CN112028625A - Zirconia ceramic material and preparation method and application thereof - Google Patents

Zirconia ceramic material and preparation method and application thereof Download PDF

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CN112028625A
CN112028625A CN202010756952.1A CN202010756952A CN112028625A CN 112028625 A CN112028625 A CN 112028625A CN 202010756952 A CN202010756952 A CN 202010756952A CN 112028625 A CN112028625 A CN 112028625A
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zirconia
ceramic material
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李毅
刘建国
吴沙欧
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Shenzhen Taotao Technology Co ltd
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Abstract

The invention provides a zirconia ceramic material and a preparation method and application thereof, wherein in the preparation method of the zirconia ceramic material, ZrO is added2Adding second phase SiC powder into the powder to prepare ZrO2-SiC composite cast film of ZrO2the-SiC composite casting membrane is used as an interlayer and clamped between adjacent zirconia casting membranes to realize toughening of a laminated structure; so that the second phase SiC is dispersedly distributed on the ZrO2In the ceramic, the dispersion toughening effect can be achieved in the whole zirconia ceramic material, so that the uniformity of the toughness of the prepared zirconia ceramic material is ensured.

Description

Zirconia ceramic material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a zirconia ceramic material and a preparation method and application thereof.
Background
The ceramic material is an inorganic non-metallic material prepared by forming and high-temperature sintering natural or synthetic compounds. It has the advantages of high melting point, high hardness, high wear resistance, oxidation resistance, etc. The ceramic can be used as a structural material and a cutter material, and can also be used as a functional material because the ceramic also has certain special properties.
The conventional ceramic material zirconia powder is prepared, the hardness and the bending strength of the zirconia ceramic are not high, and the toughness of the existing zirconia ceramic is 5-6MPa1/2The toughness of the ceramic material is also not high. The defects cause the limitation of the zirconia ceramic material in the application process, and particularly when the zirconia ceramic material is used for a shell of electronic equipment, the shell has poor wear resistance and is easy to crack, and the service life of the electronic equipment is greatly shortened.
In view of the above, a zirconia ceramic material, a preparation method and a use thereof are provided.
Disclosure of Invention
The invention aims to provide a zirconia ceramic material and a preparation method and application thereof, aiming at the defects in the prior art.
The object of the invention can be achieved by the following technical measures:
in order to achieve the above object, the present invention provides a method for preparing a zirconia ceramic material, the method comprising:
dissolving zirconia powder in an organic solvent, adding a plasticizer and a binder to prepare zirconia casting slurry, and preparing a zirconia casting membrane by using casting molding;
dissolving mixed powder of zirconium oxide powder and silicon carbide powder in the organic solvent, adding a plasticizer and a binder to prepare composite casting slurry, and preparing a composite casting membrane by using casting molding;
sequentially and alternately stacking the zirconia casting membrane and the composite casting membrane to obtain a plurality of laminated membranes, and performing isostatic pressing on the plurality of laminated membranes to form a composite ceramic biscuit;
and removing the glue from the composite ceramic biscuit and sintering to obtain the zirconia ceramic material.
Preferably, in the sintering process, the mixed gas of inert gas and oxygen is used as the sintering atmosphere, under the conditions that the total gas pressure is 0.05-0.15Mpa and the oxygen partial pressure is 140-160Pa, the mixed gas is heated to 600-1500 ℃ and the temperature is maintained for 20-40min, and then, under the conditions that the total gas pressure is 0.05-0.15Mpa, the mixed gas is heated to 1400-1500 ℃ and the temperature is maintained for 30-180 min.
Preferably, the silicon carbide content in the composite casting film is 1-15 wt%.
Preferably, the thickness ranges of the zirconia cast membrane and the composite cast membrane are both 50-200 μm.
Preferably, the zirconia powder is spherical particles or spheroidal particles with the particle size of 100-1000 nm.
Preferably, the average grain diameter of the silicon carbide powder is less than 100 nm.
The invention also provides a zirconia ceramic material, which is prepared by the preparation method of the zirconia ceramic material.
The invention also provides a shell which is made of the zirconia ceramic material.
The invention also provides electronic equipment which comprises the shell.
The invention has the beneficial effects of providing the zirconia ceramic material and the preparation method and the application thereof, wherein in the preparation method of the zirconia ceramic material, ZrO is used2Adding the powder into second phase SiC powder to prepare ZrO2-SiC composite cast film of ZrO2the-SiC composite casting membrane is used as an interlayer and clamped between adjacent zirconia casting membranes to realize toughening of a laminated structure; so that the second phase SiC is dispersedly distributed on the ZrO2In the ceramic matrix, the dispersion toughening effect can be achieved in the whole zirconia ceramic material, so that the uniformity of the toughness of the prepared zirconia ceramic material is ensured.
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FIG. 1 is a flow chart of a method for preparing a zirconia ceramic material according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the description of the present disclosure more complete and complete, the following description is given for illustrative purposes with respect to the embodiments and examples of the present invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments are intended to cover the features of the various embodiments as well as the method steps and sequences for constructing and operating the embodiments. However, other embodiments may be utilized to achieve the same or equivalent functions and step sequences.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a method for preparing a zirconia ceramic material, the method comprising the following steps:
and step S1, dissolving the zirconia powder in an organic solvent, adding a plasticizer and a binder to prepare zirconia casting slurry, and preparing the zirconia casting membrane by using casting molding. Optionally, the zirconia powder is 100-1000nm spherical or quasi-spherical particles. Optionally, the thickness of the cast zirconia membrane is in the range of 50-200 microns. The organic solvent includes but is not limited to at least one of EtOH, TOL, MEK, ethyl acetate, is capable of dissolving the binder and plasticizer, and has a certain volatility. Of course, the zirconia powder may be dissolved in water.
And step S2, dissolving the mixed powder of zirconium oxide powder and silicon carbide powder in an organic solvent, adding a plasticizer and a binder to prepare composite casting slurry, and preparing the composite casting membrane by using casting molding. Optionally, the zirconia powder is spherical particles or spheroidal particles of 100-1000 nm. Optionally, the average particle size of the silicon carbide powder is less than 100 nm. Optionally, the composite cast film sheet has a thickness in the range of 50-200 microns.
And step S3, sequentially and alternately stacking the zirconia casting membrane and the composite casting membrane to obtain a plurality of laminated membranes, and carrying out isostatic pressing on the plurality of laminated membranes to form a composite ceramic biscuit. Optionally, the content of silicon carbide in the composite casting film is 1-15 wt%.
And step S4, removing glue from the composite ceramic biscuit and sintering to obtain the zirconia ceramic material.
Preferably, in the sintering process, the composite ceramic biscuit after the binder removal is sintered by adopting a sectional sintering method, which specifically comprises the following steps:
firstly, using the mixed gas of inert gas and oxygen as the sintering atmosphere, heating to 600-800 ℃ and keeping the temperature for 20-40min under the conditions that the total gas pressure is 0.05-0.15Mpa and the oxygen partial pressure is 140-160 Pa.
Then, inert gas is used as sintering atmosphere, and the temperature is heated to 1400-1500 ℃ for 30-180 minutes under the condition that the total pressure of the gas is 0.05-0.15 Mpa.
The preparation method of the zirconium oxide ceramic material of the embodiment of the invention is in ZrO2Preparation of ZrO by adding second phase SiC into ceramic matrix2-SiC composite cast film, ZrO2the-SiC composite casting membrane is used as an interlayer and clamped between adjacent zirconia casting membranes to realize toughening of a laminated structure; so that the second phase SiC is dispersedly distributed on the ZrO2The ceramic matrix can play a role in dispersion toughening. In addition, in the sintering process, a segmented sintering method is adopted, and a certain oxygen partial pressure exists in the inert sintering atmosphere in the early stage of the sintering process, so that silicon carbide doped in a zirconia matrix is subjected to protective oxidation, a compact silicon dioxide protective film is formed on the surface of silicon carbide particles, the silicon dioxide can be used as a crystal form stabilizer in the composite material, and the toughening effect of the composite material can be ensured to be lasting and stable by increasing the normal-temperature stability of the crystal form of the zirconia.
The invention also provides a zirconia ceramic material, which is prepared by the preparation method of the zirconia ceramic material. According to the zirconia ceramic material provided by the invention, the silicon dioxide is uniformly distributed in the zirconia ceramic material, so that the toughness of the ceramic material can be enhanced, meanwhile, the silicon dioxide can be used as a crystal form stabilizer in the zirconia ceramic material, the toughening effect of the ceramic material can be ensured to be lasting and stable by increasing the normal temperature stability of the zirconia crystal form, the reliability of the zirconia ceramic material is improved, and the service life of the zirconia ceramic material is prolonged.
The invention also provides a shell which is made of the zirconia ceramic material. In the embodiment of the invention, the shell prepared by adopting the zirconia material has beautiful appearance, high-grade texture and hand feeling, and simultaneously improves the wear resistance and corrosion resistance of the shell, and in addition, the toughness of the shell is more strengthened and stable, so that the service life of the shell is greatly prolonged.
The invention also provides electronic equipment which comprises the shell according to the embodiment of the invention. Of course, those skilled in the art will appreciate that the electronic device has all of the features and advantages of the zirconia ceramic material and the housing described above, and thus, the detailed description thereof is omitted. According to the embodiment of the invention, the specific type of the electronic device is not limited, and those skilled in the art can flexibly select the electronic device according to actual needs. In some embodiments of the present invention, specific types of electronic devices include, but are not limited to, mobile phones, notebooks, game machines, and other electronic devices. Of course, it can be understood by those skilled in the art that the electronic device includes, in addition to the housing, the structure or component necessary for the conventional electronic device, and taking a mobile phone as an example, the mobile phone further includes, in addition to the housing, the structure or component necessary for the display panel, the glass cover plate, the CPU processor, the camera module, the voice module, the touch module, and the like. The understanding is further enhanced by the following specific examples and comparative examples.
Example one
Zirconia powder (ZrO) with average grain diameter less than 1 μm and purity more than 99%2Powder) is a ceramic matrix, silicon carbide powder with the average grain diameter of 100 nanometers is a ceramic toughening phase, ethyl acetate is a solvent, Butyl Benzyl Phthalate (BBP) is a plasticizer, polyvinyl butyral (PVB) is a binder, and ZrO is prepared by adopting a tape casting method2Cast film and ZrO2-SiC cast membranes. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The cast SiC films can be 7 layers each or 8 layers each, here 8 layers, as follows:
ZrO was added at a ratio of ethyl acetate 100 g and BBP 10g2100 g of powder and 14.5 g of PVB to prepare ZrO suitable for casting2Casting the slurry and preparing the ZrO with smooth and flat surface, no cracks and no pores2Cast membranes, ZrO2The average thickness of the cast film sheet was about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, 100 g of the composite powder (ZrO in the composite powder) was added2The mass ratio of the powder is 99 percent, the mass ratio of the SiC powder is 1 percent), and 14.5 g of PVB are adopted to prepare composite tape-casting slurry suitable for tape casting, and ZrO with flat and smooth surface, no cracks and no air holes is prepared at the same time2-a composite cast film sheet of SiC, the composite cast film sheet having an average thickness of about 100 microns.
ZrO2 is mixed with2Cast film and ZrO2Sequentially overlapping cast-SiC diaphragms and forming ZrO after isostatic pressing2Composite ceramic biscuit, then ZrO2And (4) carrying out glue discharging treatment on the composite ceramic biscuit.
ZrO after binder removal treatment2Sintering the composite ceramic biscuit, wherein segmented sintering is adopted in the sintering process, and the method specifically comprises the following steps:
firstly, with N2-O2The mixed gas is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the oxygen partial pressure is 160Pa, and the mixed gas is heated to 650 ℃ and is kept for 40 minutes;
then, with N2Is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the temperature is kept for 120 minutes after the temperature is heated to 1450 ℃, and the zirconia ceramic material is prepared and marked as 1#。
Example two
Zirconia powder (ZrO) with average grain diameter less than 1 μm and purity more than 99%2Powder) is ceramic matrix, and the silicon carbide powder with the average grain diameter of 100 nanometers is ceramicPreparing ZrO by tape casting method with ethyl acetate as solvent, dimethyl phthalate butyl benzyl ester (BBP) as plasticizer and polyvinyl butyral (PVB) as adhesive as toughening phase2Cast film and ZrO2-SiC cast membranes. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The number of layers of-SiC cast films is the same as in example one, and specifically as follows:
ZrO was added at a ratio of ethyl acetate 100 g and BBP 10g2100 g of powder and 14.5 g of PVB to prepare ZrO suitable for casting2Casting the slurry and preparing the ZrO with smooth and flat surface, no cracks and no pores2Cast membranes, ZrO2The average thickness of the cast film sheet was about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, 100 g of the composite powder (ZrO in the composite powder) was added2The mass percentage of the powder is 95 percent, the mass percentage of the SiC powder is 5 percent), and PVB is 14.5 g, so that the composite tape-casting slurry suitable for tape casting is prepared, and ZrO with a flat and smooth surface, no cracks and no air holes is prepared at the same time2-a composite cast film sheet of SiC, the composite cast film sheet having an average thickness of about 100 microns.
ZrO2 is mixed with2Cast film and ZrO2Sequentially overlapping cast-SiC diaphragms and forming ZrO after isostatic pressing2Composite ceramic biscuit, then ZrO2And (4) carrying out glue discharging treatment on the composite ceramic biscuit.
ZrO after binder removal treatment2Sintering the composite ceramic biscuit, wherein segmented sintering is adopted in the sintering process, and the method specifically comprises the following steps:
firstly, with N2-O2The mixed gas is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the oxygen partial pressure is 160Pa, and the mixed gas is heated to 650 ℃ and is kept for 40 minutes;
then, with N2Is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the temperature is kept for 120 minutes after the temperature is heated to 1450 ℃, and the zirconia ceramic material is prepared and marked as 2#。
EXAMPLE III
By averagingZirconium oxide powder (ZrO) with particle size less than 1 μm and purity greater than 99%2Powder) is a ceramic matrix, silicon carbide powder with the average grain diameter of 100 nanometers is a ceramic toughening phase, ethyl acetate is a solvent, Butyl Benzyl Phthalate (BBP) is a plasticizer, polyvinyl butyral (PVB) is a binder, and ZrO is prepared by adopting a tape casting method2Cast film and ZrO2-SiC cast membranes. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The number of layers of-SiC cast films is the same as in example one, and specifically as follows:
ZrO was added at a ratio of ethyl acetate 100 g and BBP 10g2100 g of powder and 14.5 g of PVB to prepare ZrO suitable for casting2Casting the slurry and preparing the ZrO with smooth and flat surface, no cracks and no pores2Cast membranes, ZrO2The average thickness of the cast film sheet was about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, 100 g of the composite powder (ZrO in the composite powder) was added2The mass percentage of the powder is 92 percent, the mass percentage of the SiC powder is 8 percent), and PVB is 14.5 g, so that the composite tape-casting slurry suitable for tape casting is prepared, and ZrO with a flat and smooth surface, no cracks and no air holes is prepared at the same time2-a composite cast film sheet of SiC, the composite cast film sheet having an average thickness of about 100 microns.
ZrO2 is mixed with2Cast film and ZrO2Sequentially overlapping cast-SiC diaphragms and forming ZrO after isostatic pressing2Composite ceramic biscuit, then ZrO2And (4) carrying out glue discharging treatment on the composite ceramic biscuit.
ZrO after binder removal treatment2Sintering the composite ceramic biscuit, wherein segmented sintering is adopted in the sintering process, and the method specifically comprises the following steps:
firstly, with N2-O2The mixed gas is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the oxygen partial pressure is 160Pa, and the mixed gas is heated to 650 ℃ and is kept for 40 minutes;
then, with N2Is sintering atmosphere with total gas pressure of 0.15MPa, is heated to 1450 ℃, is kept warm for 120 minutes, and is preparedZirconia ceramic material, marked 3#。
Example four
Zirconia powder (ZrO) with average grain diameter less than 1 μm and purity more than 99%2Powder) is a ceramic matrix, silicon carbide powder with the average grain diameter of 100 nanometers is a ceramic toughening phase, ethyl acetate is a solvent, Butyl Benzyl Phthalate (BBP) is a plasticizer, polyvinyl butyral (PVB) is a binder, and ZrO is prepared by adopting a tape casting method2Cast film and ZrO2-SiC cast membranes. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The number of layers of-SiC cast films is the same as in example one, and specifically as follows:
ZrO was added at a ratio of ethyl acetate 100 g and BBP 10g2100 g of powder and 14.5 g of PVB to prepare ZrO suitable for casting2Casting the slurry and preparing the ZrO with smooth and flat surface, no cracks and no pores2Cast membranes, ZrO2The average thickness of the cast film sheet was about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, 100 g of the composite powder (ZrO in the composite powder) was added2The mass percentage of the powder is 88 percent, the mass percentage of the SiC powder is 12 percent), and PVB is 14.5 g, so that the composite tape-casting slurry suitable for tape casting is prepared, and ZrO with flat and smooth surface, no cracks and no air holes is prepared at the same time2-a composite cast film sheet of SiC, the composite cast film sheet having an average thickness of about 100 microns.
ZrO2 is mixed with2Cast film and ZrO2Sequentially overlapping cast-SiC diaphragms and forming ZrO after isostatic pressing2Composite ceramic biscuit, then ZrO2And (4) carrying out glue discharging treatment on the composite ceramic biscuit.
ZrO after binder removal treatment2Sintering the composite ceramic biscuit, wherein segmented sintering is adopted in the sintering process, and the method specifically comprises the following steps:
firstly, with N2-O2The mixed gas is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the oxygen partial pressure is 160Pa, and the mixed gas is heated to 650 ℃ and is kept for 40 minutes;
then, with N2Is sintering atmosphere, the total pressure of gas is 0.15MPa, the temperature is heated to 1450 ℃, the temperature is preserved for 120 minutes, and the zirconia ceramic material is prepared and obtained, and the mark is 4#。
EXAMPLE five
Zirconia powder (ZrO) with average grain diameter less than 1 μm and purity more than 99%2Powder) is a ceramic matrix, silicon carbide powder with the average grain diameter of 100 nanometers is a ceramic toughening phase, ethyl acetate is a solvent, Butyl Benzyl Phthalate (BBP) is a plasticizer, polyvinyl butyral (PVB) is a binder, and ZrO is prepared by adopting a tape casting method2Cast film and ZrO2-SiC cast membranes. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The number of layers of-SiC cast films is the same as in example one, and specifically as follows:
ZrO was added at a ratio of ethyl acetate 100 g and BBP 10g2100 g of powder and 14.5 g of PVB to prepare ZrO suitable for casting2Casting the slurry and preparing the ZrO with smooth and flat surface, no cracks and no pores2Cast membranes, ZrO2The average thickness of the cast film sheet was about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, 100 g of the composite powder (ZrO in the composite powder) was added285 percent of powder, 15 percent of SiC powder and 14.5 g of PVB, and preparing composite tape-casting slurry suitable for tape casting, and preparing ZrO with flat and smooth surface, no cracks and no air holes2-a composite cast film sheet of SiC, the composite cast film sheet having an average thickness of about 100 microns.
ZrO2 is mixed with2Cast film and ZrO2Sequentially overlapping cast-SiC diaphragms and forming ZrO after isostatic pressing2Composite ceramic biscuit, then ZrO2And (4) carrying out glue discharging treatment on the composite ceramic biscuit.
ZrO after binder removal treatment2Sintering the composite ceramic biscuit, wherein segmented sintering is adopted in the sintering process, and the method specifically comprises the following steps:
firstly, with N2-O2The mixed gas is a sintering atmosphere, the total pressure of the gas is 0.15MPa, the oxygen partial pressure is 160Pa, and the mixed gas is heated to 650 ℃ and is kept for 40 minutes;
then, with N2Is sintering atmosphere, the total pressure of gas is 0.15MPa, the temperature is heated to 1450 ℃, the temperature is preserved for 120 minutes, and the zirconia ceramic material is prepared and obtained, the mark is 5#。
Comparative example 1
The preparation method comprises the steps of preparing a ZrO2-SiC tape casting membrane by using a tape casting method by using submicron zirconia powder with the average particle size of less than 1 mu m and the purity of more than 99% as a ceramic matrix, silicon carbide with the average particle size of 100 nanometers as a ceramic toughening phase, ethyl acetate as a solvent, dimethyl phthalate butyl benzyl ester BBP as a plasticizer and polyvinyl butyral ester PVB as a binder, and preparing the zirconia ceramic material by laminating, isostatic pressing, binder removal and atmosphere sintering. ZrO (ZrO)2The number of layers of the cast film sheet was the same as that of ZrO in example one2Cast film and ZrO2The total number of layers of the-SiC cast membrane is prepared as follows:
when the amount of ethyl acetate was 100 g and BBP was 10g, the composite powder (ZrO in the composite powder) was added2The mass percentage of the powder is 95%, the mass percentage of the SiC powder is 5%) 100 g and PVB14.5 g, so that the composite casting slurry suitable for casting is prepared, and meanwhile, the ZrO2-SiC casting film with a flat and smooth surface, no cracks and no air holes is prepared, and the average thickness is about 100 microns.
Sequentially overlapping ZrO2-SiC casting films and carrying out isostatic pressing to form a composite ZrO2 ceramic biscuit, and then carrying out binder removal treatment on the composite ZrO2 ceramic biscuit.
Sintering the zirconia biscuit after the binder removal treatment, wherein the sintering process comprises the following steps: n2 is used as sintering atmosphere, the total pressure of gas is 0.15MPa, the temperature is heated to 1450 ℃, and the temperature is preserved for 180 minutes. Preparation to give a zirconia ceramic Material, denoted 1'#。
Comparative example No. two
The preparation method comprises the steps of preparing a ceramic matrix from submicron zirconia powder, nano silicon carbide, ethyl acetate, dimethyl phthalate butyl benzyl ester BBP, a plasticizer and polyvinyl butyral PVB by a tape casting methodA ZrO2 cast film sheet and a ZrO2-SiC cast film sheet. And (3) laminating the casting membrane according to a preset structure, performing isostatic pressing, binder removal and sintering in an atmosphere to prepare the zirconia ceramic material. ZrO (ZrO)2Cast film and ZrO2The number of layers of-SiC cast films is the same as in example one, and specifically as follows:
when the amount of ethyl acetate is 100 g and the BBP is 10g, 100 g of ZrO2 powder and 14.5 g of PVB are added to prepare ZrO2 casting slurry suitable for casting, and a ZrO2 casting film with a flat and smooth surface, no cracks and no air holes is prepared at the same time, and the average thickness is about 100 microns.
When the amount of ethyl acetate was 100 g and BBP was 10g, the composite powder (ZrO in the composite powder) was added2The mass percentage of the powder is 95%, the mass percentage of the SiC powder is 5%) 100 g and PVB14.5 g, so that the composite casting slurry suitable for casting is prepared, and meanwhile, the ZrO2-SiC casting film with a flat and smooth surface, no cracks and no air holes is prepared, and the average thickness is about 100 microns.
And sequentially overlapping the ZrO2 casting diaphragm and the ZrO2-SiC casting diaphragm, performing isostatic pressing to form a composite ZrO2 ceramic biscuit, and then performing gel discharge treatment on the composite ZrO2 ceramic biscuit.
Sintering the zirconia biscuit after the binder removal treatment, wherein the sintering process comprises the following steps: n2 is used as sintering atmosphere, the total pressure of gas is 0.15MPa, the temperature is heated to 1450 ℃, and the temperature is preserved for 180 minutes. Preparation to give a ceramic zirconia material, denoted 2'#。
And (3) performance testing:
and (3) testing the bending strength: according to the specification of the fine ceramic bending strength test standard (GB/T6569-2006), the zirconia ceramic material 1 prepared by the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment is subjected to three-point bending on a CSS-44100 electronic universal tester#、2#、3#、4#And 5#And 1 'of zirconia ceramic material prepared in comparative example I and comparative example II'#And 2'#The bending strength of (2) was tested. Five samples of each of the above zirconia ceramic materials were taken for measurement, and see table 1, and the experimental results in table 1 are the average of the measured values of 5 samples.
And (3) testing fracture toughness: according to the regulation of (GB/T23806-2009), various zirconia ceramic materials 1 are subjected to a three-point bending fracture method by adopting a single-side notched beam on a CSS-44100 electronic universal testing machine#、2#、3#、4#、5#、1’#And 2'#The fracture toughness of five samples is tested, and the load loading direction is vertical to the laminated surface of the sample to be tested. Referring to table 1, the experimental results in table 1 are the average of the measured values of 5 samples.
And (3) anti-drop test: the zirconia ceramic materials 1 in five examples and two comparative examples were taken#、2#、3#、4#、5#、1’#And 2'#Five specimens were processed to have a length of 70mm × 30mm × 0.5mm, and each of the five specimens was brought into contact with the ground in a free-fall manner from a height of 2.5 m, and the average number of falling resistance times was determined for each of 5 specimens, as shown in table 1.
And (3) hardness testing: according to the regulations (GB/T16534-2009), various zirconia ceramic materials 1 are processed on an HVS-5 Vickers hardness tester#、2#、3#、4#、5#、1’#And 2'#The hardness of five samples of (1) was tested. Referring to table 1, the experimental results in table 1 are the average of the measured values of 5 samples.
TABLE 1
Figure BDA0002611886720000121
Figure BDA0002611886720000131
In conclusion, the zirconia ceramic material 3 prepared in example three#Under the condition that the SiC content in the ZrO2-SiC casting film is 8 percent and the sectional sintering is adopted, the fracture toughness of the composite zirconia ceramic material is optimal and reaches 16.6MPa.m1/2. Please refer to examples one to five and comparativeIn the first example, the fracture toughness of the zirconia ceramic material in all examples is higher than that of the ceramic material in the first comparative example without stacking. In addition, referring to example two and comparative example two, it was found that staged sintering can enhance the fracture toughness of the ceramic material.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A preparation method of a zirconia ceramic material is characterized by comprising the following steps:
dissolving zirconia powder in an organic solvent, adding a plasticizer and a binder to prepare zirconia casting slurry, and preparing a zirconia casting membrane by using casting molding;
dissolving mixed powder of zirconium oxide powder and silicon carbide powder in the organic solvent, adding a plasticizer and a binder to prepare composite casting slurry, and preparing a composite casting membrane by using casting molding;
sequentially and alternately stacking the zirconia casting membrane and the composite casting membrane to obtain a plurality of laminated membranes, and performing isostatic pressing on the plurality of laminated membranes to form a composite ceramic biscuit;
and removing the glue from the composite ceramic biscuit and sintering to obtain the zirconia ceramic material.
2. The method for preparing a zirconia ceramic material according to claim 1,
in the sintering process, the mixed gas of inert gas and oxygen is used as the sintering atmosphere, the mixed gas is heated to 600-fold-800 ℃ under the conditions that the total gas pressure is 0.05-0.15Mpa and the oxygen partial pressure is 140-fold-160 Pa, the temperature is kept for 20-40min, and then the mixed gas is heated to 1400-fold-1500 ℃ under the conditions that the total gas pressure is 0.05-0.15Mpa and the temperature is kept for 30-180 min.
3. The method of preparing a zirconia ceramic material according to claim 1 or 2, wherein the silicon carbide content in said composite cast membrane is 1 to 15 wt%.
4. The method of preparing a zirconia ceramic material according to claim 1, wherein said zirconia cast sheet and said composite cast sheet each have a thickness in the range of 50 to 200 μm.
5. The method for preparing zirconia ceramic material as described in claim 1, wherein the zirconia powder is 100-1000nm spherical particles or quasi-spherical particles.
6. The method of claim 1, wherein the silicon carbide powder has an average particle size of less than 100 nm.
7. A zirconia ceramic material, wherein the zirconia ceramic material is produced by the method of producing the zirconia ceramic material according to any one of claims 1 to 6.
8. A housing made from the zirconia ceramic material of claim 7.
9. An electronic device, characterized in that the electronic device comprises the housing of claim 8.
CN202010756952.1A 2020-07-31 2020-07-31 Zirconia ceramic material and preparation method and application thereof Pending CN112028625A (en)

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