CN110316968B - Fast-fired polycrystalline multicolor crystal glaze and preparation method and application thereof - Google Patents
Fast-fired polycrystalline multicolor crystal glaze and preparation method and application thereof Download PDFInfo
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- CN110316968B CN110316968B CN201910743849.0A CN201910743849A CN110316968B CN 110316968 B CN110316968 B CN 110316968B CN 201910743849 A CN201910743849 A CN 201910743849A CN 110316968 B CN110316968 B CN 110316968B
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- 239000013078 crystal Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000000919 ceramic Substances 0.000 claims abstract description 32
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 25
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 24
- 238000010304 firing Methods 0.000 claims abstract description 19
- 239000011787 zinc oxide Substances 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 12
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 12
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000010453 quartz Substances 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010433 feldspar Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 68
- 230000008569 process Effects 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000001816 cooling Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 9
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 7
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 7
- 239000003086 colorant Substances 0.000 claims description 7
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000391 smoking effect Effects 0.000 abstract description 9
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 16
- 239000002002 slurry Substances 0.000 description 11
- 238000000498 ball milling Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 239000004110 Zinc silicate Substances 0.000 description 4
- 235000019352 zinc silicate Nutrition 0.000 description 4
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 241001122767 Theaceae Species 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical class [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052611 pyroxene Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali 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
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 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
- C03C8/14—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
- C04B41/45—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)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the technical field of ceramic glaze preparation, and particularly relates to a fast-fired polycrystalline type multicolor crystal glaze, a preparation method and an application thereof, and specifically relates to a fast-fired polycrystalline type multicolor crystal glaze and a preparation method thereof, a preparation method of a fast-fired polycrystalline type multicolor crystal glaze ceramic product, a fast-fired polycrystalline type multicolor crystal glaze ceramic product and a high-temperature firing method thereof. The crystal glaze is in a supersaturated state by matching of seven metal systems of calcined light calcium carbonate (calcium), calcined light magnesium carbonate (magnesium), calcined zinc oxide (zinc), calcined titanium oxide (titanium), kaolin (silicon), quartz (silicon) and feldspar (potassium and sodium), so that the crystallization speed of the crystal glaze is improved, the crystallization area is enlarged, the problems of easy-flowing glaze and smoking (the phenomena of overcast yellow and smoking) are avoided, the crystal glaze can be normally heated to the sintering temperature on the premise of not influencing the performance of the crystal glaze, the temperature is quickly reduced to the normal temperature after the sintering is finished, the preparation period is shortened, and the effects of energy conservation and environmental protection are achieved.
Description
Technical Field
The invention belongs to the technical field of ceramic glaze preparation, and particularly relates to a fast-fired polycrystalline type multicolor crystal glaze, a preparation method and an application thereof, and specifically relates to a fast-fired polycrystalline type multicolor crystal glaze and a preparation method thereof, a preparation method of a fast-fired polycrystalline type multicolor crystal glaze ceramic product, a fast-fired polycrystalline type multicolor crystal glaze ceramic product and a high-temperature firing method thereof.
Background
The crystallized glaze is a crystal with beautiful patterns, which is generated by that the crystallized substances of the glaze are in a saturated state after the glaze is melted at high temperature in the sintering process of the product and are crystallized after being cooled. The 'rust flower', 'tea dust', 'oil drop Tianmu' and other rare crystal glazes are fired in two Song dynasties in China, people develop 'zinc silicate crystal glaze', 'calcium silicate crystal glaze' and 'rutile crystal glaze' in recent years, the crystal glaze is natural in crystal form transformation, crystal flowers are colorful and beautiful, and the crystal glaze is favored by people, however, the production crystallization conditions of the crystal glazes are strict, the process operation is complex, and enamel influencing factors are many.
Chinese patent document CN109279780A discloses a ceramic glaze resistant to strong alkali corrosion and a preparation method thereof, wherein the ceramic glaze comprises boron frit, quartz powder, spodumene, calcined zinc oxide, calcined talc powder, kaolin, zirconium silicate and a coloring agent, the preparation method comprises the steps of ball milling and sieving the components, then adding water and an electrolyte to respectively adjust the concentration and thixotropy of glaze slurry, then immersing a glaze blank in the glaze slurry, drying and then firing the glaze blank in a roller kiln to obtain the ceramic glaze. In addition, in the prior art, the preparation process of the crystal glaze generally has the problems of poor fluidity of glaze slip, strict requirements on sintering atmosphere, easy occurrence of overcast and yellow and smoking of a glaze layer in the sintering process, poor thermal stability of the crystal glaze and the like.
Disclosure of Invention
Therefore, the invention aims to overcome the defects of poor thixotropy and flowability of glaze slip, yellowing and smoking phenomena of a sintered glaze layer, poor thermal stability of a crystal glaze and the like in the prior art, thereby providing the fast-fired polycrystalline multicolor crystal glaze and the preparation method and application thereof.
Therefore, the invention provides the following technical scheme.
The invention provides a fast-fired polycrystalline multi-color crystal glaze which comprises the following raw materials in parts by weight: 0.5-1.5 parts of pigment, 15-20 parts of calcined zinc oxide, 5-10 parts of calcined titanium oxide, 10-20 parts of calcined light calcium carbonate, 10-20 parts of calcined light magnesium carbonate, 20-30 parts of feldspar, 7-9 parts of kaolin and 6-8 parts of quartz.
The colorant is at least one selected from cobalt oxide, iron oxide, chromium oxide or manganese oxide.
The invention also provides a preparation method of the fast-firing polycrystalline multi-color crystal glaze, which comprises the following steps: the raw materials are mixed according to the weight ratio, then water is added for grinding, and then the finished product glaze slip is obtained after sieving and water mixing.
The water content of the finished glaze slip is 40-50 wt%.
In addition, the invention provides a preparation method of the fast-fired polycrystalline type multicolor crystal glaze ceramic product, which comprises the steps of applying the fast-fired polycrystalline type multicolor crystal glaze or the fast-fired polycrystalline type multicolor crystal glaze prepared by the method on a blank, wherein the thickness of a glaze layer is 3-5mm, and sintering at high temperature and cooling to obtain the fast-fired polycrystalline type multicolor crystal glaze ceramic product.
Further, the fast-firing polycrystalline multi-color crystal glaze is applied on the blank body by a glaze dipping, glazing or glaze blowing method.
The cooling rate is 6.5-8 ℃/min.
The invention also provides a fast-fired polycrystalline multicolor crystal glaze ceramic product prepared by the preparation method, and the crystal glaze ceramic product can be applied to building ceramics, daily ceramics or artistic ceramics.
Further, the invention provides a high-temperature firing method of the fast-fired polycrystalline multi-color crystal glaze ceramic product, which comprises the steps of heating the temperature from room temperature to a certain temperature of 295-320 ℃ under 0.01-0.015MPa, wherein the heating time is 3-4 h; then heating to a certain temperature of 875 ℃ of 845-one, wherein the heating time is 1-1.5h, and the pressure in the process is 0.015-0.025 MPa; then heating to a certain temperature of 1135-1155 ℃, wherein the heating time is 2-2.5h, and the pressure in the process is 0.025 MPa; finally heating to 1250-1300 ℃ for 1-1.5h, wherein the pressure in the process is 0.025-0.030 MPa; the sintering method is a sintering atmosphere with sufficient oxygen.
The invention also provides a high-temperature firing method of the fast-fired polycrystalline multi-color crystal glaze ceramic product, which comprises the steps of heating the temperature from room temperature to 295-320 ℃ at 0.01-0.015MPa for 3-4 h; then heating to a certain temperature of 875 ℃ of 845-one, wherein the heating time is 1-1.5h, and the pressure in the process is 0.015-0.025 MPa; then heating to a certain temperature of 935-975 ℃, wherein the heating time is 0.5-1.0h, and the pressure in the process is 0.025 MPa; then heating to a certain temperature of 1135-1155 ℃, the heating time is 1.0-1.5h, the pressure in the process is 0.045-0.05MPa, and finally heating to a certain temperature of 1250-1300 ℃, the heating time is 1-1.5h, and the pressure in the process is 0.03-0.045 MPa; the sintering method is a sintering atmosphere with insufficient oxygen.
The technical scheme of the invention has the following advantages:
1. the fast-fired polycrystalline multicolor crystal glaze provided by the invention has the advantages that the crystal glaze is matched with seven metal systems of calcined light calcium carbonate (calcium), calcined light magnesium carbonate (magnesium), calcined zinc oxide (zinc), calcined titanium oxide (titanium), kaolin (aluminum), quartz (silicon) and feldspar (potassium and sodium), so that glaze slip is in a supersaturated state, the crystallization speed of the crystal glaze is improved, the crystallization area is enlarged, the problems of easy-flowing glaze and smoking (the phenomena of overcast and yellow smoking) are avoided, the crystal glaze can be normally heated to the sintering temperature on the premise of not influencing the performance of the crystal glaze, and the temperature is quickly reduced to the normal temperature after the sintering is finished, so that the effects of energy conservation and environmental protection are achieved; the thermal stability of the crystallized glaze is better;
according to the invention, the thixotropy of the glaze slip can be adjusted by using the calcined zinc oxide and the calcined magnesium oxide in specific proportions, and meanwhile, by adjusting the distribution ratio of the components, on the premise of not adopting an electrolyte, the fluidity of the glaze slip is improved, the precision of the thickness of a glaze layer is improved, and pores of a crystallized glaze product are avoided.
The crystal glaze can be made into various colors by introducing colorants such as iron oxide, cobalt oxide, chromium oxide or manganese oxide.
2. The invention provides a preparation method of a fast-burning polycrystalline multi-color crystal glaze ceramic product, which comprises the steps of mixing raw materials, grinding, sieving, and carrying out water mixing to obtain finished glaze slurry; glazing on the green body by adopting a method of dipping, pouring or blowing glaze, rapidly cooling the green body to normal temperature after sintering to obtain crystalline glaze, and when cooling at the speed of 6.5-8 ℃/min, forming supersaturated magnesium silicate crystals, zinc silicate crystals, perovskite crystals, pyroxene crystals and other various crystals in a high-temperature molten state on the glaze melt, wherein the crystals can rapidly separate out point-like, needle-like, rod-like, sheet-like and other various crystals from the glaze melt during cooling; in addition, the glaze slurry is added with coloring oxide, and a glaze surface with rich colors can be obtained.
The crystal glaze provided by the invention contains calcium silicate crystals, perovskite crystals, cordierite crystals, zinc silicate and other polymorphic crystals which can be quickly precipitated in the sintering process, can make the glaze layer change abundantly, and simultaneously presents a plurality of crystal forms such as point-shaped, needle-shaped, columnar, flaky crystals and the like.
In addition, in the high-temperature sintering process, the calcined light calcium carbonate and the calcined light magnesium carbonate are decomposed to generate calcium oxide and magnesium oxide, and various types of crystals formed by zinc oxide, titanium oxide, silicon substances and the like form magnesium silicate crystals, zinc silicate crystals, perovskite crystals and pyroxene crystals under the condition of sufficient or insufficient oxygen, so that the crystal glaze has the advantages of moderate crystal patterns, natural and attractive crystal forms, rich colors, crystal beauty, good firing stability, no need of adopting a heat preservation process and the like, is suitable for the production process of ceramic carving or daily ceramic tea sets or tableware products, and has good technical and economic benefits, and the crystal glaze provided by the invention is suitable for various high-temperature electric furnaces.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: 15 parts of calcined zinc oxide, 10 parts of calcined titanium oxide, 15 parts of calcined light calcium carbonate, 15 parts of calcined light magnesium carbonate, 30 parts of feldspar, 8 parts of kaolin, 7 parts of quartz and 1.5 parts of cobalt oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 45 percent, and obtaining finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, heating the temperature from room temperature to 300 ℃ under 0.01MPa, and heating for 3.5 h; then heating to 850 ℃, wherein the heating time is 1h, and the pressure in the process is 0.025 MPa; then heating to 1150 deg.C for 2.3h under 0.025 MPa; finally, heating to 1280 ℃, wherein the heating time is 1h, and the pressure in the process is 0.030 MPa; then, the temperature is reduced to normal temperature at the cooling rate of 6.9 ℃/min, and the crystallized glaze ceramic product is obtained.
Example 2
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: 15 parts of calcined zinc oxide, 10 parts of calcined titanium oxide, 15 parts of calcined light calcium carbonate, 20 parts of calcined light magnesium carbonate, 20 parts of feldspar, 8 parts of kaolin, 7 parts of quartz and 0.8 part of ferric oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 45 percent, and obtaining finished glaze slurry;
taking a blank body, carrying out glazing operation by adopting a glaze blowing mode, controlling the thickness of a glaze layer to be 3-5mm, then heating the temperature from room temperature to 320 ℃ under 0.015MPa, and heating for 4 hours; then heating to 845 ℃ for 1.5h, wherein the pressure in the process is 0.015 MPa; then heating to 1135 ℃, wherein the heating time is 2h, and the pressure in the process is 0.025 MPa; finally heating to 1300 ℃, wherein the heating time is 1.5h, and the pressure in the process is 0.025 MPa; then, the temperature is reduced to normal temperature at the cooling rate of 7.2 ℃/min, and the crystallized glaze ceramic product is obtained.
Example 3
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: calcined zinc oxide 20 parts, calcined titanium oxide 5 parts, calcined light calcium carbonate 20 parts, calcined light magnesium carbonate 10 parts, feldspar 25 parts, kaolin 8 parts, quartz 7 parts, cobalt oxide 0.8 parts and iron oxide 0.2 parts;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 45 percent, and obtaining finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, heating the temperature from room temperature to 298 ℃ under 0.01MPa, and heating for 3 h; then heating to 875 ℃ for 1.2h, wherein the pressure in the process is 0.02 MPa; then heating to 1155 ℃, wherein the heating time is 2.5h, and the pressure in the process is 0.025 MPa; finally, the temperature is raised to 1250 ℃, the temperature raising time is 1h, and the pressure in the process is 0.030 MPa; then, the temperature is reduced to normal temperature at the cooling rate of 6.9 ℃/min, and the crystallized glaze ceramic product is obtained.
Example 4
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: 20 parts of calcined zinc oxide, 10 parts of calcined titanium oxide, 15 parts of calcined light calcium carbonate, 15 parts of calcined light magnesium carbonate, 25 parts of feldspar, 8 parts of kaolin, 7 parts of quartz and 0.5 part of chromium oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 40% to obtain finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, then heating the temperature from room temperature to 300 ℃ under 0.012MPa, and heating the temperature for 3 h; then heating to 850 ℃ for 1h, wherein the pressure in the process is 0.020 MPa; then heating to 950 ℃, wherein the heating time is 0.8h, and the pressure in the process is 0.025 MPa; and then heating to 1150 ℃, wherein the temperature rise time is 1.2h, the pressure in the process is 0.045MPa, the temperature rise time is 1.5h, the pressure in the process is 0.040MPa, and then cooling to normal temperature at the temperature reduction rate of 6.6 ℃/min to obtain the crystal glaze ceramic product.
Example 5
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: 15 parts of calcined zinc oxide, 10 parts of calcined titanium oxide, 10 parts of calcined light calcium carbonate, 20 parts of calcined light magnesium carbonate, 20 parts of feldspar, 8 parts of kaolin, 7 parts of quartz and 1 part of cobalt oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 50 percent, and obtaining finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, then heating the temperature from room temperature to 295 ℃ under 0.01MPa, and heating for 3.5 hours; then heating to 875 ℃ for 1.5h, wherein the pressure in the process is 0.025 MPa; then heating to 935 ℃ for 0.5h, wherein the pressure in the process is 0.025 MPa; then heating to 1135 ℃, the temperature rise time is 1.0h, the pressure in the process is 0.05MPa, finally the temperature rise time is 1h, the pressure in the process is 0.03MPa, and then the temperature is reduced to the normal temperature at the temperature reduction rate of 8 ℃/min to obtain the crystal glaze ceramic product.
Example 6
The embodiment provides a fast-firing polycrystalline multi-color crystal glaze, which comprises the following components: 18 parts of calcined zinc oxide, 8 parts of calcined titanium oxide, 120 parts of calcined light calcium carbonate, 10 parts of calcined light magnesium carbonate, 30 parts of feldspar, 9 parts of kaolin, 6 parts of quartz and 0.5 part of chromium oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 45 percent, and obtaining finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, then heating the temperature from room temperature to 320 ℃ under 0.012MPa, and heating the temperature for 4 h; then heating to 848 ℃, wherein the heating time is 1.2h, and the pressure in the process is 0.020 MPa; then heating to 970 ℃, wherein the heating time is 0.8h, and the pressure in the process is 0.025 MPa; and then heating to 1152 ℃, wherein the heating time is 1.2h, the pressure in the process is 0.045MPa, the temperature is finally heated to 1255 ℃, the heating time is 1.5h, the pressure in the process is 0.040MPa, and then the temperature is reduced to the normal temperature at the cooling rate of 7 ℃/min to obtain the crystal glaze ceramic product. Comparative example 1
The present comparative example provides a crystalline glaze having the composition: 10 parts of calcined zinc oxide, 10 parts of calcined titanium oxide, 15 parts of calcined light calcium carbonate, 15 parts of calcined light magnesium carbonate, 35 parts of feldspar, 10 parts of kaolin, 7 parts of quartz and 1.5 parts of cobalt oxide;
the preparation and sintering method of the crystal glaze comprises the following steps,
uniformly mixing the raw materials, adding the mixture into a ball mill, adding water for ball milling, sieving the mixture by a 180-mesh sieve, adding water to adjust the water content of glaze to 45 percent, and obtaining finished glaze slurry;
taking a blank body, glazing by adopting a glaze dipping mode, controlling the thickness of a glaze layer to be 3-5mm, heating the temperature from room temperature to 300 ℃ under 0.01MPa, and heating for 3.5 h; then heating to 850 ℃, wherein the heating time is 1h, and the pressure in the process is 0.025 MPa; then heating to 1150 deg.C for 2.3h under 0.025 MPa; finally, heating to 1280 ℃, wherein the heating time is 1h, and the pressure in the process is 0.030 MPa; then, the temperature is reduced to normal temperature at the cooling rate of 6.9 ℃/min, and the crystallized glaze ceramic product is obtained.
Test examples
The test example provides the performance tests and results of the glaze slips and the crystal glaze in examples 1 to 6 and comparative example 1, the test method is as follows, and the test results are shown in table 1;
the method for testing the fluidity of the glaze slip is disclosed in GB/T23460.1-2009;
the thermal stability test method of the crystallized glaze comprises the following steps: taking 10 qualified samples to be tested in each example, putting the samples into a sample basket, putting the samples into a ceramic qualitative tester, starting the tester, keeping the temperature for 15min, stirring a handle to enable the sample basket to quickly fall into water, cooling for 5min, taking the samples out of the water, wiping the samples clean, checking whether the samples crack or not, if the samples crack or not, putting the samples into the tester, heating to the next measurement temperature (the temperature interval of two measurements is 20 ℃), repeating the test until all the 10 samples crack, recording data, and calculating the average heat-cold temperature difference (the heat-cold temperature difference is the difference between the measurement temperature and the room temperature) of the 10 samples, namely the heat stability, wherein the larger the temperature difference is, the better the heat stability is, and the purpose of changing water once every test is to keep the water temperature unchanged.
TABLE 1 results of performance test of crystalline glazes prepared in examples 1 to 6 and comparative example 1
In table 1, the glaze slips of examples 1 to 6 had good fluidity, the thermal stability of the crystal glaze was good, and no slip or smoking occurred; the composition of the crystalline glaze in comparative example 1 is not in the present invention, the fluidity of the glaze slip in comparative example 1 is relatively poor, the thermal stability of the crystalline glaze is also poor, and a slight yellowing or smoking problem occurs.
The preparation method provided by the invention has the advantages that the problems of glaze flowing and smoking are avoided, the prepared crystalline glaze has good thermal stability and fluidity, and the preparation method is energy-saving and environment-friendly.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (6)
1. A high-temperature firing method of a fast-firing polycrystalline multi-color crystal glaze ceramic product is characterized in that fast-firing polycrystalline multi-color crystal glaze is applied on a blank body, the thickness of a glaze layer is 3-5mm, and the fast-firing polycrystalline multi-color crystal glaze ceramic product is obtained after high-temperature sintering and cooling;
a high-temperature firing method for a fast-fired polycrystalline multicolor crystalline glaze ceramic product comprises,
under the pressure of 0.01-0.015MPa, the temperature is raised from room temperature to a certain temperature of 295-320 ℃, and the temperature rise time is 3-4 h; then heating to a certain temperature of 875 ℃ of 845-one, wherein the heating time is 1-1.5h, and the pressure in the process is 0.015-0.025 MPa; then heating to a certain temperature of 1135-1155 ℃, wherein the heating time is 2-2.5h, and the pressure in the process is 0.025 MPa; finally heating to 1250-1300 ℃ for 1-1.5h, wherein the pressure in the process is 0.025-0.030 MPa; the sintering method is a sintering atmosphere with sufficient oxygen, and a heat preservation process is not needed;
the fast-burning polycrystalline multicolor crystal glaze comprises the following raw materials in parts by weight: 0.5-1.5 parts of pigment, 15-20 parts of calcined zinc oxide, 5-10 parts of calcined titanium oxide, 10-20 parts of calcined light calcium carbonate, 10-20 parts of calcined light magnesium carbonate, 20-30 parts of feldspar, 7-9 parts of kaolin and 6-8 parts of quartz.
2. The method of claim 1, wherein the colorant is selected from at least one of cobalt oxide, iron oxide, chromium oxide, or manganese oxide.
3. A method according to any one of claims 1-2, comprising the steps of: the raw materials are mixed according to the weight ratio, then water is added for grinding, and then the finished product glaze slip is obtained after sieving and water mixing.
4. The method as claimed in claim 3, wherein the water content of the finished glaze slip is 40-50 wt%.
5. The method according to claim 1, wherein the fast-fired polycrystalline multi-color crystalline glaze is applied on the body by dipping, pouring or blowing.
6. The method of claim 4, wherein the rate of temperature reduction is 6.5-8 ℃/min.
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