CN102464488A - Medium-temperature-oxidized high-whiteness blue jade porcelain and preparation method thereof - Google Patents
Medium-temperature-oxidized high-whiteness blue jade porcelain and preparation method thereof Download PDFInfo
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Abstract
The invention relates to medium-temperature-oxidized high-whiteness blue jade porcelain and a preparation method thereof. According to the invention, a blank material comprises main chemical components of, by weight: 55-70 parts of SiO2, 15-25 parts of Al2O3, 2-4 parts CaO, 0.05-0.5 parts of MgO, 2-4 parts of K2O, 1.5-4 parts of Na2O, 0.1-0.5 parts of Li2O, Fe2O3 and TiO2 with a total weight smaller than 0.25% of that of the blank material, and 4-6 parts of IL. A glaze comprises main chemical components of, by weight: 60-70 parts of SiO2, 10-15 parts of Al2O3, 4-6 parts of SrO, 2-3 parts of MgO, 3-5 parts of CaO, 1-2 parts of Na2O, 4-6 parts of K2O, and 1.5-3 parts of Li2O. Compared to existing technologies, the blue-whiteness of the porcelain provided by the invention is higher than 80 DEG, and the glossiness reaches 85%. Other physical and chemical properties of the porcelain satisfy national standards. The sintering temperature of the porcelain is reduced by 100 DEG C, the qualification rate is improved by 15-18%, the oil consumption is reduced by 25%, and a production cost is reduced by approximately 1/3. The porcelain is advantaged in low cost, high yield, and good quality.
Description
Technical field
The present invention relates to a kind of high ceramic whiteware device and preparation method thereof.
Background technology
Porcelain is one of greatness invention of Ancient Times in China, and like beautiful, extremely welcome by users at home and abroad like snow for ceramic whiteware, the class of the height reflection ceramic whiteware of its whiteness, and prescription is different with calcining system, can make porcelain demonstrate yellowish-white and blue white two kinds of different whiteness manifestation.Reputation claims that the high whiteness bluish white porcelain of Dehua conventional high-temperature of " Chinese white " can be rated as " treasure in the porcelain ", and blue whiteness reaches about 70 degree, and owing to general green grass or young crops in white, porcelain is superior to showing other porcelain of yellowish-white degree, seems especially precious, always travelling trader's favor extremely both at home and abroad.But, cause the high whiteness bluish white porcelain of famous and precious for a long time Dehua high temperature to be difficult to industrialization production because of the higher porcelain manufacturing cost of blue whiteness is high, product percent of pass is low, cost an arm and a leg.Because the high whiteness bluish white porcelain of high temperature needs in the high temperature reduction atmosphere more than 1380 ℃, to burn till; Be easy to produce defectives such as spot, cigarette smoke, yin jaundice; Produce comparatively difficulty of the higher high-quality porcelain of blue whiteness in enormous quantities, thereby seriously restricted the development of the high-grade high whiteness ceramic whiteware of China for a long time.
Summary of the invention
Main purpose of the present invention is to overcome the shortcoming of prior art, through improving batching of body and glaze and firing process, provide a kind of in the high whiteness turquoise of warm oxidation porcelain and preparation method thereof, the blue whiteness of the porcelain of preparation is high, and reduces firing temperature, and is energy-saving and cost-reducing.
One, blank
Of the present invention a kind of in the high whiteness turquoise of warm oxidation porcelain be on the basis of the high whiteness bluish white porcelain of conventional high-temperature, to carry out technological innovation.The tradition bluish white porcelain is easy to generate shortcomings such as spot, sootiness, yin jaundice in process of production, and energy consumption is high, causes production cost high, and product percent of pass is low, costs an arm and a leg.To these characteristics; The applicant uses for reference a large amount of domestic and international ceramic advanced production technology data through consulting, and on the basis of repeatedly experiment, high temperature bluish white porcelain blank formulation is reformed and innovated; Through adding low temperature mineral, multiple oxide compound; Change the physics-chem characteristic of base glaze, solve a firing technology technology difficult problem, burn till high whiteness turquoise porcelain 1275 ℃ ± 10 ℃ of middle temperature oxydizing flame.Therefore rationally selecting raw mineral materials for use is one of very crucial work of this project.
The applicant analyzes the reason of the easy spot that occurs, sootiness, yin jaundice in the production of high temperature bluish white porcelain, and the high temperature bluish white porcelain is in order to reduce Fe
3+Painted, Fe
2O
3+ CO → 2FeO+CO
2The employing reducing atmosphere burns till, in the sintering process transition of oxydizing flame and reducing flame as deal with improperly or reduce too high, the strong reduction zone of deficiency, firing temperature heat up too fast, the too early vitreous of glaze, pore sealing and secondary oxidation all can make product yellowing phenomenon occur; Reduce later stage reducing atmosphere overrich in addition, CO at high temperature produces to decompose and causes the glaze carbon distribution to form sootiness, 2CO → CO
2+ C (carbon black) or reduction period furnace temperature are low excessively, the glaze layer is blocked up also can produce sootiness.The compound of iron, metallic iron exists in the base glaze with larger particles and colour developing is the major cause that spot forms.Learn that through analysis the control of high temperature firing atmosphere is improper to be the major cause that porcelain glaze yin jaundice and sootiness produce, the existence of iron contamination is the major cause that spot produces.High temperature reduction atmosphere is burnt till the energy consumption that not only can improve product, and the while flue gas contains CO and can increase the weight of the pollution to environment.Therefore the general technical route that warm oxidation is burnt till in the feasibility study process of this project, just having confirmed to adopt; Adopt oxidizing atmosphere to burn till and to avoid the wayward product defects that brings of high temperature reduction atmosphere; Fuel is got back and is fully burnt, and reduces to flue gas minimum to the pollution level of surrounding environment.Temperature is burnt till in the employing, and firing temperature descends about 100 ℃, can cut down the consumption of energy greatly, and is energy-conservation 25%, shortens firing period, prolongs kiln, kiln furnitures work-ing life, reduces production costs, and improves the competitiveness of product in market.In order to reach the porcelain of the high whiteness of project product; Many schemes have been proposed in the process of argumentation; Through comparing and test, confirm at last to adopt through adding the painted way of carrying out physics complementary color of coloring oxide to ferrotitanium, alleviate the influence of iron cpd to the porcelain whiteness.
High temperature bluish white porcelain blank generally is made up of kaolin and quartz, feldspar, for the target of warm oxidation in reaching, reduces the firing temperature of blank; Just must reform the flux component in the blank formulation; According to the physical chemistry of silicate principle, accomplish the series of physical chemical transformation, sintering will carry out fast; Need liquid phase to participate in, should increase flux component for this reason, improve the blank fineness.Based on the eutectic point principle, component is many more, and eutectic point is low more, and the temperature that liquid phase promptly occurs is low more.Therefore select polynary composite fluxing agent for use, make the demand that warm oxidation is burnt till in its adaptation, generally adopt potassium felspar sand, can obtain better glossiness, whiteness and transparency, more quartzyly can melt at high temperature bluish white porcelain blank andesine.Melt temperature a wider range of potassium felspar sand, melt temperature is higher, but can increase the thermal expansivity of base substrate, reduces anti-opening and elastic performance.Introduce the part albite for this reason and replace potassium felspar sand, the initial melting temperature of albite is lower than potassium felspar sand, does not have new crystalline phase to produce during fusing; The liquid phase viscosity that forms is lower, the rising of its viscosity with temperature and reducing rapidly, and albite is fast to the dissolution rate of quartz, clay, mullite when high temperature; Solubleness is also bigger; Help the porcelainization and raising translucency of porcelain base, the fluxing action of albite is better than potassium felspar sand, can reduce the sintering temperature of base substrate.The cooling-down effect albite is better than potassium felspar sand, and the porcelain body transparency is high, and quality is fine and smooth, eliminates defectives such as pin hole, glaze bubble easily.Add Na in the glaze
2The too much easy especially crackle of O can only be introduced the part albite for this reason.Containing lithium minerals also is good flux, and lithium ion radius ratio potassium, sodium ion radius are little, and the chemically reactive of lithium is higher than potassium, sodium, and the effect of its flux is more much better than than potassium, sodium; The ability of lithium matter liquation dissolving quartz is also very big, can reduce liquation viscosity to contain lithium minerals as flux, significantly reduces sintering temperature, maturing temperature and the thermal expansivity of base substrate, adopts triphane to introduce.Adopt area, Dehua kaolin to belong to the high silicon-type of rich potassium in the present invention, under 1100 ℃, triphane and metakaolinite, quartz reaction generate β-triphane Solid solution and mullite, help into porcelain.The SiO in β-triphane Solid solution wherein
2Content the more, its thermal expansivity is littler.
The introducing of triphane simultaneously has very great help to thermostability, intensity and the density that improves the porcelain base, and its mechanism is: triphane receives SiO in the kaolinite
2With SiO in the quartz
2, quartz constantly is melted in the melt, suppressed residual quartz and transformed, free SiO in the melt to cristobalite
2Content reduces, and causes the cristobalite can be because of silicon supersaturation crystallization in the melt.Triphane has reduced the crystal conversion of β-quartz to alpha-quartz, makes β-quartz stable in broader temperature province, and β-quartzy coefficient of expansion is very low, and this is of great importance to reduction porcelain base thermal expansivity, raising thermal shock resistance.On the other hand, because the adding of triphane reduces blank andesine consumption, thermal expansivity also can reduce.The strong fusibleness of triphane impels base substrate to produce more glassy phase, improves density of product and intensity.Introduce according to porcelain and to contain lithium minerals, reduce the temperature that liquid phase appears in base substrate, mullite can occur under 1000 ℃.Through comparison to mine resources, composition analysis, quality situation and the communications and transportation etc. of porcelain stone in Dehua feldspar, land for growing field crops feldspar, Ninghua feldspar, Xianyou feldspar, the waterside; Porcelain stone and Xinjiang triphane are as base substrate flux in selected at last land for growing field crops feldspar, Ninghua feldspar, the waterside; Land for growing field crops feldspar and Ninghua feldspar ore reserve are abundant; All more than 300,000 tons, steady quality is main with potassium felspar sand; The porcelain stone firing temperature is lower in the waterside, contains the part albite, helps reducing the base substrate firing temperature, and it is higher that the Xinjiang triphane contains the lithium amount, is China's quality triphane mineral deposit preferably.
Kaolinic quality has decisive role to the whiteness of porcelain; Therefore very prudent to the selection of kaolin raw material; Through the kaolinic analysis in various places is compared, comprehensive various factors is chosen the kaolin of Bao Keng ore deposit, Dehua, ore deposit, hollow hole, three locations, Ge Keng ore deposit at last and is used kaolin as base.Through firing test, above-mentioned three kinds of kaolinic burnings back whiteness are all at 90 more than the whiteness unit, and ore reserve are big, and steady quality can satisfy requirement of mass production, and the kaolinic whiteness in hollow hole is more higher than the whiteness of other two places.The quartzy land for growing field crops of adopting is quartzy, and steady quality meets requirement of products.
The blank raw material chemical constitution is as shown in the table:
The raw mineral materials of selecting respectively taken a sample 10 tons process subsequent use.Bao Keng (No. 1), hollow hole (No. 2), lattice hole (No. 3) kaolin all adopted the machine treadle-operated tilt hammer for hulling rice 24 hours, and it is subsequent use to go into ball milling soil storehouse later with the 0.5cm sieve behind the treadle-operated tilt hammer for hulling rice.Stone class raw material all adopts fragmentation, rolling, and it is subsequent use to cross 8 mesh sieves warehouse-in.Stone class raw material is first water flushing before fragmentation, and the earth that will adhere to is cleaned, and then chooses, and rejects detrimental impurity such as iron-bearing mineral and mica.In the course of processing to raw material, note industrial hygiene, raw material is stacked the place and will be cleaned totally, various raw material pile up separately, each manufacturing procedure place, machinery, instrument should clean totally, avoid the particularly introducing of irony of impurity in the course of processing.
Fig. 1 is a raw material work flow skeleton diagram.
All take a sample 5kg ball milling 30 hours of every kind of raw material after the processing, mill are after 250 mesh sieve iron removal by filtration, and screen over-size is not more than 0.02%, and the mud after the filtration pours suction in the plaster mould, oven dry, grind up shape, and it is subsequent use to post label in the wealthy mouthful of bottle of packing into.Earlier carry out the debugging of base substrate firing temperature, whiteness with strip.
Through a large amount of blank formulation tests, the following blank formulation of final formation is formed:
Kaolin 40-55 part, feldspar 15-30 part, porcelain stone 1-3 part, triphane 2-6 part, quartzy 20-30 part.
The chemical constitution of blank is following:
SiO
255-70 part, Al
2O
315-25 part, CaO 2-4 part, MgO 0.05-0.5 part, K
2O 2-4 part, Na
2O 1.5-4 part, Li
2O 0.1-0.5 part, Fe
2O
3+ TiO
2Less than 0.25% of blank gross weight, IL 4-6 part.
Two, glaze
As everyone knows; In ceramic industry, adopt plumbous oxide to have very superior performance in the glaze as flux, all be applied for a long time; But containing lead glaze brings certain harm can for people's health; Along with people's is all the more paid attention to healthy, and various countries have made more and more stricter regulation to objectionable impurities stripping quantities such as the plumbous cadmiums of pottery, continues to use traditional leaded system and is difficult to satisfy the requirement that harsh day by day plumbous quantity of cadmium release allows limit value.Therefore in glaze development of the present invention, carry out the research and development of leadless glaze and lead and cadmium free pigment.The present invention takes lithium, strontium, system on silicon glaze, Li
2O introduces with triphane; Li
2O introduces can reduce thermal expansivity, and glaze fit is good, improves glaze texture.SrO, BaO have strong fluxing action in glaze, specific refractory power is bigger, can guarantee Gloss of Glazes degree and brightness, melt temperature a wider range, and SrO is with SrCO
3, BaO is with BaCO
3Introduce; MgO introduces to burn talcum simultaneously, utilizes MgO to improve the elasticity of glaze layer, improves thermostability, whiteness, transparency, reduces firing temperature, increases the flowability of glaze, and air scavenge in the favourable sintering process overcomes glaze pin hole, glaze bubble defective easily.Therefore in the glaze formula of this project, adopt Li
2O, SrO, BaO, MgO polycomponent mineralizer replace PbO fully, can guarantee the glaze glossiness; Adjustment Li
2O and K
2O, Na
2The ratio of O can guarantee the coupling of the base glaze coefficient of expansion and suiting of firing temperature; Add a spot of kaolin and improve the suspension property of glaze, not enough SiO
2Adopt quartzy the introducing.
According to test of many times, it is following to obtain best glaze formula:
Feldspar 35-50 part, triphane 4-10 part, Wingdale 5-15 part, quartzy 15-30 part, kaolin 2-8 part, talcum 4-10 part, SrCO
35-15 part, BaCO
31-5 part.
The main chemical compositions parts by weight are following in the glaze: SiO
260-70 part; Al
2O
310-15 part; SrO 4-6 part; BaO 2-3 part; MgO 1-3 part; CaO 3-5 part; Na
2O 1-2 part; K
2O 4-6 part; Li
2O 1.5-3 part.
Glaze is made an experiment and can know, glaze glossiness＞85% of the glaze of this prescription, body and glaze associativity is good, glaze plane defects such as free of pinholes, 200-20 ℃ of heat exchange once do not split.Record various glaze performances and all can reach predetermined target value; This glaze belongs to the transparent medium temperature glaze of lithium strontium silicon, has a beginning to melt temperature height, burn-off rate is fast, high temperature viscosity is little characteristics, through producing checking; This glaze formula can satisfy the demand of producing in enormous quantities, is practicable.
This glaze is not leaded, and belonging to the lithium strontium does not have the boron glaze, in actual production, the dried glaze phenomenon can not occur and split the glaze phenomenon.In the test of 200 ℃ of-20 ℃ of chillings, glaze does not split, and the base glaze combines good, and the under glazed color development is bright-coloured, and the glaze transparency is high, and temperature flowing property is strong, good springiness, characteristics that physical strength is high.The glaze fineness is controlled to be 250 mesh screen residues less than 0.005%, and it is subsequent use to cross 160 mesh sieves after the deironing.The decoration of this project product adopts under glazed to decorate, and under glazed pigment is selected not leaded cadmium pigment as far as possible, and the project product has been realized the target that lead and cadmium free is decorated basically, has improved the class of product.
In a word, the present invention adopts the lower melting point raw material improving on the high whiteness bluish white porcelain of Dehua conventional high-temperature batching of body and glaze basis, reduces iron titanium oxide and introduces, and changes base glaze chemical constitution, reduces firing temperature.The present invention adopts under glazed to decorate and the temperature automatically controlled and strict control oil-gas ratin of computer, and warm oxidizing atmosphere is burnt till in the realization.Practice result shows that this project is burnt till porcelain at 1275 ± 10 ℃ under the oxidizing atmosphere, and vitreous becomes porcelain fully, and water-intake rate reaches in 0.5%, is up to state standards.The content of ferrotitanium from complete processing control raw material; Adopt advanced iron removal technology; Guarantee that iron level reaches than low degree; Add and use transition element oxide compound complementary color method, can reach fully and eliminate iron, the painted influence of titanium, fire the new porcelain kind of bright-coloured, the pure high blue whiteness true to nature of picture color under glaze light jade-like stone profit, the general ultramarine tone of Bai Liwei, the glaze.
The blue whiteness of the porcelain of the present invention's preparation is up to more than 80 degree, and glossiness reaches 85%, other physicochemical property National standard; And firing temperature reduces by 100 ℃, and qualification rate improves 15%-18%, fuel-economizing 25%; Production cost descends about 1/3, has that cost is low, output is high, the measured advantage of matter.The at home and abroad high whiteness bluish white porcelain of alternative high temperature and other high temperature ceramic whiteware products on the market.
Description of drawings
Fig. 1 is a raw material work flow skeleton diagram of the present invention;
Fig. 2 is a firing temperature graphic representation of the present invention.
Embodiment
Embodiment one
Blank ingredients by weight umber is following: 48 parts of kaolin, 21 parts of feldspars, 2 parts of porcelain stones, 4 parts of triphanes, quartzy 25 parts.
Wherein kaolin selects for use 3 parts of the kaolin in precious hole, 40 parts of the kaolin in hollow hole, lattice to cheat 5 parts of kaolin; Feldspar is selected 11 parts of Ninghua feldspars, 10 parts of land for growing field crops feldspars for use; Porcelain stone is selected porcelain stone in the waterside for use; Quartz selects for use the land for growing field crops quartzy.
The chemical weight item of blank is following:
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | TiO 2 | CaO | MgO | K 2O | Na 2O | Li 2O | IL |
| Form | 64.81 | 21.57 | 0.03 | 0.01 | 3.24 | 0.09 | 2.79 | 2.35 | 0.27 | 4.96 |
Each item performance index of blank are as follows:
Glaze ingredients by weight umber is following: 43 parts of feldspars, 6 parts of triphanes, 10 parts in Wingdale, quartzy 21 parts, 5 parts of kaolin, 6 parts in talcum, SrCO
310 parts, BaCO
33 parts.
The chemical weight item of glaze is following:
In oxidizing atmosphere, burn till, firing temperature is 1275 ± 10 ℃.
The firing temperature graphic representation is shown in accompanying drawing 2, and X-coordinate firing time unit is h among the figure, and ordinate zou firing temperature unit is 100 ℃.
Product the key technical indexes after burning till is following:
Thermostability: 200 ℃ of-20 ℃ of heat exchanges are not once split
Whiteness: blue whiteness >=80 a whiteness unit
Firing atmosphere: oxidizing atmosphere
Water-intake rate:＜0.5%
Lead release :≤2mg/L
Quantity of cadmium release :≤0.2mg/L
Fuel-economizing:＞25%.
Embodiment two
Blank ingredients by weight umber is following: 42 parts of kaolin, 20 parts of feldspars, 2.5 parts of porcelain stones, 3 parts of triphanes, quartzy 25 parts.
Glaze ingredients by weight umber is following: 40 parts of feldspars, 8 parts of triphanes, 6 parts in Wingdale, quartzy 25 parts, 4 parts of kaolin, 8 parts in talcum, SrCO
312 parts, BaCO
34 parts.
In oxidizing atmosphere, burn till, firing temperature is 1275 ± 10 ℃.
Product the key technical indexes after burning till is following:
Thermostability: 200 ℃ of-20 ℃ of heat exchanges are not once split
Whiteness: blue whiteness >=80 a whiteness unit
Firing atmosphere: oxidizing atmosphere
Water-intake rate:＜0.5%
Lead release :≤2mg/L
Quantity of cadmium release :≤0.2mg/L
Fuel-economizing:＞25%.
Embodiment three
Blank ingredients by weight umber is following: 50 parts of kaolin, 25 parts of feldspars, 1.5 parts of porcelain stones, 5 parts of triphanes, quartzy 22 parts.
Glaze ingredients by weight umber is following: 45 parts of feldspars, 6 parts of triphanes, 12 parts in Wingdale, quartzy 18 parts, 6 parts of kaolin, 5 parts in talcum, SrCO
37 parts, BaCO
32 parts.
In oxidizing atmosphere, burn till, firing temperature is 1275 ± 10 ℃.
Product the key technical indexes after burning till is following:
Thermostability: 200 ℃ of-20 ℃ of heat exchanges are not once split
Whiteness: blue whiteness >=80 a whiteness unit
Firing atmosphere: oxidizing atmosphere
Water-intake rate:＜0.5%
Lead release :≤2mg/L
Quantity of cadmium release :≤0.2mg/L
Fuel-economizing:＞25%.
Above-mentionedly be merely several embodiment of the present invention, but design concept of the present invention is not limited thereto, allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should belong to the behavior of invading protection domain of the present invention.
Claims (4)
1. the high whiteness turquoise of warm oxidation porcelain in a kind is characterized in that:
The main chemical compositions parts by weight are following in its blank: SiO
255-70 part, Al
2O
315-25 part, CaO 2-4 part, MgO 0.05-0.5 part, K
2O 2-4 part, Na
2O 1.5-4 part, Li
2O 0.1-0.5 part, Fe
2O
3+ TiO
2Less than 0.25% of blank gross weight, IL 4-6 part;
The main chemical compositions parts by weight are following in its glaze: SiO
260-70 part; Al
2O
310-15 part; SrO 4-6 part; BaO 2-3 part; MgO 1-3 part; CaO 3-5 part; Na
2O 1-2 part; K
2O 4-6 part; Li
2O 1.5-3 part.
2. as claimed in claim 1 a kind of in the high whiteness turquoise of warm oxidation porcelain, it is characterized in that: said blank ingredients by weight umber is following: kaolin 40-55 part, feldspar 15-30 part, porcelain stone 1-3 part, triphane 2-6 part, quartzy 20-30 part.
3. as claimed in claim 1 a kind of in the high whiteness turquoise of warm oxidation porcelain, it is characterized in that: said glaze ingredients by weight umber is following: feldspar 35-50 part, triphane 4-10 part; Wingdale 5-15 part, quartzy 15-30 part, kaolin 2-8 part; Talcum 4-10 part, SrCO
35-15 part, BaCO
31-5 part.
A claim 1 or 2 or 3 described in the preparation method of the high whiteness turquoise of warm oxidation porcelain, it is characterized in that: in oxidizing atmosphere, burn till, firing temperature is 1275 ± 10 ℃.
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