CN100519475C - Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method - Google Patents

Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method Download PDF

Info

Publication number
CN100519475C
CN100519475C CNB031140971A CN03114097A CN100519475C CN 100519475 C CN100519475 C CN 100519475C CN B031140971 A CNB031140971 A CN B031140971A CN 03114097 A CN03114097 A CN 03114097A CN 100519475 C CN100519475 C CN 100519475C
Authority
CN
China
Prior art keywords
hours
slurry
agent
curtain coating
ball milling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB031140971A
Other languages
Chinese (zh)
Other versions
CN1534001A (en
Inventor
周和平
党桂彬
吴崇隽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZHUHAI YUEKE JINGHUA ELECTRONIC CERAMICS CO Ltd
Original Assignee
ZHUHAI YUEKE JINGHUA ELECTRONIC CERAMICS CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ZHUHAI YUEKE JINGHUA ELECTRONIC CERAMICS CO Ltd filed Critical ZHUHAI YUEKE JINGHUA ELECTRONIC CERAMICS CO Ltd
Priority to CNB031140971A priority Critical patent/CN100519475C/en
Publication of CN1534001A publication Critical patent/CN1534001A/en
Application granted granted Critical
Publication of CN100519475C publication Critical patent/CN100519475C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Compositions Of Oxide Ceramics (AREA)

Abstract

A process for preparing the zirconium oxide ceramics by doctor blading method includes calcining the square-crystal zirconium oxide powder at 600-800 deg.C for 1-3 hr, proportionally mixing it with disperser, solvent and homogenizing agent, ball grinding for 10 hr, adding plasticizer and defoaming agent, ball grinding for 10 hr, vacuum stirring for defoaming, doctor blading, drying at 60-100 deg.C for 2-3 hr, degumming by heating to 600 deg.C and holding the temp for 4 hr, and sintering at temp lower than 1540 deg.C for 2-4 hr.

Description

Prepare the method for zirconia ceramics and the product that obtains by this method thereof by casting method
Technical field
The present invention relates to a kind ofly prepare the method for zirconia ceramics and the product that obtains by this method thereof by casting method.
Background technology
Flow casting molding (Tape Casting) is a kind of forming method that can obtain high quality, ultra-thin type ceramic substrate, at present can the many thin slice stupaliths of moulding except that zirconium white, and as aluminum oxide, aluminium nitride, barium titanate etc.Be characterized in process stabilizing, production efficiency height, can realize automatic continuous production, quality product is also higher simultaneously, and the scale operation cost is low.The conventional thickness that general ceramic substrate requires is 0.4-1.0mm, and dimensional precision is higher.It is very strict to the requirement of ceramic powder average particle size particle size that production reaches the curtain coating ceramic substrate of this thickness, and the average particle size particle size that laser method is surveyed powder must be stabilized in 2-3 μ m.When the powder average particle size particle size less than 2 μ m, serious cracking or at all can not be used for carrying out flow casting molding 0.4-1.0mm substrate during by present casting method moulding, its reason is as follows:
1. the zirconium white micro mist of present partially stabilized cubic crystalline phase is to use wet chemistry method production basically, and the powder active height can effectively reduce sintering temperature.But the zirconium white micro mist average particle size particle size that this method is produced is generally less than 1 μ m, and it is serious to reunite usually, is difficult for disperseing.Being configured to equal flowing property casting slurry like this needs a large amount of solvents effectively to disperse powder, forms certain fluidity.Cause the solid load (mainly being inorganic material content) of slurry relatively very low like this, finally cause all severe exacerbations of the processability of green compact and the ceramic body performance behind the sintering.Therefore this powder can not satisfy the needs that present traditional curtain coating is produced.
2. can cause all serious cracking of curtain coating process when the solid load of slurry is low, drying is very difficult, and green compact are Texturized easily when dry.Sintering warpage simultaneously is also corresponding bigger, and product size is restive, and yield rate is extremely low.Therefore this powder can not directly be adapted to the large-scale production of the zirconia ceramics substrate of big area, high-precision requirement.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the method for zirconia ceramics and the product that obtains by this method thereof by casting method.
Above-mentioned purpose of the present invention be adopt following technical scheme with to realize:
A kind ofly prepare the method for zirconia ceramics by casting method, its basic step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 1-3 hour;
(2). pretreated zirconium white micro mist adds ball mill, be that basic calculation adds dispersion agent 1-3% by weight percentage with the zirconia powder body weight then, solvent 50-60%, levelling agent 0.5-3%, ball milling was made slurry in 10 hours one time, to add softening agent 2-8% respectively in the above-mentioned slurry again, secondary ball milling was made curtain coating slurry in 10 hours behind the binding agent 3-10%, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent is a dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 10-30 minute, control slurry viscosity 10000-30000mPa.s, on large-scale casting machine, carry out curtain coating then, descended dry 2-3 hour at 60 ℃-100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 0.5-1.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 2-4 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
According to the present invention, its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 1 hour;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 1% then, solvent 50%, levelling agent 0.5%, ball milling was made slurry in 10 hours one time, to add softening agent 2% respectively in the above-mentioned slurry again, binding agent 3% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 10 minutes, control slurry viscosity 10000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 60 ℃-100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 0.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 2 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
According to the present invention, its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 2 hours;
(2). pretreated zirconium white micro mist adds ball mill, add corresponding dispersion agent 2% then, solvent 55%, levelling agent 2%, ball milling was made slurry in 10 hours one time, to add softening agent 6% respectively in the above-mentioned slurry again, binding agent 6% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 20 minutes, control slurry viscosity 20000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 80 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 3 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
According to the present invention, its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 3 hours;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 3% then, solvent 60%, levelling agent 3%, ball milling was made slurry in 10 hours one time, in an above-mentioned slurry, add softening agent 8% respectively again, binding agent 10% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 30 minutes, control slurry viscosity 30000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 3 hours at 100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 4 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
According to the present invention, the weight percent of the zirconia ceramics of being produced composition is:
ZrO 2 94.6%
Y 2O 3 5.2%
Surplus is Al 2O 3
According to the present invention, the performance of the zirconia ceramics that is produced is as follows:
Performance perameter testing performance index method
Volume density (Kg/m 3) 〉=6.02 GB2413-81
Volume specific resistance (Ω .cm25 ℃) 〉=10 13Agilent high resistant tester
The accurate LCR tester of dielectric loss (7.5GHz) 0.001-0.002 Agilent
The anti-folding of bending strength (MPa) 〉=800 experimental machine
Surfaceness R Max≤ 0.2 μ m surfaceness or profile tester
Parallelism MAX (mm) 0.10 parallelism tester
Coefficient of linear expansion
10 -6mm/℃(RT~1000) 9.5-10.5 GB5594.3
The accurate LCR tester of specific inductivity (1MHz) 28.0-29.0 Agilent
Thermal conductivity (20 ℃) is the pulse laser method (W/m.K) 〉=2.0
Planeness (mm) (~/ 25 (length)) 0.04/25 testing flatness instrument
Squareness MAX (mm) 0.10 squareness tester
The ivory white range estimation of color.
According to the present invention, the zirconia ceramics cutter of being produced that is obtained, its weight percent composition is:
ZrO 2 94.6%
Y 2O 3 5.2%
Surplus is Al 2O 3
Because the present invention carries out pre-treatment by the zirconium white micro mist to partially stabilized cubic crystalline phase, under the prerequisite that guarantees the powder sintering performance, effectively reduced the specific surface area of powder, improved the solid load of slurry.And adopt unique flow casting molding prescription and dispersant with high efficiency, realized the production of superfine zirconia powder (average particle size particle size 0.5 μ m) large-scale industrialization curtain coating.Adopt this method can be in enormous quantities, low-cost high-strength, high frequency microwave device, comprise stripline loop and wave filter, use the zirconia ceramics substrate, thickness 0.2-1.0mm and other microwaves economize on electricity device.The zirconia ceramics substrate of being produced is smooth smooth.
Embodiment
Embodiment one:
A kind ofly prepare the method for zirconia ceramics by casting method, its basic step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 1 hour;
(2). pretreated zirconium white micro mist adds ball mill, be that basic calculation adds dispersion agent 1% by weight percentage with the zirconia powder body weight then, solvent 50%, levelling agent 0.5%, ball milling was made slurry in 10 hours one time, to add softening agent 2% respectively in the above-mentioned slurry again, binding agent 3% back secondary ball milling was made curtain coating slurry in 10 hours, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent is a dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 10-30 minute, control slurry viscosity 10000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 60 ℃-100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 0.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 2 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
Embodiment two
Its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 2 hours;
(2). pretreated zirconium white micro mist adds ball mill, add corresponding dispersion agent 2% then, solvent 55%, levelling agent 2%, ball milling was made slurry in 10 hours one time, to add softening agent 6% respectively in the above-mentioned slurry again, binding agent 6% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 20 minutes, control slurry viscosity 20000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 80 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 3 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
Embodiment three:
Its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 3 hours;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 3% then, solvent 60%, levelling agent 3%, ball milling was made slurry in 10 hours one time, in an above-mentioned slurry, add softening agent 8% respectively again, binding agent 10% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 30 minutes, control slurry viscosity 30000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 3 hours at 100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 4 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
The present invention adopts the weight percent of the zirconia ceramics of casting method production to form:
ZrO 2 94.6%
Y 2O 3 5.2%
Surplus is Al 2O 3
The zirconia ceramics chemical constitution that adopts casting method to produce is as follows:
Chemical constitution ZrO 2Y 2O 3Al 2O 3
Weight percent 94.6% 5.2% surpluses.
The main performance index and the testing method of the zirconia ceramics of employing curtain coating legal system are as follows:
Performance perameter testing performance index method
Volume density (Kg/m 3) 〉=6.02 GB2413-81
Volume specific resistance (25 ℃ of Ω .cm) 〉=10 13Agilent high resistant tester
The accurate LCR tester of dielectric loss (7.5GHz) 0.001-0.002 Agilent
The anti-folding of bending strength (MPa) 〉=800 experimental machine
Surfaceness R Max≤ 0.2 μ m surfaceness or profile tester
Parallelism MAX (mm) 0.10 parallelism tester
Coefficient of linear expansion
10 -6mm/℃(RT~1000) 9.5-10.5 GB5594.3
The accurate LCR tester of specific inductivity (1MHz) 28.0-29.0 Agilent
Thermal conductivity (20 ℃) is the pulse laser method (W/m.K) 〉=2.0
Planeness (mm) (~/ 25 (length)) 0.04/25 testing flatness instrument
Squareness MAX (mm) 0.10 squareness tester
The ivory white range estimation of color.

Claims (7)

1, a kind ofly prepare the method for zirconia ceramics by casting method, its basic step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 1-3 hour;
(2). pretreated zirconium white micro mist adds ball mill, be that basic calculation adds dispersion agent 1-3% by weight percentage with the zirconia powder body weight then, solvent 50-60%, levelling agent 0.5-3%, ball milling was made slurry in 10 hours one time, to add softening agent 2-8% respectively in the above-mentioned slurry again, secondary ball milling was made curtain coating slurry in 10 hours behind the binding agent 3-10%, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent is a dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 10-30 minute, control slurry viscosity 10000-30000mPa.s, on large-scale casting machine, carry out curtain coating then, descended dry 2-3 hour at 60 ℃-100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 0.5-1.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 2-4 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
2, according to claim 1ly a kind ofly prepare the method for zirconia ceramics by casting method, its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 1 hour;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 1% then, solvent 50%, levelling agent 0.5%, ball milling was made slurry in 10 hours one time, to add softening agent 2% respectively in the above-mentioned slurry again, binding agent 3% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 10 minutes, control slurry viscosity 10000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 60 ℃-100 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 0.5 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 2 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
3, according to claim 1ly a kind ofly prepare the method for zirconia ceramics by casting method, its basic step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 2 hours;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 2% then, solvent 55%, levelling agent 2%, ball milling was made slurry in 10 hours one time, to add softening agent 6% respectively in the above-mentioned slurry again, binding agent 6% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 20 minutes, control slurry viscosity 20000mPa.s, on large-scale casting machine, carry out curtain coating then, following dry 2 hours at 80 ℃ simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1 ℃/min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 3 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
4, according to claim 1ly a kind ofly prepare the method for zirconia ceramics by casting method, its step is as follows:
(1). with the zirconium white micro mist of the partially stabilized cubic crystalline phase of wet chemistry method production 600-800 ℃ down calcining carried out pre-treatment in 3 hours;
(2). pretreated zirconium white micro mist adds ball mill, add dispersion agent 3% then, solvent 60%, levelling agent 3%, ball milling was made slurry in 10 hours one time, to add softening agent 8% respectively in the above-mentioned slurry again, binding agent 10% back secondary ball milling was made curtain coating slurry in 10 hours, below all be weight percentage, with the zirconia powder body weight is basic calculation, above-mentioned dispersion agent is Viscotrol C or phosphoric acid ester, binding agent is a polyvinyl butyral acetal, softening agent is the mixture of dibutyl phthalate and o-phthalic acid dibutyl ester, weight ratio 1:1, solvent are dehydrated alcohol, and levelling agent is a pimelinketone;
(3). the casting slurry behind the ball milling is rich in a large amount of bubbles, must be through vacuum stirring de-bubble 30 minutes, control slurry viscosity 30000mPa.s, on large-scale casting machine, carry out curtain coating then, under 100 ° of C dry 3 hours simultaneously, be prepared into the zirconia ceramics green compact, green compact after the curtain coating are placed on that the temperature rise rate with 1.5 ℃ of min is raised to 600 ℃ from room temperature on the load bearing board, be incubated 4 hours binder removals, then less than 1540 ℃ of following sintering 4 hours, substrate behind the sintering is through sandblast and smooth processing, and thickness is 0.2-1.0mm.
5, the product that is obtained according to claim 1 or 2 or 3 or 4 described methods is characterized in that: the weight percent of the zirconia ceramics of being produced is formed and is:
ZrO 2 94.6%
Y 2O 3 5.2%
Surplus is Al 2O 3
6, product according to claim 5, it is characterized in that: the performance of the zirconia ceramics that is produced is as follows:
Performance perameter testing performance index method
Volume density (Kg/m 3) 〉=6.02 GB2413-81
Volume specific resistance (25 ℃ of Ω .cm) 〉=10 13Agilent high resistant tester
The accurate LCR tester of dielectric loss (7.5GHz) 0.001-0.002 Agilent
The anti-folding of bending strength (MPa) 〉=800 experimental machine
Surfaceness R Max≤ 0.2 μ m surfaceness or profile tester
Parallelism MAX (mm) 0.10 parallelism tester
Coefficient of linear expansion
10 -8mm/℃(RT~1000) 9.5-10.5 GB5594.3
The accurate LCR tester of specific inductivity (1MHz) 28.0-29.0 Agilent
Thermal conductivity (20 ℃) is the pulse laser method (W/m.K) 〉=2.0
Planeness (mm) (~/ 25 (length)) 0.04/25 testing flatness instrument
Squareness MAX (mm) 0.10 squareness tester
The ivory white range estimation of color.
7, the zirconia ceramics cutter that is obtained according to claim 1 or 2 or 3 or 4 described methods, its weight percent are formed:
ZrO 2 94.6%
Y 2O 3 5.2%
Surplus is Al 2O 3
CNB031140971A 2003-04-02 2003-04-02 Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method Expired - Fee Related CN100519475C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB031140971A CN100519475C (en) 2003-04-02 2003-04-02 Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB031140971A CN100519475C (en) 2003-04-02 2003-04-02 Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method

Publications (2)

Publication Number Publication Date
CN1534001A CN1534001A (en) 2004-10-06
CN100519475C true CN100519475C (en) 2009-07-29

Family

ID=34283935

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB031140971A Expired - Fee Related CN100519475C (en) 2003-04-02 2003-04-02 Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method

Country Status (1)

Country Link
CN (1) CN100519475C (en)

Families Citing this family (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101328068B (en) * 2008-07-28 2010-12-22 浙江大学 Preparation of boric microwave dielectric ceramic aqueous tape casting diaphragm
CN101870577B (en) * 2010-06-25 2013-01-02 沈阳大学 Preparation method of magnesium phase-enriched cordierite water-based tape casting slurry
CN101927656B (en) * 2010-07-20 2014-12-24 李思渊 Ceramic stamp
CN102503444B (en) * 2011-11-15 2013-03-27 中国电子科技集团公司第十三研究所 Non-aqueous tape casting slurry and preparation method thereof
CN102627474B (en) * 2012-04-18 2013-07-03 深圳顺络电子股份有限公司 Treatment method for burning board
CN102718498B (en) * 2012-07-04 2013-11-06 珠海微晶新材料科技有限公司 Coating preparation method for flakey aluminum oxide ceramic
CN102718497B (en) * 2012-07-04 2014-01-15 珠海微晶新材料科技有限公司 Coating preparation method for flaky zirconium oxide ceramic
CN103435358B (en) * 2013-08-29 2015-03-25 中国人民解放军国防科学技术大学 Organic composition added in preparation of tape-casting slurry and application of organic composition
CN103951421A (en) * 2014-04-25 2014-07-30 东风电子科技股份有限公司 Casting slurry and method for preparing zirconia substrate for NOx sensor by using same
CN104098341A (en) * 2014-07-11 2014-10-15 中国第一汽车股份有限公司 Preparation method of porous yttrium-stabilized zirconium oxide for sensor
CN104446457A (en) * 2014-11-18 2015-03-25 潮州三环(集团)股份有限公司 Modified zirconium oxide ceramic material and application thereof
CN104771206B (en) * 2015-05-07 2017-03-08 珠海市香之君科技股份有限公司 Knife blade and the processing method of scalpel
CN105032348B (en) * 2015-07-07 2017-12-22 中国科学院水生生物研究所 A kind of redox graphene/nano zirconium dioxide composite adsorption dephosphorization agent and preparation method
CN105503182A (en) * 2015-12-18 2016-04-20 珠海市香之君科技股份有限公司 Cutter blank forming technology of ceramic surgical blade
CN107399969A (en) * 2016-05-19 2017-11-28 张尚权 A kind of method that curtain coating in situ prepares zirconia ceramics piece
CN105881700A (en) * 2016-05-26 2016-08-24 郑州中瓷科技有限公司 High-strength ceramic substrate and preparation method and production line thereof
CN106977201A (en) * 2017-03-30 2017-07-25 南京云启金锐新材料有限公司 High-purity high-strength high-ductility zirconia composite ceramics ultra thin plate and preparation method thereof
CN107698253B (en) * 2017-11-11 2020-03-27 郑州方铭高温陶瓷新材料有限公司 Preparation method of thermal protection ceramic plate applied to rocket launching platform
CN110862260B (en) * 2018-08-28 2021-03-26 比亚迪股份有限公司 Electronic product shell, preparation method thereof and mobile phone rear cover
CN110357623A (en) * 2019-07-16 2019-10-22 广东捷成科创电子股份有限公司 A kind of fine grain and high-intensitive novel zirconia ceramic product and preparation method thereof
CN111925215A (en) * 2020-07-20 2020-11-13 宁波伏尔肯科技股份有限公司 Preparation method of enhanced layered ceramic bulletproof piece
CN112661504B (en) * 2020-12-28 2023-01-31 长裕控股集团股份有限公司 Preparation method of zirconia dental material
CN112876245A (en) * 2021-01-28 2021-06-01 深圳陶陶科技有限公司 Preparation method of zirconia ceramic
CN114702306B (en) * 2022-04-22 2022-12-13 湖南省新化县鑫星电子陶瓷有限责任公司 Preparation method of 95 alumina ceramic substrate and product thereof
CN116462516A (en) * 2023-03-14 2023-07-21 乐山职业技术学院 Silicon nitride ceramic and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6068828A (en) * 1997-06-13 2000-05-30 Nippon Shokubai Co., Ltd. Zirconia powder, method for producing the same, and zirconia ceramics using the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6068828A (en) * 1997-06-13 2000-05-30 Nippon Shokubai Co., Ltd. Zirconia powder, method for producing the same, and zirconia ceramics using the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
氧化钇掺杂四方氧化锆电性能的研究. 刘继进等.硅酸盐学报,第31卷第3期. 2003 *
流延法制备YSZ电解质薄膜研究. 梁广川等.陶瓷学报,第21卷第1期. 2000 *

Also Published As

Publication number Publication date
CN1534001A (en) 2004-10-06

Similar Documents

Publication Publication Date Title
CN100519475C (en) Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method
CN100503507C (en) Low temperature sintered 99 aluminium oxide ceramic and its production method and use
CN111747756B (en) Nitride ceramic tape-casting slurry and nitride ceramic substrate prepared from same
EP0708068B1 (en) Method for controlling firing shrinkage of ceramic green body
CN107857595A (en) Silicon nitride ceramics slurry and preparation method thereof and the application for preparing Silicon Nitride Slips by Tape Casting
CN105622093B (en) Ceramic material and preparation method thereof, resonator, filter and radio frequency remote equipment
EP0659705A1 (en) Sintered ceramic article formed mainly of alumina
WO2020052453A1 (en) Silicon nitride ceramic material for mobile phone back plate and preparation method therefor
CN112608154A (en) Silicon nitride ceramic slurry and preparation method and application thereof
CN100457678C (en) Dielectric adjustable material of ceramics burned together at low temperature, and preparation method
CN108409336A (en) Silicon nitride ceramics and preparation method thereof
CN115028460B (en) Preparation method of high-heat-conductivity silicon nitride ceramic substrate
CN102173784B (en) Method for preparing sodium bismuth titanate-barium titanate composite dielectric ceramic through sol cladding method
CN108218422A (en) Wear-resistant ceramic tape casting slurry and its application process
CN115849885B (en) High-purity high-strength alumina ceramic substrate and preparation method thereof
US20240002294A1 (en) Alkaline porous ceramic matrix and preparation method thereof, electronic-cigarette vaporization core, and electronic cigarette
CN114736012B (en) Low dielectric microwave dielectric ceramic with ultrahigh Q value and LTCC material thereof
CN114835473B (en) Alumina ceramic and preparation method thereof
CN110981480A (en) High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof
CN115124343A (en) Zirconia solid solution yttria ceramic, preparation method and application thereof
KR20190023485A (en) Aluminum nitride sintered body and method for manufacturing the same
CN113105216A (en) Injection-molded zirconium-aluminum composite ceramic and preparation method thereof
CN110511025B (en) Preparation method of NN-based piezoelectric ceramic
CN113582694A (en) Method for forming yttrium aluminum garnet type microwave dielectric ceramic by using Isobam system gel injection molding
CN111499359A (en) Production process of alumina ceramic

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090729

Termination date: 20200402