CN115353381B - Large-size zirconia antistatic ceramic and preparation method and application thereof - Google Patents

Large-size zirconia antistatic ceramic and preparation method and application thereof Download PDF

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CN115353381B
CN115353381B CN202211043267.XA CN202211043267A CN115353381B CN 115353381 B CN115353381 B CN 115353381B CN 202211043267 A CN202211043267 A CN 202211043267A CN 115353381 B CN115353381 B CN 115353381B
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陈文彬
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Hunan Sheng Ci Technology Co ltd
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Abstract

The invention discloses a large-size zirconia antistatic ceramic and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing zirconium oxychloride octahydrate, yttrium salt, cerium salt, ethanol, hydrogen peroxide and a dispersing agent, and performing spray granulation and calcination to obtain cerium-yttrium stable zirconia; mixing cerium-yttrium stabilized zirconia, zinc oxide, aluminum sol, silica sol and a dispersing agent, and performing spray granulation and calcination to obtain antistatic ceramic powder; and forming the anti-static ceramic powder, and then carrying out powder embedding sintering to obtain the large-size zirconia anti-static ceramic. The preparation method can effectively prevent sintering defects, is beneficial to preparing large-size zirconia antistatic ceramics, and the prepared large-size zirconia antistatic ceramics has higher density, better mechanical property and lower surface resistivity, and is suitable for preparing chip ceramic suckers and ceramic arms with excellent performance.

Description

Large-size zirconia antistatic ceramic and preparation method and application thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a large-size zirconia antistatic ceramic and a preparation method and application thereof.
Background
At present, the antistatic materials widely used in engineering application mainly comprise a polymer composite material, an antistatic glaze and an antistatic ceramic material. However, the polymer composite material and the antistatic glaze have defects in the aspects of high temperature resistance, durability, abrasion resistance and the like, and the application of the polymer composite material and the antistatic glaze in the fields with more strict requirements on working environments and the like, such as the fields of high temperature and high pressure, high friction frequency, aerospace and the like, is limited. The antistatic zirconia ceramic is a novel antistatic product, has excellent performances in various aspects, is wear-resistant and corrosion-resistant, has high safety performance, has the advantages of fire resistance, water resistance, stable chemical properties and the like, and is widely applied to the fields of instruments, petrochemical industry, electrical equipment, aerospace, information energy and the like. At present, the zirconia-based antistatic ceramic is mainly prepared by filling conductive particles, the preparation is simple, and the electrical property can be adjusted according to the application, for example, chinese patent document CN201711234878.1 reports an antistatic ceramic and a preparation method and application thereof, the antistatic zirconia ceramic is prepared by taking rare metal oxides such as niobium oxide, indium oxide and the like as conductive fillers, however, the oxides are very scarce resources and are widely applied in other high and new technologies, and the price of the antistatic zirconia ceramic is continuously increased. In order to reduce the use of such oxides, the current solution is to use silicon carbide, zirconium nitride, conductive carbon black, graphite, carbon nanotubes, etc. as conductive fillers, but the sintering process of such anti-static ceramics must be performed under vacuum or protective gas conditions, and the sintering temperature is very high, which will result in the increase of manufacturing cost, and is not beneficial to industrial production. The zinc oxide is a common chemical product, is low in price, is easy to be semi-conducted and can be used as a conductive filler, but the addition of the zinc oxide can obviously reduce the mechanical property of the zirconia ceramic, and the tetragonal zirconia is promoted to be converted into monoclinic zirconia in the sintering process, so that the sintering cracking is caused, and the preparation of the large-size zirconia antistatic ceramic is very difficult.
Therefore, how to overcome the difficulties, such as expensive production equipment, poor mechanical property of the anti-static ceramic, sintering cracking and the like, and find a large-size zirconia anti-static ceramic and a preparation method thereof are of great significance for realizing the application of the large-size zirconia anti-static ceramic in ceramic chip suckers and ceramic arms.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the large-size zirconia antistatic ceramic with higher density, better mechanical property and lower surface resistivity, and the preparation method and the application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme.
A preparation method of large-size zirconia antistatic ceramic is characterized by comprising the following steps:
s1, mixing zirconium oxychloride octahydrate, yttrium salt, cerium salt, ethanol, hydrogen peroxide and a dispersing agent to obtain zirconium sol;
s2, carrying out spray granulation and drying on the zirconium sol obtained in the step S1 to obtain dry gel particles;
s3, calcining the xerogel particles obtained in the step S2 at 600-1000 ℃ to obtain cerium-yttrium-stabilized zirconia;
s4, mixing the cerium-yttrium-stabilized zirconia, the zinc oxide, the aluminum sol, the silica sol and the dispersing agent obtained in the step S3, and performing ball milling treatment to obtain mixed slurry;
s5, carrying out spray granulation and drying on the mixed slurry obtained in the step S4 to obtain particles;
s6, calcining the particles obtained in the step S5 at 600-1000 ℃ to obtain antistatic ceramic powder;
and S7, forming the anti-static ceramic powder obtained in the step S6, and sintering at 1200-1500 ℃, wherein the sintering mode is powder burying sintering, and the powder burying sintering is mixed powder of zinc oxide and graphite to obtain the large-size zirconia anti-static ceramic.
Preferably, in the step S1, the mass of the zirconium oxychloride octahydrate is 25 to 45% of the sum of the mass of the zirconium oxychloride octahydrate and the mass of the hydrogen peroxide, the mass of the hydrogen peroxide is 55 to 75% of the sum of the mass of the zirconium oxychloride octahydrate and the mass of the hydrogen peroxide, the addition amount of the yttrium salt is 1 to 5% of the mass of the zirconium oxychloride octahydrate, the addition amount of the cerium salt is 1 to 3% of the mass of the zirconium oxychloride octahydrate, the addition amount of the ethanol is 20 to 60% of the mass of the hydrogen peroxide, and the addition amount of the dispersant is 0.1 to 0.5% of the mass of the zirconium oxychloride octahydrate; h in the hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%.
Preferably, in the step S4, the addition amount of each raw material is, by mass percentage, 55% to 85% of cerium-yttrium-stabilized zirconia, 5% to 30% of zinc oxide, 5% to 20% of alumina sol, 1% to 5% of silica sol, and 0.1% to 0.5% of dispersant.
In the preparation method of the large-size zirconia antistatic ceramic, preferably, in step S7, the mass percentage of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 20% to 50%.
Preferably, in the step S1, the yttrium salt is yttrium nitrate, the cerium salt is cerium nitrate, the dispersant includes at least one of ammonium citrate, polyvinylpyrrolidone and polyethylene glycol, and the mixing temperature is 50 ℃ to 90 ℃;
and/or in the step S2, the temperature of the spray granulation is 110-300 ℃, the drying temperature is 50-100 ℃, and the particle size of the xerogel particles is 30-100 μm.
In the above preparation method of the large-size zirconia antistatic ceramic, preferably, in step S3, the calcination time is 1h to 5h, the particle size of the cerium yttrium stabilized zirconia is 30 μm to 100 μm, and the average grain size of the cerium yttrium stabilized zirconia is 10nm to 100nm. According to the cerium-yttrium-stabilized zirconia, the particle size of the cerium-yttrium-stabilized zirconia is optimized to be 30-100 microns, so that a blank body is favorably formed; the average grain size of the cerium-yttrium-stabilized zirconia is optimized to be 10 nm-100 nm, so that the sintering temperature is favorably reduced, and the mechanical property of the antistatic ceramic is improved.
Preferably, in the step S4, the dispersant includes at least one of ammonium citrate, polyvinylpyrrolidone and polyethylene glycol, the ball milling treatment time is 12 to 48 hours, the ball milling treatment is wet ball milling, and the material-water ball ratio of the wet ball milling is 1: 0.5 to 1: 1 to 3;
and/or in the step S5, the temperature of the spray granulation is 110-300 ℃, the drying temperature is 50-100 ℃, and the particle size of the particles is 50-150 mu m.
In the above preparation method of the large-size zirconia antistatic ceramic, preferably, in step S6, the calcination time is 1h to 5h, and the following treatment is further included after the calcination: sieving the calcined product with a 180-mesh sieve;
and/or in the step S7, the forming comprises at least one of dry pressing, isostatic pressing, casting and extrusion, and the sintering time is 2-5 h.
As a general technical concept, the invention also provides the large-size zirconia antistatic ceramic prepared by the preparation method of the large-size zirconia antistatic ceramic.
As a general technical concept, the invention also provides application of the large-size zirconia antistatic ceramic in ceramic chip suckers and ceramic arms.
Compared with the prior art, the invention has the advantages that:
(1) The invention discloses a preparation method of large-size zirconia antistatic ceramic, which comprises the steps of firstly preparing cerium yttrium stabilized zirconia by adopting a sol-gel process, wherein the cerium yttrium stabilized zirconia has fine crystal grains, lower sintering temperature and excellent mechanical property after sintering, and yttrium salt and cerium salt jointly stabilize the zirconia to inhibit the tetragonal zirconia from being converted into monoclinic zirconia in the sintering process of the antistatic ceramic, so that sintering cracking is prevented, and the mechanical property of the antistatic ceramic is improved. Then, the preparation method of the invention introduces alumina sol and silica sol to form an aluminum oxide/silicon dioxide coating layer on the surfaces of zinc oxide and zirconia powder, wherein firstly, the aluminum oxide can dope the zinc oxide, thereby improving the conductive capability of the zinc oxide and finally promoting the reduction of the resistivity of the antistatic ceramic; secondly, the introduction of the silicon dioxide can reduce the sintering temperature and promote the sintering densification, thereby improving the mechanical property of the anti-static ceramic and reducing the surface resistivity, and meanwhile, the silicon dioxide and the aluminum oxide can form mullite whiskers in situ in the matrix, thereby effectively improving the fracture toughness of the anti-static ceramic; thirdly, the coating layer can inhibit the direct contact of the zinc oxide and the zirconium oxide, thereby reducing the influence of the zinc oxide on the phase change of the zirconium oxide in the sintering process, improving the mechanical property of the antistatic ceramic and preventing sintering cracking; fourthly, the alumina particles with even dispersion can form dispersion toughening effect on the ceramic matrix, and can also promote the improvement of mechanical property; fifthly, the coating layer can inhibit the volatilization of zinc oxide to a certain extent, thereby improving the density of the anti-static ceramic and reducing the surface resistivity. More importantly, the preparation method provided by the invention adopts a powder burying sintering mode to sinter the large-size anti-static ceramic, and the buried powder is mixed powder of zinc oxide and graphite, so that on one hand, the powder burying sintering can provide a more uniform temperature gradient and reduce the friction between a ceramic blank and a burning bearing plate, and the anti-static ceramic can be effectively prevented from deforming or cracking in the sintering process; on the other hand, zinc oxide in the embedded powder is partially gasified when being heated at high temperature to form local saturated vapor pressure, so that the volatilization of the zinc oxide in the ceramic matrix can be effectively inhibited, and evaporation-condensation mass transfer can be promoted at the initial stage of sintering, so that the density of a sample is improved, the densification rate is accelerated, the grain size is reduced, the mechanical property of the ceramic is improved, and the resistivity is reduced; meanwhile, the zinc oxide permeated into the ceramic matrix can promote the formation of a conductive path and can also reduce the surface resistivity; furthermore, carbon atoms in the graphite can enter the zirconium oxide through diffusion mass transfer at high temperature, so that the zirconium oxide has a remarkable stabilizing effect on tetragonal phase zirconium oxide, the densification of the anti-static ceramic can be promoted, the mechanical property can be improved, and the carbon penetrating into the ceramic matrix can also promote the formation of a conductive network so as to reduce the surface resistivity. The large-size zirconia antistatic ceramic prepared by the preparation method has higher compactness, better mechanical property and lower surface resistivity, and is suitable for preparing chip ceramic suckers and ceramic arms with excellent performance.
(2) According to the preparation method disclosed by the invention, the mass percentage of the zinc oxide in the mixed powder of the zinc oxide and the graphite is optimized to be 20-50%, so that the compactness and the mechanical property of the large-size zirconia antistatic ceramic are further improved, and the resistivity is reduced, because: when the mass percentage of the zinc oxide is lower than 20%, local saturated vapor pressure is difficult to form, and the volatilization of the zinc oxide in the ceramic matrix cannot be effectively inhibited; when the zinc oxide is contained in an amount of more than 50% by mass, the embedded powder may be sintered and bonded to the ceramic substrate, thereby causing sintering defects or causing non-uniformity in surface resistivity.
Detailed Description
The invention is further described below with reference to specific preferred examples, without thereby limiting the scope of protection of the invention. The materials and equipment used in the following examples are commercially available.
Example 1:
the invention relates to a preparation method of large-size zirconia for preventing static electricity, which comprises the following steps:
(1) 25000g of zirconium oxychloride octahydrate, 15000g of ethanol, 50000g of hydrogen peroxide, 850g of yttrium nitrate, 500g of cerium nitrate and 75g of polyvinylpyrrolidone are weighed and placed in a double-layer glass reaction kettle, the temperature is raised to 70 ℃, stirring is carried out, and after bubbling is stopped, the zirconium sol can be obtained. Wherein, hydrogen peroxide in hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%.
(2) Spray granulating and drying the zirconium sol obtained in the step (1) to obtain dry gel particles; wherein the temperature of a spray drying tower for spray granulation is 250 ℃, the temperature of a drying oven for drying is 60 ℃, and the size distribution of the xerogel particles is 30-100 mu m.
(3) Placing the xerogel particles obtained in the step (2) into a muffle furnace, and calcining for 3 hours at 1000 ℃ to obtain cerium-yttrium-stabilized zirconia particles; the cerium yttrium stabilized zirconia has an average crystal grain size of 70nm to 100nm and a particle size of 30 μm to 100 μm.
(4) 8700g of cerium-yttrium-stabilized zirconia powder, 1000g of zinc oxide powder, 1850g of aluminum sol (3 nm,15% commercially available), 150g of silica sol (5 nm,20% commercially available) and 50g of polyvinylpyrrolidone were weighed into a drum-type ball mill jar, 8300g of deionized water and 30000g of zirconia balls were added, and ball milling was performed for 12 hours to obtain a mixed slurry.
(5) Performing spray granulation and drying on the mixed slurry obtained in the step (4) to obtain zinc oxide and cerium yttrium stabilized zirconia particles coated by silica gel and aluminum gel; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the drying temperature is 50 ℃, and the particle size distribution of the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel is 50-150 μm.
(6) And (3) placing the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel obtained in the step (5) into a muffle furnace, calcining for 3 hours at 600 ℃, and sieving the calcined product by a 180-mesh sieve to obtain the antistatic ceramic powder.
(7) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (6) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing is 50MPa, the dwell time is 2 minutes, the pressure of isostatic pressing is 250MPa, the dwell time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(8) Placing the anti-static ceramic biscuit obtained in the step (7) into a sagger with a cover and filled with zinc oxide/graphite powder, sending the sagger into a silicon-molybdenum rod furnace, and sintering the sagger for 3 hours at 1350 ℃ to obtain large-size zirconia anti-static ceramic; the sintering mode is powder burying sintering, the buried powder is mixed powder of zinc oxide and graphite, and the mass fraction of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 25%.
Example 2:
the invention relates to a preparation method of large-size zirconia antistatic coating, which comprises the following steps:
(1) 25000g of zirconium oxychloride octahydrate, 15000g of ethanol, 50000g of hydrogen peroxide, 930g of yttrium nitrate, 530g of cerium nitrate and 75g of polyvinylpyrrolidone are weighed and placed in a double-layer glass reaction kettle, the temperature is raised to 70 ℃, stirring is carried out, and after bubbling is stopped, the zirconium sol can be obtained. Wherein, H in hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%.
(2) And (2) performing spray granulation and drying on the zirconium sol obtained in the step (1) to obtain dry gel particles, wherein the temperature of a spray drying tower for spray granulation is 250 ℃, the drying temperature is 60 ℃, and the size distribution of the dry gel particles is 30-100 mu m.
(3) Placing the xerogel particles obtained in the step (2) into a muffle furnace, and calcining for 3 hours at 1000 ℃ to obtain cerium-yttrium-stabilized zirconia particles; the grain size of the cerium yttrium stabilized zirconia is 70 nm-100 nm.
(4) 8150g of cerium-yttrium stabilized zirconia powder, 1500g of zinc oxide powder, 1920g of alumina sol (3nm, 15%), 150g of silica sol (5nm, 20%) and 50g of polyvinylpyrrolidone are weighed and placed in a drum-type ball milling tank, 8280g of deionized water and 30000g of zirconia balls are added, and after ball milling is carried out for 12 hours, mixed slurry is obtained.
(5) Performing spray granulation and drying on the mixed slurry obtained in the step (4) to obtain zinc oxide and cerium yttrium stabilized zirconia particles coated by silica gel and aluminum gel; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the drying temperature is 50 ℃, and the particle size distribution of the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel is 50-150 μm.
(6) And (4) placing the zinc oxide and cerium-yttrium stable zirconia particles coated by the silica gel and the aluminum gel obtained in the step (5) into a muffle furnace, calcining for 3 hours at 600 ℃, and sieving the calcined product by a 180-mesh sieve to obtain the antistatic ceramic powder.
(7) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (6) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing is 50MPa, the pressure maintaining time is 2 minutes, the pressure of isostatic pressing is 250MPa, the pressure maintaining time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(8) Placing the anti-static ceramic biscuit obtained in the step (7) into a sagger with a cover and filled with zinc oxide/graphite powder, sending the sagger into a silicon-molybdenum rod furnace, and sintering the sagger for 3 hours at 1350 ℃ to obtain large-size zirconia anti-static ceramic; the sintering mode is powder burying sintering, the buried powder is mixed powder of zinc oxide and graphite, and the mass fraction of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 30%.
Example 3:
the invention relates to a preparation method of large-size zirconia for preventing static electricity, which comprises the following steps:
(1) 25000g of zirconium oxychloride octahydrate, 15000g of ethanol, 50000g of hydrogen peroxide, 1000g of yttrium nitrate, 570g of cerium nitrate and 75g of polyvinylpyrrolidone are weighed and placed in a double-layer glass reaction kettle, the temperature is raised to 70 ℃, stirring is carried out, and after bubbling is stopped, the zirconium sol can be obtained. Wherein, hydrogen peroxide in hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%.
(2) Spray granulating and drying the zirconium sol obtained in the step (1) to obtain dry gel particles; wherein the temperature of a spray drying tower for spray granulation is 250 ℃, the drying temperature is 60 ℃, and the size distribution of the xerogel particles is 30-100 mu m.
(3) Placing the xerogel particles obtained in the step (2) into a muffle furnace, and calcining for 3 hours at 800 ℃ to obtain cerium-yttrium-stabilized zirconia particles; the grain size of the cerium-yttrium stabilized zirconia is 50 nm-80 nm.
(4) 7570g of cerium yttrium stabilized zirconia powder, 2000g of zinc oxide powder, 2000g of alumina sol (3nm, 15%), 150g of silica sol (5nm, 20%) and 50g of polyvinylpyrrolidone are weighed and placed in a drum-type ball milling tank, 8280g of deionized water and 30000g of zirconia balls are added, and after ball milling is carried out for 12 hours, mixed slurry is obtained.
(5) Performing spray granulation and drying on the mixed slurry obtained in the step (4) to obtain zinc oxide and cerium yttrium stabilized zirconia particles coated by silica gel and aluminum gel; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the drying temperature is 50 ℃, and the particle size distribution of the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel is 50-150 μm.
(6) And (3) placing the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel obtained in the step (5) into a muffle furnace, calcining for 3 hours at 600 ℃, and sieving the calcined product by a 180-mesh sieve to obtain the antistatic ceramic powder.
(7) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (6) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing molding is 50MPa, the pressure maintaining time is 2 minutes, the pressure of isostatic pressing molding is 250MPa, the pressure maintaining time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(8) Placing the anti-static ceramic biscuit obtained in the step (7) into a sagger with a cover and filled with zinc oxide/graphite powder, sending the sagger into a silicon-molybdenum rod furnace, and sintering the sagger at 1300 ℃ for 3 hours to obtain large-size zirconia anti-static ceramic; the sintering mode is powder burying sintering, the buried powder is mixed powder of zinc oxide and graphite, and the mass fraction of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 35%.
Example 4:
the invention relates to a preparation method of large-size zirconia for preventing static electricity, which comprises the following steps:
(1) 25000g of zirconium oxychloride octahydrate, 15000g of ethanol, 50000g of hydrogen peroxide, 1050g of yttrium nitrate, 600g of cerium nitrate and 75g of polyvinylpyrrolidone are weighed and placed in a double-layer glass reaction kettle, the temperature is raised to 70 ℃, stirring is carried out, and after bubbling is stopped, the zirconium sol can be obtained. Wherein, two areOxygen in water H 2 O 2 The mass concentration of (2) is 30%.
(2) Spray granulating and drying the zirconium sol obtained in the step (1) to obtain dry gel particles; wherein the temperature of a spray drying tower for spray granulation is 250 ℃, the drying temperature is 60 ℃, and the size distribution of the xerogel particles is 30-100 mu m.
(3) Placing the xerogel particles obtained in the step (2) into a muffle furnace, and calcining for 3 hours at 800 ℃ to obtain cerium-yttrium-stabilized zirconia particles; the grain size of the cerium yttrium stabilized zirconia is 50 nm-80 nm.
(4) 7160g of cerium yttrium stabilized zirconia powder, 2500g of zinc oxide powder, 2050g of alumina sol (3 nm, 15%), 150g of silica sol (5 nm, 20%) and 50g of polyvinylpyrrolidone were weighed and placed in a drum-type ball mill pot, 8140g of deionized water and 30000g of zirconia balls were added, and after ball milling for 12 hours, mixed slurry was obtained.
(5) Performing spray granulation and drying on the mixed slurry obtained in the step (4) to obtain zinc oxide and cerium yttrium stabilized zirconia particles coated by silica gel and aluminum gel; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the drying temperature is 50 ℃, and the particle size distribution of the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel is 50-150 μm.
(6) And (3) placing the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel obtained in the step (5) into a muffle furnace, calcining for 3 hours at 600 ℃, and sieving the calcined product by a 180-mesh sieve to obtain the antistatic ceramic powder.
(7) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (6) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing molding is 50MPa, the pressure maintaining time is 2 minutes, the pressure of isostatic pressing molding is 250MPa, the pressure maintaining time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(8) Placing the anti-static ceramic biscuit obtained in the step (7) into a sagger with a cover and filled with zinc oxide/graphite powder, sending the sagger into a silicon-molybdenum rod furnace, and sintering the sagger at 1300 ℃ for 3 hours to obtain large-size zirconia anti-static ceramic; the sintering mode is buried powder sintering, the buried powder is mixed powder of zinc oxide and graphite, and the mass fraction of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 40%.
Example 5:
the invention relates to a preparation method of large-size zirconia antistatic coating, which comprises the following steps:
(1) 25000g of zirconium oxychloride octahydrate, 15000g of ethanol, 50000g of hydrogen peroxide, 1050g of yttrium nitrate, 600g of cerium nitrate and 75g of polyvinylpyrrolidone are weighed and placed in a double-layer glass reaction kettle, the temperature is raised to 70 ℃, stirring is carried out, and after bubbling is stopped, the zirconium sol can be obtained. Wherein, H in hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%.
(2) Carrying out spray granulation and drying on the zirconium sol obtained in the step (1) to obtain dry gel particles; wherein the temperature of a spray drying tower for spray granulation is 250 ℃, the drying temperature is 60 ℃, and the size distribution of the xerogel particles is 30-100 mu m.
(3) Placing the xerogel particles obtained in the step (2) into a muffle furnace, and calcining for 3 hours at 800 ℃ to obtain cerium-yttrium-stabilized zirconia particles; the grain size of the cerium yttrium stabilized zirconia is 50 nm-80 nm.
(4) 7160g of cerium-yttrium-stabilized zirconia powder, 2500g of zinc oxide powder, 2050g of aluminum sol (3 nm, 15%), 150g of silica sol (5 nm, 20%) and 50g of polyvinylpyrrolidone are weighed and placed in a drum-type ball milling tank, 8140g of deionized water and 30000g of zirconia balls are added, and after ball milling is carried out for 12 hours, mixed slurry is obtained.
(5) Performing spray granulation and drying on the mixed slurry obtained in the step (4) to obtain zinc oxide and cerium yttrium stabilized zirconia particles coated by silica gel and aluminum gel; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the drying temperature is 50 ℃, and the particle size distribution of the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel is 50-150 μm.
(6) And (3) placing the zinc oxide and cerium yttrium stabilized zirconia particles coated by the silica gel and the aluminum gel obtained in the step (5) into a muffle furnace, calcining for 3 hours at 600 ℃, and sieving the calcined product by a 180-mesh sieve to obtain the antistatic ceramic powder.
(7) Molding:
(7.1) 9000g of the antistatic ceramic powder obtained in the step (6), 2700g of deionized water, 45g of vegetable oil and 225g of hydroxyethyl cellulose are weighed and placed in a kneader, and stirring is carried out for 2 hours to obtain the plastic pug.
(7.2) extruding the plastic pug obtained in the step (7.1) by using vacuum pugging equipment to obtain an anti-static ceramic wet blank; the dimensions of the wet green were 250X 20mm.
(7.3) firstly, sequentially placing the anti-static ceramic wet blank obtained in the step (7.2) in an oven at 40 ℃ and 60 ℃ for 12 hours respectively for primary drying, and then placing the ceramic wet blank in an oven at 80 ℃ for drying until the weight is not changed any more, so as to obtain a dry blank.
(7.4) sealing the dry blank obtained in the step (7.3), and placing the sealed dry blank into an isostatic pressing machine for forming to obtain an anti-static ceramic blank, wherein the isostatic pressing forming pressure is 150MPa, and the pressure maintaining time is 15min;
(8) Placing the antistatic ceramic blank obtained in the step (7.4) into a sagger with a cover and filled with zinc oxide/graphite powder, sending the sagger into a silicon-molybdenum rod furnace, and sintering the sagger at 1300 ℃ for 3 hours to obtain large-size zirconia antistatic ceramic; the sintering mode is powder burying sintering, the buried powder is mixed powder of zinc oxide and graphite, and the mass fraction of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 40%.
In this example, the molding manner in step (7) is extrusion molding, and the vegetable oil and the hydroxyethyl cellulose are added mainly to adjust the viscosity, thereby obtaining a plastic paste.
Comparative example 1:
a preparation method of zirconia ceramic comprises the following steps:
(1) 10000g of yttrium-stabilized zirconia powder (model 3YSZ, 100nm), 3000g of deionized water, 50g of polyvinylpyrrolidone and 30000g of zirconia balls are weighed and placed in a drum-type ball milling tank for ball milling for 12 hours to obtain mixed slurry.
(2) Carrying out spray granulation and drying on the mixed slurry obtained in the step (1) to obtain antistatic ceramic powder; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the temperature of a drying oven is 50 ℃, and the particle size distribution of the antistatic ceramic powder is 50-150 mu m.
(3) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (2) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing molding is 50MPa, the pressure maintaining time is 2 minutes, the pressure of isostatic pressing molding is 250MPa, the pressure maintaining time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(4) And (4) placing the anti-static ceramic biscuit obtained in the step (3) in a silicon-molybdenum rod furnace, and sintering for 3 hours at the temperature of 1480 ℃ to obtain the zirconia ceramic.
Comparative example 2:
a preparation method of zirconia ceramic comprises the following steps:
(1) 9250g of yttrium-stabilized zirconia powder (3YSZ, 100nm), 500g of zinc oxide powder (100 nm), 200g of alumina powder (100 nm), 50g of white carbon black (30 nm) and 50g of polyvinylpyrrolidone are weighed and placed in a drum-type ball milling tank, 3000g of deionized water and 30000g of zirconia balls are added, and ball milling is carried out for 12 hours, so as to obtain mixed slurry.
(2) Carrying out spray granulation and drying on the mixed slurry obtained in the step (1) to obtain antistatic ceramic powder; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the temperature of a drying oven is 50 ℃, and the particle size distribution of the antistatic ceramic powder is 50-150 mu m.
(3) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (2) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing is 50MPa, the dwell time is 2 minutes, the pressure of isostatic pressing is 250MPa, the dwell time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(4) And (4) placing the anti-static ceramic biscuit obtained in the step (3) into a silicon-molybdenum rod furnace, and sintering for 3 hours at 1450 ℃ to obtain the zirconia ceramic.
Comparative example 3:
a preparation method of zirconia ceramic comprises the following steps:
(1) 8250g of yttrium-stabilized zirconia powder (3YSZ, 100nm), 1500g of zinc oxide powder (100 nm), 200g of alumina powder (100 nm), 50g of white carbon black (30 nm) and 50g of polyvinylpyrrolidone are weighed and placed in a drum-type ball milling tank, 3000g of deionized water and 30000g of zirconia balls are added, and ball milling is carried out for 12 hours to obtain mixed slurry.
(2) Carrying out spray granulation and drying on the mixed slurry obtained in the step (1) to obtain antistatic ceramic powder; wherein the temperature of a spray drying tower for spray granulation is 230 ℃, the temperature of a drying oven is 50 ℃, and the particle size distribution of the antistatic ceramic powder is 50-150 mu m.
(3) Carrying out dry pressing-isostatic pressing on the anti-static ceramic powder obtained in the step (2) to obtain an anti-static ceramic biscuit; wherein the pressure of dry pressing molding is 50MPa, the pressure maintaining time is 2 minutes, the pressure of isostatic pressing molding is 250MPa, the pressure maintaining time is 5 minutes, and the size of the blank is 400 multiplied by 250 multiplied by 20mm.
(4) And (4) placing the anti-static ceramic biscuit obtained in the step (3) in a silicon-molybdenum rod furnace, and sintering for 3 hours at 1400 ℃ to obtain the zirconia ceramic.
TABLE 1 comparison of Performance data of Large-sized zirconia antistatic ceramics of examples 1 to 5 and zirconia ceramics of comparative examples 1 to 3
Sample(s) Sintering conditions Relative density (%) Bending strength (MPa) Surface resistivity (omega. Cm)
Example 1 Has no obvious defect 98.5 750 2.04×10 8
Example 2 Has no obvious defect 98.2 667 6.34×10 7
Example 3 Has no obvious defect 97.8 592 1.03×10 7
Example 4 Has no obvious defect 97.5 549 4.86×10 6
Example 5 Has no obvious defect 97.3 524 5.7×10 6
Comparative example 1 Has no obvious defect 99.5 1100 3.15×10 13
Comparative example 2 No obvious effectDefect of 97.2 458 2.68×10 10
Comparative example 3 Cracking of 93 273 6.04×10 8
As can be seen from Table 1, the large-sized zirconia antistatic ceramics of examples 1 to 5 had a relative density of at least 97.3%, a bending strength of at least 524MPa, and a surface resistivity of at most 2.04X 10 8 The above data are superior to the zirconia ceramics of comparative examples 2 and 3, and the ceramics of examples 1-5 have no significant defects during sintering. The introduction of zinc oxide can significantly reduce the mechanical properties and porosity of zirconia ceramics, even cause sintering cracking, and the main reasons are as follows: on the one hand, zinc oxide absorbs the stabilizing elements in zirconium oxide causing it to transform from a tetragonal phase to a monoclinic phase, on the other hand, zinc oxide is volatile at high temperatures. In order to solve the problems, the invention provides a preparation method of large-size zirconia antistatic ceramic, firstly, cerium yttrium stabilized zirconia with fine grains is prepared by a sol-gel method, which can effectively inhibit the crystal phase transformation in the sintering process, and in addition, the sintering temperature of the fine-grain zirconia is low, which can prevent zinc oxide from volatilizing at high temperature; then, the coating layer is used for inhibiting the zinc oxide from directly contacting with the zirconium oxide, so that the crystal phase transformation of the zirconium oxide in the sintering process can be inhibited, and meanwhile, the coating layer can also inhibit the volatilization of the zinc oxide; finally, sintering is carried out by adopting a powder-embedding sintering mode, on one hand, saturated zinc oxide vapor pressure can be generated, so that zinc oxide volatilization is inhibited, and grain refinement is promoted, on the other hand, the tetragonal zirconia is promoted to be stable by carbon permeation, and the surface resistivity is reduced. Thus, the preparation method of the inventionThe method can effectively prevent the generation of sintering defects and is beneficial to preparing large-size zirconia antistatic ceramics; the prepared large-size zirconia antistatic ceramic has higher density, better mechanical property and lower surface resistivity, and is suitable for preparing chip ceramic suckers and ceramic arms with excellent performance.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modifications, equivalent substitutions, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention are within the scope of the technical scheme of the present invention.

Claims (7)

1. The preparation method of the large-size zirconia antistatic ceramic is characterized by comprising the following steps of:
s1, mixing zirconium oxychloride octahydrate, yttrium salt, cerium salt, ethanol, hydrogen peroxide and a dispersing agent to obtain zirconium sol;
s2, carrying out spray granulation and drying on the zirconium sol obtained in the step S1 to obtain dry gel particles;
s3, calcining the xerogel particles obtained in the step S2 at 600-1000 ℃ to obtain cerium-yttrium-stabilized zirconia;
s4, mixing the cerium-yttrium-stabilized zirconia, the zinc oxide, the aluminum sol, the silica sol and the dispersing agent obtained in the step S3, and performing ball milling treatment to obtain mixed slurry;
s5, carrying out spray granulation and drying on the mixed slurry obtained in the step S4 to obtain particles;
s6, calcining the particles obtained in the step S5 at 600-1000 ℃ to obtain antistatic ceramic powder;
s7, forming the anti-static ceramic powder obtained in the step S6, and sintering at 1200-1500 ℃, wherein the sintering mode is powder burying sintering, and the powder burying sintering is mixed powder of zinc oxide and graphite to obtain large-size zirconia anti-static ceramic;
in the step S1, the mass of the zirconium oxychloride octahydrate is 25% -45% of the mass sum of the zirconium oxychloride octahydrate and the hydrogen peroxide, the mass of the hydrogen peroxide is 55% -75% of the mass sum of the zirconium oxychloride octahydrate and the hydrogen peroxide, the addition amount of the yttrium salt is 1% -5% of the mass of the zirconium oxychloride octahydrate, the addition amount of the cerium salt is 1% -3% of the mass of the zirconium oxychloride octahydrate, the addition amount of the ethanol is 20% -60% of the mass of the hydrogen peroxide, and the addition amount of the dispersing agent is 0.1% -0.5% of the mass of the zirconium oxychloride octahydrate; h in the hydrogen peroxide 2 O 2 The mass concentration of (2) is 30%;
in the step S4, the addition amount of each raw material comprises, by mass percent, 55-85% of cerium-yttrium stabilized zirconia, 5-30% of zinc oxide, 5-20% of alumina sol, 1-5% of silica sol and 0.1-0.5% of dispersant;
in the step S7, the mass percentage of the zinc oxide in the mixed powder of the zinc oxide and the graphite is 20-50%.
2. The method for preparing large-size zirconia antistatic ceramic according to claim 1, wherein in step S1, the yttrium salt is yttrium nitrate, the cerium salt is cerium nitrate, the dispersant comprises at least one of ammonium citrate, polyvinylpyrrolidone and polyethylene glycol, and the mixing temperature is 50 ℃ to 90 ℃;
and/or in the step S2, the temperature of spray granulation is 110-300 ℃, the drying temperature is 50-100 ℃, and the particle size of the xerogel particles is 30-100 μm.
3. The method for preparing large-size zirconia antistatic ceramic according to claim 1, wherein in step S3, the calcination time is 1-5 h, the particle size of the cerium yttrium stabilized zirconia is 30-100 μm, and the average grain size of the cerium yttrium stabilized zirconia is 10-100 nm.
4. The method for preparing the large-size zirconia antistatic ceramic according to the claim 1, wherein in the step S4, the dispersant comprises at least one of ammonium citrate, polyvinylpyrrolidone and polyethylene glycol, the ball milling time is 12h to 48h, the ball milling is a wet ball milling, and the ratio of the material to the water ball of the wet ball milling is 1: 0.5 to 1: 1 to 3;
and/or in the step S5, the temperature of spray granulation is 110-300 ℃, the drying temperature is 50-100 ℃, and the particle size of the particles is 50-150 μm.
5. The method for preparing large-size zirconia antistatic ceramic according to claim 1, wherein in step S6, the calcination time is 1-5 h, and the following treatment is further included after the calcination: sieving the calcined product with a 180-mesh sieve;
and/or in the step S7, the forming comprises at least one of dry pressing, isostatic pressing, casting and extrusion, and the sintering time is 2-5 h.
6. A large-sized zirconia antistatic ceramic obtained by the method for preparing a large-sized zirconia antistatic ceramic according to any one of claims 1 to 5.
7. Use of the large-sized zirconia antistatic ceramic according to claim 6 in ceramic chip chucks and ceramic arms.
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