CN112028638B - Ceramic material and preparation method and application thereof - Google Patents
Ceramic material and preparation method and application thereof Download PDFInfo
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- CN112028638B CN112028638B CN202010758268.7A CN202010758268A CN112028638B CN 112028638 B CN112028638 B CN 112028638B CN 202010758268 A CN202010758268 A CN 202010758268A CN 112028638 B CN112028638 B CN 112028638B
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Abstract
The invention provides a ceramic material and a preparation method and application thereof, wherein the preparation method of the ceramic material comprises the following steps: the method comprises the steps of obtaining a first diaphragm by carrying out tape casting on ceramic slurry, cutting the first diaphragm into a plurality of second diaphragms, stacking the plurality of second diaphragms in a layered staggered stacking mode to obtain a first stacked diaphragm and a second stacked diaphragm with different layers, obtaining a first ceramic biscuit and a second ceramic biscuit by respectively carrying out isostatic pressing and glue discharging treatment, forming first ceramic by using the first ceramic biscuit with a large number of layers through one-time sintering treatment, coating the first ceramic on the second ceramic biscuit with a small number of layers to cover the surface of the first ceramic, and then obtaining the second ceramic by using secondary sintering. The outer layer of the ceramic material prepared by the preparation method of the invention has higher hardness than the core part and lower toughness and strength than the core part, so that the ceramic material has high hardness, high toughness and wear resistance.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a 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 and the like, and can be used as a structural material; ceramics also have certain special properties and can be used as functional materials.
The conventional ceramic has low hardness and bending strength and low toughness, so that the ceramic material has limitation in the application process, particularly when the ceramic material is used for a shell of electronic equipment, the shell has poor wear resistance, and cracks are easy to appear if the ceramic material falls off in the use process, so that the service life of the electronic equipment is greatly shortened.
In view of this, a new ceramic material, a method for its preparation and its use are provided.
Disclosure of Invention
The present invention aims to overcome the above defects of the prior art and provide a ceramic material, a preparation method and an application thereof.
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 ceramic material, the method comprising:
mixing ceramic powder and an additive, carrying out ball milling to obtain casting slurry, and carrying out casting molding on the casting slurry to obtain a first membrane;
cutting the first membrane into a plurality of second membranes, and respectively stacking the second membranes in a layering staggered stacking mode to form a first stacked membrane and a second stacked membrane, wherein the number of stacked layers of the first stacked membrane is larger than that of the second stacked membrane;
The first stacked diaphragm and the second stacked diaphragm are subjected to isostatic pressing and glue discharging in sequence to obtain a first ceramic biscuit and a second ceramic biscuit respectively;
the first ceramic biscuit is sintered for one time to obtain first ceramic;
and sequentially laminating the second ceramic biscuit, the first ceramic and the second ceramic biscuit to enable the first ceramic to be clamped between two layers of the second ceramic biscuits, putting the second ceramic biscuits into a die for prepressing, and then performing secondary sintering to obtain the second ceramic.
Preferably, the stacking a plurality of the second membrane sheets in a layered staggered manner to form a first stacked membrane sheet and a second stacked membrane sheet respectively includes: in the process of layering and staggered stacking, an aluminum oxide layer is stacked between adjacent second membrane arrangement layers and comprises an aluminum oxide membrane layer and/or an aluminum oxide spraying layer;
and/or, during the layering and dislocation stacking process, the second membrane sheets adjacent to each layer are partially overlapped.
Preferably, the primary sintering is air sintering, and the conditions of the primary sintering include: and heating and sintering the first ceramic biscuit in an air atmosphere, and when the sintering temperature is raised to a first highest sintering temperature, preserving the temperature for 30-60min, and then cooling, wherein the first highest sintering temperature is 1350-1600 ℃.
Preferably, the conditions of the primary sintering further include: in the heating process, when the sintering temperature is increased from room temperature to 1000 ℃, the heating speed is 10-15 ℃/min, and the temperature is kept at 1000 ℃ for 60 min; when the sintering temperature is increased from 1000 ℃ to 1200 ℃, the temperature increasing speed is 10-15 ℃/min, and the temperature is kept at 1200 ℃ for 60 min; when the sintering temperature is increased from 1200 ℃ to the first highest sintering temperature, the temperature increasing speed is 5-10 ℃/min;
in the cooling process, when the sintering temperature is reduced to 1200 ℃ from the first highest sintering temperature, the cooling speed is 5-10 ℃/min; and cooling along with the furnace when the sintering temperature is reduced to 1200 ℃.
Preferably, the secondary sintering is spark plasma sintering, and the secondary sintering conditions include: when the sintering temperature is increased to 1000 ℃, starting to apply pressure of 30-50MPa, when the sintering temperature is increased to the second highest sintering temperature, starting to preserve heat and finish pressurizing, preserving heat for 1-10min, cooling to 800 ℃, then unloading pressure, and then cooling along with the furnace; wherein the second maximum sintering temperature is greater than or equal to 1300 ℃ and less than 1350 ℃.
Preferably, the conditions of the secondary sintering further include: in the temperature rising process, when the sintering temperature rises from room temperature to 800 ℃, the temperature rising speed is 15-20 ℃/min; when the sintering temperature is increased from 800 ℃ to 1000 ℃, the temperature increasing speed is 30-40 ℃/min; when the sintering temperature is increased from 1000 ℃ to the second highest sintering temperature, the temperature increasing speed is 40-50 ℃/min;
In the cooling process, when the sintering temperature is reduced to 800 ℃ from the second highest sintering temperature, the cooling speed is 30-40 ℃/min.
Preferably, the first film sheet casting conditions include: the casting temperature is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane is 100-500 mu m.
The invention also provides a ceramic material prepared by the preparation method of the ceramic material.
The invention also provides a cover body which is prepared from the ceramic material.
The invention also provides electronic equipment which comprises the cover body.
The invention has the beneficial effects that the ceramic material and the preparation method and the application thereof are provided, and the preparation method of the ceramic material comprises the following steps: the method comprises the steps of carrying out tape casting molding on ceramic slurry to obtain a first diaphragm, cutting the first diaphragm into a plurality of second diaphragms, stacking the plurality of second diaphragms in a layered staggered stacking mode, respectively obtaining a first stacked diaphragm and a second stacked diaphragm with different layers, respectively carrying out isostatic pressing and glue removing treatment to obtain a first ceramic biscuit and a second ceramic biscuit, forming first ceramic by using the first ceramic biscuit with a plurality of layers through one-time sintering treatment, coating the first ceramic on the second ceramic biscuit with a small number of layers to cover the surface of the first ceramic, and then obtaining second ceramic by using secondary sintering. The outer layer of the ceramic material prepared by the preparation method of the invention has higher hardness than the core part, but lower toughness and strength than the core part, so that the ceramic material has high hardness, high toughness and wear resistance.
Drawings
FIG. 1 is a flow chart of a method for preparing a ceramic material according to an embodiment of the present invention.
FIG. 2 is a schematic structural view of a first stacked membrane and a second stacked membrane stacked in a layered and staggered manner according to an embodiment of the present invention.
FIG. 3 is a schematic view showing a stacked structure of a first stacked membrane sheet and a second stacked membrane sheet of a comparative example 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.
The invention provides a preparation method of a ceramic material, which comprises the following steps:
and step S1, mixing and ball-milling the ceramic powder and the additive to obtain casting slurry, and carrying out casting molding on the casting slurry to obtain the first diaphragm. Optionally, the ceramic powder includes, but is not limited to, at least one of zirconia powder, silicon nitride powder, nano-system alumina powder, silicon carbide powder, and complex phase ceramic powder. Optionally, the ceramic powder may be doped with a portion of a stabilizer, which is yttria. Optionally, the additives include dispersants and plasticizers. Optionally, the casting conditions for casting the casting slurry to form the first membrane sheet include: the casting temperature is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane is 100-500 mu m. In the embodiment of the invention, the casting membrane prepared by casting has less defects and uniform components, the microstructure of the sintered ceramic is more uniform than that of the ceramic prepared by dry pressing, and the sintered ceramic has less microscopic defects (pores) and better performance.
Step S2, cutting the first membrane into a plurality of second membranes, and stacking the plurality of second membranes in a layered staggered stacking manner to form a first stacked membrane and a second stacked membrane, wherein the number of stacked layers of the first stacked membrane is larger than that of the second stacked membrane. Preferably, the second membrane is rectangular with the same size. Optionally, the second diaphragm has a size of 100mmx100 mm.
Specifically, as shown in fig. 2, the square second membrane is stacked and laid in a staggered layering and stacking manner, where the staggered layering and stacking manner is as follows: in the transverse direction, the plurality of second film sheets are sequentially and adjacently connected to form second film sheet arrangement layers A, B and C, and no gap is left between the adjacent second film sheets; and arranging and laminating a plurality of second film sheets in the longitudinal direction, wherein the joints n of the second film sheets in the adjacent second film sheet arrangement layers are staggered with each other. Alternatively, in the transverse direction, adjacent second membranes at least partially overlap when being arranged, for example, the joint n between the second membrane 11 and the second membrane 12 should be formed after a part of the second membrane 11 and a part of the second membrane 12 overlap, and the overlapped part is used for supplementing cracks formed by material loss when the abutting surface of the second membrane 11 and the second membrane 12 abuts is sintered. The second membrane is stacked in a layered and staggered manner in the subsequent sintering process, so that the expansion of cracks is hindered or the path of the expansion is lengthened, and the mechanical properties such as fracture toughness and the like of the prepared ceramic material can be improved.
And step S3, carrying out isostatic pressing and glue discharging on the first stacked membrane and the second stacked membrane in sequence to respectively obtain a first ceramic biscuit and a second ceramic biscuit.
Step S4, the first ceramic biscuit is sintered for one time to obtain first ceramic; and sequentially laminating the second ceramic biscuit, the first ceramic and the second ceramic biscuit to enable the first ceramic to be clamped between two layers of the second ceramic biscuits, putting the second ceramic biscuits into a die for prepressing, and then sintering for the second time to obtain the second ceramic. After the first ceramic is obtained and subjected to surface grinding, the two outer surfaces of the ground first ceramic are covered with a second ceramic biscuit so that the first ceramic serves as a core and the second ceramic biscuit serves as an outer layer to clamp the core inside. The obtained second ceramic is subjected to subsequent machining to obtain the ceramic material.
Preferably, the primary sintering is air sintering, and the conditions of the primary sintering include: and heating and sintering the first ceramic biscuit in an air atmosphere, and when the sintering temperature is raised to a first maximum sintering temperature, preserving heat for 30-60min, and then cooling, wherein the first maximum sintering temperature is 1350-1600 ℃.
Preferably, the conditions of the primary sintering further include: in the temperature rising process, when the sintering temperature rises from room temperature to 1000 ℃, the temperature rising speed is 10-15 ℃/min, and the temperature is kept at 1000 ℃ for 60 min; when the sintering temperature is increased from 1000 ℃ to 1200 ℃, the temperature increasing speed is 10-15 ℃/min, and the temperature is kept at 1200 ℃ for 60 min; when the sintering temperature is increased from 1200 ℃ to the first highest sintering temperature, the temperature increasing speed is 5-10 ℃/min;
In the cooling process, when the sintering temperature is reduced to 1200 ℃ from the first highest sintering temperature, the cooling speed is 5-10 ℃/min; and cooling along with the furnace when the sintering temperature is reduced to 1200 ℃.
Preferably, the secondary sintering is spark plasma sintering, and the secondary sintering conditions include: when the sintering temperature is increased to 1000 ℃, starting to apply pressure of 30-50MPa, when the sintering temperature is increased to the second highest sintering temperature, starting to preserve heat and finish pressurizing, preserving heat for 1-10min, cooling to 800 ℃, then unloading pressure, and then cooling along with the furnace; wherein the second highest sintering temperature is greater than or equal to 1300 ℃ and less than 1350 ℃.
Preferably, the conditions of the secondary sintering further include: in the temperature rising process, when the sintering temperature rises from room temperature to 800 ℃, the temperature rising speed is 15-20 ℃/min; when the sintering temperature is increased from 800 ℃ to 1000 ℃, the temperature increasing speed is 30-40 ℃/min; when the sintering temperature is increased from 1000 ℃ to the second highest sintering temperature, the temperature increasing speed is 40-50 ℃/min;
in the cooling process, when the sintering temperature is reduced to 800 ℃ from the second highest sintering temperature, the cooling speed is 30-40 ℃/min.
Wherein the second highest sintering temperature of the spark plasma sintering is lower than the first highest sintering temperature of the air atmosphere sintering, so that the core part (first ceramic) is equivalent to aging treatment in a short time in the spark plasma sintering process. The short-time aging treatment has the following effects: on one hand, the method is favorable for forming stable tetragonal phase (zirconia), the metastable tetragonal phase (zirconia) is subjected to martensite transformation under the induction of external force, the transformation from the tetragonal phase to the monoclinic phase is realized, and the volume expansion of ceramic crystal grains forms compressive stress on the inside, so that the strength of the ceramic material is improved; secondly, the grain structure is more complete, the grain size is increased in a small range, the grain size formed in the embodiment of the invention is between 1.8 and 2 microns and is lower than the critical transformation size of tetragonal phase (zirconia) by 2.2 microns, when the grain size is smaller than the critical transformation size of ceramic (zirconia), the stress induced phase transformation amount is increased along with the increase of the grain size under the induction of external force, the phase transformation amount is larger, the fracture toughness of the ceramic material is larger, and when the grain size is between 1.8 and 2 microns, the tetragonal phase (zirconia) is more favorably existed, and in the size range, the content of the tetragonal phase (zirconia) is relatively larger.
For the surface material (second ceramic biscuit formation), spark plasma sintering is used for rapid densification to form fine grains, which is beneficial to improving the hardness and thus also improving the wear resistance of the material. In conclusion, the surface layer has fine crystal grains and the core part has relatively large crystal grains, the surface layer has higher hardness than the core part and lower toughness and strength than the core part, and thus the ceramic with high hardness and high toughness is prepared.
On the basis of the above embodiment, it is preferable that, in the step S2, during the process of stacking the plurality of second membrane sheets in a staggered manner, an aluminum oxide layer is stacked between the adjacent second membrane sheet alignment layers A, B, C. Optionally, the alumina layer comprises an alumina film layer and/or an alumina spray coating. When the alumina layer is an alumina membrane layer, as shown in fig. 2, alumina membranes are stacked between the adjacent second membrane alignment layers A, B, C in the longitudinal direction, and the thickness of the alumina membranes is about 50 μm, although the thinner the thickness of the alumina membranes is, the better the thickness is; when the aluminum oxide layer is an aluminum oxide spray coating layer, an aluminum oxide solution (which may also be simple-substance aluminum powder, and aluminum powder may also form aluminum oxide after sintering) prepared from a volatile solution is sprayed into the gap formed between the adjacent second membrane arrangement layers, and other components in the aluminum oxide solution volatilize (aluminum oxide powder is dissolved by alcohol). After sintering, the alumina is doped into the adjacent second membrane arrangement layer (namely, the ceramic material), so that gaps or holes formed among the second membranes formed by the ceramic can be avoided, the interface strength among the second membranes is improved, and the mechanical properties such as strength, toughness and the like of the prepared ceramic material are improved.
According to the preparation method of the ceramic material, the first stacked membrane and the second stacked membrane with different layers are respectively formed in a layered staggered stacking mode, the first ceramic biscuit and the second ceramic biscuit are respectively obtained through isostatic pressing and glue discharging, the first ceramic biscuit with the large layer number is processed through air sintering to form the first ceramic, the second ceramic biscuit with the small layer number is coated with the first ceramic to cover the surface of the first ceramic, and then secondary sintering is carried out through spark plasma sintering to obtain the second ceramic. The outer layer (formed from the second ceramic biscuit) of the ceramic material is made with fine crystal grains and the core (formed from the first ceramic biscuit) is made with relatively large crystal grains, so that the outer layer of the ceramic material is made with a higher hardness than the core but with a lower toughness and strength than the core, thereby giving the ceramic material a high hardness, a high toughness and a wear resistance.
The invention also provides a ceramic material, which is prepared by the preparation method of the ceramic material. The surface layer of the ceramic material provided by the invention has higher hardness than the core part, and the toughness and the strength of the ceramic material are lower than those of the core part, so that the ceramic material has high hardness, high toughness and wear resistance.
The invention also provides a cover body which is made of the ceramic material. In the embodiment of the invention, the cover body prepared by the ceramic material has high-grade texture and hand feeling, and simultaneously, the high hardness, high toughness and wear resistance of the cover body are improved, so that the service life of the cover body is greatly prolonged.
The invention further provides an electronic device, which includes the cover body according to the embodiment of the invention. Of course, those skilled in the art will appreciate that the electronic device has all the features and advantages of the ceramic material and the cover body described above, and the description thereof is omitted here. According to the embodiment of the invention, the specific type of the electronic device has no limitation requirement, and a person skilled in the art can flexibly select the electronic device according to actual requirements. In some embodiments of the present invention, specific types of electronic devices include, but are not limited to, mobile phones, notebooks, game machines, and the like. Of course, it can be understood by those skilled in the art that the electronic device includes necessary structures or components of a conventional electronic device besides the front housing, and for example, the mobile phone includes necessary structures or components of a display panel, a glass cover plate, a CPU processor, a camera module, a voice module, a touch module, and the like besides the front housing.
Further understanding is provided below by way of specific examples and comparative examples.
Example one
Step S1, mixing and ball-milling zirconia powder with the average particle size of 0.642 mu m and containing 3 mol% of yttria, a dispersant, a plasticizer and ball-milling liquid in a ball mill, wherein zirconia balls are used as grinding balls (the material-ball ratio is 1: 2), the rotating speed of the ball mill is 400 r/min, and the ball-milling time is 24 hours until the zirconia powder is uniformly dispersed in the solution to form casting slurry. Pouring the casting slurry into a hopper of a casting machine, adjusting the height of a scraper, casting the casting slurry on a base band under the drive of the scraper, wherein the casting temperature in the casting process is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane after casting is about 100-500 mu m.
Step S2, cutting the first film sheet into a square of 100mmx100mm to obtain a plurality of second film sheets, stacking the plurality of second film sheets in a layered staggered stacking manner, and stacking 40 layers of casting films and 20 layers of casting films respectively to obtain a first stacked film sheet and a second stacked film sheet correspondingly.
And step S3, cutting the first stacked membrane and the second stacked membrane into regular shapes, and then sequentially carrying out isostatic pressing and binder removal to obtain a zirconium oxide biscuit I and a zirconium oxide biscuit II.
And step S4, sintering the zirconia biscuit to prepare the zirconia ceramic.
And step S41, sintering in air atmosphere to obtain the first zirconia ceramic. The method specifically comprises the following steps:
and (3) placing the zirconia biscuit I in a sintering furnace, and heating and sintering in an air atmosphere, wherein the maximum sintering temperature is 1500 ℃. The heating rate and holding time of different temperature sections are as follows (T1 is the sintering temperature in the air sintering process): keeping the temperature for 60min at the room temperature of less than T1 and less than or equal to 1000 ℃ and at the temperature of 15 ℃/min; t1 is more than 1000 ℃ and less than or equal to 1200 ℃, 10 ℃/min, and the temperature is kept for 60 min; t1 is more than 1200 ℃ and less than or equal to 1500 ℃, the temperature is kept for 30-60min at 5 ℃/min; and after the heat preservation at 1500 ℃, cooling to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling along with the furnace to obtain the zirconia ceramic I.
And step S42, performing spark plasma sintering to obtain a second zirconia ceramic. The method specifically comprises the following steps:
The upper surface and the lower surface of the zirconia ceramic I are ground to be used as a core part of a ceramic sample, and the upper surface and the lower surface of the zirconia ceramic I are covered with a zirconia biscuit II. And wrapping the zirconia biscuit II with the zirconia ceramic I, prepressing in a mould, and sintering in a plasma sintering furnace. When the temperature rises to 1000 ℃, the pressurization is started, when the heat preservation is started, the pressurization is finished, the pressure is 40MPa, and the pressure relief is started after the heat preservation is finished. The temperature rise speed and the heat preservation time of different temperature sections are as follows (T2 is the sintering temperature in the spark plasma sintering process): the room temperature is less than T2 and less than or equal to 800 ℃, and the temperature is 20 ℃/min; t2 is more than 800 ℃ and less than or equal to 1000 ℃, 40 ℃/min; keeping the temperature at 1000 ℃ and T2 being less than or equal to 1300 ℃ and 50 ℃/min for 1-10 min; and after the heat preservation at 1300 ℃ is finished, cooling to 800 ℃ at a cooling speed of 40 ℃/min, and then cooling along with the furnace to obtain the zirconium oxide ceramic II. And grinding, polishing and other machining processes are carried out on the zirconia ceramic II to obtain a zirconia ceramic material sample 1.
Example two
Step S1, mixing and ball-milling zirconia powder with the average particle size of 0.642 mu m and containing 3 mol% of yttria, a dispersant, a plasticizer and ball-milling liquid in a ball mill, wherein zirconia balls are used as grinding balls (the material-ball ratio is 1: 2), the rotating speed of the ball mill is 400 r/min, and the ball-milling time is 24 hours until the zirconia powder is uniformly dispersed in the solution to form casting slurry. Pouring the casting slurry into a hopper of a casting machine, adjusting the height of a scraper, casting the casting slurry on a base band under the driving of the scraper, wherein the casting temperature in the casting process is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane after casting is about 100-500 mu m.
Step S2, cutting the first film sheet into a square of 100mmx100mm to obtain a plurality of second film sheets, stacking the plurality of second film sheets in a layered staggered stacking manner, and stacking 40 layers of casting films and 20 layers of casting films respectively to obtain a first stacked film sheet and a second stacked film sheet correspondingly.
And step S3, cutting the first stacked membrane and the second stacked membrane into regular shapes, and then sequentially carrying out isostatic pressing and binder removal to obtain a zirconium oxide biscuit I and a zirconium oxide biscuit II.
And step S4, sintering the zirconia biscuit in an air atmosphere to prepare the zirconia ceramic.
The method comprises the following specific steps: wrapping the zirconia biscuit II with the zirconia ceramic biscuit I, pre-pressing in a mold, placing in a sintering furnace, and heating and sintering in an air atmosphere, wherein the maximum sintering temperature is 1500 ℃. The heating rate and the holding time of different temperature sections are as follows (T1 is the sintering temperature in the air sintering process): keeping the temperature for 60min at the room temperature of less than T1 and less than or equal to 1000 ℃ and at the temperature of 15 ℃/min; t1 is more than 1000 ℃ and less than or equal to 1200 ℃, 10 ℃/min, and the temperature is kept for 60 min; t1 is more than 1200 ℃ and less than or equal to 1500 ℃, the temperature is kept for 30-60min at 5 ℃/min; and after the heat preservation at 1500 ℃, cooling to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling along with the furnace to obtain the zirconia ceramic. And grinding, polishing and other machining processes are carried out on the zirconia ceramic to obtain a zirconia ceramic material sample 2.
EXAMPLE III
Step S1, mixing and ball-milling zirconia powder with the average particle size of 0.642 mu m and containing 3 mol% of yttria, a dispersant, a plasticizer and ball-milling liquid in a ball mill, wherein zirconia balls are used as grinding balls (the material-ball ratio is 1: 2), the rotating speed of the ball mill is 400 r/min, and the ball-milling time is 24 hours until the zirconia powder is uniformly dispersed in the solution to form casting slurry. Pouring the casting slurry into a hopper of a casting machine, adjusting the height of a scraper, casting the casting slurry on a base band under the drive of the scraper, wherein the casting temperature in the casting process is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane after casting is about 100-500 mu m.
Step S2, cutting the first film sheet into a square of 100mmx100mm to obtain a plurality of second film sheets, stacking the plurality of second film sheets in a layered staggered stacking manner, and stacking 40 layers of casting films and 20 layers of casting films respectively to obtain a first stacked film sheet and a second stacked film sheet correspondingly.
And step S3, cutting the first stacked membrane and the second stacked membrane into regular shapes, and then sequentially carrying out isostatic pressing and binder removal to obtain a zirconium oxide biscuit I and a zirconium oxide biscuit II.
Step S4, sintering the zirconia biscuit by discharge plasma to prepare zirconia ceramics.
The method comprises the following specific steps: and wrapping the zirconia biscuit II with the zirconia ceramic I, prepressing in a mould, and sintering in a plasma sintering furnace. When the temperature rises to 1000 ℃, the pressurization is started, when the heat preservation is started, the pressurization is finished, the pressure is 40MPa, and the pressure relief is started after the heat preservation is finished. The heating rate and the holding time of different temperature sections are as follows (T2 is the sintering temperature in the spark plasma sintering process): the room temperature is less than T2 and less than or equal to 800 ℃, and the temperature is 20 ℃/min; t2 is less than or equal to 1000 ℃ at 800 ℃, 40 ℃/min; keeping the temperature at 1000 ℃ and T2 being less than or equal to 1300 ℃ and 50 ℃/min for 1-10 min; and after the heat preservation at 1300 ℃ is finished, cooling to 800 ℃ at a cooling speed of 40 ℃/min, and then cooling along with the furnace to obtain the zirconium oxide ceramic II. And grinding, polishing and other machining processes are carried out on the zirconia ceramic II to obtain a zirconia ceramic material sample 3.
Comparative example
Step S1, mixing and ball-milling zirconia powder with the average particle size of 0.642 mu m and containing 3 mol% of yttria, a dispersant, a plasticizer and ball-milling liquid in a ball mill, wherein zirconia balls are used as grinding balls (the material-ball ratio is 1: 2), the rotating speed of the ball mill is 400 r/min, and the ball-milling time is 24 hours until the zirconia powder is uniformly dispersed in the solution to form casting slurry. Pouring the casting slurry into a hopper of a casting machine, adjusting the height of a scraper, casting the casting slurry on a base band under the driving of the scraper, wherein the casting temperature in the casting process is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane after casting is about 100-500 mu m.
Step S2, sequentially stacking 40 layers and 20 layers of the first film to obtain a first stacked film and a second stacked film, respectively, please refer to the stacking manner in fig. 3.
And step S3, cutting the first stacked membrane and the second stacked membrane into regular shapes, and then sequentially carrying out isostatic pressing and binder removal to obtain a zirconium oxide biscuit I and a zirconium oxide biscuit II.
And step S4, sintering the zirconia biscuit to prepare the zirconia ceramic.
And step S41, sintering in air atmosphere to obtain the first zirconia ceramic. The method comprises the following specific steps:
and (3) placing the zirconia biscuit I in a sintering furnace, and heating and sintering in an air atmosphere, wherein the maximum sintering temperature is 1500 ℃. The heating rate and holding time of different temperature sections are as follows (T1 is the sintering temperature in the air sintering process): keeping the temperature for 60min at the room temperature of less than T1 and less than or equal to 1000 ℃ at 15 ℃/min; t1 is more than 1000 ℃ and less than or equal to 1200 ℃, 10 ℃/min, and the temperature is kept for 60 min; t1 is more than 1200 ℃ and less than or equal to 1500 ℃, the temperature is kept for 30-60min at 5 ℃/min; and after the heat preservation at 1500 ℃, cooling to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling along with the furnace to obtain the zirconia ceramic I.
And step S42, performing spark plasma sintering to obtain a second zirconia ceramic. The method specifically comprises the following steps:
the upper surface and the lower surface of the zirconia ceramic I are ground to be used as a core part of a ceramic sample, and the upper surface and the lower surface of the zirconia ceramic I are covered with a zirconia biscuit II. And wrapping the zirconia biscuit II with the zirconia ceramic I, prepressing in a mould, and sintering in a plasma sintering furnace. When the temperature rises to 1000 ℃, the pressurization is started, when the heat preservation is started, the pressurization is finished, the pressure is 40MPa, and the pressure relief is started after the heat preservation is finished. The heating rate and the holding time of different temperature sections are as follows (T2 is the sintering temperature in the spark plasma sintering process): the room temperature is less than T2 and less than or equal to 800 ℃, and the temperature is 20 ℃/min; t2 is less than or equal to 1000 ℃ at 800 ℃, 40 ℃/min; keeping the temperature at 1000 ℃ and T2 being less than or equal to 1300 ℃ and 50 ℃/min for 1-10 min; and after the heat preservation at 1300 ℃ is finished, cooling to 800 ℃ at a cooling speed of 40 ℃/min, and then cooling along with the furnace to obtain the zirconium oxide ceramic II. And grinding, polishing and other machining processes are carried out on the zirconia ceramic II to obtain a zirconia ceramic material sample 4.
Detection result of performance of zirconia ceramic material
The mechanical properties of the zirconia ceramic materials prepared in the above examples one, two, three and comparative examples, sample 1, sample 2, sample 3 and sample 4, respectively, were examined. The detection results are shown in table 1:
TABLE 1
Please compare the mechanical property data of sample 1, sample 2 and sample 3 in table 1 with sample 4, it can be seen that the density, bending strength, hardness and fracture toughness of the zirconia ceramic material obtained by two times of sintering after layered, staggered and stacked are all higher than those of the zirconia ceramic material directly stacked. In addition, the density, the bending strength, the hardness and the fracture toughness of the zirconia ceramic material which is prepared by respectively carrying out air sintering and spark plasma sintering on the sample 1 in the table 1, compared with the mechanical property data of the sample 2 and the sample 3 after layering, staggered and stacking are higher than those of the zirconia ceramic material which is prepared by carrying out air sintering or uniform spark plasma sintering twice. In conclusion, the zirconia ceramic material prepared by the preparation method of the zirconia ceramic material provided by the embodiment of the invention has mechanical properties of high hardness, high fracture toughness, wear resistance and the like.
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 (10)
1. A method for preparing a ceramic material, the method comprising:
mixing ceramic powder and an additive, carrying out ball milling to obtain casting slurry, and carrying out casting molding on the casting slurry to obtain a first membrane;
cutting the first membrane into a plurality of second membranes, and respectively stacking the second membranes in a layering staggered stacking mode to form a first stacked membrane and a second stacked membrane, wherein the number of stacked layers of the first stacked membrane is larger than that of the second stacked membrane;
the first stacked membrane and the second stacked membrane are subjected to isostatic pressing and glue discharging in sequence to obtain a first ceramic biscuit and a second ceramic biscuit respectively;
the first ceramic biscuit is subjected to primary sintering to obtain first ceramic; the primary sintering is air sintering;
sequentially laminating the second ceramic biscuit, the first ceramic and the second ceramic biscuit to enable the first ceramic to be clamped between two layers of the second ceramic biscuits, putting the second ceramic biscuits into a die for prepressing, and then performing secondary sintering to obtain second ceramic; the secondary sintering is spark plasma sintering; the second highest sintering temperature of the secondary sintering is lower than the first highest sintering temperature of the primary sintering.
2. A process for the preparation of a ceramic material as claimed in claim 1,
the mode of piling up a plurality of the second diaphragm in the layering dislocation pile respectively forms first stack diaphragm and second and piles up the diaphragm, includes: in the process of layering and staggered stacking, an aluminum oxide layer is stacked between adjacent second membrane arrangement layers and comprises an aluminum oxide membrane layer and/or an aluminum oxide spraying layer;
and/or, during the layering and dislocation stacking process, the second membrane sheets adjacent to each layer are partially overlapped.
3. A process for the preparation of a ceramic material according to claim 1 or 2,
the conditions of the primary sintering comprise: and heating and sintering the first ceramic biscuit in an air atmosphere, and when the sintering temperature is raised to a first highest sintering temperature, preserving the temperature for 30-60min, and then cooling, wherein the first highest sintering temperature is 1350-1600 ℃.
4. A process for the preparation of a ceramic material as claimed in claim 3,
the conditions of the primary sintering further comprise: in the temperature rising process, when the sintering temperature rises from room temperature to 1000 ℃, the temperature rising speed is 10-15 ℃/min, and the temperature is kept at 1000 ℃ for 60 min; when the sintering temperature is increased from 1000 ℃ to 1200 ℃, the temperature increasing speed is 10-15 ℃/min, and the temperature is kept at 1200 ℃ for 60 min; when the sintering temperature is increased from 1200 ℃ to the first highest sintering temperature, the temperature increasing speed is 5-10 ℃/min;
In the cooling process, when the sintering temperature is reduced to 1200 ℃ from the first highest sintering temperature, the cooling speed is 5-10 ℃/min; and cooling along with the furnace when the sintering temperature is reduced to 1200 ℃.
5. Process for the preparation of a ceramic material according to claim 4,
the secondary sintering conditions include: when the sintering temperature rises to 1000 ℃, starting to apply pressure of 30-50MPa, when the sintering temperature rises to the second highest sintering temperature, starting to preserve heat and finish pressurization, preserving heat for 1-10min, cooling to 800 ℃, then relieving pressure, and then cooling along with the furnace; wherein the second maximum sintering temperature is greater than or equal to 1300 ℃ and less than 1350 ℃.
6. Process for the preparation of a ceramic material according to claim 5,
the conditions of the secondary sintering further comprise: in the temperature rising process, when the sintering temperature rises from room temperature to 800 ℃, the temperature rising speed is 15-20 ℃/min; when the sintering temperature is increased from 800 ℃ to 1000 ℃, the temperature increasing speed is 30-40 ℃/min; when the sintering temperature is increased from 1000 ℃ to the second highest sintering temperature, the temperature increasing speed is 40-50 ℃/min;
in the cooling process, when the sintering temperature is reduced to 800 ℃ from the second highest sintering temperature, the cooling speed is 30-40 ℃/min.
7. A process for the preparation of a ceramic material as claimed in claim 1,
the first film sheet casting conditions include: the casting temperature is 50-90 ℃, the casting speed is 0.5-5m/min, and the thickness of the first membrane is 100-500 mu m.
8. Ceramic material, characterized in that it is obtained by a method for the preparation of a ceramic material according to any one of claims 1 to 7.
9. A cap, characterized in that it is made of the ceramic material according to claim 8.
10. An electronic device characterized in that it comprises a cover according to claim 9.
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