CN108751985A - Gray oxide zircon ceramic feedstock composition, gray oxide zircon ceramic and preparation method thereof - Google Patents
Gray oxide zircon ceramic feedstock composition, gray oxide zircon ceramic and preparation method thereof Download PDFInfo
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- CN108751985A CN108751985A CN201810522624.8A CN201810522624A CN108751985A CN 108751985 A CN108751985 A CN 108751985A CN 201810522624 A CN201810522624 A CN 201810522624A CN 108751985 A CN108751985 A CN 108751985A
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Abstract
The present invention relates to a kind of gray oxide zircon ceramic feedstock compositions, gray oxide zircon ceramic and preparation method thereof.A kind of gray oxide zircon ceramic feedstock composition, including zirconia ceramics material of main part and additive；The additive includes at least one of aluminium oxide and gallium oxide, nickel oxide and manganese oxide；In the gray oxide zircon ceramic feedstock composition, the mass percentage of at least one of the aluminium oxide and gallium oxide is 0.01%~20%, the mass percentage of the nickel oxide is 0.01%~4%, and the mass percentage of the manganese oxide is 0.01%~3%.It is not easy to collapse when above-mentioned gray oxide zircon ceramic feedstock composition processing scarce.
Description
Technical field
The present invention relates to a kind of gray oxide zircon ceramic feedstock compositions, gray oxide zircon ceramic and preparation method thereof.
Background technology
Zirconium dioxide is due to excellent mechanics, calorifics and electric property, in structural material, optical material, the quick member of oxygen
It has a wide range of applications in terms of part and fuel cell.In recent years, gray oxide zircon ceramic is with its excellent mechanical performance and wear-resisting
Performance becomes new lover's material, is widely used in fields such as decoration, electronic products.However, existing gray oxide zirconium
Ceramics are difficult to, and are easy to collapse in process scarce so that yield rate is told somebody what one's real intentions are, to limit answering for gray oxide zircon ceramic
With, and at present almost without gray oxide zircon ceramic.
Invention content
Based on this, it is necessary to provide and be not easy to collapse scarce gray oxide zircon ceramic feedstock composition, grey when a kind of processing
Zirconia ceramics and preparation method thereof.
A kind of gray oxide zircon ceramic feedstock composition, including zirconia ceramics material of main part and additive；The addition
Agent includes at least one of aluminium oxide and gallium oxide, nickel oxide and manganese oxide；The gray oxide zircon ceramic feedstock composition
In, the mass percentage of at least one of the aluminium oxide and gallium oxide is 0.01%~20%, the matter of the nickel oxide
It is 0.01%~4% to measure percentage composition, and the mass percentage of the manganese oxide is 0.01%~3%.
The addition of special formulation is added in above-mentioned gray oxide zircon ceramic feedstock composition in zirconia ceramics material of main part
Agent improves processing performance, and additive includes at least one of aluminium oxide and gallium oxide, iron oxide and cobalt oxide, several components
Proportioning is reasonable, the crystal grain of zirconium oxide can be made firmly to combine each other, therefore can improve fracture toughness so that intensity and toughness
Reach good balance, can significantly improve processing performance, through measuring, made of gray oxide zircon ceramic feedstock composition
The toughness and hardness matching degree of gray oxide zircon ceramic are preferable, are easily worked, be less prone to collapse it is scarce；In addition, nickel oxide, manganese oxide
As the primary raw material of grey colorant, it can cooperate with and play a role at high temperature, form the grey ceramics with spinel structure,
With excellent high-temperature stability, will not occur decomposing at a temperature of 1500 DEG C and gamut, and evenness；It is logical
It crosses and is adjusted the gray oxide zirconium that can form different tones pottery to the ratio of above-mentioned zirconia ceramics material of main part and additive
Porcelain.
The additive further includes magnesia, calcium oxide, zinc oxide, barium monoxide and oxidation in one of the embodiments,
At least one of strontium；In the gray oxide zircon ceramic feedstock composition, the magnesia, calcium oxide, zinc oxide, barium monoxide
And the mass percentage of at least one of strontium oxide strontia is 0.01~15%.
The additive further includes yttrium oxide in one of the embodiments, the gray oxide zircon ceramic material combination
The mass percentage of yttrium oxide described in object is 2.5%~7.85%.
At least one in the magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia in one of the embodiments,
Kind mass percentage be 0.1%~5%, the mass percentage of at least one of the aluminium oxide and gallium oxide is
0.3%~6%, the mass percentage of the nickel oxide is 0.1%~3%, and the mass percentage of the manganese oxide is
0.01%~1.6%, the mass percentage of the yttrium oxide is 3%~6.3%.
The gray oxide zircon ceramic feedstock composition includes 0.01%~10% oxidation in one of the embodiments,
Aluminium.
The zirconia ceramics material of main part is the zirconium oxide containing hafnium oxide in one of the embodiments,.
It is 0.05 μm~1.50 μm that the gray oxide zircon ceramic feedstock composition, which is D50, in one of the embodiments,
Specific surface area is 6m2/ g~25m2The powder of/g.
The gray oxide zircon ceramic that above-mentioned gray oxide zircon ceramic feedstock composition is prepared.
In one of the embodiments, the gray oxide zircon ceramic be converted into polishing after 0.5mm equivalent thickness,
Light transmittance < 20% under 550nm wavelength, SCI chromatic values are L >=43, -10≤a≤2, -10≤b≤6.
A kind of preparation method of gray oxide zircon ceramic, includes the following steps：
Above-mentioned gray oxide zircon ceramic feedstock composition is uniformly mixed and obtains premix；And
By the premix molding and be sintered obtain gray oxide zircon ceramic.
Specific implementation mode
Below in conjunction with specific implementation mode to gray oxide zircon ceramic feedstock composition, gray oxide zircon ceramic and its system
Preparation Method is further described in detail.
The gray oxide zircon ceramic feedstock composition of one embodiment, including zirconia ceramics material of main part and additive.
Additive includes at least one of magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia, aluminium oxide and gallium oxide
At least one, nickel oxide and manganese oxide.
Zirconia ceramics material of main part is mainly zirconium oxide.Certainly, in order to improve the performance of zirconia ceramics material of main part,
It is also possible to mix some other components in zirconium oxide.
In some embodiments, zirconia ceramics material of main part further includes hafnium oxide, and zirconia ceramics material of main part is
Zirconium oxide containing hafnium oxide.The quality percentage of hafnium oxide contains in zirconia ceramics material of main part in one of the embodiments,
Amount is 5%.
The mass percentage of at least one of aluminium oxide and gallium oxide is in gray oxide zircon ceramic feedstock composition
0.01%~20%.The mass percentage of at least one of aluminium oxide and gallium oxide is in one of the embodiments,
0.3%~6%.Certainly in other embodiments, the mass percentage of at least one of aluminium oxide and gallium oxide is
1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%,
18% or 19%.
In some embodiments, gray oxide zircon ceramic feedstock composition includes 0.01%~10% aluminium oxide.Into
One step, the mass percentage of aluminium oxide is 1%~7% in gray oxide zircon ceramic feedstock composition.Certainly in others
In embodiment, the mass percentage of aluminium oxide is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
Further, the mass percentage of gallium oxide is 1%~5% in gray oxide zircon ceramic feedstock composition.When
So in other examples, the mass percentage of gallium oxide is 0.5%, 1%, 2%, 3%, 4% or 5%.
In some embodiments, additive further includes in magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia
It is at least one.Preferably, in gray oxide zircon ceramic feedstock composition, magnesia, calcium oxide, zinc oxide, barium monoxide and oxidation
The mass percentage of at least one of strontium is 0.01%~15%.
At least one of magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia in one of the embodiments,
Mass percentage is 0.1%~5%.Certainly in other embodiments, magnesia, calcium oxide, zinc oxide, barium monoxide and oxygen
The mass percentage for changing at least one of strontium is 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%,
9%, 10%, 11%, 12%, 13% or 14%.
In gray oxide zircon ceramic feedstock composition, the mass percentage of nickel oxide is 0.01%~3%.In some realities
It applies in mode, the mass percentage of nickel oxide is 0.1%~3%, certainly in other examples, the quality hundred of nickel oxide
It is 0.1%, 0.5%, 1%, 1.5%, 2% or 2.5% to divide content.
In gray oxide zircon ceramic feedstock composition, the mass percentage of manganese oxide is 0.01%~3%.In some realities
It applies in mode, the mass percentage of manganese oxide is 0.01%~1.6%, certainly in other examples, the matter of manganese oxide
It is 0.1%, 0.5%, 1%, 1.5%, 2% or 2.5% to measure percentage composition.
In some embodiments, additive further includes yttrium oxide.Yttrium oxide in gray oxide zircon ceramic feedstock composition
Mass percentage be 2.5%~7.85%.Further, in gray oxide zircon ceramic feedstock composition yttrium oxide quality
Percentage composition is 3%~6.3%.Certainly in other embodiments, the mass percentage of yttrium oxide be 3%, 3.5%,
4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7% or 7.5%.
It is 0.05 μm~1.50 μm that gray oxide zircon ceramic feedstock composition, which is D50, in one of the embodiments, compares table
Area is 6m2/ g~25m2The powder of/g.
It should be noted that in above-mentioned gray oxide zircon ceramic feedstock composition, by adjusting zirconia ceramics main body material
The content of material so that the gross mass percentage composition of all components meets 100%.
Certainly, in order to further enhance the performance of gray oxide zircon ceramic, the component of other modifications can also be added, herein
It does not repeat one by one.
In order to obtain the gray oxide zircon ceramic of different tones, zirconia ceramics material of main part and additive can be contained
Amount and the concrete composition of additive are adjusted, to obtain the gray oxide zircon ceramic of different tones.
The addition of special formulation is added in above-mentioned gray oxide zircon ceramic feedstock composition in zirconia ceramics material of main part
Agent improves processing performance, and additive includes at least one of magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia, oxygen
Change at least one of aluminium and gallium oxide, nickel oxide and manganese oxide, several reasonable mixture ratio of components, can make zirconium oxide crystal grain that
This is firmly combined, therefore can improve fracture toughness so that intensity and toughness reach good balance, can significantly improve and add
Work performance, through measuring, the toughness and hardness of gray oxide zircon ceramic made of gray oxide zircon ceramic feedstock composition
It is preferable with degree, be easily worked, be less prone to collapse it is scarce.In addition, the primary raw material of nickel oxide, manganese oxide as grey colorant, it can
Collaboration plays a role at high temperature, forms the black ceramic with spinel structure, has excellent high-temperature stability, even if
Will not occur decomposing at a temperature of 1500 DEG C and gamut, and evenness；By to above-mentioned zirconia ceramics material of main part
And the ratio of additive is adjusted the gray oxide zircon ceramic that can form different tones.
It is understood that the technical solution of multiple embodiments of foregoing description without conflicting with each other can be into
Row combination application.
Above-mentioned gray oxide zircon ceramic composition is by the way that zirconia ceramics material of main part to be mixed to get with additive.
The gray oxide zircon ceramic of one embodiment is prepared by above-mentioned gray oxide zircon ceramic feedstock composition.
Gray oxide zircon ceramic is converted into the equivalent thickness of the 0.5mm after polishing, 550nm in one of the embodiments,
Light transmittance < 20% under wavelength, SCI chromatic values are L >=43, -10≤a≤2, -10≤b≤6.
For above-mentioned gray oxide zircon ceramic through measuring, toughness and hardness matching degree are preferable, are easily worked, are less prone to and collapse
It lacks.
The preparation method of above-mentioned gray oxide zircon ceramic, includes the following steps：
Step S110, gray oxide zircon ceramic feedstock composition is uniformly mixed and obtains premix.
Gray oxide zircon ceramic feedstock composition is the gray oxide zircon ceramic feedstock composition of above-described embodiment description.
The grinding of each raw material of zirconia ceramics material of main part and additive is sufficiently mixed in one of the embodiments,
To premix.Further, grinding can be sand milling, ball milling.Further, ball milling is wet ball grinding or dry ball milling.
Additive is precipitated by mixing the corresponding salting liquid of each raw material with aqueous slkali in one of the embodiments,
Reaction, is precipitated and calcines to obtain.Grinding obtains premix after ceramic zirconium oxide ceramic body material is mixed with additive.
Further, aqueous slkali is sodium hydroxide solution.Salting liquid be at least one of chloride solution or nitrate solution, herein
The corresponding meaning is that the corresponding salting liquid of copper oxide is copper chloride solution or copper nitrate solution.Further, grinding can be sand
Mill, ball milling.Further ball milling is wet ball grinding or dry ball milling.
Step S120, by premix molding and be sintered obtain gray oxide zircon ceramic.
Premix is granulated in one of the embodiments, to obtain ceramic powder, isostatic cool pressing compression moulding is sintered later
Obtain gray oxide zircon ceramic.Further, the pressure of isostatic cool pressing compression moulding is 100MPa.Further, the work of sintering
Skill parameter is：1430 DEG C are risen to the heating rate of 2 DEG C/min, heat preservation 1.5h is sintered.
In one of the embodiments, by premix and acrylic resin, stearic acid and paraffin be mixed to get masterbatch, will
Injection moulding obtains biscuit after masterbatch is kneaded, and biscuit is carried out dumping later and sintering obtains gray oxide zircon ceramic.Preferably,
In masterbatch, the mass percentage of acrylic resin is 8.5%, and stearic mass percentage is 2%, and paraffin is common stone
The mass percentage of wax, paraffin is 6.5%.Preferably, the technological parameter of mixing is：It is kneaded 3 hours at 180 DEG C.Preferably,
The technological parameter of dumping is：With the heating rate of 0.1 DEG C/min rises to 200 DEG C, the heating rate of 0.4 DEG C/min rises by 200 DEG C
To 400 DEG C, 400 DEG C keep the temperature 2 hours dumpings.Preferably, the technological parameter of sintering is：1360 DEG C of heat preservations 1.5 are risen to 2 DEG C/min
Hour.
Above-mentioned several embodiments, the merely illustrative several preparation methods for listing gray oxide zircon ceramic, need
Illustrate, gray oxide zircon ceramic is not limited to use above-mentioned preparation method, other preparation methods preparation in the industry may be used.
The preparation method of above-mentioned gray oxide zircon ceramic, easy to operate, the gray oxide zircon ceramic being prepared is being processed
During be not easy to collapse it is scarce.Harsh preparation method ability must be used by changing the gray oxide zircon ceramic of current similar demand
It avoids collapsing scarce drawback.
It is specific embodiment below.
Content in following embodiment is mass percentage, and number is mass fraction.Such as without spy in following embodiment
Different explanation does not include then that other in addition to inevitable impurity do not point out component.
The zirconia ceramics material of main part used in following embodiment is the zirconium oxide containing hafnium oxide；Contain hafnium oxide
In zirconium oxide, mass percentage of the hafnium oxide in the zirconium oxide containing hafnium oxide is 5%.
Embodiment 1
The composition of gray oxide zircon ceramic feedstock composition and the specific surface area of zirconia ceramics material of main part are shown in Table 1.
It is dried to obtain premix after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling；By premix
Granulation obtains ceramic powder；Ceramic powder is pressed into tablet with 100MPa isostatic cool pressings, after with the heating rate liter of 2 DEG C/min
To 1430 DEG C, heat preservation 1.5h obtains gray oxide zircon ceramic.
Embodiment 2
The composition of gray oxide zircon ceramic feedstock composition and the specific surface area of zirconia ceramics material of main part are shown in Table 1.
Premix, premix and poly- third are obtained after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling
Olefine resin, stearic acid and common paraffin are kneaded at 180 DEG C obtains masterbatch for 3 hours, and the content of acrylic resin is in masterbatch
8.5%, stearic content is 2%, and the content of common paraffin is 6.5%.Masterbatch is injection moulded.It is heated up with 0.1 DEG C/min
Rate rise to 200 DEG C, 0.4 DEG C/min rise to 400 DEG C by 200 DEG C, 400 DEG C of heat preservations, 2 hours dumpings, then risen to 2 DEG C/min
1360 DEG C of heat preservations obtain gray oxide zircon ceramic in 1.5 hours.
Embodiment 3
To containing Ni (NO3)2、Al(NO3)3、Mn(NO3)2、Ca(NO3)2Solution in excessive NaOH solution is added dropwise while stirring,
Precipitation mixture washing and drying calcines to obtain colorant powder.By toner material, Y2O3, zirconia ceramics material of main part be mixed to get grey oxygen
Change zircon ceramic feedstock composition.The composition of gray oxide zircon ceramic feedstock composition and the specific surface of zirconia ceramics material of main part
Product is shown in Table 1.
It is dried to obtain premix after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling；By premix
Granulation obtains ceramic powder；Ceramic powder is pressed into tablet with 100MPa isostatic cool pressings, after with the heating rate liter of 2 DEG C/min
To 1450 DEG C, heat preservation 1.5h obtains gray oxide zircon ceramic.
Embodiment 4
The composition of gray oxide zircon ceramic feedstock composition gray oxide zircon ceramic feedstock composition and zirconia ceramics master
The specific surface area of body material is shown in Table 1.
Premix, premix and poly- third are obtained after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling
Olefine resin, stearic acid and common paraffin are kneaded at 170 DEG C obtains masterbatch for 3 hours, and the content of acrylic resin is in masterbatch
6%, stearic content is 1.5%, and the content of common paraffin is 7%.Masterbatch is injection moulded.It is heated up with 0.1 DEG C/min fast
Rate rise to 200 DEG C, 0.4 DEG C/min rise to 400 DEG C by 200 DEG C, 400 DEG C of heat preservations, 2 hours dumpings, then 1400 are risen to 2 DEG C/min
DEG C heat preservation obtains gray oxide zircon ceramic in 2 hours.
Embodiment 5
The composition of gray oxide zircon ceramic feedstock composition and the specific surface area of zirconia ceramics material of main part are shown in Table 1.
It is dried to obtain premix after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling；By premix
Granulation obtains ceramic powder；Ceramic powder is pressed into tablet with 100MPa isostatic cool pressings, after with the heating rate liter of 2 DEG C/min
To 1480 DEG C, heat preservation 2h obtains gray oxide zircon ceramic.
Embodiment 6
The composition of gray oxide zircon ceramic feedstock composition and the specific surface area of zirconia ceramics material of main part are shown in Table 1.
It is dried to obtain premix after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling；By premix
Granulation obtains ceramic powder；Ceramic powder is pressed into tablet with 100MPa isostatic cool pressings, after with the heating rate liter of 2 DEG C/min
To 1480 DEG C, heat preservation 2h obtains gray oxide zircon ceramic.
Embodiment 7
The composition of gray oxide zircon ceramic feedstock composition and the specific surface area of zirconia ceramics material of main part are shown in Table 1.
It is dried to obtain premix after gray oxide zircon ceramic feedstock composition is sufficiently mixed dispersion with ball milling；By premix
Granulation obtains ceramic powder；Ceramic powder is pressed into tablet with 100MPa isostatic cool pressings, after with the heating rate liter of 2 DEG C/min
To 1480 DEG C, heat preservation 2h obtains gray oxide zircon ceramic.
It is put into spectrophotometer, surveys after gray oxide zircon ceramic piece prepared by the Examples 1 to 7 of 0.5mm thickness is polished
The visible light transmittance within the scope of its 550nm is measured, the CIE (International Commission on Illumination) using D65 light sources is found out using color meter
L*, a*, b* chromatic value, the results are shown in Table 1.Relative density is tested using drainage density tester, using universal material pulling force
Machine tests four-point bending intensity, uses climatic chamber and XRD to test ageing properties (being evaluated with monoclinic phase content), using SENB
Method tests fracture toughness, tests hardness using Vickers, the results are shown in Table 1.
Table 1
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of gray oxide zircon ceramic feedstock composition, which is characterized in that including zirconia ceramics material of main part and additive；
The additive includes at least one of aluminium oxide and gallium oxide, nickel oxide and manganese oxide；The gray oxide zircon ceramic is former
In feed composition, the mass percentage of at least one of the aluminium oxide and gallium oxide is 0.01%~20%, the oxygen
The mass percentage for changing nickel is 0.01%~4%, and the mass percentage of the manganese oxide is 0.01%~3%.
2. gray oxide zircon ceramic feedstock composition according to claim 1, which is characterized in that the additive further includes
At least one of magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia；The gray oxide zircon ceramic feedstock composition
In, the mass percentage of at least one of the magnesia, calcium oxide, zinc oxide, barium monoxide and strontium oxide strontia is 0.01~
15%.
3. gray oxide zircon ceramic feedstock composition according to claim 1, which is characterized in that the additive further includes
Yttrium oxide, the mass percentage of yttrium oxide described in the gray oxide zircon ceramic feedstock composition are 2.5%~7.85%.
4. gray oxide zircon ceramic feedstock composition according to claim 2, which is characterized in that the magnesia, oxidation
The mass percentage of at least one of calcium, zinc oxide, barium monoxide and strontium oxide strontia is 0.1%~5%, the aluminium oxide and oxygen
The mass percentage for changing at least one of gallium is 0.3%~6%, the mass percentage of the nickel oxide is 0.1%~
3%, the mass percentage of the manganese oxide is 0.01%~1.6%, the mass percentage of the yttrium oxide is 3%~
6.3%.
5. gray oxide zircon ceramic feedstock composition according to claim 1, which is characterized in that the gray oxide zirconium pottery
Porcelain feedstock composition includes 0.01%~10% aluminium oxide.
6. gray oxide zircon ceramic feedstock composition according to claim 1, which is characterized in that the zirconia ceramics master
Body material is the zirconium oxide containing hafnium oxide.
7. gray oxide zircon ceramic feedstock composition according to claim 1, which is characterized in that the gray oxide zirconium pottery
Porcelain feedstock composition is that D50 is 0.05 μm~1.50 μm, specific surface area 6m2/ g~25m2The powder of/g.
8. the gray oxide zirconium pottery that claim 1~7 any one of them gray oxide zircon ceramic feedstock composition is prepared
Porcelain.
9. gray oxide zircon ceramic according to claim 8, which is characterized in that the gray oxide zircon ceramic is converted into throwing
Light transmittance < 20% under the equivalent thickness of 0.5mm after light, 550nm wavelength, SCI chromatic values be L >=43, -10≤a≤2, -
10≤b≤6。
10. a kind of preparation method of gray oxide zircon ceramic, which is characterized in that include the following steps：
Claim 1~7 any one of them gray oxide zircon ceramic feedstock composition is uniformly mixed and obtains premix；And
By the premix molding and be sintered obtain gray oxide zircon ceramic.
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