CN108033789A - A kind of black zirconia ceramics material compositions and its application - Google Patents
A kind of black zirconia ceramics material compositions and its application Download PDFInfo
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Abstract
The invention discloses a kind of black zirconia ceramics material compositions, the component of following mass percentage is included:Iron oxide 0.01 4%, cobalt oxide 0.01 3.5%, aluminium oxide 0.01 15%, zinc oxide 0 3.5%, yittrium oxide 2 7%, titanium oxide 0 4%, silica 0.01 1.0%, surplus are the zirconium oxide containing hafnium oxide.The colouring agent that the present invention passes through the addition black inside zirconia ceramics powder, the granularity of the added silica of control and aluminium oxide, improve the covering power and blackness of zirconia ceramics, reduce its light transmittance, improve it and be molded the mechanical strength of porcelain body, ensure excellent effect of both product colour and intensity.Meanwhile the invention also discloses the black zirconia ceramics and the preparation method of the black zirconia ceramics being prepared using the black zirconia ceramics material compositions.
Description
Technical field
The present invention relates to a kind of ceramic material powder and its application, especially a kind of black zirconia ceramics material compositions
And its application.
Background technology
Zirconium dioxide is due to excellent mechanics, calorifics, electric property, in structural material, optical element, oxygen sensitive element
Have a wide range of applications with fuel cell etc..In recent years, as people are to the high speed development of ornament demand, black oxidation
Zircon ceramic becomes high-grade decoration with its excellent mechanical performance, chromatic colour, metallic luster and the features such as acted on without allergy
New lover's material, has vast market prospect in high-grade watch chain, bangle, phone housing etc..But the black of common process production
Zirconia ceramics there are brittleness is big, intensity is low, Color uniformity is poor, blackness is insufficient, translucency is good, color mileage is insufficient etc. no
Good shortcoming, can not meet the requirement of the appearance elements such as high blackness mobile phone board.
Color and intensity are always ceramic appearance member two large problems urgently to be resolved hurrily.In terms of color, existing technical side
Case is by zirconia ceramics in vacuum, reducing atmosphere or inert atmosphere black, and Lacking oxygen is formed, so as to form the point of colour center
Defect, produces the sink effect to light.It is the colorant oxide such as doping iron, cobalt, nickel in zirconium oxide to compare similar technology, is led to
Absorption of the addition colorant raising to light is crossed, so as to improve the covering power and blackness of zirconia material.In terms of intensity, the prior art
Scheme is usually that directly will prepare slurry after zirconium oxide and the direct ball milling of other additives, to the additive amount and granularity of silica
Detailed anatomy is not done, the intensity and brittleness for causing shaping porcelain body do not conform to ideal yet.
Using vacuum drying oven, reducing atmosphere stove or inert atmosphere stove, it is necessary to sinter zirconium oxide into porcelain in atmosphere, then upper
State in sintering furnace and black, the cost of production technology has so been significantly greatly increased, the product that special shape and thickness differ is being sent out
Easily because a series of problems, such as colour center inhomogeneities causes aberration occur, causes product blackness insufficient during black.And in oxygen
Change the colorant oxide such as doping iron, cobalt, nickel in zirconium, since each oxide is inconsistent to the absorbing wavelength of light, be easy to cause black
Not black, there is situations such as partially red, partially blue, partially green in product colour.And institute's oxygenates easily react with yttrium, zirconium, oxygen is destroyed
Change the stability of zirconium, be easy to cause product Transformation Cracking.It is more tight to colorant additive amount and temperature requirement in preparation process
Lattice, once management and control is bad to be easy for occurring the problems such as color between batch differs.
The content of the invention
A kind of high intensity, high blackness, height are provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art part
The zirconia ceramics material composition of light-proofness.
To achieve the above object, the technical solution taken of the present invention is:A kind of black zirconia ceramics material compositions, bag
Component containing following mass percentage:Iron oxide 0.01-4%, cobalt oxide 0.01-3.5%, aluminium oxide 0.01-15%, oxidation
Zinc 0-3.5%, yittrium oxide 2-7%, titanium oxide 0-4%, silica 0.01-1.0%, surplus are zirconium oxide.
In black zirconia ceramics material compositions of the present invention, glass phase in zirconium oxide can be increased by adding silica, from
And the crack tip of the plasticity passive oxidation zirconium by glass, it can finally significantly improve the toughness and bending strength for being molded porcelain body.
Meanwhile the content of silica should be controlled below 1.0%.Because glass is mutually excessive, by causing, the brittleness for being molded porcelain body is obvious
Increase.It moreover, dioxide-containing silica is excessive, may assemble in sintering process, reduce the glossiness of shaping porcelain body, and
Destroy the homogeneity of its color.The black zirconia ceramics material improves pottery on the basis of the blackness of ceramics and covering power is ensured
The warping resistance intensity of the intensity of porcelain, especially three can reach more than 1600Mpa;In addition, the powder is ensureing ceramic blackness and screening
On the basis of Gai Li, avoid using chromium compound is contained, especially without Cr VI, porcelain product have environmental-friendly performance after making its shaping.
Preferably, the composition does not include chromium oxide and nickel oxide.The powder is ensureing ceramic blackness and covering power base
On plinth, avoid using chromium compound is contained, especially without Cr VI, porcelain product have environmental-friendly performance after making its shaping.
Preferably, the composition includes the component of following mass percentage:Iron oxide 0.5-4%, cobalt oxide 0.5-
3.5%th, aluminium oxide 1-10%, zinc oxide 0.01-2%, yittrium oxide 3-6%, titanium oxide 0-4%, silica 0.01-1.0%,
Surplus is the zirconium oxide containing hafnium oxide.
Present inventor has found that each component of above-mentioned content can ensure the composition by a large amount of creative works
The ceramics strength that is prepared, hardness, L values, into porcelain density reach preferable unification.
Preferably, the black zirconia ceramics material compositions are powder, and powder D50 granularities are 0.1-1.5 μm, than
Surface area is 5-18m2/g。
Preferably, the granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 of the silica
Granularity is 0.1-1 μm.
Preferably, the granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide
For 0.1-1 μm.
Silica/alumina can play toughening effect in ceramic powder, be mixed with zirconium oxide in the form of size particles
Close, improve compactness between particle, reduce its porosity, so as to reduce shrinking percentage in shaping porcelain body sintering process, greatly improve into
The consistency of type porcelain body, makes shaping porcelain body have superior flexural strength.Using the molding porcelain body of this programme, it sinters front and rear
Shrinking percentage can reach 15-30%.
Preferably, the silica, aluminium oxide are respectively silicon dioxide powder, the aluminium oxide as obtained by being granulated and prepare
Powder, the silicon dioxide powder, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball
Mill, Ball-stirring mill, sieving removal of impurities, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Meanwhile the present invention also provides a kind of black zirconia ceramics, the black zirconia ceramics to include above-mentioned black
Zirconia ceramics material composition.
Preferably, the black zirconia ceramics be polishing thickness 0.1-1.0mm, 550nm wavelength under light transmittance < 0.3,
OD values > 4.0, the potsherd of chromatic value L≤35.The a values of the potsherd are that 0.5 ± 1, b values are -0.5 ± 1.
In addition, the present invention also provides a kind of preparation method of above-mentioned black zirconia ceramics, comprise the following steps:
(1) by black zirconia ceramics material compositions contained by each component mixing, obtain black zirconia ceramics material
Composition;
(2) the black zirconia ceramics material compositions that step (1) obtains are molded, roasting obtains black zirconia
Ceramics;
In the step (2) be shaped to tape casting, it is dry-pressing formed, injection moulding, hot-forming or gel injection into
Type.
Preferably, gel injection shaping is shaped in the step (2), the gel injection shaping includes following step
Suddenly:
The black zirconia ceramics material compositions that step (1) obtains are uniformly mixed by (2a) with solvent, organic additive, are matched somebody with somebody
Slurry is made, wherein, the solvent is water, the organic additive is acrylamide, in acrylate, Methacrylamide extremely
Few one kind;
After (2b) adds initiator, catalyst in the slurry that step (2a) obtains, slurry is injected in mould, wherein,
The initiator is at least one of ammonium persulfate, potassium peroxydisulfate;
Mould room temperature is placed 5-10min by (2c), after shaping to be solidified, the dry 2-6h at 40-80 DEG C, up to described black
Color zirconia ceramics base substrate.
This method gel injection technique, using organic monomer cross-linked polymeric, forms black zirconia porcelain body, and component is uniform,
Even density, defect are few.In addition, technique is simple, and it is easy to operate, do not increase production process and workload, it can be achieved that volume production.Using this
The black zirconia ceramics that invention the method is prepared, into porcelain density >=5.8g/cm3, 3 flexural strengths >=
1600Mpa, Vickers hardness >=1200.
Compared with prior art, beneficial effects of the present invention are:
The present invention by adding the colouring agent of black inside zirconia ceramics powder, the added silica of control and
The granularity of aluminium oxide, improves the covering power and blackness of zirconia ceramics, reduces its light transmittance, improves it and is molded the machinery of porcelain body by force
Degree, ensures excellent effect of both product colour and intensity.The black zirconia ceramics material ensure ceramics blackness and
On the basis of covering power, the intensity of ceramics is improved, especially 3 warping resistance intensity can reach more than 1600Mpa;In addition, the powder
On the basis of ceramic blackness and covering power is ensured, avoid using chromium compound is contained, especially without Cr VI, make porcelain product after its shaping
With environmental-friendly performance.
The preparation method of black zirconia ceramics material of the present invention, technique is prepared simply, easy to operate, does not increase production
Process and workload have preferable stability, can realize homogenizing for product, and do not increase the later stage, it can be achieved that volume production
Moulding process and the final strength and fracture toughness for not influencing zirconia ceramics.
Embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 0.01%, cobalt oxide 0.01%, aluminium oxide 0.01%, zinc oxide 0%, yittrium oxide 2%, titanium oxide 0%,
Silica 0.01%, surplus are zirconium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 0.1 μm, compare surface
Product is 5m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica are
0.1-1μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-1 μ
m;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the silica
Powder, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, is screened out excessively
Miscellaneous, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Embodiment 2
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 2%, cobalt oxide 2%, aluminium oxide 7.5%, zinc oxide 1.7%, yittrium oxide 4.5%, titanium oxide 2%, two
Silica 0.3%, surplus are the zirconium oxide containing hafnium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 1.5 μm, compare surface
Product is 18m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica
For 0.1-1 μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-
1μm;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the titanium dioxide
Silica flour, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, sieving
Removal of impurities, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Embodiment 3
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 1%, cobalt oxide 1.5%, aluminium oxide 10%, zinc oxide 2.5%, yittrium oxide 6%, titanium oxide 1%, dioxy
SiClx 0.4%, surplus are the zirconium oxide containing hafnium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 0.5 μm, compare surface
Product is 12m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica
For 0.1-1 μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-
1μm;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the titanium dioxide
Silica flour, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, sieving
Removal of impurities, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Embodiment 4
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 4%, cobalt oxide 3.5%, aluminium oxide 15%, zinc oxide 3.5%, yittrium oxide 7%, titanium oxide 4%, dioxy
SiClx 1.0%, surplus are the zirconium oxide containing hafnium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 1 μm, specific surface area
For 15m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica are
0.1-1μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-1 μ
m;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the silica
Powder, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, is screened out excessively
Miscellaneous, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Embodiment 5
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 4%, cobalt oxide 3.5%, aluminium oxide 10%, zinc oxide 2%, yittrium oxide 6%, titanium oxide 4%, titanium dioxide
Silicon 1%, surplus are the zirconium oxide containing hafnium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 1 μm, specific surface area
For 15m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica are
0.1-1μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-1 μ
m;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the silica
Powder, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, is screened out excessively
Miscellaneous, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
Embodiment 6
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following mass percentage:
Iron oxide 0.5%, cobalt oxide 0.5%, aluminium oxide 10%, zinc oxide 0.01%, yittrium oxide 3%, titanium oxide 1%,
Silica 0.4%, surplus are the zirconium oxide containing hafnium oxide.
The black zirconia ceramics material compositions of the present embodiment are powder, and powder D50 granularities are 0.5 μm, compare surface
Product is 12m2/g;The granularity of the silica is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the silica
For 0.1-1 μm;The granularity of the aluminium oxide is less than the granularity of the zirconium oxide, wherein, the D97 granularities of the aluminium oxide are 0.1-
1μm;Silicon dioxide powder, the alumina powder of the silica, aluminium oxide respectively as obtained by being granulated and prepare, the titanium dioxide
Silica flour, the preparation method of alumina powder are:Additive is added in silica, aluminium oxide, by ball milling, Ball-stirring mill, sieving
Removal of impurities, mist projection granulating, it is 0.5-1.5g/cm to obtain apparent density3Silicon dioxide powder, alumina powder.
The performance test of 7 black zirconia ceramics of embodiment
The present embodiment sets test group 1~6 and control group, the black zirconia ceramics material difference of the test group 1~6
It is prepared using the black zirconia ceramics material compositions of embodiment 1~6, the black oxidation of test group 1~6 and control group
Zircon ceramic is prepared using same preparation method, and the preparation method comprises the following steps:
(1) by black zirconia ceramics material compositions contained by each component mixing, obtain black zirconia ceramics material
Composition;
(2) the black zirconia ceramics material compositions that step (1) obtains are molded, roasting obtains black zirconia
Ceramics;
Gel injection shaping is shaped in the step (2), the gel injection shaping includes the following steps:
The black zirconia ceramics material compositions that step (1) obtains are uniformly mixed by (2a) with solvent, organic additive, are matched somebody with somebody
Slurry is made, wherein, the solvent is water, the organic additive is acrylamide, in acrylate, Methacrylamide extremely
Few one kind;
After (2b) adds initiator, catalyst in the slurry that step (2a) obtains, slurry is injected in mould, wherein,
The initiator is at least one of ammonium persulfate, potassium peroxydisulfate;
Mould room temperature is placed 5-10min by (2c), after shaping to be solidified, the dry 2-6h at 40-80 DEG C, up to described black
Color zirconia ceramics base substrate.
Control group is existing relatively common black zirconia ceramics, and the black zirconia ceramics material compositions contain
The component of following mass percentage:
Iron oxide 2%, cobalt oxide 0.8%, chromium oxide 2%, aluminium oxide 1%, nickel oxide 0.5%, manganese oxide 0.5%, oxygen
Change zinc 2%, yittrium oxide 5%, titanium oxide 0.5%, silica 0.5%, cerium oxide 1%, strontium oxide strontia 3%, calcium oxide 2%, oxygen
Change magnesium 4%, surplus is the zirconium oxide containing hafnium oxide;In the zirconium oxide containing hafnium oxide, hafnium oxide is described containing aerobic
It is 10% to change the mass percentage in the zirconium oxide of hafnium.
The black zirconia ceramics material compositions of the present embodiment are powder, and the powder D50 granularities are 1.2 μm, compare table
Area is 9m2/g。
Test group 1~6 is identical with the molding mode that control group uses, the black zirconia pottery of test group 1~6 and control group
The polishing thickness of porcelain also all same (being 0.5mm).The black zirconia ceramics of test group 1~6 and control group are surveyed respectively
Light transmittance under 550nm wavelength, OD values, chromatic value, into porcelain density, 3 flexural strengths and Vickers hardness, the test result such as institute of table 1
Show.
The performance test results of 1 black zirconia ceramics of table
As seen from the results in Table 1, black zirconia ceramics of the invention have higher intensity and hardness, higher covering power
With blackness, relatively low light transmittance;Wherein, the black zirconia ceramics of test group 2,3,5,6, effect are preferable.
Embodiment 7
According to the method in embodiment 6, using the ceramics obtained in embodiment 3 as control, test group 1~17, examination are set
Test in group 1~17 in addition to the content of silica is different, other compositions are identical with the ceramic component in embodiment 3, experiment
The content of silica and its 3 flexural strengths, Vickers hardnesses are as shown in table 2 in group 1~17:
The content and its 3 flexural strengths, Vickers hardnesses of aluminium oxide, yittrium oxide in 2 test group of table and control group
From table 2 it can be seen that under conditions of other conditions are the same, in ceramic material of the present invention, when the silica
Mass percentage when being 0.5-1%, 3 flexural strengths and hardness are preferable.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, those of ordinary skill in the art should
Understand, can be to technical scheme technical scheme is modified or replaced equivalently, without departing from the essence of technical solution of the present invention
And scope.
Claims (6)
1. a kind of black zirconia ceramics material compositions, it is characterised in that include the component of following mass percentage:Oxidation
Iron 0.01-4%, cobalt oxide 0.01-3.5%, aluminium oxide 0.01-15%, zinc oxide 0-3.5%, yittrium oxide 2-7%, titanium oxide
0-4%, silica 0.01-1.0%, surplus are the zirconium oxide containing hafnium oxide.
2. black zirconia ceramics material compositions as claimed in claim 1, it is characterised in that the composition does not include oxygen
Change chromium and nickel oxide.
3. black zirconia ceramics material compositions as claimed in claim 1 or 2, it is characterised in that include following quality hundred
Divide the component of content:Iron oxide 0.5-4%, cobalt oxide 0.5-3.5%, aluminium oxide 1-10%, zinc oxide 0.01-2%, yittrium oxide
3-6%, titanium oxide 0-4%, silica 0.01-1.0%, surplus are the zirconium oxide containing hafnium oxide.
4. black zirconia ceramics material compositions as claimed in claim 3, it is characterised in that the black zirconia ceramics
Material compositions are powder, and powder D50 granularities are 0.1-1.5 μm, specific surface area 5-18m2/g。
A kind of 5. black zirconia ceramics that composition as described in claim 1-4 is any is prepared, it is characterised in that institute
Black zirconia ceramics are stated as obtained by prepared by following preparation method:
(1) by black zirconia ceramics material compositions contained by each component mixing, obtain black zirconia ceramics combination of materials
Thing;
(2) the black zirconia ceramics material compositions that step (1) obtains are molded, roasting obtains black zirconia pottery
Porcelain;
Tape casting, dry-pressing formed, injection moulding, the shaping of hot-forming or gel injection are shaped in the step (2).
6. the preparation method of black zirconia ceramics as claimed in claim 5, it is characterised in that in the step (2) into
Type is molded for gel injection, and the gel injection shaping includes the following steps:
The black zirconia ceramics material compositions that step (1) obtains are uniformly mixed by (2a) with solvent, organic additive, are configured to
Slurry, wherein, the solvent is water, and the organic additive is at least one in acrylamide, acrylate, Methacrylamide
Kind;
After (2b) adds initiator, catalyst in the slurry that step (2a) obtains, slurry is injected in mould, wherein, it is described
Initiator is at least one of ammonium persulfate, potassium peroxydisulfate;
Mould room temperature is placed 5-10min by (2c), after shaping to be solidified, the dry 2-6h at 40-80 DEG C, up to the black oxygen
Change zircon ceramic base substrate.
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