CN110028245A - A kind of zirconium oxide low temperature yellow glaze and preparation method thereof - Google Patents
A kind of zirconium oxide low temperature yellow glaze and preparation method thereof Download PDFInfo
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- CN110028245A CN110028245A CN201910455184.3A CN201910455184A CN110028245A CN 110028245 A CN110028245 A CN 110028245A CN 201910455184 A CN201910455184 A CN 201910455184A CN 110028245 A CN110028245 A CN 110028245A
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- zirconium oxide
- low temperature
- glaze
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- temperature yellow
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 239000000919 ceramic Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 21
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 6
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000004327 boric acid Substances 0.000 claims abstract description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 3
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000011521 glass Substances 0.000 claims description 52
- 238000000498 ball milling Methods 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 102220043159 rs587780996 Human genes 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 239000004615 ingredient Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical class CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 2
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 230000001680 brushing effect Effects 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical class CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Dental Prosthetics (AREA)
- Glass Compositions (AREA)
Abstract
A kind of zirconium oxide low temperature yellow glaze and preparation method thereof, belongs to special cermacis, gear division reparation, ceramic ornament field.Zirconium oxide low temperature yellow glaze is zirconium oxide low temperature yellow glaze, is made by being sintered 20~40min to the glazing of zirconia ceramics surface, at 700~900 DEG C；Zirconium oxide low temperature yellow glaze includes base glaze and zirconium pr-yellow material, and zirconium pr-yellow material accounts for 1~15wt.% of base glaze；The raw material and its mass fraction that base glaze includes are as follows: 55-70 parts of silica, 5-8 parts of aluminium hydroxide, 5-10 parts of sodium carbonate, 3-8 parts of lithium carbonate, 3-8 parts of barium carbonate, 3-8 parts of basic zinc carbonate, 2-8 parts of zirconium oxide, 1-3 parts of cerium oxide, 2-8 parts of boric acid, 0.5-1 parts of niobium pentaoxide.This method has mirror effect in the yellow glaze of low temperature and short time sintering preparation, and glossiness is high, and colour stable, the coefficient of expansion matches with zirconium oxide, and particle is fine and smooth, is easy rest.This method is simple, effective.
Description
Technical field
The invention belongs to special cermacis field, gear division reparation field, ceramic ornament field, in particular to a kind of zirconium oxide is used
Low temperature yellow glaze and preparation method thereof.
Background technique
Zirconia ceramics has outstanding mechanical performance, and flexural strength can reach 1200MPa, be widely used in the industry
In various components, metal material is gradually replaced in certain industries.Since zirconia ceramics has preferable glossiness and special
Texture and translucence, also be used to make shell (watch case, mobile phone shell of ceramic ornament and intelligent wearable device
Deng), the demand of colored zirconia is continuously increased, and colored zirconia ceramics can be realized by the way that colorant is added in the feed,
One layer of glaze can be burnt on white oxide zirconium surface, this method is not only able to realize coloring, while can also improve surface light
Damp degree.Zirconia ceramics also has good biocompatibility, has been widely used in oral restoration industry, for making tooth
The fixed dentures such as hat, inlay, pontic, the color of teeth of people is generally partially yellow, and the face of zirconium oxide prosthesis may be implemented in yellow glaze
Color is more life-like, while also can increase the glossiness of dummy, is more nearly nature tooth.Due to zirconia ceramics heat resistanceheat resistant vibration property
Difference, low temperature glazing sintering is the trend of zirconium oxide glazing, while can also save time and cost.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of zirconium oxide low temperature yellow glaze and preparation method thereof.We
Method can be sintered at low temperature, and sintering time is short, can make the zirconium oxide of preparation in lower temperature and shorter time
Reach mirror effect with low temperature yellow glaze, glossiness is more than 85 (apparatus measures angle is 60 °), colour stable, after making sintering
Color is more stable, and the coefficient of expansion matches with zirconium oxide, and particle is fine and smooth, is easy rest.The preparation method is simple, effective.
A kind of zirconium oxide of the invention low temperature yellow glaze is zirconium oxide low temperature yellow glaze, by making pottery to zirconium oxide
The low temperature yellow glaze of zirconium oxide made from the glazing of porcelain surface, sintering；Wherein, the zirconium oxide low temperature yellow glaze includes base
Plinth glaze and zirconium pr-yellow material, wherein the mass percent that zirconium pr-yellow material accounts for base glaze is 1~15%；
The mass fraction of raw material and each raw material that the base glaze includes are as follows: 55-70 parts of silica, hydroxide
5-8 parts of aluminium, 5-10 parts of sodium carbonate, 3-8 parts of lithium carbonate, 3-8 parts of barium carbonate, 3-8 parts of basic zinc carbonate, 2-8 parts of zirconium oxide, oxidation
1-3 parts of cerium, 2-8 parts of boric acid, 0.5-1 parts of niobium pentaoxide.
Zirconium oxide low temperature yellow glaze, thermal expansion coefficient is 9.5 ± 0.5 × 10-6/ K, with zirconia ceramics phase
Matching.
Zirconium oxide low temperature yellow glaze, applicable zirconia ceramics are the relatively compact of relative density >=90%
Zirconia ceramics.
Zirconium oxide low temperature yellow glaze is 60 ° in apparatus measures angle, glossiness >=85.
A kind of preparation method of zirconium oxide low temperature yellow glaze of the invention, comprising the following steps:
Step 1: ingredient
By the zirconium oxide raw material and proportion of base glaze in low temperature yellow glaze, raw material is weighed, raw material is uniformly mixed,
Obtain mixture；
Step 2: preparation base glaze
Mixture is placed in 1400~1600 DEG C and is melted, after keeping the temperature 40~90min, water quenching obtains glass frit；
By glass frit after broken, grinding, ball milling, drying, glass powder is obtained, as basic glaze；The glass powder
Granularity D50=2~20 μm；
Step 3: preparing zirconium oxide low temperature yellow glaze
It by glass powder and zirconium pr-yellow material, is uniformly mixed according to a ratio, obtains zirconium oxide low temperature yellow glaze；Wherein, institute
Granularity D50=2~20 μm of the zirconium oxide stated low temperature yellow glaze；
Step 4: glazing, sintering
Zirconium oxide low temperature yellow glaze is added in organic solution, stirring obtains zirconium oxide low temperature yellow glaze liquid；Its
In, the solid content of the zirconium oxide low temperature yellow glaze in zirconium oxide low temperature yellow glaze liquid is 60~70wt.%；
By zirconium oxide with the glaze liquid glazing of low temperature yellow on zirconia ceramics surface, be placed in 700~900 DEG C be sintered 20~
40min cools to room temperature with the furnace, takes out, and obtains the zirconium oxide low temperature yellow glaze of zirconia ceramics surface attachment.
In the step 1, described is uniformly mixed using ball milling mixing；Wherein, ball milling parameter are as follows: horizontal ball mill,
100~200r/min of rotational speed of ball-mill, Ball-milling Time are 4~5h, and in mass ratio, material ball ratio is (2.5~3): 1.
In the step 2, the ball milling, rotational speed of ball-mill is 350~400r/min, and Ball-milling Time is 30~40min.
In the step 4, the organic solution is ethylene glycol, propylene glycol, 1,3 butanediols, polyethylene glycol 200 or poly-
The one or more of ethylene glycol 400.
In the step 4, before sintering, preheated, preheating temperature be 350~500 DEG C, preheating time be 2~
3min, its purpose is that organic solvent in glaze liquid is made sufficiently to volatilize completely.
In the step 4, the sintering, heating rate is 30~40 DEG C/min.
In described step 4, the zirconia ceramics is the relatively compact zirconia ceramics of relative density >=90%.
A kind of zirconium oxide of the invention low temperature yellow glaze and preparation method thereof, the beneficial effect is that:
1) glazing effect of zirconia ceramics yellow is realized；2) coefficient of expansion is consistent with zirconium oxide, will not generate stress and lead
Cause cracking；3) the glazing sintering that zirconium oxide can be achieved in lower temperature and shorter soaking time, reaches mirror surface luster effect
Fruit, using intelligent -118 measurement Gloss measurements of reputation moral number Grossmeters is more than 85 (apparatus measures angle is 60 °)；4)
Sintering front and back colour consistency is good；5) particle is fine and smooth, is easy rest；6) it is added and zirconium pr-yellow material colours jointly, after making sintering
Color is more stable.Meanwhile present invention process process is simple, and it is easy to operate, it is at low cost, there are significant environmental benefit, economic benefit
And social benefit.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, the glossiness of the zirconium oxide low temperature yellow glaze of preparation, using reputation moral number Grossmeters intelligence
Energy type -118 measures, and apparatus measures angle is 60 °.
Embodiment 1
A kind of preparation method of zirconium oxide low temperature yellow glaze, comprising the following steps:
Step 1: ingredient
Each raw material is weighed according to the ratio of table 1, the raw material weighed up is then put into horizontal ball grinder, ball milling 4h, after ball milling
It sieves with 100 mesh sieve, is further uniformly mixed, obtain mixture；Wherein, in mass ratio, material ball ratio 2.5:1；
Step 2: preparation base glaze
Then, mixture is poured into corundum crucible, is put into sintering furnace, in 1500 DEG C of sintering 1h, then fallen glass metal
Enter and obtains glass frit in water；
By the broken simultaneously ball milling of glass frit, rotational speed of ball-mill 350r/min, Ball-milling Time 40min obtain glass by drying
Glass powder；D50=10 μm of the granularity of glass powder.
Step 3: preparing zirconium oxide low temperature yellow glaze
By after drying glass powder and zirconium pr-yellow material according to table 2 ratio mix, obtain zirconium oxide low temperature yellow glaze
Material；Wherein, D50=10 μm of granularity of zirconium oxide low temperature yellow glaze；
Step 4: glazing, sintering
Claim 5 part 1 in beaker, 3 butanediols and 5 parts of polyethylene glycol 400s are stirred evenly with glass bar, obtain organic solution；
Zirconium oxide low temperature yellow glaze is mixed with the organic solution stirred evenly, reconciles into proper viscosity, consolidate
The zirconium oxide low temperature yellow glaze liquid that content is 60%；By zirconium oxide with the glaze liquid brushing of low temperature yellow on zirconia ceramics surface,
It is sintered according to the sintering procedure of table 3, can achieve final effect.Table 4 is thermal expansion coefficient test result, and table 5 is glossiness
Test result.
Embodiment 2
A kind of preparation method of zirconium oxide low temperature yellow glaze, comprising the following steps:
Step 1: ingredient
Each raw material is weighed according to the ratio of table 1, the raw material weighed up is then put into horizontal ball grinder, ball milling 4h, after ball milling
It sieves with 100 mesh sieve, is further uniformly mixed, obtain mixture；Wherein, in mass ratio, material ball ratio 3:1；
Step 2: preparation base glaze
Then, mixture is poured into corundum crucible, is put into sintering furnace, in 1400 DEG C of sintering 1.5h, then by glass metal
It is poured into water to obtain glass frit；
By the broken simultaneously ball milling of glass frit, rotational speed of ball-mill 350r/min, Ball-milling Time 40min obtain glass by drying
Glass powder；D50=20 μm of the granularity of glass powder.
Step 3: preparing zirconium oxide low temperature yellow glaze
By after drying glass powder and zirconium pr-yellow material according to table 2 ratio mix, obtain zirconium oxide low temperature yellow glaze
Material；Wherein, D50=20 μm of granularity of zirconium oxide low temperature yellow glaze；
Step 4: glazing, sintering
Claim 5 parts of propylene glycol and 5 parts of polyethylene glycol 400s in beaker, is stirred evenly with glass bar, obtain organic solution；
Zirconium oxide low temperature yellow glaze is mixed with the organic solution stirred evenly, reconciles into proper viscosity, consolidate
The zirconium oxide low temperature yellow glaze liquid that content is 70%；By zirconium oxide with the glaze liquid brushing of low temperature yellow on zirconia ceramics surface,
It is sintered according to the sintering procedure of table 3, can achieve final effect.Table 4 is thermal expansion coefficient test result, and table 5 is glossiness
Test result.
Embodiment 3
A kind of preparation method of zirconium oxide low temperature yellow glaze, comprising the following steps:
Step 1: ingredient
Each raw material is weighed according to the ratio of table 1, the raw material weighed up is then put into horizontal ball grinder, rotational speed of ball-mill is
100r/min, ball milling 5h are sieved with 100 mesh sieve after ball milling, are further uniformly mixed, obtain mixture；Wherein, in mass ratio, pellet
Than for 2.5:1；
Step 2: preparation base glaze
Then, mixture is poured into corundum crucible, is put into sintering furnace, in 1600 DEG C of sintering 40min, then by glass metal
It is poured into water to obtain glass frit；
By the broken simultaneously ball milling of glass frit, rotational speed of ball-mill 400r/min, Ball-milling Time 30min obtain glass by drying
Glass powder；D50=2 μm of the granularity of glass powder.
Step 3: preparing zirconium oxide low temperature yellow glaze
By after drying glass powder and zirconium pr-yellow material according to table 2 ratio mix, obtain zirconium oxide low temperature yellow glaze
Material；Wherein, D50=2 μm of granularity of zirconium oxide low temperature yellow glaze；
Step 4: glazing, sintering
Claim 5 parts of ethylene glycol and 5 parts of polyethylene glycol 200s in beaker, is stirred evenly with glass bar, obtain organic solution；
Zirconium oxide low temperature yellow glaze is mixed with the organic solution stirred evenly, reconciles into proper viscosity, consolidate
The zirconium oxide low temperature yellow glaze liquid that content is 65%；By zirconium oxide with the glaze liquid brushing of low temperature yellow on zirconia ceramics surface,
It is sintered according to the sintering procedure of table 3, can achieve final effect.Table 4 is thermal expansion coefficient test result, and table 5 is glossiness
Test result.
Embodiment 4
A kind of preparation method of zirconium oxide low temperature yellow glaze, comprising the following steps:
Step 1: ingredient
Each raw material is weighed according to the ratio of table 1, the raw material weighed up is then put into horizontal ball grinder, rotational speed of ball-mill is
200r/min, ball milling 4.5h are sieved with 100 mesh sieve after ball milling, are further uniformly mixed, obtain mixture；Wherein, in mass ratio, expect
Ball ratio is 2.5:1；
Step 2: preparation base glaze
Then, mixture is poured into corundum crucible, is put into sintering furnace, in 1550 DEG C of sintering 60min, then by glass metal
It is poured into water to obtain glass frit；
By the broken simultaneously ball milling of glass frit, rotational speed of ball-mill 350r/min, Ball-milling Time 80min obtain glass by drying
Glass powder；D50=5 μm of the granularity of glass powder.
Step 3: preparing zirconium oxide low temperature yellow glaze
By after drying glass powder and zirconium pr-yellow material according to table 2 ratio mix, obtain zirconium oxide low temperature yellow glaze
Material；Wherein, D50=5 μm of granularity of zirconium oxide low temperature yellow glaze；
Step 4: glazing, sintering
Claim 5 part 1 in beaker, 3 butanediols and 5 parts of polyethylene glycol 200s are stirred evenly with glass bar, obtain organic solution；
Zirconium oxide low temperature yellow glaze is mixed with the organic solution stirred evenly, reconciles into proper viscosity, consolidate
The zirconium oxide low temperature yellow glaze liquid that content is 78%；By zirconium oxide with the glaze liquid brushing of low temperature yellow on zirconia ceramics surface,
It is sintered according to the sintering procedure of table 3, can achieve final effect.Table 4 is thermal expansion coefficient test result, and table 5 is glossiness
Test result.
Embodiment 5
A kind of preparation method of zirconium oxide low temperature yellow glaze, comprising the following steps:
Step 1: ingredient
Each raw material is weighed according to the ratio of table 1, the raw material weighed up is then put into horizontal ball grinder, rotational speed of ball-mill is
150r/min, ball milling 4.5h are sieved with 100 mesh sieve after ball milling, are further uniformly mixed, obtain mixture；Wherein, in mass ratio, expect
Ball ratio is 2.5:1；
Step 2: preparation base glaze
Then, mixture is poured into corundum crucible, is put into sintering furnace, in 1450 DEG C of sintering 50min, then by glass metal
It is poured into water to obtain glass frit；
By the broken simultaneously ball milling of glass frit, rotational speed of ball-mill 400r/min, Ball-milling Time 30min obtain glass by drying
Glass powder；D50=8 μm of the granularity of glass powder.
Step 3: preparing zirconium oxide low temperature yellow glaze
By after drying glass powder and zirconium pr-yellow material according to table 2 ratio mix, obtain zirconium oxide low temperature yellow glaze
Material；Wherein, D50=8 μm of granularity of zirconium oxide low temperature yellow glaze；
Step 4: glazing, sintering
Claim 5 parts of ethylene glycol and 3 parts of polyethylene glycol 400s in beaker, is stirred evenly with glass bar, obtain organic solution；
Zirconium oxide low temperature yellow glaze is mixed with the organic solution stirred evenly, reconciles into proper viscosity, consolidate
The zirconium oxide low temperature yellow glaze liquid that content is 60%；By zirconium oxide with the glaze liquid brushing of low temperature yellow on zirconia ceramics surface,
It is sintered according to the sintering procedure of table 3, can achieve final effect.Table 4 is thermal expansion coefficient test result, and table 5 is glossiness
Test result.
1 glass powder of table proportion
2 glass powder of table and zirconium pr-yellow material match
3 sintering procedure of table
| Embodiment | Preheating temperature | Preheating time | Heating rate | Maximum temperature | Soaking time |
| 1 | 400 | 3min | 30℃/min | 800 | 25min |
| 2 | 400 | 2min | 30℃/min | 750 | 30min |
| 3 | 400 | 3min | 40℃/min | 850 | 25min |
| 4 | 400 | 3min | 40℃/min | 700 | 40min |
| 5 | 400 | 2min | 35℃/min | 900 | 20min |
4 thermal expansion coefficient of table
| Corresponding embodiment | Thermal expansion coefficient |
| 1 | 9.8×10-6/K |
| 2 | 9.7×10-6/K |
| 3 | 9.5×10-6/K |
| 4 | 9.5×10-6/K |
| 5 | 9.3×10-6/K |
5 glossiness of table
| Corresponding embodiment | Glossiness |
| 1 | 93 |
| 2 | 96 |
| 3 | 101 |
| 4 | 91 |
| 5 | 88 |
Claims (10)
- Be zirconium oxide low temperature yellow glaze 1. a kind of zirconium oxide low temperature yellow glaze, by the glazing of zirconia ceramics surface, It is sintered zirconium oxide low temperature yellow glaze obtained；It is characterized in that, the zirconium oxide low temperature yellow glaze includes parent glaze Material and zirconium pr-yellow material, wherein the mass percent that zirconium pr-yellow material accounts for base glaze is 1~15%；The mass fraction of raw material and each raw material that the base glaze includes are as follows: 55-70 parts of silica, aluminium hydroxide 5- 8 parts, 5-10 parts of sodium carbonate, 3-8 parts of lithium carbonate, 3-8 parts of barium carbonate, 3-8 parts of basic zinc carbonate, 2-8 parts of zirconium oxide, cerium oxide 1- 3 parts, 2-8 parts of boric acid, 0.5-1 parts of niobium pentaoxide.
- 2. zirconium oxide as described in claim 1 low temperature yellow glaze, which is characterized in that zirconium oxide low temperature yellow Glaze, thermal expansion coefficient is 9.5 ± 0.5 × 10-6/ K, matches with zirconia ceramics.
- 3. zirconium oxide as described in claim 1 low temperature yellow glaze, which is characterized in that zirconium oxide low temperature yellow Glaze, applicable zirconia ceramics are the relatively compact zirconia ceramics of relative density >=90%.
- 4. zirconium oxide as described in claim 1 low temperature yellow glaze, which is characterized in that zirconium oxide low temperature yellow Glaze is 60 ° in apparatus measures angle, glossiness >=85.
- 5. the preparation method of low temperature yellow glaze of zirconium oxide described in Claims 1 to 4 any one, which is characterized in that including Following steps:Step 1: ingredientBy the zirconium oxide raw material and proportion of base glaze in low temperature yellow glaze, raw material is weighed, raw material is uniformly mixed, is obtained Mixture；Step 2: preparation base glazeMixture is placed in 1400~1600 DEG C and is melted, after keeping the temperature 40~90min, water quenching obtains glass frit；By glass frit after broken, grinding, ball milling, drying, glass powder is obtained, as basic glaze；The grain of the glass powder Spend D50=2~20 μm；Step 3: preparing zirconium oxide low temperature yellow glazeIt by glass powder and zirconium pr-yellow material, is uniformly mixed according to a ratio, obtains zirconium oxide low temperature yellow glaze；Wherein, described Granularity D50=2~20 μm of zirconium oxide low temperature yellow glaze；Step 4: glazing, sinteringZirconium oxide low temperature yellow glaze is added in organic solution, stirring obtains zirconium oxide low temperature yellow glaze liquid；Wherein, The solid content of zirconium oxide low temperature yellow glaze in zirconium oxide low temperature yellow glaze liquid is 60~70wt.%；By zirconium oxide with the glaze liquid glazing of low temperature yellow on zirconia ceramics surface, be placed in 700~900 DEG C be sintered 20~ 40min cools to room temperature with the furnace, takes out, and obtains the zirconium oxide low temperature yellow glaze of zirconia ceramics surface attachment.
- 6. the zirconium oxide as claimed in claim 5 preparation method of low temperature yellow glaze, which is characterized in that in the step 1, Described is uniformly mixed using ball milling mixing；Wherein, ball milling parameter are as follows: horizontal ball mill, 100~200r/min of rotational speed of ball-mill, Ball-milling Time is 4~5h, and in mass ratio, material ball ratio is (2.5~3): 1.
- 7. the zirconium oxide as claimed in claim 5 preparation method of low temperature yellow glaze, which is characterized in that in the step 2, The ball milling, rotational speed of ball-mill are 350~400r/min, and Ball-milling Time is 30~40min.
- 8. the zirconium oxide as claimed in claim 5 preparation method of low temperature yellow glaze, which is characterized in that in the step 4, The organic solution is the one or more of ethylene glycol, propylene glycol, 1,3 butanediols, polyethylene glycol 200 or polyethylene glycol 400.
- 9. the zirconium oxide as claimed in claim 5 preparation method of low temperature yellow glaze, which is characterized in that in the step 4, Before sintering, it is preheated, preheating temperature is 350~500 DEG C, and preheating time is 2~3min.
- 10. the zirconium oxide as claimed in claim 5 preparation method of low temperature yellow glaze, which is characterized in that the step 4 In, the sintering, heating rate is 30~40 DEG C/min.
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Effective date of registration: 20231227 Address after: No. 34 Jinniushan Street West, Xishi District, Yingkou City, Liaoning Province, 115000 Patentee after: Liaoning sinawa dental porcelain block Technology Co.,Ltd. Address before: 110168 Liaoning province Shenyang Hunnan Hunnan Road No. 9 Patentee before: SHENYANG JIANZHU University |