CN106467413A - The resintering method that imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain is fired based on nano-sized iron oxide glaze and its serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain fired - Google Patents
The resintering method that imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain is fired based on nano-sized iron oxide glaze and its serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain fired Download PDFInfo
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Abstract
The present invention relates to based on the nano-sized iron oxide glaze resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain and its serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain fired.The inventive method passes through to add nano-sized iron oxide in base glaze, it is fired after direct glazing in the form of the glaze basis, overcome that in current resintering Song Jun official's porcelain technique, yield rate is low, burning process is complicated, color is excessively bright-coloured, color development is too straight, the shortcomings of opaque effect is inconspicuous, and the present invention passes through mass ratio in base glaze for the nano-sized iron oxide, the isoparametric color controlling adjustment to can reach control glaze layer of firing temperature, makes resintering pottery implements assume the purpose of series Song Jun official's enamel color such as pale blue, reddish black, sky blue, grey indigo plant.Except this, diffusivity is strong in pottery glaze firing for nano material, be conducive to coloring agent equally distributed feature in pottery glaze layer, so that the pottery product colour generation fired is uniform, and can effectively reduce glaze layer viscosity during glaze firing, avoid pottery surface that the defects such as pore occur, that improves pottery fires success rate.
Description
Technical field
The invention belongs to ceramic technology field, more particularly, to based on nano-sized iron oxide glaze fire imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain resintering method and its
The serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain fired.
Background technology
According to relevant historical document, pottery is created from the Tang Dynasty and being burnt, and reaches to the Northern Song Dynasty prosperous, ranks among first of five big porcelain of Song dynasty.Pottery
Glaze colours changes unpredictably, be blue or green as blue sky, white as beautiful jade, red like Caulis et folium euphorbiae milii, purple such as Flos Rosae Rugosae, gloss such as Achatess, dignified deep,
Implicit resistance to see, implication of endless appeal.The reddish black glaze colours that especially official kilns of Song Dynasty presents, with its simply thick and heavy style, obtains people's
Extensively praise.Ancients are once with " surpassing jade like beautiful non-jade ", the artistic style to evaluate it such as " the sun shines again after the rain, and cloud breaks just ".Its base
This quality is the different Celeste opalescence glaze of the various depths, and color is followed successively by bluish white, pale blue, reddish black, sky blue, grey from deep to shallow
Blue.
Excavate Song's kiln ruins through science and confirm, the kiln firing Song Jun government porcelain kiln is a kind of pair of emulsus fire box kiln, moulding is unique few
See, exclusive by pottery kiln.Its construction feature is to take to dig the method built on the spot, and flue, after kiln, belongs to half downward flame
Furnace construction.In terms of the ruins of kiln, an ancient unit of weight kiln product in ancient times burns till for firewood, and furnace chamber capacity is little, and chimney is short, relies in kiln
Negative pressure weaker generation reducing atmosphere.Celeste glaze is mainly by ferrum element colour generation, and all relies on mineral to provide in ferrum element at that time, past
It is difficult to control to toward because of the difference using iron concentration in raw material, tire, glaze and firing atmosphere and glaze.Although so gathering around during Song
There is so unique kiln, but still cannot reverse the situation of pottery " ten kilns nine do not become ", retention Song Jun official's porcelain so far is very
Few.Trace it to its cause, tire, glaze and firing atmosphere and temperature all can have influence on the colour generation of pottery, the influence factor of wherein glaze is the most straight
Connect.The burning process of unique exquisite kiln, mysterious glaze formula and complexity has achieved the Song Jun official's porcelain spreading thousand.
Because the burning techniques of Song Jun official's porcelain are lost, mostly Anhydrite can be added as colour former in glaze blue at present, but Yin Qise
Coloured silk is excessively bright-coloured, and color development is too straight, and opaque effect is inconspicuous, is difficult to be accepted by common people.Although resintering Song Jun official's porcelain successful case
Example (horse is exposed to the sun, Li Fubin. and the Northern Song Dynasty double fire box an ancient unit of weight kiln bavin burns Principle Discussion, 2005 Chinese Yuzhou Jun Yao scientific seminar papers
Collection), but burning process is considerably complicated.Pile firewood in major and minor fire box first, by the product of biscuiting together with saggar after allowing
Swing in firing chamber, finally close wicket.After igniting, main fire box firewood gradually burns, meanwhile, the firewood in secondary fire box be heated by
Gradually carbonization, releases a large amount of carbon monoxides in carbonization process.At this moment the acute catarrhal conjunctivitis of secondary fire box, in hall, the firewood of carbonization starts so
Around heating curve runs according to set scheme all the time.Through one day night, after 4 tons of firewoods burn down, same with major-minor fire box
When firing chamber is heated, furnace temperature has reached 1270 DEG C about of the temperature that pottery is fired finally.But fired during kiln discharge 56 works
5 finished products are only had in product.As can be seen here, current resintering technology is also very immature, there is poor controllability, glaze colours and texture not
The low shortcoming of good, yield rate, lacks the support of the science data such as color contrast simultaneously.
In fact, the basic glaze colours of an ancient unit of weight kiln major part product is the deep or light blue-opalescent glaze differing, mainly chun glaze Phase separation
As a result, in continuous glass matrix, left floating another kind of small size droplet-like and continuous second phase glass, in pottery glaze
This structure be famous American pottery scholar Kingery discovery first, and give Phase separation in K2O-CaO-
Al2O3-SiO2Region on quarternary phase diagram, becomes one of most important theories basis of modern pottery scientific research.Chun glaze dispersion phase
Particle diameter in 60nm to 200nm, the opalescence blueness exactly glaze layer of chun glaze these dispersed phase particles to visible spectrum intermediate waves light
Scattering process cause.If particle size close to visible wavelength to the several times of visible light wave wavelength when, the light intensity of scattering with
The selectivity of lambda1-wavelength relation is not notable, and the scattering seen from different directions is white, does not assume color, here it is newborn
Turbid phenomenon；If contrary particle size is less than the wavelength of incident illumination, particle then carries out selectivity scattering (Rayleigh scattering) to light wave,
Long wave scattering of light is weak, and shortwave light scattering is strong, so that glaze is in reddish black, sky blue etc., here it is opalescence phenomenon.So, ancient
People, in preparing glaze, can be milled into quality Ore after very thin powdery to use, because granule is more tiny, light scattering be got over
By force, chromophoric characteristic is better.In recent years, with the development of nanosecond science and technology, by the research of nano material introducing ceramic field gradually
It is taken seriously.Due to nano material some fundamental characteristics distinctive, it is easy to spread more evenly across in chun glaze.By making pottery common
Add a certain proportion of nano material in ceramic material, be conducive to densification, the homogenization of ceramic material the Nomenclature Composition and Structure of Complexes, simultaneously excellent
Change thermophysical property and optical property of material etc..Nanometer powder specific surface area is big, and chemism is high, advantageously reduces ceramic material
The firing temperature of material, the sintering becoming good promotes material.At present, existing Application of micron prepares pottery to pottery glaze
A kind of method firing pottery by additional nano material under oxidizing atmosphere of report, such as Application No. 2011104352877 is special
Profit, its specific practice is：Nano simple substance copper is equably imposed on by idiosome surface by outer coating method, by the use of Nanometer Copper as reduction
Agent, using temperature programming Muffle furnace, burns out under oxidizing atmosphere and produces from the shallow pottery having opal effect to deep various bluenesss
Product.The main purpose of this invention is to provide a kind of eco-friendly oxidizing atmosphere burning process, adds a kind of nontoxic non-colorant to help
Agent, burns out the pottery having blue-opalescent effect, but it is no matter all reach far away the product of Song Jun official's porcelain in terms of colourity, texture etc.
Matter.
Therefore, using the characteristic of nano material, find new solution resintering and go out to reach Song Jun official's porcelain quality and effect, have
The serial pottery product that collection is worth, innovation and upgrading to pottery industry are significant.
Content of the invention：
Problem to be solved by this invention is the characteristic how utilizing nano material, finds new solution resintering and goes out to reach or connect
Nearly Song Jun official's porcelain quality and the serial pottery product of effect.
For solving above-mentioned technical problem, the technical solution used in the present invention is：
There is provided a kind of based on nano-sized iron oxide glaze fire imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain resintering method it is characterised in that：Base glaze adds
Plus the nano oxidized iron material of 0.5wt%～2.0wt%, fire imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain.
By such scheme, after nano oxidized iron material dispersed acquisition nano-sized iron oxide glaze in base glaze, by once
The mode dipping in glaze is fired in idiosome surface glazing.
By such scheme, in intensification sintering procedure, control more than 1000-1060 DEG C and less than 1240-1260 DEG C of firing temperature model
Enclosing the firing atmosphere in interval is reducing atmosphere.
By such scheme, the firing time that reducing atmosphere is fired in intensification sintering procedure, is kept to be 5-6h.
By such scheme, above-mentioned fire for：When being warming up to 1000-1060 DEG C under the conditions of natural atmosphere, control climate is also
Primordial Qi atmosphere then heats to 1240-1260 DEG C, continues intensification afterwards again and carry out abundant vitreous process under the conditions of natural atmosphere, from
So cooling can obtain imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain products.In this sintering procedure, initial temperature-rise period mainly makes idiosome naturally rise warming middle-JIAO
Venting mechanical water and constitution water；The design then passing through intermediary reduction atmosphere intensification sintering procedure can make glaze paint drastically melt, and
Coloured under reducing atmosphere, gas in system can be discharged in this intensification sintering procedure simultaneously；Then carry out again at intensification vitreous
Reason, Temperature fall has obtained imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain products.
By such scheme, the described time being warming up to 1000-1060 DEG C is 3-5h.
By such scheme, described vitreous is processed as under the conditions of natural atmosphere being continuously heating to 1260-1280 DEG C, and here heats up
During carry out vitreous process.
By such scheme, described vitreous process time is 0.5-1h.
By such scheme, the present invention fires heat riser used and electrically mixes kiln for high temperature.High temperature electrically mixes kiln and is different from
Conventional kiln, on the one hand it adopts electric energy as heating energy source, and firing temperature is easy to control, and can be heated up with precise control and drop
Warm curve, meanwhile, whenever necessary by being burnt with the use of liquefied petroleum gas, and by controlling air inlet amount, can make
Liquefied petroleum gas burn incompletely produces CO, produces reducing atmosphere, is thus also easy to control firing atmosphere.
The above-mentioned serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain being prepared based on the resintering method that nano-sized iron oxide glaze fires imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain is provided.
By such scheme, described serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain color transition is uniformly natural, colour generation is uniform, and colour generation has pale blue, sky
Blue or green, sky blue, grey blue series, in tomography glaze paint, uniformly, ferrum element is uniformly distributed bubble distribution in whole glaze layer.
Beneficial effects of the present invention：
The inventive method passes through to add nano-sized iron oxide in base glaze, after its direct glazing in the form of the glaze basis
Fire, overcome that in current resintering Song Jun official's porcelain technique, yield rate is low, burning process is complicated, color is excessively bright-coloured, color development too
Directly, the shortcomings of opaque effect is inconspicuous, and the present invention passes through mass ratio in base glaze for the nano-sized iron oxide, firing temperature etc.
The adjustment that controls of parameter can reach the color controlling glaze layer, makes resintering pottery implements assume pale blue, reddish black, sky blue, grey indigo plant etc. and is
The purpose of row Song Jun official's enamel color.Except this, diffusivity is strong in pottery glaze firing for nano material, be conducive to coloring agent in pottery glaze
Equally distributed feature in layer is so that the pottery product colour generation fired is uniform, and can effectively reduce glaze layer viscosity during glaze firing,
Avoid pottery surface that the defects such as pore occur, that improves pottery fires success rate.
Advantages of the present invention：
1st, in directly nano oxidized iron material being added to parent glaze in the form of the glaze basis, glaze can accurately be controlled
The content of middle nano-sized iron oxide, in idiosome surface glazing by way of once dipping in glaze, hair color effect is more preferable.
2nd, it is uniformly dispersed in base glaze using nano material, in pottery glaze firing, diffusivity is strong, be conducive to coloring agent to exist
Be uniformly distributed in pottery glaze layer, more sensitive to atmosphere in pyroreaction the features such as, the pottery product colour generation fired and color mistake
Cross more uniform, natural.
3rd, can effectively reduce glaze layer viscosity during glaze firing, reduce the defects such as the pore that pottery surface occurs, substantially increase an ancient unit of weight
The success rate that porcelain is fired.
4th, pass through to change the color of the state modulator glaze layers such as mass ratio in base glaze for the nano-sized iron oxide, firing temperature, make
Resintering pottery implements can assume series Song Jun official's enamel color such as pale blue, reddish black, sky blue, grey indigo plant.With collection Song dynasty pottery piece pair
It is respectively less than 1 than aberration, particularly the △ a and △ b value of reflection reddish blue value is all close to 0.
5th, the present invention is kiln furnace used mixes kiln using electric, can control heating rate and atmosphere well.And clean no
Pollution, when solving conventional kiln using firewood, coal or heated by natural gas, itself volatilization gas of these fuel cause to pottery
Pollution the problems such as.Process is simple, metal quality thing content are controlled, high yield rate is it is easy to produce in batches.
Brief description
Fig. 1-1, the photochrome of the fired pottery implements of embodiment 1
Fig. 1-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 1
Fig. 1-3, the fired pottery implements of embodiment 1 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is contrast collection Song Jun ceramics
Fig. 1-4, the scanning electron microscope (SEM) photograph of the fired pottery implements glaze paint of embodiment 1
Fig. 1-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 1
Fig. 2-1, the photochrome of the fired pottery implements of embodiment 2
Fig. 2-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 2
Fig. 2-3, the fired pottery implements of embodiment 2 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is contrast collection Song Jun ceramics
Fig. 2-4, the scanning electron microscope (SEM) photograph of the fired pottery implements glaze paint of embodiment 2
Fig. 2-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 2
Fig. 3-1, the photochrome of the fired pottery implements of embodiment 3
Fig. 3-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 3
Fig. 3-3, the fired pottery implements of embodiment 3 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is contrast collection Song Jun ceramics
Fig. 3-4, the scanning electron microscope (SEM) photograph of the fired pottery implements glaze paint of embodiment 3
Fig. 3-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 3
Fig. 4-1, the photochrome of the fired pottery implements of embodiment 4
Fig. 4-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 4
Fig. 4-3, the fired pottery implements of embodiment 4 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is contrast collection Song Jun ceramics
Fig. 4-4, the scanning electron microscope (SEM) photograph of the fired pottery implements glaze paint of embodiment 4
Fig. 4-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 4
Fig. 5-1, the photochrome of the fired pottery implements of embodiment 5
Fig. 5-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 5
Fig. 5-3, the fired pottery implements of embodiment 5 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is fired pottery device by contrast collection Song Jun ceramics Fig. 5-4, embodiment 5
The scanning electron microscope (SEM) photograph of thing glaze paint
Fig. 5-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 5
Fig. 6-1, the photochrome of the fired pottery implements of embodiment 6
Fig. 6-2, the photochrome enlarged drawing of the fired pottery implements of embodiment 6
Fig. 6-3, the fired pottery implements of embodiment 6 and Song dynasty pottery piece comparison diagram, wherein：The complete pottery implements in the left side are
The product that the embodiment of the present invention is fired, the relic on the right is contrast collection Song Jun ceramics
Fig. 6-4, the scanning electron microscope (SEM) photograph of the fired pottery implements glaze paint of embodiment 6
Fig. 6-5, fired pottery implements glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram of embodiment 6
Fig. 7-1, the photochrome of the fired pottery implements of comparative example 1
Fig. 7-2, the photochrome enlarged drawing of the fired pottery implements of comparative example 1
The scanning electron microscope (SEM) photograph of the pottery thing glaze paint that Fig. 7-3, comparative example 1 are fired
Pottery thing glaze paint EDS Surface scan Fe, Si, Al Elemental redistribution schematic diagram that Fig. 7-4, comparative example 1 are fired.
Specific implementation method：
Further explain how to reach the porcelain of Song Jun government porcelain kiln glaze colours and enamel by the inventive method below by example.
Embodiment 1
Preparatory work of experiment：Draw traditional type with conventional potter's clay, then through 1000 DEG C of high-temperature firing Cheng Tao, naturally cold in kiln
But, obtain biscuit.Glaze raw material prepares：Will the hard raw material such as Anhydrite, quartz, calcite used by the locality of Yuzhou carry out choosing-
Coarse crushing (using jaw crusher)-in (edge runner mill) in small, broken bits standby；Will be in small, broken bits standby in Os Bovis seu Bubali, Talcum calcining.
Base glaze preparation method：With mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc
Mixing, in addition (particle diameter is 30 nanometers to the nano-sized iron oxide of additional gross mass 0.5%, and purity is 99.9%, Shanghai paddy field
Material Science and Technology Ltd. provides), mix homogeneously, obtain mixing glaze.Base glaze raw material is had by great Song government porcelain kiln porcelain industry share
Limit company provides (seeing attached list 1).
By mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball mill, and wet ball grinding is processed, and glaze fineness crosses 160
Mesh sieve screen over-size is less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing, thickness
Control in 1mm about, enter kiln after being dried；It is fired, specially：Under the conditions of natural atmosphere room temperature start to warm up to
1050 DEG C, heating-up time 5h, then by the control to air inflow, make liquefied petroleum gas burn incompletely produce CO, control
Firing atmosphere processed then proceedes to be warming up to 1250 DEG C for reducing atmosphere, heating-up time 5h, then is warming up under the conditions of natural atmosphere
1280 DEG C, stop heating up, heating-up time 1h, natural cooling, obtain pale blue color pottery (Fig. 1-1,1-2).
Summarize：Obtained implements color is pale blue color, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E value)
It is only 0.19, with Song Jun government porcelain kiln ceramics (74S36) closely (Fig. 1-3), particularly △ a and the almost nil (table of △ b value
1), scanning electron microscope (Zeiss EVO LS-15) observes glaze layer surface texture and bubble, X-ray power spectrum (Bruker XFlash
Detector 5010) research glaze layer elemental distribution.Scanning electron microscopic observation shows that its tomography glaze paint bubble is uniformly distributed (figure
1-4), EDS Surface scan shows that its glaze paint ferrum element is uniformly distributed (Fig. 1-5) in whole glaze layer, fires successfully.
Embodiment 2
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc, additional gross mass
1.0% nano-sized iron oxide, mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired (with embodiment 1), natural cooling, obtain Celeste pottery
(Fig. 2-1,2-2).
4. summarize：Obtained implements color is Celeste, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E
Value) it is only 0.38, with Song Jun government porcelain kiln ceramics (04Y98) closely (Fig. 2-3), particularly △ a and △ b value are almost nil
(table 2), is uniformly distributed (Fig. 2-4) with its tomography glaze paint bubble of scanning electron microscopic observation, EDS Surface scan shows its glaze paint ferrum unit
Element is uniformly distributed in whole glaze layer, and iron content increases (2-5), fires successfully.
Embodiment 3
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc, additional gross mass
1.5% nano-sized iron oxide, mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired (with embodiment 1), natural cooling, obtain sky blue pottery
(Fig. 3-1,3-2).
4. summarize：Obtained implements color is sky blue, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E
Value) it is only 0.05, with Song Jun government porcelain kiln ceramics (74S71) closely (Fig. 3-3), particularly △ a and △ b value are almost nil
(table 3), is uniformly distributed (Fig. 3-4) with its tomography glaze paint bubble of scanning electron microscopic observation, EDS Surface scan shows its glaze paint ferrum unit
Element is uniformly distributed in whole glaze layer, and iron content substantially increases (Fig. 3-5), fires successfully.
Embodiment 4
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc, additional gross mass
1.5% nano-sized iron oxide, mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired, specially：Under the conditions of natural atmosphere room temperature start to warm up to
1050 ± 10 DEG C, heating-up time 5h, then by the control to air inflow, so that liquefied petroleum gas burn incompletely is produced
CO, controls firing atmosphere to then proceed to be warming up to 1240 DEG C for reducing atmosphere, heating-up time 5h, then under the conditions of natural atmosphere
It is warming up to 1260 DEG C, stop heating up, heating-up time 0.5h, natural cooling, obtain sky blue pottery (Fig. 4-Isosorbide-5-Nitrae-2).
4. summarize：Obtained implements color is sky blue, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E
Value) it is only 0.33, with Song Jun government porcelain kiln ceramics (04Y05) closely (Fig. 4-3), particularly △ a and △ b value are almost nil
(table 4), is uniformly distributed (Fig. 4-4) with its tomography glaze paint bubble of scanning electron microscopic observation, EDS Surface scan shows its glaze paint ferrum unit
Element is uniformly distributed (Fig. 4-5) in whole glaze layer, fires successfully.
Embodiment 5
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 59% Anhydrite, 30% quartz, 10% calcite, 1% Os Bovis seu Bubali ash, additional gross mass 1.5%
Nano-sized iron oxide, mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired (with embodiment 1), specially：Room temperature under the conditions of natural atmosphere
Start to warm up to 1050 ± 10 DEG C, heating-up time 4h, then by the control to air inflow, make liquefied petroleum gas burn incompletely
To produce CO, to control firing atmosphere to then proceed to be warming up to 1250 ± 10 DEG C for reducing atmosphere, heating-up time 6h, then in nature
It is warming up to 1280 DEG C under atmospheric condition, stop heating up, heating-up time 1h, natural cooling, natural cooling, obtain sky blue an ancient unit of weight
Porcelain (Fig. 5-1,5-2).
4. summarize：Obtained implements color is sky blue, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E
Value) it is only 0.61, with Song Jun government porcelain kiln ceramics (04J125) closely (Fig. 5-3), particularly △ a and △ b value are almost
Zero (table 5), is uniformly distributed with its tomography glaze paint bubble of scanning electron microscopic observation, EDS Surface scan shows its glaze paint ferrum element whole
Individual glaze layer is uniformly distributed (Fig. 5-4,5-5), fires successfully.
Embodiment 6
Numbering 2015040906
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc, additional gross mass
2.0% nano-sized iron oxide, altogether 102.0%, mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired (with embodiment 1), natural cooling, obtain dusty blue pottery
(Fig. 6-1,6-2).
4. summarize：Obtained implements color is dusty blue, and uniformly, spectrophotometric color measurement instrument result shows color development：Aberration (△ E
Value) it is 0.96, with Song Jun government porcelain kiln ceramics (04J94) closely (Fig. 6-3), particularly △ a and △ b value are almost nil
(table 6), is uniformly distributed with its tomography glaze paint bubble of scanning electron microscopic observation, EDS Surface scan shows its glaze paint ferrum element whole
Glaze layer is uniformly distributed, and iron content increases (Fig. 6-4,6-5), fires successfully.
Embodiment 7
Substantially the same manner as Example 1, the nano-sized iron oxide that simply additional nano-sized iron oxide is 80 nanometers for particle diameter.Its
Implements color obtained by firing is pale blue color, and uniformly, with Song Jun government porcelain kiln ceramics (74S36) closely, scanning is electric for color development
Sem observation shows that its tomography glaze paint bubble is uniformly distributed, and EDS Surface scan shows that its glaze paint ferrum element is uniformly distributed in whole glaze layer,
Fire successfully.
Comparative example 1
1. Preparatory work of experiment：With embodiment 1.
2. with mass percent, by 65% Anhydrite, 15% quartz, 15% calcite, 5% calcination of talc, altogether 100.0%,
Mix homogeneously.
3. press mixing glaze：Ball：Water=1:1.5:0.7 mass ratio, adds ball milling, and wet ball grinding is processed, glaze fineness mistake
180 mesh sieve screen over-sizes are less than 0.06wt%, and glaze slip water content control is in 45wt%.By the biscuit calcined with dipping in glaze method glazing,
THICKNESS CONTROL, in 1mm, enters kiln after being dried and is fired, specially：Under the conditions of natural atmosphere room temperature start to warm up to
1050 DEG C, heating-up time 5h, then by the control to air inflow, make liquefied petroleum gas burn incompletely produce CO, control
Firing atmosphere processed then proceedes to be warming up to 1250 DEG C for reducing atmosphere, heating-up time 5h, then is warming up under the conditions of natural atmosphere
1280 DEG C, stop heating up, heating-up time 1h, natural cooling, obtain being not added with nano-sized iron oxide clear frit pottery (Fig. 7-
1,7-2).
4. summarize：Obtained implements be clear frit pottery, with its tomography glaze paint bubble distribution of scanning electron microscopic observation uneven,
EDS Surface scan shows that its glaze paint does not contain ferrum element (Fig. 7-3,7-4).
In sum：Nano-sized iron oxide plays main quality effect during Song Jun official's porcelain is imitated and burnt, with nano-sized iron oxide in glaze
The increase of content, pottery glaze colours is gradually deepened.By controlling mass ratio in base glaze for the nano-sized iron oxide, firing temperature etc.
Parameter, successfully burns out serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain products with glaze colours such as pale blue, reddish black, sky blue, grey indigo plants, with the collection Song dynasty
Pottery piece compared colour difference (△ E value) is respectively less than 1 (note：In GB/T 3532-2009 household china aberration be less than or equal to 1 for excellent
Deng product)., all close to 0, resintering is successfully for the △ a and △ b value of particularly reflection reddish blue value.With scanning electron microscopic observation tomography glaze paint
Bubble distribution is uniform, EDS power spectrum shows that its ferrum element is uniformly distributed in whole glaze layer.
Subordinate list 1：Parent glaze raw material chemical composition used by the embodiment of the present invention
Subordinate list 2：Embodiment 1 sample and collection Song Jun ceramics 74S36 color contrast
Subordinate list 3：Embodiment 2 sample and collection Song Jun ceramics 04Y98 color contrast
Subordinate list 4：Embodiment 3 sample and collection Song Jun ceramics 74S71 color contrast
Subordinate list 5：Embodiment 4 sample and collection Song Jun ceramics 04Y05 color contrast
Subordinate list 6：Embodiment 5 sample and collection Song Jun ceramics 04J125 color contrast
Subordinate list 7：Embodiment 6 sample and collection Song Jun ceramics 04J94 color contrast
Note：L* lightness index (luminance axis), represents black and white, and 0 is black, and 100 is white, is Lycoperdon polymorphum Vitt between 0-100.
A* chromaticity index (red green axle), on the occasion of for redness, negative value is green.
B* chromaticity index (champac axle), on the occasion of for yellow, negative value is blueness.
Δ L=L* (embodiment)-L* (contrast collection Song Jun ceramics).
Δ a=a* (embodiment)-a* (contrast collection Song Jun ceramics).
Δ b=b* (embodiment)-b* (contrast collection Song Jun ceramics).
Δ E is the size of total color difference.
Claims (10)
1. a kind of resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze：It is characterized in that：Add the nano oxidized iron material of 0.5wt%～2.0wt% in base glaze, fire imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain.
2. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 1：It is characterized in that：After nano oxidized iron material dispersed acquisition nano-sized iron oxide glaze in base glaze, fired in idiosome surface glazing by way of once dipping in glaze.
3. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 1：It is characterized in that：The firing atmosphere in more than 1000-1060 DEG C and less than 1240-1260 DEG C of baking temperature range interval is controlled to be reducing atmosphere in intensification sintering procedure.
4. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 3：It is characterized in that：The firing time keeping reducing atmosphere in intensification sintering procedure is 5-6h.
5. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 1 or 3：It is characterized in that：Described fire for：When being warming up to 1000-1060 DEG C under the conditions of natural atmosphere, control climate is then heated to 1240-1260 DEG C for reducing atmosphere, continue intensification afterwards again under the conditions of natural atmosphere and carry out abundant vitreous process, Temperature fall can obtain imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain products.
6. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 5：It is characterized in that：The described time being warming up to 1000-1060 DEG C is 3-5h.
7. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 5：It is characterized in that：Described vitreous is processed as under the conditions of natural atmosphere being continuously heating to 1260-1280 DEG C, carries out vitreous process in this temperature-rise period.
8. the resintering method firing imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain based on nano-sized iron oxide glaze according to claim 5：It is characterized in that：Described vitreous process time is 0.5-1h.
9. serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain of being fired based on nano-sized iron oxide glaze it is characterised in that：It is being prepared based on the resintering method that nano-sized iron oxide glaze fires imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain described in any claim in claim 1-8.
10. according to claim 9 series imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain it is characterised in that：Described serial imitation Song-Dynasty-style typeface an ancient unit of weight official's porcelain color transition is uniformly natural, colour generation is uniform, and colour generation has pale blue, reddish black, sky blue, grey blue series, and in tomography glaze paint, uniformly, ferrum element is uniformly distributed bubble distribution in whole glaze layer.
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