CN107056282B - Yttrium-stabilized zirconia slurry, preparation method thereof and preparation method of yttrium-stabilized zirconia blank - Google Patents
Yttrium-stabilized zirconia slurry, preparation method thereof and preparation method of yttrium-stabilized zirconia blank Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/12—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein one or more rollers exert pressure on the material
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Abstract
The invention relates to yttrium-stabilized zirconia slurry, a preparation method thereof and a preparation method of a yttrium-stabilized zirconia blank. An yttrium stabilized zirconia slurry comprises the following components in percentage by weight: 70% -90% of yttrium-stabilized zirconia powder; 6.5 to 25 percent of solvent; 0.5 to 5 percent of surfactant; 0.5 to 1.5 percent of defoaming agent; 2% -8% of adhesive; and 0.5 to 2.5 percent of plasticizer; wherein the solvent comprises water and an organic solvent, the organic solvent is selected from at least one of tert-butyl carbitol acetate, n-propyl acetate, olive oil, glycerol, ethanol, hexanediol, isobutanol and terpineol, and the percentage content of water in the solvent is 70-95%; the surfactant is at least one selected from oleic acid, castor oil, methacrylate, triethanolamine, triolein, herring oil and ammonium acrylate copolymer salt. The yttrium-stabilized zirconia slurry is environment-friendly and the forming process is relatively simple.
Description
Technical Field
The invention relates to yttrium-stabilized zirconia slurry, a preparation method thereof and a preparation method of a yttrium-stabilized zirconia blank.
Background
The manufacturing technology of the automobile oxygen sensor chip is the core technology of the automobile oxygen sensor, and the quality of the chip directly influences the quality of the oxygen sensor, so that a good ceramic substrate is required to be prepared. At present, the commonly used preparation process of the ceramic matrix is to manufacture yttrium stable zirconia slurry into a large-area, thin and flat ceramic chip by a Tape Casting method (Tape Casting), and then to cut the ceramic chip.
The tape casting method is a main industrialized scheme at present, and the traditional yttrium stabilized zirconia slurry tape casting process has the defects that the used organic solvent (such as toluene, xylene and the like) has toxicity and high production cost, and the density of a biscuit is low due to high organic content in the slurry. Because the solid content of the yttrium-stabilized zirconia slurry is low, the thickness of a film formed by tape casting is small, a plurality of films need to be laminated and compounded for use when the yttrium-stabilized zirconia slurry is used, and the complexity of a forming process is increased.
Disclosure of Invention
Accordingly, there is a need for an environmentally friendly yttrium-stabilized zirconia slurry with a relatively simple molding process, a method for preparing the same, and a method for preparing an yttrium-stabilized zirconia green body.
An yttrium stabilized zirconia slurry comprises the following components in percentage by weight:
wherein the solvent comprises water and an organic solvent, the organic solvent is selected from at least one of tert-butyl carbitol acetate, n-propyl acetate, olive oil, glycerol, ethanol, hexanediol, isobutanol and terpineol, and the mass percentage of the water in the solvent is 70-95%; the surfactant is at least one selected from oleic acid, castor oil, methacrylate, triethanolamine, triolein, herring oil and ammonium acrylate copolymer salt.
In one embodiment, the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 92:8 to 97: 3.
In one embodiment, the yttrium-stabilized zirconia powder has a particle size of less than 9 μm.
In one embodiment, the defoaming agent is selected from at least one of polyoxypropylene glycerol ether, phenylacetic acid lauryl alcohol, polyether modified silicone and polysiloxane.
In one embodiment, the binder is selected from at least one of polyvinyl butyral, ethyl cellulose, hydroxypropyl methylcellulose, acrylates, polymethacrylates, hydrogenated castor oil, and polyvinyl alcohol.
In one embodiment, the plasticizer is selected from at least one of dioctyl phthalate, dibutyl phthalate, polyethylene glycol, dibenzoate, butyl stearate, and propylene phosphate.
A method of making the yttrium-stabilized zirconia slurry of any one of the preceding claims, comprising the steps of:
mixing the yttrium-stabilized zirconia powder, a solvent, a surfactant and a defoaming agent, and then ball-milling for 8-24 hours to obtain a premix; and
and adding the plasticizer and the adhesive into the premix, and continuously performing ball milling for 8-24 hours to obtain yttrium stable zirconia slurry.
In one embodiment, the method further comprises the following steps: and (3) carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry for 30-60 minutes.
The preparation method of the yttrium-stabilized zirconia blank comprises the step of rolling, drying and forming the yttrium-stabilized zirconia slurry to obtain the yttrium-stabilized zirconia blank.
In one embodiment, the yttrium-stabilized zirconia green body has a thickness of 0.2mm to 0.5 mm.
The yttrium-stabilized zirconia slurry takes water as a main solvent, has the advantages of environmental friendliness and low cost, and is relatively environment-friendly; the yttrium-stabilized zirconia slurry has the solid content of 70-90%, the viscosity of 180078-350102 cps, high solid content and high viscosity, and can be used for preparing a blank with the thickness of 0.2-0.5 mm in one step by adopting a rolling method, so that the forming process is simplified.
Drawings
Fig. 1 is an SEM photograph of the green body prepared in example 2.
Detailed Description
The yttrium-stabilized zirconia slurry, the preparation method thereof, and the preparation method of the yttrium-stabilized zirconia green body will be described in further detail below mainly with reference to specific examples.
An embodiment of the yttrium stabilized zirconia slurry comprises the following components in weight percent:
wherein the solvent comprises water and an organic solvent. The organic solvent is at least one of tert-butyl carbitol acetate, n-propyl acetate, olive oil, glycerol, ethanol, hexanediol, isobutanol and terpineol, and the mass percentage of water in the solvent is 70-95%.
The surfactant is at least one selected from oleic acid, castor oil, methacrylate, triethanolamine, triolein, herring fish oil and ammonium acrylate copolymer salt. In one embodiment, the methacrylate is selected from at least one of dimethylaminoethyl methacrylate, sodium methacrylate, dimethylaminoethyl bromide quaternary ammonium methacrylate-styrene copolymer and 2-hydroxyethyl methacrylate. The acrylate copolymer ammonium salt is at least one selected from acrylic acid-acrylate copolymer containing quaternary ammonium salt, alkylphenol polyoxyethylene ether acrylic acid copolymer containing quaternary ammonium salt, polysiloxane-acrylate copolymer containing quaternary ammonium salt and styrene acrylic acid copolymer containing quaternary ammonium salt.
In one embodiment, the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 92:8 to 97: 3. Of course, the yttrium-stabilized zirconia powder is either commercially available or prepared according to methods known to those skilled in the art, and the appropriate ZrO is selected as desired2、Y2O3Yttria in a molar ratio stabilizes the zirconia.
In one embodiment, the yttrium-stabilized zirconia powder has a particle size of less than 9 μm. Preferably, the particle size of the yttrium-stabilized zirconia powder is 0.4 to 1.5 μm.
In one embodiment, the defoaming agent is selected from at least one of polyoxypropylene glycerol ether, phenylacetic acid lauryl alcohol, polyether modified silicone and polysiloxane. The polyether modified organic silicon is at least one selected from polyether modified organic silicon KP-140, polyether modified organic silicon JH-935, polyether modified organic silicon LM-110 and Wack polyether modified organic silicon SD, wherein the organic silicon KP-140, the organic silicon JH-935, the organic silicon LM-110 and the organic silicon SD are all commercially available. The polysiloxane is at least one selected from polydimethylsiloxane, methyl alkyl polysiloxane, phenyl trimethyl siloxane, methyl vinyl polysiloxane and PEG-8 dimethicone water soluble siloxane.
In one embodiment, the binder is selected from at least one of polyvinyl butyral (PVB), ethyl cellulose, hydroxypropyl methyl cellulose, acrylates, polymethacrylates, hydrogenated castor oil, and polyvinyl alcohol (PVA). The acrylate is at least one selected from methyl acrylate, ethyl acrylate, 2-methyl methacrylate and 2-ethyl methacrylate. The polymethacrylate is at least one selected from polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate and polyethylene glycol methacrylate.
In one embodiment, the plasticizer is selected from at least one of dioctyl phthalate (DOP), dibutyl phthalate (DBP), polyethylene glycol, dibenzoate, butyl stearate, and propylene phosphate. The polyethylene glycol is at least one selected from polyethylene glycol 550, polyethylene glycol 1000, polyethylene glycol 6000, and polyethylene glycol 10000.
In one embodiment, the yttrium-stabilized zirconia slurry has a solid content of 70-90% and a viscosity of 180078 cps-350102 cps.
The yttrium-stabilized zirconia slurry takes water as a main solvent, and the used organic solvent has low toxicity, has the advantages of environmental friendliness and low cost, and is relatively environment-friendly; the solid content of the yttrium-stabilized zirconia slurry is 70-90%, the viscosity of the slurry is 180078-350102 cps, the solid content is high, the viscosity is high, a rolling method can be adopted to prepare a blank with the thickness of 0.2-0.5 mm in one step, a multilayer film laminating mode is not required to be adopted for preparation, and the forming process is simplified; the prepared green body has high density and good compactness.
The preparation method of the yttrium-stabilized zirconia slurry comprises the following steps:
step S110, mixing yttrium-stabilized zirconia powder, a solvent, a surfactant and a defoaming agent, and then ball-milling for 6-24 hours to obtain a premix.
In one embodiment, zirconium balls are added for ball milling. Further, the mass ratio of the zirconium balls to the yttrium-stabilized zirconia powder is 2: 1-5: 1.
and step S120, adding the plasticizer and the adhesive into the premix, and continuing ball milling for 8-24 hours to obtain yttrium stabilized zirconia slurry.
In one embodiment, the pellets are separated after the ball milling is completed.
And step S130, carrying out vacuum defoaming on the yttrium stabilized zirconia slurry for 30-60 minutes.
In one embodiment, the vacuum defoaming is carried out under the condition of-0.06 MPa to-0.09 MPa.
The preparation method of the yttrium stable zirconia slurry is simple to operate.
A preparation method of a yttrium-stabilized zirconia film comprises the step of rolling, drying and forming the yttrium-stabilized zirconia slurry to obtain a yttrium-stabilized zirconia blank.
Preferably, the thickness of the yttrium-stabilized zirconia green body is 0.2mm to 0.5 mm.
Preferably, when rolling, the roll shaft spacing is controlled to be 0.25 mm-0.62 mm, and the rotating speed is controlled to be 100 rpm-150 rpm.
Preferably, the drying temperature is 120-150 ℃, and the drying time is 60-90 min.
According to the preparation method of the yttrium-stabilized zirconia blank, the blank with the thickness of 0.2-0.5 mm is prepared in one step, a multilayer film laminating mode is not needed, the forming process is simplified, and the prepared blank is high in density and good in compactness.
The following are specific examples:
the parts in the following examples are parts by mass.
Example 1
(1) Preparing slurry: mixing 70 parts of yttrium-stabilized zirconia powder, 18 parts of solvent, 1 part of castor oil and 1 part of polydimethylsiloxane, adding 140 parts of zirconium balls, carrying out ball milling for 12 hours, adding 8 parts of ethyl cellulose and 2 parts of polyethylene glycol 550, carrying out ball milling for 12 hours, separating the balls to obtain yttrium-stabilized zirconia slurry, and carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry for 30 minutes under-0.06 MPa, wherein the solvent comprises 30 parts of absolute ethyl alcohol and 70 parts of water, and the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 97: 3.
(2) controlling the distance between the roll shafts to be 0.25mm, the rotating speed to be 140rpm, the drying temperature to be 120 ℃, and the drying time to be 60min, rolling and drying the yttrium stabilized zirconia slurry to obtain a compact blank with the thickness of 0.2mm, and cutting the compact blank according to the size of 140mm in width and 140mm in length for subsequent electrode printing.
Example 2
(1) Preparing slurry: mixing 75 parts of yttrium-stabilized zirconia powder, 13.5 parts of solvent, 0.75 part of triethanolamine and 0.75 part of polyoxypropylene glycerol ether, adding 225 parts of zirconium balls, carrying out ball milling for 8 hours, adding 8 parts of polyvinyl alcohol and 2 parts of DOP, continuing ball milling for 16 hours, separating the balls to obtain yttrium-stabilized zirconia slurry, and carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry under-0.07 MPa for 30 minutes, wherein the solvent comprises 15 parts of n-propyl acetate and 85 parts of water, and the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 95: 5.
(2) controlling the distance between the roll shafts to be 0.35mm, the rotating speed to be 130rpm, the drying temperature to be 130 ℃, and the drying time to be 70min, rolling and drying the yttrium stabilized zirconia slurry to obtain a compact blank with the thickness of 0.3mm, and cutting the compact blank according to the size of 140mm in width and 140mm in length for subsequent electrode printing.
Example 3
(1) Preparing slurry: mixing 80 parts of yttrium-stabilized zirconia powder, 9.35 parts of solvent, 1.1 parts of styrene acrylic copolymer and 0.55 part of polyether modified organic silicon LM-110, adding 320 parts of zirconium balls, carrying out ball milling for 24 hours, adding 7.65 parts of PVB and 1.35 parts of butyl stearate, continuing ball milling for 8 hours, separating the balls to obtain yttrium-stabilized zirconia slurry, and carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry for 30 minutes under-0.08 MPa, wherein the solvent comprises 20 parts of absolute ethyl alcohol and 80 parts of water, and the molar ratio of zirconium oxide to yttrium oxide in the yttrium-stabilized zirconia powder is 95: 5.
(2) controlling the distance between the roll shafts to be 0.34mm, the rotating speed to be 130rpm, the drying temperature to be 130 ℃, and the drying time to be 70min, rolling and drying the yttrium stabilized zirconia slurry to obtain a compact blank with the thickness of 0.3mm, and cutting the compact blank according to the size of 140mm in width and 140mm in length for subsequent electrode printing.
Example 4
(1) Preparing slurry: mixing 85 parts of yttrium-stabilized zirconia powder, 8.5 parts of solvent, 1 part of dimethylaminoethyl methacrylate and 0.5 part of methyl alkyl polysiloxane, adding 425 parts of zirconium balls, carrying out ball milling for 18 hours, adding 3.75 parts of hydroxypropyl methyl cellulose and 1.25 parts of polyethylene glycol 1000, continuing ball milling for 12 hours, separating the balls to obtain yttrium-stabilized zirconia slurry, and carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry for 30 minutes under the condition of-0.08 MPa, wherein the solvent comprises 10 parts of glycerol and 90 parts of water, and the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 92: 8.
(2) controlling the distance between the roll shafts to be 0.51mm, the rotating speed to be 120rpm, the drying temperature to be 140 ℃, and the drying time to be 80min, rolling and drying the yttrium stabilized zirconia slurry to obtain a compact blank with the thickness of 0.4mm, and cutting the compact blank according to the size of 140mm in width and 140mm in length for subsequent electrode printing.
Example 5
(1) Then, 90 parts of YSZ powder (molar ratio of zirconia to yttria: 95: 5), 6.5 parts of solvent (n-propyl acetate: 15:85), 0.5 part of surfactant (acrylic acid-acrylate copolymer), 0.5 part of defoaming agent (methyl vinyl polysiloxane), and 450 parts of zirconium balls were put into a ball mill pot and ball-milled for 16 hours.
(2) 2 parts of binder (ethyl cellulose) and 0.5 part of plasticizer (butyl stearate) were added to the ball mill pot and ball milled again for 16 hours.
(3) And after the ball milling is finished, filtering and discharging by using 200-mesh filter cloth, and testing the viscosity of the slurry.
(4) And performing ball separation to obtain yttrium-stabilized zirconia slurry, and performing vacuum defoaming on the yttrium-stabilized zirconia slurry for 30 minutes under the condition of-0.09 MPa.
(5) Controlling the distance between the roll shafts to be 0.62mm, controlling the rotating speed to be 100rpm, controlling the drying temperature to be 150 ℃, controlling the drying time to be 90min, rolling and drying the yttrium stabilized zirconia slurry to obtain a compact blank with the thickness of 0.5mm, and cutting the blank according to the size of 140mm in width and 140mm in length for subsequent electrode printing.
The viscosity of the yttrium-stabilized zirconia slurry obtained in examples 1 to 5 was measured by an NDJ rotational viscometer, AND the solid content of the yttrium-stabilized zirconia slurry obtained in examples 1 to 5 was measured by an AND slurry solid content detector, AND the results are shown in table 1:
TABLE 1
| Order of item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Solid content | 70％ | 75％ | 80％ | 85％ | 90％ |
| Viscosity (cps) | 180078 | 221450 | 264203 | 310142 | 350102 |
Fig. 1 is an SEM picture of the green body of example 2, and it can be seen from fig. 1 that the green body has good ceramic forming property and high density.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. An yttrium-stabilized zirconia slurry, characterized by comprising, in weight percent:
wherein the solvent comprises water and an organic solvent, the organic solvent is selected from at least one of tert-butyl carbitol acetate, n-propyl acetate, olive oil, glycerol, ethanol, hexanediol, isobutanol and terpineol, and the mass percentage of the water in the solvent is 70-95%; the surface active agent is selected from at least one of oleic acid, castor oil, methacrylate, triethanolamine, triolein, herring fish oil and acrylate copolymer ammonium salt, the plasticizer is selected from at least one of dioctyl phthalate, dibutyl phthalate, polyethylene glycol, dibenzoate, butyl stearate and allyl phosphate, and the yttrium-stabilized zirconia slurry can be used for preparing a green body with the thickness of 0.2-0.5 mm by a rolling method in one step.
2. The yttrium-stabilized zirconia slurry according to claim 1, wherein the molar ratio of zirconia to yttria in the yttrium-stabilized zirconia powder is 92:8 to 97: 3.
3. The yttrium-stabilized zirconia slurry according to claim 1, wherein said yttrium-stabilized zirconia powder has a particle size of less than 9 μm.
4. The yttrium-stabilized zirconia slurry according to claim 1, wherein said antifoaming agent is at least one selected from the group consisting of polyoxypropylene glycerol ether, lauryl phenylacetate, polyether-modified silicone and polysiloxane.
5. The yttrium-stabilized zirconia slurry according to claim 1, wherein said binder is at least one selected from the group consisting of polyvinyl butyral, ethyl cellulose, hydroxypropyl methylcellulose, acrylates, polymethacrylates, hydrogenated castor oil, and polyvinyl alcohol.
6. A method of preparing an yttrium-stabilized zirconia slurry according to any one of claims 1 to 5, comprising the steps of:
mixing the yttrium-stabilized zirconia powder, a solvent, a surfactant and a defoaming agent, and then ball-milling for 8-24 hours to obtain a premix; and
and adding the plasticizer and the adhesive into the premix, and continuously performing ball milling for 8-24 hours to obtain yttrium stable zirconia slurry.
7. The method of preparing an yttrium-stabilized zirconia slurry according to claim 6, further comprising the step of: and (3) carrying out vacuum defoaming on the yttrium-stabilized zirconia slurry for 30-60 minutes.
8. A method for preparing a yttrium-stabilized zirconia green body, which is characterized in that the yttrium-stabilized zirconia green body is obtained by rolling, drying and forming the yttrium-stabilized zirconia slurry according to any one of claims 1 to 5.
9. The method for preparing an yttrium-stabilized zirconia green body according to claim 8, wherein the thickness of the yttrium-stabilized zirconia green body is 0.2mm to 0.5 mm.
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