CN115340367B - Alumina ceramic and preparation method and application thereof - Google Patents

Alumina ceramic and preparation method and application thereof Download PDF

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CN115340367B
CN115340367B CN202210987360.XA CN202210987360A CN115340367B CN 115340367 B CN115340367 B CN 115340367B CN 202210987360 A CN202210987360 A CN 202210987360A CN 115340367 B CN115340367 B CN 115340367B
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alumina ceramic
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陈文彬
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Hunan Sheng Ci Technology Co ltd
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Abstract

The invention belongs to the field of ceramic materials, and particularly relates to alumina ceramic, and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, adding water, a dispersing agent and a bonding agent into a ceramic composition for ball milling to obtain slurry, wherein the ceramic composition comprises the following components in percentage by mass: 65-95% of aluminum oxide, 3-30% of titanium dioxide, 0.2-1.5% of silicon dioxide, 0.2-3% of sintering aid and 0-5% of zinc oxide; s2, carrying out spray granulation on the slurry to obtain composite alumina powder; s3, carrying out dry press molding on the composite alumina powder, and then carrying out cold isostatic pressing molding to obtain a biscuit; s4, pre-sintering the biscuit in an oxygen-free atmosphere, and then performing hot isostatic pressing sintering to obtain the alumina ceramic. The alumina ceramic prepared by the preparation method has the characteristics of excellent antistatic property, high strength and high hardness.

Description

Alumina ceramic and preparation method and application thereof
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to alumina ceramic, and a preparation method and application thereof.
Background
In the increasingly developed electronic industry age today, various microelectronic and optoelectronic originals are very widely used. Static electricity is a common physical phenomenon, and electrostatic discharge can damage electronic elements, change the electrical properties of semiconductor components and damage electronic systems, so that the whole equipment is failed or malfunctioned; at the same time, when the static charges are released, static sparks are generated, and flammable and explosive materials are easy to ignite, so that great danger and economic loss are caused. The loss caused by static electricity hazard is more and more serious, so people pay attention to the anti-static phenomenon.
The ceramic material has the characteristics of good wear resistance, light weight, high strength, strong radiation resistance, acid and alkali resistance, corrosion resistance and difficult aging, and is an ideal antistatic material, so the high-performance antistatic ceramic has wide market prospect.
The antistatic ceramic is a new type antistatic material, and compared with the antistatic coating used before, the plastic has higher strength, wear resistance and corrosion resistance, is a permanent antistatic material, and is mainly applied to the fields of aviation, electronics, computers, chemical industry and the like, and is the most ideal antistatic material at present. The current research on antistatic ceramics is mainly focused on zirconia antistatic ceramics, and few researches on alumina antistatic ceramics are available.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide alumina ceramic, a preparation method and application thereof, and the alumina ceramic prepared by the preparation method has the characteristics of excellent antistatic performance, high strength and high hardness.
In order to achieve the above purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing alumina ceramic, comprising the steps of:
s1, adding water, a dispersing agent and a bonding agent into a ceramic composition for ball milling to obtain slurry, wherein the ceramic composition comprises the following components in percentage by mass: 65% -95% (e.g., may be 65%, 75%, 80%, 90%, 95%, etc.), 3% -30% (e.g., may be 3%, 5%, 15%, 20%, 30%, etc.), 0.2% -1.5% (e.g., may be 0.2%, 1%, 1.5%, etc.), 0.2% -3% (e.g., may be 0.2%, 1%, 2%, 3%, etc.), 0% -5% (e.g., may be 0, 1%, 2%, 3%, 4%, 5%, etc.), 0% -5% zinc oxide;
s2, carrying out spray granulation on the slurry to obtain composite alumina powder;
s3, carrying out dry press molding on the composite alumina powder, and then carrying out cold isostatic pressing molding to obtain a biscuit;
s4, pre-sintering the biscuit in an oxygen-free atmosphere, and then performing hot isostatic pressing sintering to obtain the alumina ceramic.
The preparation method provided by the invention is simple to operate and low in equipment requirement, and the prepared alumina ceramic has the characteristics of excellent antistatic property, high strength and high hardness.
In the preparation method of the alumina ceramic, as a preferred embodiment, the ceramic composition comprises the following components in percentage by mass:
Figure BDA0003802713360000021
the alumina ceramic prepared by the embodiment of the invention has excellent antistatic performance.
In the above method for preparing alumina ceramic, as a preferred embodiment, the sintering aid includes at least one of yttrium oxide, calcium oxide, niobium oxide, and cerium oxide.
In the above method for preparing alumina ceramic, as a preferred embodiment, the dispersant includes at least one of ammonium polyacrylate and ammonium citrate.
In the above method for preparing alumina ceramic, as a preferred embodiment, the binder includes at least one of polyvinyl alcohol and polyvinyl pyrrolidone.
In the above-mentioned method for producing alumina ceramic, as a preferred embodiment, the dispersant is added in an amount of 0.2 to 1wt% (for example, may be 0.2wt%, 0.4wt%, 0.6wt%, 0.8wt%, 1wt%, or the like) based on the total amount of the components in the ceramic composition.
In the above-mentioned method for producing alumina ceramic, as a preferred embodiment, the binder is added in an amount of 0.2 to 1.2wt% (for example, 0.2wt%, 0.4wt%, 0.6wt%, 0.8wt%, 1wt%, 1.2wt%, or the like) based on the total amount of the components in the ceramic composition.
In the above method for preparing alumina ceramic, as a preferred embodiment, in step S1, the volume ratio of the balls, the material and the water is (2-4): (0.5-1.5), wherein the material includes the ceramic composition, the dispersant and the binder.
In the above method for preparing alumina ceramic, as a preferred embodiment, in step S1, the adding water, dispersant and binder to the ceramic composition is ball-milled to obtain slurry, which includes:
placing the ceramic composition into a ball milling tank, adding the water and the dispersing agent, and mixing at a speed of 60-300 r.min -1 The rotational speed of (e.g. may be 60 r.min -1 、100r·min -1 、150r·min -1 、200r·min -1 、250r·min -1 Or 300 r.min -1 ) Ball milling for 40-80 hours (such as ball milling for 40 hours, 50 hours, 60 hours, 70 hours or 80 hours, etc.), adding the adhesive, and continuing ball milling for 5-15 hours (such as ball milling for 5 hours, 10 hours or 15 hours, etc.), thus obtaining the slurry.
In the above method for preparing alumina ceramic, as a preferred embodiment, the spray granulation process is as follows: the inlet temperature is 200-300 ℃ (for example, the inlet temperature can be 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃ or 300 ℃ and the like), the outlet temperature is 100-200 ℃ (for example, the outlet temperature can be 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃ or 200 ℃ and the like), the negative pressure is 40-60 Pa (for example, the negative pressure can be 40Pa, 50Pa or 60Pa and the like), the atomizer frequency is 15-25 HZ (for example, the atomizer frequency can be 15HZ, 20HZ or 25HZ and the like), the atomizer rotating speed is 8000-9000 r/min (for example, the atomizer rotating speed can be 8000r/min, 8500r/min or 9000r/min and the like), and the feed pump speed is 25-30 mL/min.
In the above-mentioned method for producing alumina ceramic, as a preferred embodiment, in step S2, the slurry is passed through a 150 to 250 mesh screen (for example, 150 mesh screen, 200 mesh screen, 250 mesh screen, or the like) before the spray granulation.
In the above-mentioned method for producing alumina ceramic, in step S2, after the spray granulation, the powder obtained by the spray granulation is screened by a double-layer screen, the composite alumina powder is used as a screen material, the upper layer screen mesh of the double-layer screen is 60 to 90 mesh (for example, the upper layer screen mesh may be 60 mesh, 70 mesh, 80 mesh or 90 mesh), and the lower layer screen mesh is 150 to 250 mesh (for example, the lower layer screen mesh is 150 mesh, 200 mesh or 250 mesh). Taking undersize of the upper layer sieve, then adopting the lower layer sieve to further sieve, and taking the undersize as composite alumina powder.
In the above method for preparing alumina ceramic, as a preferred embodiment, the conditions for dry press molding include: the dry press molding pressure is 5 to 50MPa (for example, the molding pressure can be 5MPa, 10MPa, 20MPa, 30MPa, 40MPa or 50MPa, etc.), and the holding time is 3 to 10min (for example, 3min, 5min, 7min, 9min or 10min, etc.).
In the above method for preparing alumina ceramic, as a preferred embodiment, the conditions for cold isostatic pressing include: the cold isostatic pressing pressure is 150-350MPa (for example, the cold isostatic pressing pressure is 150MPa, 200MPa, 250MPa, 300MPa or 350MPa, etc.), and the holding time is 5-15 min (for example, 5min, 7min, 9min, 11min, 13min or 15min, etc.).
According to the embodiment of the invention, the density of the biscuit can be controlled within the range of 40-55% of the theoretical density of the alumina ceramic by limiting the conditions of dry isostatic pressing and cold isostatic pressing.
According to the embodiment of the invention, the large-size alumina ceramic can be prepared by limiting the process of molding and then sintering, for example, the size of the alumina ceramic can be a cylinder with the diameter of 800mm and the thickness of 30mm or a cuboid with the length of 1200mm, the width of 500mm and the thickness of 30 mm.
In the above method for producing alumina ceramic, as a preferred embodiment, the oxygen-free atmosphere is at least one of argon, nitrogen, hydrogen, carbon monoxide, and vacuum atmosphere.
In the above method for preparing alumina ceramic, as a preferred embodiment, the pre-sintering process includes: the temperature is raised from room temperature to 1400 to 1600 ℃ over 20 to 60 hours (for example, 20 hours, 30 hours, 40 hours, 50 hours, 60 hours, etc.), and the temperature is kept for 2 to 8 hours (for example, 2 hours, 4 hours, 6 hours, 8 hours, etc.), and finally the temperature is naturally cooled to room temperature.
In the above method for producing alumina ceramic, as a preferred embodiment, the pressure of the hot isostatic pressing sintering is 100 to 200mpa (for example, 100 mpa, 120 mpa, 140 mpa, 160 mpa, 180 mpa, 200mpa, or the like), the atmosphere of the hot isostatic pressing sintering is argon, the temperature of the hot isostatic pressing sintering is 1300 to 1450 ℃ (for example, the temperature may be 1300 ℃, 1350 ℃, 1400 ℃, 1450 ℃, or the like), and the time of the hot isostatic pressing sintering is 10 to 20 hours (for example, 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, or the like).
In the above method for preparing alumina ceramic, in step S4, the green body is first embedded in an embedding powder and pre-sintered in an oxygen-free atmosphere, wherein the embedding powder includes at least one of graphene, graphite, silicon carbide, and tungsten carbide.
According to the embodiment of the invention, the black alumina ceramic with uniform color can be prepared by burying and sintering the biscuit powder, so that the resistance of the alumina ceramic is reduced, and the antistatic performance of the alumina ceramic is improved.
In the above-mentioned method for producing alumina ceramics, as a preferred embodiment, alumina ceramics having different surface resistances and different colors can be obtained by adjusting the kind of the oxygen-free atmosphere in step S4.
In a second aspect, the present invention provides an alumina ceramic prepared by the method for preparing an alumina ceramic according to the first aspect.
The alumina ceramic provided by the invention has the advantages of antistatic property, high strength and high hardness.
In the above alumina ceramic, as a preferred embodiment, the surface resistance of the alumina ceramic is 10 5 ~10 10 Ohm, e.g. the aluminium oxide ceramic has a surface resistance of 10 5 Ohm, 10 6 Ohm, 10 7 Ohm, 10 8 Ohm, 10 9 Ohm or 10 10 Ohmic, etc.
In the alumina ceramic, as a preferable embodiment, the flexural strength of the alumina ceramic is 350 to 600 mpa, and for example, the strength may be 350mpa, 380 mpa, 450 mpa, 500 mpa, 600 mpa, or the like.
In the alumina ceramic, as a preferable embodiment, the alumina ceramic has a vickers hardness of 1500 to 1800HV, for example, 1500HV, 1600HV, 1700HV, 1800HV, or the like.
In the above alumina ceramic, as a preferred embodiment, the density of the alumina ceramic is 3.6 to 4.4 g/cc.
In a third aspect, the present invention provides the use of an alumina ceramic according to the second aspect for the preparation of an antistatic material.
By using the alumina ceramic provided by the invention, the damage of static electricity to electronic components can be prevented and controlled in the production process of assembling and connecting spacecraft electronic products, and the damage of the components is prevented from directly affecting the quality and reliability of the spacecraft.
Compared with the prior art, the invention has the beneficial technical effects that the invention at least comprises one of the following:
(1) The preparation method provided by the invention is simple to operate and low in equipment requirement, and the prepared alumina ceramic has the characteristics of excellent antistatic property, high strength and high hardness.
(2) The alumina ceramic prepared by the invention has the advantages of wear resistance, high temperature resistance, corrosion resistance, long-term stability of resistance at normal temperature, low cost and wide application in electronic ceramics, functional ceramics, semiconductor chip industry and structural ceramics.
Drawings
FIG. 1 is a schematic view showing the appearance of alumina ceramics prepared in examples 1 to 4 of the present invention;
FIG. 2 is a schematic view showing the appearance of the alumina ceramic prepared in comparative example 1 of the present invention;
FIG. 3 is a schematic view showing the appearance of the alumina ceramic prepared in example 5 of the present invention;
FIG. 4 is a schematic view showing the appearance of alumina ceramic prepared in example 6 of the present invention.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The experimental reagents used in the following examples are all conventional biochemical reagents unless otherwise specified; the dosage of the experimental reagent is the dosage of the reagent in the conventional experimental operation if no special description exists; the experimental methods are conventional methods unless otherwise specified.
In a first aspect, an embodiment of the present invention provides a method for preparing alumina ceramic, including the steps of:
s1, placing the ceramic composition into a ball milling tank, and adding the water and the dispersing agent into the ball milling tank to obtain a ceramic composition with a particle size of 60-300 r.min -1 The adhesive is added after the ball milling is carried out for 40 to 80 hours at the rotating speed, and the ball milling is continued for 5 to 15 hours, so as to obtain slurry, wherein the sintering aid comprises at least one of yttrium oxide, calcium oxide, niobium oxide and cerium oxide, the dispersing agent comprises at least one of ammonium polyacrylate and ammonium citrate, the adhesive comprises at least one of polyvinyl alcohol and polyvinyl pyrrolidone, and the ceramic composition comprises the following components in percentage by mass: 65 to 95 percent of aluminum oxide, 3 to 30 percent of titanium dioxide, 0.2 to 1.5 percent of silicon dioxide, 0.2 to 3 percent of sintering aid and 0 to 5 percent of zinc oxide, wherein the addition amount of the dispersing agent is 0.2 to 1 percent of the total amount of all components in the ceramic composition, the addition amount of the adhesive is 0.2 to 1.2 percent of the total amount of all components in the ceramic composition, and the volume ratio of the ball, the material and the water is (2 to 4) to (0.5 to 1.5).
S2, passing the slurry through a 150-250 mesh screen for spray granulation, then screening powder obtained through spray granulation through a double-layer screen, wherein a screen space is composite alumina powder, the upper layer screen mesh number of the double-layer screen is 60-90 meshes, the lower layer screen mesh number is 150-250 meshes, and the spray granulation process comprises the following steps: the inlet temperature is 200-300 ℃, the outlet temperature is 100-200 ℃, the negative pressure is 40-60 Pa, the atomizer frequency is 15-25 HZ, the atomizer rotating speed is 8000-9000 r/min, and the feeding pump speed is 25-30 mL/min.
S3, carrying out dry press molding on the composite alumina powder, and then carrying out cold isostatic pressing molding to obtain a biscuit, wherein the dry press molding conditions comprise: the dry-pressing forming pressure is 5-50 MPa, the dwell time is 3-10 min, and the cold isostatic pressing conditions comprise: the cold isostatic pressing pressure is 150-350MPa, and the pressure maintaining time is 5-15 min.
S4, embedding the biscuit into buried powder, presintering in an oxygen-free atmosphere, and then performing hot isostatic pressing sintering, wherein the alumina ceramics with different surface resistances can be obtained by adjusting the type of the oxygen-free atmosphere, the oxygen-free atmosphere is at least one of argon, nitrogen, hydrogen, carbon monoxide and vacuum atmosphere, and the presintering process comprises the following steps: heating from room temperature to 1400-1600 ℃ for 20-60 hours, preserving heat for 2-8 hours, and naturally cooling to room temperature, wherein the pressure of hot isostatic pressing sintering is 100-200 megapascals, the atmosphere of hot isostatic pressing sintering is argon, the temperature of hot isostatic pressing sintering is 1300-1450 ℃, the time of hot isostatic pressing sintering is 10-20 hours, and the buried powder comprises at least one of graphene, graphite, silicon carbide and tungsten carbide.
The preparation method provided by the embodiment of the invention is simple to operate and low in equipment requirement, and the prepared alumina ceramic has the characteristics of excellent antistatic performance, high strength and high hardness, and under the condition that the alumina ceramic does not comprise the nano second conductive phase, the prepared alumina ceramic has excellent antistatic performance and excellent mechanical property.
In a second aspect, the present invention provides an alumina ceramic prepared by the method of the first aspect, the alumina ceramic having a surface resistance of 10 5 ~10 10 Ohm, the bending strength of the alumina ceramic is 350-600 megaPa, the Vickers hardness of the alumina ceramic is 1500-1800 HV, and the density of the alumina ceramic is 3.6-4.4 g/cubic centimeterAnd (5) rice.
In a third aspect, the present invention provides the use of an alumina ceramic according to the second aspect for the preparation of an antistatic material.
Example 1
Raw materials: ceramic composition comprising 90wt% of alumina, 5wt% of titanium dioxide, 1wt% of silicon dioxide, 2wt% of yttrium oxide and 2wt% of zinc oxide.
The preparation method of the alumina ceramic provided by the embodiment of the invention comprises the following steps:
s1, accurately weighing aluminum oxide (purity 99.98%), titanium dioxide (purity 99.9%), silicon dioxide (purity 99.9%), yttrium oxide (purity 99.9%) and zinc oxide (purity 99%) according to raw material composition, putting into a ball milling tank, adding deionized water and a proper amount of dispersing agent (ammonium polyacrylate and ammonium citrate in a mass ratio of 1:1), wherein the adding amount of the dispersing agent is 0.4wt% of the total amount of all components in the ceramic composition, mixing for 60 hours by using a ball mill, and rotating at 150 r.min -1 And then adding an adhesive (polyvinyl alcohol and polyvinyl pyrrolidone in a mass ratio of 1:1), wherein the addition amount of the adhesive is 0.5 weight percent of the total amount of all components in the ceramic composition, and the volume ratio of balls, materials (the ceramic composition, a dispersing agent and the adhesive) and deionized water is 3:1:0.8, and continuing ball milling and mixing for 10 hours to obtain the slurry.
S2, sieving the slurry obtained in the step S1 with a 200-mesh screen, and then performing spray granulation to prepare dry composite alumina powder, wherein the spray granulation process comprises the following steps: the inlet temperature is 260 ℃, the outlet temperature is 120 ℃, the negative pressure is 50Pa, the frequency of an atomizer is 20HZ, the rotating speed of the atomizer is 8500r/min, the feeding pump speed is 25mL/min, and the powder obtained by spray granulation is subjected to double-layer screening by a 80-mesh screen and a 200-mesh screen, so that a qualified product is obtained between the two, namely the composite alumina powder obtained by the embodiment.
S3, putting the composite alumina powder prepared in the step S2 into a die to perform dry pressing preforming, wherein the forming pressure is 20MPa, the pressure maintaining time is 5min, and then putting the preformed blank into a cold isostatic press to perform pressing after vacuum packaging, so that the density of the blank is more uniform and compact, the pressure is 150MPa, and the pressure is ensuredPressing for 10min to obtain biscuit with density of 1.9g/cm 3
S4, placing the biscuit obtained in the step S3 into a crucible, embedding the biscuit into embedded powder (the mass ratio of graphite to silicon carbide is 3:1) which is composed of graphite and silicon carbide, then heating to 1400 ℃ from room temperature for 20 hours under the mixed atmosphere of argon and hydrogen (the volume ratio of the argon to the hydrogen is 1:1), preserving heat for 3 hours, and finally naturally cooling to room temperature to sinter to obtain a pre-sintered body.
And (3) carrying out hot isostatic pressing sintering on the pre-sintered body for 15 hours under the conditions of argon atmosphere and the pressure of 100 megapascals and the temperature of 1300 ℃ to obtain the alumina ceramic. The aluminum oxide ceramic has a black color and a uniform color as shown in fig. 1.
Example 2
Raw materials: ceramic composition comprising 80wt% of alumina, 15wt% of titanium dioxide, 1wt% of silicon dioxide, 2wt% of yttrium oxide and 2wt% of zinc oxide.
The preparation method of the alumina ceramic provided by the embodiment of the invention is exactly the same as that of the embodiment 1.
The aluminum oxide ceramic prepared in this example is schematically shown in fig. 1.
Example 3
Raw materials: ceramic composition comprising 75wt% of alumina, 20wt% of titanium dioxide, 1wt% of silicon dioxide, 2wt% of yttrium oxide and 2wt% of zinc oxide.
The preparation method of the alumina ceramic provided by the embodiment of the invention is exactly the same as that of the embodiment 1.
The aluminum oxide ceramic prepared in this example is schematically shown in fig. 1.
Example 4
Raw materials: ceramic composition comprising 65wt% of alumina, 30wt% of titania, 1wt% of silica, 2wt% of yttria and 2wt% of zinc oxide.
The preparation method of the alumina ceramic provided by the embodiment of the invention is exactly the same as that of the embodiment 1.
The aluminum oxide ceramic prepared in this example is schematically shown in fig. 1.
Example 5
Raw materials: exactly the same as in example 1.
The preparation method of the alumina ceramic provided in the embodiment of the invention is basically the same as that in the embodiment 1, except that in the step S4, during the preparation of the pre-sintered body, the atmosphere is nitrogen.
An external view of the alumina ceramic prepared in this example is schematically shown in FIG. 3.
Example 6
Raw materials: exactly the same as in example 1.
The preparation method of the alumina ceramic provided in the embodiment of the present invention is basically the same as that in embodiment 1, except that in step S4, during the preparation of the pre-sintered body, the atmosphere is carbon monoxide.
An external view of the alumina ceramic prepared in this example is schematically shown in fig. 4.
Example 7
Raw materials: substantially the same as in example 1, except that 92% by weight of alumina was not included.
Alumina ceramic was prepared with reference to the preparation method of alumina ceramic provided in example 1.
Example 8
Raw materials: exactly the same as in example 1.
The preparation method of the alumina ceramic provided by the embodiment of the invention is basically the same as that of the embodiment 1, except that in the step S4, the powder embedding operation is not performed in the process of preparing the presintered body.
Comparative example 1
Raw materials: exactly the same as in example 1.
The preparation method of the alumina ceramic provided in the embodiment of the present invention is basically the same as that in embodiment 1, except that in step S4, the atmosphere is an air atmosphere during the preparation of the pre-sintered body.
Fig. 2 is a schematic view showing the appearance of the alumina ceramic prepared in this comparative example, and as can be seen from fig. 2, the alumina ceramic is white and yellowish, and the color is uneven.
Comparative example 2
Raw materials: ceramic composition comprising 100wt% alumina.
Alumina ceramic was prepared with reference to the preparation method of alumina ceramic provided in example 1.
Comparative example 3
Raw materials: ceramic composition comprising 50wt% of alumina, 45wt% of titania, 1wt% of silica, 2wt% of yttria and 2wt% of zinc oxide.
Alumina ceramic was prepared with reference to the preparation method of alumina ceramic provided in example 1. The strength is very high but the resistance is too small to meet the antistatic standard.
Comparative example 4
Raw materials: ceramic composition comprising 90% by weight of alumina, 1% by weight of silica, 2% by weight of yttria and 7% by weight of zinc oxide.
Alumina ceramic was prepared with reference to the preparation method of alumina ceramic provided in example 1. The resistance and example 1 were not changed and the strength was much reduced.
Test case
The properties of the alumina ceramics prepared in the examples and comparative examples of the present invention were tested at room temperature, and the results are shown in tables 1 and 2.
The surface resistance test adopts a surface resistance tester; the bending strength adopts a bending strength tester, and the testing method is a three-point bending strength testing method; hardness testing was performed using a vickers hardness tester.
TABLE 1
Figure BDA0003802713360000111
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Figure BDA0003802713360000121
TABLE 2
Figure BDA0003802713360000122
As can be seen from tables 1 and 2, the alumina ceramics prepared in examples 1 to 6 have not only excellent antistatic properties but also high strength and hardness; as is clear from comparative example 1, when the sintering atmosphere is air, the surface resistance of the alumina ceramic is too high, and the alumina ceramic does not have antistatic performance; as is clear from comparative example 3, when the titanium dioxide content is too high, the surface resistance of the alumina ceramic is too small, and the alumina ceramic does not have antistatic performance; as is apparent from example 1 and comparative example 4, when zinc oxide is replaced with a part of titanium oxide, not only the antistatic property of the alumina ceramic is not reduced, but also the strength and hardness of the alumina ceramic are improved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.

Claims (8)

1. The preparation method of the alumina ceramic is characterized by comprising the following steps:
s1, adding water, a dispersing agent and a bonding agent into a ceramic composition for ball milling to obtain slurry, wherein the ceramic composition comprises the following components in percentage by mass: 75-90% of aluminum oxide, 5-20% of titanium dioxide, 0.2-1.5% of silicon dioxide, 0.2-3% of sintering aid and 1-3% of zinc oxide;
s2, carrying out spray granulation on the slurry to obtain composite alumina powder;
s3, carrying out dry press molding on the composite alumina powder, and then carrying out cold isostatic pressing molding to obtain a biscuit;
s4, embedding the biscuit into embedded powder, presintering in an oxygen-free atmosphere, and then performing hot isostatic pressing sintering to obtain the aluminum oxide ceramic, wherein the embedded powder comprises at least one of graphene, graphite, silicon carbide and tungsten carbide.
2. The method for preparing alumina ceramic according to claim 1, wherein the sintering aid comprises at least one of yttrium oxide, calcium oxide, niobium oxide, and cerium oxide;
and/or the dispersing agent comprises at least one of ammonium polyacrylate and ammonium citrate;
and/or the adhesive comprises at least one of polyvinyl alcohol and polyvinyl pyrrolidone;
and/or the anaerobic atmosphere is at least one of argon, nitrogen, hydrogen, carbon monoxide and vacuum atmosphere.
3. The method for preparing alumina ceramic according to claim 1, wherein the spray granulation process is as follows: the inlet temperature is 200-300 ℃, the outlet temperature is 100-200 ℃, the negative pressure is 40-60 Pa, the atomizer frequency is 15-25 HZ, the atomizer rotating speed is 8000-9000 r/min, and the feeding pump speed is 25-30 mL/min.
4. The method for producing an alumina ceramic according to claim 1, wherein the dry press molding conditions include: the dry pressing forming pressure is 5-50 MPa, and the pressure maintaining time is 3-10 min;
and/or the conditions for cold isostatic pressing include: the cold isostatic pressing pressure is 150-350MPa, and the pressure maintaining time is 5-15 min.
5. The method of preparing alumina ceramic according to claim 1, wherein the pre-sintering process comprises: heating from room temperature to 1400-1600 ℃ for 20-60 hours, preserving heat for 2-8 hours, and naturally cooling to room temperature;
and/or the pressure of the hot isostatic pressing sintering is 100-200 MPa, the atmosphere of the hot isostatic pressing sintering is argon, the temperature of the hot isostatic pressing sintering is 1300-1450 ℃, and the time of the hot isostatic pressing sintering is 10-20 hours.
6. An alumina ceramic, characterized in that the alumina ceramic is prepared by the preparation method of the alumina ceramic according to any one of claims 1 to 5.
7. The alumina ceramic of claim 6, wherein the alumina ceramic has a surface resistance of 10 5 ~10 9 Ohmic;
and/or the bending strength of the alumina ceramic is 350-600 megapascals;
and/or the Vickers hardness of the alumina ceramic is 1500-1800 HV;
and/or the alumina ceramic has a density of 3.6 to 4.4 g/cc.
8. Use of an alumina ceramic according to claim 6 or 7 for the preparation of an antistatic material.
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