体置入马弗炉中进行热脱脂，热脱脂的升温曲线为：在4h内从室温升至80℃，保温1.5～3h；然后在3h内从80℃升至150℃，保温1.5～3h；接着在4h内从150℃升至250℃，保温1.5～3h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从250℃升至350℃，保温2.5～3.5h；接着在4h内从350℃升至450℃，保温2.5～3.5h；最后在4h内从450℃升至500℃，保温2.5～3.5h；整个热脱脂过程控制在44h内。
  9. 根据权利要求8所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(4.2)热脱脂过程采用埋粉方式进行，埋粉采用的粉体为α-Al2O3粉、氧化锆粉、γ-Al2O3粉、活性碳粉中的任意一种。
  10. 根据权利要求9所述的注射成型制备透明陶瓷部件的方法，其特征在于，所述步骤(5)采用气氛烧结、热压烧结或者常压烧结后再通过热等静压烧结方式中的任意一种方式进行。
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