CN110540424B - Feed for zirconia ceramic injection molding and preparation method thereof - Google Patents
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- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/6567—Treatment time
Abstract
The invention discloses a feed for zirconia ceramic injection molding and a preparation method thereof, wherein the feed is prepared from yttrium-stabilized zirconia powder and an organic mixture, wherein the yttrium-stabilized zirconia powder accounts for 75-92 wt%, and the organic mixture accounts for 8-25 wt%. According to the invention, the organic zirconium precursor is creatively introduced to optimize the zirconia ceramic feed, the organic zirconium precursor has good fluidity and brings 30 wt% of zirconia yield after being fired, the problems of high organic matter content and multiple firing defects in the traditional zirconia ceramic feed are solved, and the zirconia ceramic feed with high solid content and good fluidity is obtained.
Description
Technical Field
The invention relates to the field of precise ceramic preparation, in particular to a feed for zirconia ceramic injection molding and a preparation method thereof.
Background
The zirconia ceramic is a novel high-technology ceramic, has the conditions of high strength, hardness, high temperature resistance, acid and alkali corrosion resistance, high chemical stability and the like of precision ceramics, and also has higher toughness than common ceramics, so that the zirconia ceramic is widely applied to various industries, such as shaft seal bearings, cutting assemblies, dies, automobile parts and the like, and even can be used in artificial joints. Particularly, in recent years, with the development of communication technology, 5G communication is commercialized in 2020, interference from metal is very severe, and the 3D zirconia ceramic mobile phone back plate has the characteristics of no signal shielding, high hardness, strong appearance, excellent heat dissipation close to metal materials and the like, and becomes an important choice for mobile phone enterprises to enter the 5G era of march, and the zirconia ceramic has wider application.
However, the zirconia ceramic structural member has the characteristics of low production yield and poor dimensional accuracy controllability, so that the large-scale application of the zirconia ceramic structural member is greatly limited, particularly, the zirconia ceramic structural member with a complex shape is more difficult to produce in batches, the required accuracy is difficult to effectively control in the ceramic production process, the dimensional accuracy of the structural member can only be realized by means of machining, and the zirconia ceramic has high hardness and high brittleness, so that the complex structure such as a thin-wall structure and a curved-surface structure is extremely difficult to machine, the cost is high, and the capacity is severely limited. In the industry, the qualification rate of the zirconia ceramic structural part with the complex shape is less than 20 percent, and the main reason is from the characteristic of poor controllability of ceramic forming and sintering processes.
The blank of the zirconia ceramic structural component with the complex shape formed by the currently and generally adopted dry pressing and isostatic pressing processes has poor dimensional accuracy, and a large dimensional allowance needs to be reserved for machining; the existing injection molding process is also difficult to produce the zirconia ceramic structural member in batch, and the main reasons are that the content of zirconia feeding organic matters is high, and the organic matters are difficult to be completely eliminated in the sintering process, so that the zirconia ceramic structural member subjected to injection molding has many pore defects and low density, and the product performance cannot meet the requirements; the shrinkage and consistency of the ceramic structural member caused by large shrinkage of the sintering size are uncontrollable, and the difficulty which cannot be overcome by the existing zirconia ceramic system is overcome. The defect is caused by a 'tire of a zirconia ceramic system', the sintering shrinkage of the existing zirconia ceramic system is up to 20%, the size change temperature zone is narrow, the size of the zirconia ceramic structural part is not changed only in the sintering temperature zone of 10-20 ℃, the fluctuation of the sintering temperature obviously has great influence on the size shrinkage and deformation of the zirconia ceramic structural part, and the industrialization process of the zirconia ceramic structural part is also directly restricted. Therefore, the zirconia ceramic system needs to be adjusted so that the dimensional accuracy is truly controllable.
Disclosure of Invention
In order to solve the technical problems, the embodiment of the invention provides a feed for zirconia ceramic injection molding and a preparation method thereof, wherein an organic zirconium precursor introduced into the feed has high solid content and good flow property, and the yield of zirconia of 30% is introduced after the organic zirconium precursor is sintered at high temperature, so that paraffin components in a traditional zirconia ceramic feed system can be completely replaced, and the problems of high organic matter content such as paraffin and the like and high defect after sintering of the traditional zirconia ceramic feed system are solved. In addition, the sintering size of the ceramic blank formed by injection molding is reduced, the shrinkage consistency in the height and diameter directions is good, and the controllable sintering shrinkage and consistency of the zirconia ceramic structural member are realized.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a feed for zirconia ceramic injection molding is prepared from yttrium-stabilized zirconia powder and an organic mixture.
Preferably: 75-92 wt% of yttrium-stabilized zirconia powder and 8-25 wt% of organic mixture.
Preferably: the content (mol ratio) of yttrium oxide in the yttrium-stabilized zirconia powder is 2-4 mol%.
Preferably: the organic mixture is composed of an organic zirconium precursor, an organic binder and a dispersing agent.
Preferably: the organic zirconium precursor accounts for 40-94 wt%, the organic binder accounts for 3-40 wt%, and the dispersant accounts for 3-20 wt% of the organic mixture.
Preferably: the organic zirconium precursor is ZrO (OH)2And (3) precursor.
Preferably: the organic binder is selected from more than one of High Density Polyethylene (HDPE), ethylene-vinyl acetate copolymer (EVA), polyvinylpyrrolidone (PVP), polyvinyl butyral (PVB), atactic polypropylene (APP) and polypropylene (PP).
Preferably: the dispersant is more than one of Stearic Acid (SA), Oleic Acid (OA) and carboxyl stearic acid (HSA).
The invention also provides a preparation method of the feed for zirconia ceramic injection molding, which adopts an original high-pressure injection ceramic molding process, and ceramic blanks are degreased under the conditions of constant temperature and humidity water vapor, so that the potential safety hazard of environmental protection caused by using environmental protection oil to degrease a traditional zirconia ceramic feeding system is solved, the near-net-size molding of large-size, high-performance and complex-shaped ceramic precision parts is realized, and the application range of zirconia ceramic structural parts is greatly expanded.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the preparation method of the feed for zirconia ceramic injection molding comprises the following steps:
(1) melting, stirring and mixing an organic zirconium precursor, an organic binder and a dispersing agent, and cooling for later use to obtain an organic mixture;
(2) carrying out ball milling on yttrium stabilized zirconia powder, and then carrying out spray drying;
(3) and (3) adding the dried yttrium-stabilized zirconia powder obtained in the step (2) into the organic mixture prepared in the step (1) and mixing.
Preferably: the melting temperature of the step (1) is 160-250 ℃.
Preferably: and (3) in the step (2), a horizontal ceramic ball mill, a stirring mill and a sand mill are used for ball milling, and the ball milling time is 1-18 hours.
Preferably: the mixing temperature in the step (3) is 130-180 ℃.
A preparation method of an yttrium-stabilized zirconia ceramic material comprises the following steps:
(1) after granulating the prepared feed, feeding the granulated feed into a hopper of a high-pressure injection molding machine, applying high temperature and high pressure to inject the granulated feed into a mold, and opening the mold to obtain a ceramic blank;
(2) degreasing the ceramic blank prepared in the step (1);
(3) and (3) drying the degreased ceramic blank in the step (2), carrying out glue discharging treatment, and then heating for sintering to obtain the yttrium-stabilized zirconia ceramic material.
Preferably: the injection pressure in the step (1) is 20-50 MPa, and the injection temperature is 120-180 ℃.
Preferably: in the step (2), the degreasing temperature and the humidity of the ceramic blank are respectively 60-90 ℃ and 40-80% of humidity.
Preferably: the step (3) is specifically as follows: and (3) drying the ceramic blank degreased in the step (2), preserving heat at 650 ℃ for 2 hours for glue removal treatment, wherein the heating rate is 20 ℃/h, then heating to 1470-1620 ℃ for sintering, the heating rate is 120-180 ℃/h, and the heat preservation time is 2-16 hours.
The invention has the beneficial effects that:
the feed for zirconia ceramic injection molding claimed in this embodiment originally introduces the organic zirconium precursor to optimize the zirconia ceramic feed, solves the problems of high organic content (the organic content is up to more than 15 wt%) and multiple firing defects (the organic volatilization leaves many pore defects) in the traditional zirconia ceramic feed, and obtains the zirconia ceramic feed with high solid content (the organic zirconium precursor introduces 30 wt% of zirconia yield, and reduces the pore defects caused by the organic volatilization) and good fluidity.
The zirconia ceramic material prepared by the feed for zirconia ceramic injection molding claimed in this embodiment is prepared by a high-pressure injection molding process, and a ceramic blank is degreased under the conditions of constant temperature and humidity and water vapor, so that the potential safety hazard of environmental protection caused by using environment-friendly oil to degrease a traditional zirconia ceramic feeding system is solved, the precision of the prepared product is high, the near-net-size molding of a zirconia ceramic structural member is realized, the sintering shrinkage and consistency of the zirconia ceramic structural member are controllable, and the size fluctuation values of the sintered products in the same batch and different batches are less than one percent.
The zirconia ceramic prepared by the feed for zirconia ceramic injection molding claimed in the embodiment realizes low-deformation sintering of the zirconia ceramic three-dimensional precision structural member, and the product can meet the requirements of metal and high polymer materials on dimensional precision in batches without processing, thereby greatly expanding the application field of the zirconia ceramic and having the potential of widely replacing metal, high polymer materials and the like.
Detailed Description
In order to better understand the technical solution of the present invention, the following embodiments are provided to further explain the present invention.
Example 1
Mixing the raw materials according to the mass percentage, taking 85 wt% of ZrO (OH)2Adding a precursor, 10 wt% of polyvinylpyrrolidone (PVP) and 5 wt% of stearic acid into a mixer, melting at 180 ℃, stirring, fully mixing uniformly, cooling for later use to obtain an organic mixture, and preparing the low-deformation high-precision zirconia ceramic material by the following steps:
(1) putting 3mol of yttrium-stabilized zirconia powder into a 200KG horizontal ceramic ball mill for ball milling for 16 hours, and carrying out spray granulation after ball milling;
(2) putting the yttrium-stabilized zirconia powder after spray granulation into a mixing roll, adding an organic mixture with the powder mass fraction of 12 wt%, and uniformly mixing at 180 ℃;
(3) granulating the mixed raw materials in a granulator to obtain ceramic feed with the diameter of 3mm and the height of 5mm, feeding the ceramic feed into a hopper of a high-pressure injection molding machine through an automatic feeding machine, injecting the ceramic feed into a precision mold under the conditions that the injection pressure is 40MPa and the injection temperature is 150 ℃, and opening the mold to obtain a ceramic blank;
(4) degreasing the ceramic blank under the conditions of constant temperature and constant humidity of 70 ℃ and 60 percent of humidity;
(5) drying the degreased ceramic blank at the temperature of 100 ℃, putting the ceramic blank into a pushed slab kiln through a mechanical arm, carrying out heat preservation on the ceramic blank at the temperature of 650 ℃ for 2 hours for glue removal treatment at the heating rate of 20 ℃/h, then heating to the temperature of 1470-1550 ℃ for sintering, wherein the heating rate is 120-180 ℃/h, and the heat preservation time is 2-16 hours, so that the low-deformation high-precision yttrium-stabilized zirconia ceramic material can be prepared.
Table 1 dimensional shrinkage of example 1
Example 2
According to the mass percentageTaking 82 wt% of ZrO (OH)2Adding a precursor, 8 wt% of high-density polyethylene (HDPE), 5 wt% of polypropylene (PP) and 5 wt% of stearic acid into a mixer, melting at 180 ℃, stirring, fully mixing uniformly, cooling for later use to obtain an organic mixture, and preparing the low-deformation high-precision zirconia ceramic material by the following steps:
(1) after 2mol of yttrium-stabilized zirconia powder (2YSZ) components are mixed, putting the mixture into a 200KG horizontal ceramic ball mill for ball milling for 16 hours, and carrying out spray granulation after ball milling;
(2) putting the zirconia powder after spray granulation into a mixing roll, adding an organic mixture with the powder mass fraction of 12 percent, and uniformly mixing at the temperature of 180 ℃;
(3) granulating the mixed raw materials in a granulator to obtain ceramic feed with the diameter of 3mm and the height of 5mm, feeding the ceramic feed into a hopper of a high-pressure injection molding machine through an automatic feeding machine, injecting the ceramic feed into a precision mold under the conditions that the injection pressure is 40MPa and the injection temperature is 150 ℃, and opening the mold to obtain a ceramic blank;
(4) degreasing the ceramic blank under the conditions of constant temperature and constant humidity of 70 ℃ and 60 percent of humidity;
(5) drying the degreased ceramic blank at the temperature of 100 ℃, putting the ceramic blank into a pushed slab kiln through a mechanical arm, carrying out heat preservation on the ceramic blank at the temperature of 650 ℃ for 2 hours for glue removal treatment at the heating rate of 20 ℃/h, then heating to the temperature of 1560-1620 ℃ for sintering, wherein the heating rate is 120, the heat preservation time is 2-16 hours, and the low-deformation high-precision zirconia ceramic material can be prepared.
Table 2 shrinkage of the dimensions of example 2
Example 3
The same features of this embodiment as those of embodiment 1 or embodiment 2 are not described again, and the different features of this embodiment from those of the above embodiments are: mixing the raw materials according to the mass percentage, taking 75 weight percent of ZrO (OH)2Precursor, 20 wt% high density polyethyleneAt least one of HDPE, ethylene-vinyl acetate copolymer EVA, polyvinylpyrrolidone PVP, polyvinyl butyral PVB, random polypropylene APP and polypropylene PP and at least one of 5 wt% of stearic acid SA, oleic acid OA and carboxyl stearic acid HSA are added into a mixer to be melted at 160 ℃.
(1) The ball milling time in (1) is 5 hours, and the mixing temperature is 130 ℃.
(2) Adding an organic mixture with the powder mass fraction of 12 wt%, and uniformly mixing at the temperature of 130 ℃.
(3) The injection pressure is 20MPa, and the injection temperature is 125 ℃.
(4) The medium ceramic blank is degreased under the conditions of a temperature of 60 ℃ and a humidity of 40 percent at a constant temperature and a constant humidity.
Example 4
The same features of this embodiment as those of any of embodiments 1 to 3 are not described again, and the features of this embodiment that are different from those of the above embodiments are: taking 85 wt% of ZrO (OH)2The precursor, 10 wt% of at least one of High Density Polyethylene (HDPE), ethylene-vinyl acetate copolymer (EVA), polyvinylpyrrolidone (PVP), polyvinyl butyral (PVB), random polypropylene (APP) and polypropylene (PP), and 5 wt% of at least one of Stearic Acid (SA), Oleic Acid (OA) and carboxyl stearic acid (HSA) are added into a mixer and melted at 160 ℃.
(1) The ball milling time in (1) is 18 hours, and the mixing temperature is 180 ℃.
(2) Adding an organic mixture with the powder mass fraction of 28 wt%, and uniformly mixing at the temperature of 200 ℃.
(3) The injection pressure was 50MPa and the injection temperature was 175 ℃.
(4) The medium ceramic blank is degreased under the conditions of temperature of 90 ℃ and humidity of 70 percent at constant temperature and constant humidity.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (8)
1. The feed for zirconia ceramic injection molding is characterized by being prepared from yttrium-stabilized zirconia powder and an organic mixture, wherein the yttrium-stabilized zirconia powder accounts for 75-92 wt%, and the organic mixture accounts for 8-25 wt%;
wherein, the content of yttrium oxide in the yttrium-stabilized zirconia powder accounts for 2-4 mol%;
the organic mixture consists of an organic zirconium precursor, an organic binder and a dispersant, wherein the organic zirconium precursor accounts for 40-94 wt%, the organic binder accounts for 3-40 wt% and the dispersant accounts for 3-20 wt% of the components of the organic mixture.
2. The feed for zirconia ceramic injection molding according to claim 1, characterized in that: the organic binder is selected from more than one of high-density polyethylene, ethylene-vinyl acetate copolymer, polyvinylpyrrolidone, polyvinyl butyral, atactic polypropylene and polypropylene, and the dispersant is more than one of stearic acid, oleic acid and carboxyl stearic acid.
3. A method for preparing a feedstock for injection molding of zirconia ceramics as claimed in any one of claims 1 to 2, characterized in that: the method comprises the following steps:
(1) melting, stirring and mixing an organic zirconium precursor, an organic binder and a dispersing agent, and cooling for later use to obtain an organic mixture;
(2) carrying out ball milling on yttrium stabilized zirconia powder, and then carrying out spray drying;
(3) and (3) adding the spray-dried yttrium-stabilized zirconia powder obtained in the step (2) into the organic mixture prepared in the step (1) and mixing to obtain the yttrium-stabilized zirconia powder.
4. The method for preparing a feed material for zirconia ceramic injection molding according to claim 3, characterized in that: the melting temperature of the step (1) is 160-250 ℃.
5. The method for preparing a feed material for zirconia ceramic injection molding according to claim 3, characterized in that: and (3) in the step (2), a horizontal ceramic ball mill, a stirring mill and a sand mill are used for ball milling, and the ball milling time is 1-18 hours.
6. The method for preparing a feed material for zirconia ceramic injection molding according to claim 3, characterized in that: the mixing temperature in the step (3) is 130-180 ℃.
7. A preparation method of an yttrium-stabilized zirconia ceramic material comprises the following steps:
(1) granulating the feed material of any one of claims 1-2, feeding into a hopper of a high-pressure injection molding machine, applying high temperature and high pressure, injecting into a mold, and opening the mold to obtain a ceramic blank;
(2) degreasing the ceramic blank prepared in the step (1);
(3) and (3) drying the degreased ceramic blank in the step (2), carrying out glue discharging treatment, and then heating for sintering to obtain the yttrium-stabilized zirconia ceramic material.
8. The process for preparing yttrium-stabilized zirconia ceramic material according to claim 7, wherein: the injection pressure in the step (1) is 20-50 MPa, and the injection temperature is 120-180 ℃; the step (3) is specifically as follows: and (3) drying the ceramic blank degreased in the step (2), preserving heat at 650 ℃ for 2 hours for glue removal treatment, wherein the heating rate is 20 ℃/h, then heating to 1470-1620 ℃ for sintering, the heating rate is 120-180 ℃/h, and the heat preservation time is 2-16 hours.
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| CN111233488B (en) * | 2020-02-24 | 2023-12-08 | 长裕控股集团股份有限公司 | Surface modified zirconia injection molding solvent degreasing feed and preparation method and application thereof |
| CN112608147A (en) * | 2020-11-25 | 2021-04-06 | 科益展智能装备有限公司 | Integral zirconia ceramic cutting tool material and preparation method thereof |
| CN112679209B (en) * | 2020-12-28 | 2023-04-14 | 长裕控股集团股份有限公司 | Preparation method of black zirconia ceramic material |
| CN113149626B (en) * | 2021-05-13 | 2023-06-30 | 武汉理工大学 | Feed for quartz ceramic injection molding and preparation method thereof |
| CN116082037A (en) * | 2022-09-06 | 2023-05-09 | 江西虔悦新材料有限公司 | Nano zirconium-based ceramic injection molding feed and preparation method and application thereof |
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