CN110028245B - Low-temperature yellow glaze for zirconia and preparation method thereof - Google Patents
Low-temperature yellow glaze for zirconia and preparation method thereof Download PDFInfo
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- CN110028245B CN110028245B CN201910455184.3A CN201910455184A CN110028245B CN 110028245 B CN110028245 B CN 110028245B CN 201910455184 A CN201910455184 A CN 201910455184A CN 110028245 B CN110028245 B CN 110028245B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 48
- 238000005245 sintering Methods 0.000 claims abstract description 45
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 17
- USEGQPUGEPSVQL-UHFFFAOYSA-N [Pr].[Zr] Chemical compound [Pr].[Zr] USEGQPUGEPSVQL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 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
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 3
- 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
- 229910000420 cerium oxide Inorganic materials 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
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 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
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-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
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 48
- 239000011521 glass Substances 0.000 claims description 47
- 238000002156 mixing Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 8
- 239000001052 yellow pigment Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005259 measurement Methods 0.000 claims description 5
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 5
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 4
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000010419 fine particle Substances 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 description 10
- 239000010431 corundum Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 7
- 238000007873 sieving Methods 0.000 description 5
- 239000012856 weighed raw material Substances 0.000 description 5
- 238000004040 coloring Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Classifications
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- 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
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
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- 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 low-temperature yellow glaze for zirconia and a preparation method thereof belong to the fields of special ceramics, dental restoration and ceramic ornaments. The low-temperature yellow glaze for the zirconia is a low-temperature yellow glaze for the zirconia, and is prepared by glazing the surface of zirconia ceramic and sintering at 700-900 ℃ for 20-40 min; the low-temperature yellow glaze for the zirconium oxide comprises a base glaze and a zirconium praseodymium yellow material, wherein the zirconium praseodymium yellow material accounts for 1-15 wt% of the base glaze; the basic glaze comprises the following raw materials in parts by weight: 55-70 parts of silicon dioxide, 5-8 parts of aluminum 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 and 0.5-1 part of niobium pentoxide. The yellow glaze prepared by sintering at low temperature and short time has the advantages of mirror surface effect, high glossiness, stable color, matching expansion coefficient with zirconia, fine particles and easy glaze hanging. The method is simple and effective.
Description
Technical Field
The invention belongs to the fields of special ceramics, dental restoration and ceramic ornaments, and particularly relates to a low-temperature yellow glaze for zirconium oxide and a preparation method thereof.
Background
The zirconia ceramics have excellent mechanical property, the flexural strength can reach 1200MPa, and the zirconia ceramics are widely applied to various parts in industry and gradually replace metal materials in certain industries. Because zirconia ceramics have better glossiness, special texture and translucency, and are also used for manufacturing ceramic ornaments and shells (watchcases, mobile phone shells and the like) of intelligent wearable equipment, the demand of colored zirconia is continuously increased, the colored zirconia ceramics can be realized by adding a colorant into raw materials, and a layer of glaze can be burnt on the surface of white zirconia, so that the method not only can realize coloring, but also can improve the surface glossiness. The zirconia ceramics also has good biocompatibility, is widely applied to the oral cavity restoration industry, is used for manufacturing fixed false teeth such as crowns, inlays, bridges and the like, the color of the teeth of people is generally yellow, and the yellow glaze can realize more vivid color of the zirconia restoration and can also increase the glossiness of the restoration to be more close to natural teeth. Because of the poor thermal shock resistance of zirconia ceramics, the low-temperature glazing and sintering is the trend of zirconia glazing, and simultaneously, the time and the cost can be saved.
Disclosure of Invention
In order to solve the problems, the invention provides a low-temperature yellow glaze for zirconia and a preparation method thereof. The method can be used for sintering at low temperature, the sintering time is short, the prepared low-temperature yellow glaze for zirconium oxide can achieve the mirror surface effect at low temperature and in a short time, the glossiness of the glaze exceeds 85 (the measurement angle of an instrument is 60 degrees), the color is stable, the color is more stable after sintering, the expansion coefficient is matched with that of zirconium oxide, the particles are fine and smooth, and glaze hanging is easy. The preparation method is simple and effective.
The low-temperature yellow glaze for zirconia is a low-temperature yellow glaze for zirconia, and is prepared by glazing and sintering the surface of zirconia ceramic; the low-temperature yellow glaze for zirconia comprises a base glaze and a zirconium praseodymium yellow material, wherein the zirconium praseodymium yellow material accounts for 1-15% of the base glaze in mass percent;
the basic glaze comprises the following raw materials in parts by weight: 55-70 parts of silicon dioxide, 5-8 parts of aluminum 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 and 0.5-1 part of niobium pentoxide.
The low-temperature yellow glaze for zirconia has a thermal expansion coefficient of 9.5 +/-0.5 multiplied by 10-6and/K, matching with the zirconia ceramic.
The low-temperature yellow glaze for zirconia is applicable to zirconia ceramics which are relatively compact and have the relative density of more than or equal to 90 percent.
The low-temperature yellow glaze for zirconia has an instrument measurement angle of 60 degrees and a glossiness of more than or equal to 85 degrees.
The invention discloses a preparation method of low-temperature yellow glaze for zirconium oxide, which comprises the following steps:
step 1: ingredients
Weighing raw materials according to the raw materials and the proportion of the basic glaze in the low-temperature yellow glaze for zirconium oxide, and uniformly mixing the raw materials to obtain a mixture;
step 2: preparation of basic glaze
Melting the mixture at 1400-1600 ℃, preserving heat for 40-90 min, and performing water quenching to obtain a glass frit;
crushing, grinding, ball milling and drying the glass frit to obtain glass powder serving as basic glaze; the granularity D50 of the glass powder is 2-20 mu m;
and step 3: low-temperature yellow glaze for preparing zirconium oxide
Uniformly mixing the glass powder and the zirconium praseodymium yellow pigment according to the proportion to obtain a low-temperature yellow glaze material for zirconium oxide; the granularity D50 of the low-temperature yellow glaze for zirconium oxide is 2-20 mu m;
and 4, step 4: glazing and sintering
Adding the low-temperature yellow glaze for zirconium oxide into the organic solution, and stirring to obtain low-temperature yellow glaze liquid for zirconium oxide; the solid content of the low-temperature yellow glaze for zirconia in the low-temperature yellow glaze liquid for zirconia is 60-70 wt.%;
glazing the zirconia on the surface of the zirconia ceramic by using the low-temperature yellow glaze liquid, sintering at 700-900 ℃ for 20-40 min, cooling to room temperature along with a furnace, and taking out to obtain the low-temperature yellow glaze for zirconia attached to the surface of the zirconia ceramic.
In the step 1, the mixture is uniformly mixed by ball milling; wherein, the ball milling parameters are as follows: the ball milling speed of the horizontal ball mill is 100-200 r/min, the ball milling time is 4-5 h, and the material ball ratio is (2.5-3): 1.
in the step 2, the ball milling is carried out, wherein the ball milling rotating speed is 350-400 r/min, and the ball milling time is 30-40 min.
In the step 4, the organic solution is one or more of ethylene glycol, propylene glycol, 1, 3-butanediol, polyethylene glycol 200 or polyethylene glycol 400.
In the step 4, before sintering, preheating is carried out, wherein the preheating temperature is 350-500 ℃, and the preheating time is 2-3 min, and the purpose is to fully and completely volatilize the organic solvent in the glaze liquid.
In the step 4, the temperature rise rate of the sintering is 30-40 ℃/min.
In the step 4, the zirconia ceramics is relatively compact zirconia ceramics with the relative density of more than or equal to 90 percent.
The low-temperature yellow glaze for zirconium oxide and the preparation method thereof have the beneficial effects that:
1) the yellow glazing effect of the zirconia ceramics is realized; 2) the expansion coefficient is consistent with that of zirconia, and cracking caused by stress can not be generated; 3) glazing and sintering of zirconium oxide can be realized at a lower temperature and within a shorter heat preservation time, a mirror surface glossiness effect is achieved, and a glossiness measured value measured by a reputation digital glossiness meter intelligent-118 is over 85 (the instrument measurement angle is 60 degrees); 4) the color consistency is good before and after sintering; 5) the particles are fine and smooth, and glaze hanging is easy; 6) and the pigment and zirconium praseodymium yellow are added for coloring together, so that the color is more stable after sintering. Meanwhile, the method has the advantages of simple process flow, convenient operation, low cost and obvious environmental benefit, economic benefit and social benefit.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the gloss of the prepared low-temperature yellow glaze for zirconia was measured by a reputation digital gloss meter intelligent-118, and the instrumental measurement angle thereof was 60 °.
Example 1
A preparation method of low-temperature yellow glaze for zirconia comprises the following steps:
step 1: ingredients
Weighing the raw materials according to the proportion in the table 1, then putting the weighed raw materials into a horizontal ball milling tank, carrying out ball milling for 4 hours, sieving by a 100-mesh sieve after ball milling, and further uniformly mixing to obtain a mixture; wherein, the material ball ratio is 2.5:1 according to the mass ratio;
step 2: preparation of basic glaze
Then, pouring the mixture into a corundum crucible, putting the corundum crucible into a sintering furnace, sintering for 1h at 1500 ℃, and then pouring the glass liquid into water to obtain glass frit;
crushing and ball-milling the glass frit, wherein the ball-milling speed is 350r/min, the ball-milling time is 40min, and drying to obtain glass powder; the particle size D50 of the glass frit was 10 μm.
And step 3: low-temperature yellow glaze for preparing zirconium oxide
Mixing the dried glass powder with the zirconium praseodymium yellow pigment according to the proportion in the table 2 to obtain a low-temperature yellow glaze for zirconium oxide; wherein the granularity D50 of the low-temperature yellow glaze for zirconia is 10 mu m;
and 4, step 4: glazing and sintering
Weighing 5 parts of 1, 3-butanediol and 5 parts of polyethylene glycol 400 in a beaker, and uniformly stirring by using a glass rod to obtain an organic solution;
mixing the low-temperature yellow glaze for zirconium oxide with the uniformly stirred organic solution, and blending to obtain low-temperature yellow glaze liquid for zirconium oxide with solid content of 60%; zirconia is coated on the surface of zirconia ceramic by using low-temperature yellow glaze liquid, and sintering is carried out according to the sintering procedure in the table 3, so that the final effect can be achieved. Table 4 shows the results of the thermal expansion coefficient test, and table 5 shows the results of the gloss test.
Example 2
A preparation method of low-temperature yellow glaze for zirconia comprises the following steps:
step 1: ingredients
Weighing the raw materials according to the proportion in the table 1, then putting the weighed raw materials into a horizontal ball milling tank, carrying out ball milling for 4 hours, sieving by a 100-mesh sieve after ball milling, and further uniformly mixing to obtain a mixture; wherein, the material ball ratio is 3:1 according to the mass ratio;
step 2: preparation of basic glaze
Then, pouring the mixture into a corundum crucible, putting the corundum crucible into a sintering furnace, sintering for 1.5 hours at 1400 ℃, and then pouring the glass liquid into water to obtain glass frit;
crushing and ball-milling the glass frit, wherein the ball-milling speed is 350r/min, the ball-milling time is 40min, and drying to obtain glass powder; the particle size D50 of the glass frit was 20 μm.
And step 3: low-temperature yellow glaze for preparing zirconium oxide
Mixing the dried glass powder with the zirconium praseodymium yellow pigment according to the proportion in the table 2 to obtain a low-temperature yellow glaze for zirconium oxide; wherein the granularity D50 of the low-temperature yellow glaze for zirconia is 20 mu m;
and 4, step 4: glazing and sintering
Weighing 5 parts of propylene glycol and 5 parts of polyethylene glycol 400 in a beaker, and uniformly stirring by using a glass rod to obtain an organic solution;
mixing the low-temperature yellow glaze for zirconium oxide with the uniformly stirred organic solution, and blending to obtain a low-temperature yellow glaze liquid for zirconium oxide with a solid content of 70%; zirconia is coated on the surface of zirconia ceramic by using low-temperature yellow glaze liquid, and sintering is carried out according to the sintering procedure in the table 3, so that the final effect can be achieved. Table 4 shows the results of the thermal expansion coefficient test, and table 5 shows the results of the gloss test.
Example 3
A preparation method of low-temperature yellow glaze for zirconia comprises the following steps:
step 1: ingredients
Weighing the raw materials according to the proportion shown in the table 1, then putting the weighed raw materials into a horizontal ball milling tank, carrying out ball milling at the ball milling rotation speed of 100r/min for 5 hours, sieving by using a 100-mesh sieve after ball milling, and further uniformly mixing to obtain a mixture; wherein, the material ball ratio is 2.5:1 according to the mass ratio;
step 2: preparation of basic glaze
Then, pouring the mixture into a corundum crucible, putting the corundum crucible into a sintering furnace, sintering for 40min at 1600 ℃, and then pouring the glass liquid into water to obtain glass frit;
crushing and ball-milling the glass frit, wherein the ball-milling speed is 400r/min, the ball-milling time is 30min, and drying to obtain glass powder; the particle size D50 of the glass frit was 2 μm.
And step 3: low-temperature yellow glaze for preparing zirconium oxide
Mixing the dried glass powder with the zirconium praseodymium yellow pigment according to the proportion in the table 2 to obtain a low-temperature yellow glaze for zirconium oxide; wherein the granularity D50 of the low-temperature yellow glaze for zirconia is 2 mu m;
and 4, step 4: glazing and sintering
Weighing 5 parts of ethylene glycol and 5 parts of polyethylene glycol 200 in a beaker, and uniformly stirring by using a glass rod to obtain an organic solution;
mixing the low-temperature yellow glaze for zirconium oxide with the uniformly stirred organic solution, and blending to obtain a low-temperature yellow glaze liquid for zirconium oxide with a solid content of 65%; zirconia is coated on the surface of zirconia ceramic by using low-temperature yellow glaze liquid, and sintering is carried out according to the sintering procedure in the table 3, so that the final effect can be achieved. Table 4 shows the results of the thermal expansion coefficient test, and table 5 shows the results of the gloss test.
Example 4
A preparation method of low-temperature yellow glaze for zirconia comprises the following steps:
step 1: ingredients
Weighing the raw materials according to the proportion shown in the table 1, then putting the weighed raw materials into a horizontal ball milling tank, performing ball milling at the ball milling rotation speed of 200r/min for 4.5 hours, sieving by using a 100-mesh sieve after ball milling, and further uniformly mixing to obtain a mixture; wherein, the material ball ratio is 2.5:1 according to the mass ratio;
step 2: preparation of basic glaze
Then, pouring the mixture into a corundum crucible, putting the corundum crucible into a sintering furnace, sintering for 60min at 1550 ℃, and then pouring the glass liquid into water to obtain glass frit;
crushing and ball-milling the glass frit, wherein the ball-milling speed is 350r/min, the ball-milling time is 80min, and drying to obtain glass powder; the particle size D50 of the glass frit was 5 μm.
And step 3: low-temperature yellow glaze for preparing zirconium oxide
Mixing the dried glass powder with the zirconium praseodymium yellow pigment according to the proportion in the table 2 to obtain a low-temperature yellow glaze for zirconium oxide; wherein the granularity D50 of the low-temperature yellow glaze for zirconia is 5 mu m;
and 4, step 4: glazing and sintering
Weighing 5 parts of 1, 3-butanediol and 5 parts of polyethylene glycol 200 in a beaker, and uniformly stirring by using a glass rod to obtain an organic solution;
mixing the low-temperature yellow glaze for zirconium oxide with the uniformly stirred organic solution, and blending to obtain low-temperature yellow glaze liquid for zirconium oxide with solid content of 78%; zirconia is coated on the surface of zirconia ceramic by using low-temperature yellow glaze liquid, and sintering is carried out according to the sintering procedure in the table 3, so that the final effect can be achieved. Table 4 shows the results of the thermal expansion coefficient test, and table 5 shows the results of the gloss test.
Example 5
A preparation method of low-temperature yellow glaze for zirconia comprises the following steps:
step 1: ingredients
Weighing the raw materials according to the proportion shown in the table 1, then putting the weighed raw materials into a horizontal ball milling tank, performing ball milling at the ball milling rotation speed of 150r/min for 4.5 hours, sieving by using a 100-mesh sieve after ball milling, and further uniformly mixing to obtain a mixture; wherein, the material ball ratio is 2.5:1 according to the mass ratio;
step 2: preparation of basic glaze
Then, pouring the mixture into a corundum crucible, putting the corundum crucible into a sintering furnace, sintering for 50min at 1450 ℃, and then pouring the glass liquid into water to obtain glass frit;
crushing and ball-milling the glass frit, wherein the ball-milling speed is 400r/min, the ball-milling time is 30min, and drying to obtain glass powder; the particle size D50 of the glass frit was 8 μm.
And step 3: low-temperature yellow glaze for preparing zirconium oxide
Mixing the dried glass powder with the zirconium praseodymium yellow pigment according to the proportion in the table 2 to obtain a low-temperature yellow glaze for zirconium oxide; wherein the granularity D50 of the low-temperature yellow glaze for zirconia is 8 mu m;
and 4, step 4: glazing and sintering
Weighing 5 parts of ethylene glycol and 3 parts of polyethylene glycol 400 in a beaker, and uniformly stirring by using a glass rod to obtain an organic solution;
mixing the low-temperature yellow glaze for zirconium oxide with the uniformly stirred organic solution, and blending to obtain low-temperature yellow glaze liquid for zirconium oxide with solid content of 60%; zirconia is coated on the surface of zirconia ceramic by using low-temperature yellow glaze liquid, and sintering is carried out according to the sintering procedure in the table 3, so that the final effect can be achieved. Table 4 shows the results of the thermal expansion coefficient test, and table 5 shows the results of the gloss test.
TABLE 1 glass powder ratio
TABLE 2 glass powder to zirconium praseodymium yellow pigment ratio
TABLE 3 sintering procedure
| Examples | Preheating temperature | Preheating time | Rate of temperature rise | Maximum temperature | Time of heat preservation |
| 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 |
TABLE 4 coefficient of thermal expansion
| Corresponding embodiment | Coefficient of thermal expansion |
| 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 |
TABLE 5 gloss values
| Corresponding embodiment | Degree of gloss |
| 1 | 93 |
| 2 | 96 |
| 3 | 101 |
| 4 | 91 |
| 5 | 88 |
Claims (10)
1. A low-temperature yellow glaze for zirconia is a low-temperature yellow glaze for zirconia, and is prepared by glazing the surface of zirconia ceramic and sintering at 700-900 ℃ for 20-40 min; the low-temperature yellow glaze for zirconia is characterized by comprising a base glaze and a zirconium praseodymium yellow material, wherein the zirconium praseodymium yellow material accounts for 1-15% of the base glaze in percentage by mass;
the basic glaze comprises the following raw materials in parts by weight: 55-70 parts of silicon dioxide, 5-8 parts of aluminum 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 and 0.5-1 part of niobium pentoxide.
2. The low-temperature yellow glaze for zirconia according to claim 1, wherein the low-temperature yellow glaze for zirconia has a coefficient of thermal expansion of 9.5 ± 0.5 x 10-6and/K, matching with the zirconia ceramic.
3. The low-temperature yellow glaze for zirconia according to claim 1, wherein the low-temperature yellow glaze for zirconia is suitable for zirconia ceramics which are relatively dense and have a relative density of not less than 90%.
4. The low-temperature yellow glaze for zirconia according to claim 1, wherein the low-temperature yellow glaze for zirconia has a gloss of 85 or more at an instrumental measurement angle of 60 °.
5. The method for preparing the low-temperature yellow glaze for zirconium oxide according to any one of claims 1 to 4, comprising the steps of:
step 1: ingredients
Weighing raw materials according to the raw materials and the proportion of the basic glaze in the low-temperature yellow glaze for zirconium oxide, and uniformly mixing the raw materials to obtain a mixture;
step 2: preparation of basic glaze
Melting the mixture at 1400-1600 ℃, preserving heat for 40-90 min, and performing water quenching to obtain a glass frit;
crushing, grinding, ball milling and drying the glass frit to obtain glass powder serving as basic glaze; the granularity D50 of the glass powder is 2-20 μm;
and step 3: low-temperature yellow glaze for preparing zirconium oxide
Uniformly mixing the glass powder and the zirconium praseodymium yellow pigment according to the proportion to obtain a low-temperature yellow glaze material for zirconium oxide; the granularity D50 of the low-temperature yellow glaze for the zirconium oxide is = 2-20 μm;
and 4, step 4: glazing and sintering
Adding the low-temperature yellow glaze for zirconium oxide into the organic solution, and stirring to obtain low-temperature yellow glaze liquid for zirconium oxide; the solid content of the low-temperature yellow glaze for zirconia in the low-temperature yellow glaze liquid for zirconia is 60-70 wt.%;
glazing the zirconia on the surface of the zirconia ceramic by using the low-temperature yellow glaze liquid, sintering at 700-900 ℃ for 20-40 min, cooling to room temperature along with a furnace, and taking out to obtain the low-temperature yellow glaze for zirconia attached to the surface of the zirconia ceramic.
6. The method for preparing the low-temperature yellow glaze for zirconium oxide according to claim 5, wherein in the step 1, the mixing is performed by ball milling; wherein, the ball milling parameters are as follows: the ball milling speed of the horizontal ball mill is 100-200 r/min, the ball milling time is 4-5 h, and the material ball ratio is (2.5-3): 1.
7. the method for preparing the low-temperature yellow glaze for zirconium oxide according to claim 5, wherein in the step 2, the ball milling is performed at a ball milling rotation speed of 350-400 r/min for 30-40 min.
8. The method for preparing low-temperature yellow glaze for zirconium oxide according to claim 5, wherein in the step 4, the organic solution is one or more of ethylene glycol, propylene glycol, 1, 3-butanediol, polyethylene glycol 200 or polyethylene glycol 400.
9. The method for preparing low-temperature yellow glaze for zirconium oxide according to claim 5, wherein in the step 4, the glaze is preheated before sintering, wherein the preheating temperature is 350-500 ℃ and the preheating time is 2-3 min.
10. The method for preparing low-temperature yellow glaze for zirconium oxide according to claim 5, wherein in the step 4, the sintering is performed at a temperature rise rate of 30-40 ℃/min.
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| CN110698068B (en) * | 2019-11-25 | 2021-08-17 | 大埔县怡丰园实业有限公司 | Yellow high-gloss glaze for ceramics and preparation method thereof |
| CN111182754A (en) * | 2020-01-19 | 2020-05-19 | Oppo（重庆）智能科技有限公司 | Electronic equipment shell, manufacturing method thereof and electronic equipment |
| CN113387727A (en) * | 2021-06-30 | 2021-09-14 | 成都贝施美生物科技有限公司 | Zirconia surface treatment process |
| CN113402302B (en) * | 2021-07-08 | 2022-09-30 | 上海森艺医疗科技有限公司 | Dyeing material, preparation method thereof and application thereof to zirconium dioxide all-ceramic tooth |
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| EP2000443A1 (en) * | 2007-05-29 | 2008-12-10 | Sociedad Anonima Minera Catalano-Aragonesa | Metallic glaze composition |
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