CN105130502A - Method for firing photochromic jun porcelain under oxidizing atmosphere condition - Google Patents
Method for firing photochromic jun porcelain under oxidizing atmosphere condition Download PDFInfo
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Abstract
The invention provides a method for firing photochromic jun porcelain under an oxidizing atmosphere condition. The method is characterized in that micro-nano materials are added to serve as additives, and the jun porcelain with the photochromic effect is fired in the oxidizing atmosphere at the condition of 1,260 DEG C to 1,300 DEG C. The micro-nano material additives are micro-nano silicate, and the mass of the micro-nano silicate is 5% to 30% of the mass of an enamel layer. The color-change micro-nano silicate is prepared with an in-situ solid-phase reaction method, the preparing temperature ranges from 1,300 DEG C to 1,400 DEG C, and the particle size of the micro-nano silicate ranges from 0.5 micrometer to 5 micrometers. The micro-nano silicate is neodymium silicate, and the chemical formula is M2Nd8(SiO4)6O2, wherein M is calcium elements or strontium elements or barium elements.
Description
Invention field
The invention belongs to silicate ceramics field, relate to a kind of method firing photochromic pottery under oxidizing atmosphere condition.
Technical background
Pottery, as first of Song dynasty five your name's porcelain, has splendid sight and reserve value.Deep artistic expressions such as " transmutation ", " hacking " and " opalescence " of its uniqueness and deeply liking by Song dynasty imperial palace, archaism has " there is wealth ten thousand strings of cash in family, not as pottery a slice ".But after the Song dynasty is destroyed, the development of pottery is almost sluggish, until Qing Dynasty's pottery is just restored, reenters the visual field of people.Arrived founding of New, pottery industry obtains vigorous growth; In recent years, pottery is constantly sent using the identity of the rarity of state by as state's gift.
Research shows, " transmutation ", " opalescence " and " hacking " of pottery is inseparable with the colorant content in its glaze, glaze firing technique gentle body atmosphere etc.In recent decades, domestic and international many ceramic research persons, by modern analysis and test method, have extensively studied the impact on pottery enamel such as different colorant, atmosphere and glaze layer microstructure morphology, and have inquired into transmutation mechanism further.Such as, the cobalt blue adding trace in glaze, as tinting material, can obtain reddish black or sky blue pottery under oxidizing atmosphere; Pottery is made to present redness because the cupric oxide in glaze is partially reduced for Red copper oxide under reducing atmosphere.
In recent years, along with the raising of people's living standard and the develop rapidly of science and technology, traditional pottery colour generation and the change of moulding can not meet the requirement of pottery fan far away.For this reason, the pottery product of development of new functionalization can promote further developing of pottery and even whole ceramic industry energetically.
Summary of the invention
The object of this invention is to provide and a kind ofly under oxidizing atmosphere condition, burn out the technique with photochromic effect pottery product.
Realize the technical scheme of the object of the invention: a kind of method firing variable color pottery, is characterized in that, additional a kind of micro Nano material makes additive, fires the pottery with photochromic effect under oxidizing atmosphere.
The present invention's additive used is a kind of micro nanometer silicon hydrochlorate, and micro nanometer silicon hydrochlorate amount accounts for the 5%-30% of glaze layer quality proportion.
The micro nanometer silicon hydrochlorate that the present invention is used, adopt the preparation of original position solid reaction process, preparation temperature is 1300-1400 DEG C, and its particle diameter is at 0.5-5 micron.
The present invention's micro nanometer silicon hydrochlorate used is a kind of silicon neodymate, and chemical formula is M
2nd
8(SiO
4)
6o
2, wherein M is calcium, strontium and barium divalent metal element.
The present invention's kiln used is retort furnace, and temperature of glaze firing is 1260-1300 DEG C, and the atmosphere of employing is air, avoids the pollution of industrial reduction kiln to environment and the waste of the energy.
Variable color powder preparation: adopt original position solid reaction process preparative chemistry formula to be Ca
2nd
8(SiO
4)
6o
2silicon neodymium acid calcium powder; Weigh calcium carbonate, Neodymium trioxide and silicon-dioxide respectively according to stoichiometric ratio, the raw material after weighing put into agate mortar, adds a small amount of dehydrated alcohol, clockwise with alternately grind 30min counterclockwise, make it fully mix; Put into air dry oven, design temperature is 120 DEG C, dry 3h; Take out dried powder, again adopt aforesaid way to grind one time, for subsequent use after dry; Mixed raw material is loaded corundum crucible and puts into retort furnace, temperature rise rate 5 DEG C/min, sintering temperature 1350 DEG C, insulation 30min, then furnace cooling, prepare required variable color silicon neodymate powder;
Variable color pottery preparation process: according to account for glaze mass ratio be 20% silicon neodymate powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1300 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.
The present invention pottery embryo used is provided by Xuchang pottery research institute of China, and glaze is an ancient unit of weight glaze base glaze.
The present invention's analytical test means used: adopt x-ray diffractometer to analyze crystal thing phase composite after the thing phase composite of micro nanometer silicon hydrochlorate prepared by original position solid state reaction and glaze firing in glaze layer; Utilize scanning electronic microscope mirror study micro nanometer silicon hydrochlorate and glaze layer section microscopic appearance, in conjunction with the Elemental redistribution of different loci in X-ray energy spectrum research glaze layer.
Accompanying drawing explanation
Fig. 1-1, embodiment 1 to fire variable color silicon neodymium acid calcium powder color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions;
Fig. 1-2, embodiment 1 fire the XRD diffracting spectrum that variable color silicon neodymium acid calcium powder XRD analysis figure: a is prepared silicon neodymium acid calcium powder; B is standard P DF card collection of illustrative plates;
Fig. 1-3, embodiment 1 fire variable color silicon neodymium acid calcium powder microscopic appearance figure;
Fig. 1-4, embodiment 1 to fire variable color pottery color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions;
Glaze layer section microscopic appearance figure under the low magnification condition of Fig. 1-5, embodiment 1;
Glaze layer section microscopic appearance figure and energy spectrum analysis under Fig. 1-6, embodiment 1 high-amplification-factor condition;
Fig. 1-7, embodiment 1 glaze layer powder XRD analysis figure: a are the XRD diffracting spectrum of glaze layer powder; B is standard P DF card collection of illustrative plates;
Fig. 2-1, embodiment 2 to fire variable color pottery color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions;
Fig. 3-1, embodiment 3 to fire variable color pottery test piece color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions;
Silicon neodymium acid strontium powder color changeable effect figure: a that Fig. 4-1, embodiment 4 are fired is under indoor daylight lamp condition; B is under sunlight conditions;
XRD analysis figure: a of the silicon neodymium acid strontium powder that Fig. 4-2, embodiment 4 are fired is the XRD diffracting spectrum of prepared silicon neodymium acid strontium powder; B is standard P DF card collection of illustrative plates;
Fig. 4-3, embodiment 4 to fire variable color pottery color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions;
Fig. 5-1, embodiment 5 to fire variable color pottery color changeable effect figure: a be under indoor daylight lamp condition; B is under sunlight conditions.
Embodiment
Further illustrate how under oxidizing atmosphere condition, to fire the pottery with color changeable effect by additional micro nanometer silicon hydrochlorate below by embodiment.
Plant the method firing variable color pottery, it is characterized in that, additional a kind of micro Nano material makes additive, fires the pottery with photochromic effect under oxidizing atmosphere.
The present invention's additive used is a kind of micro nanometer silicon hydrochlorate, and micro nanometer silicon hydrochlorate amount accounts for the 5%-30% of glaze layer quality proportion.
The micro nanometer silicon hydrochlorate that the present invention is used, adopt the preparation of original position solid reaction process, preparation temperature is 1300-1400 DEG C, and its particle diameter is at 0.5-5 micron.
The present invention's micro nanometer silicon hydrochlorate used is a kind of silicon neodymate, and chemical formula is M
2nd
8(SiO
4)
6o
2, wherein M is calcium, strontium and barium divalent metal element.
The present invention's kiln used is retort furnace, and temperature of glaze firing is 1260-1300 DEG C, and the atmosphere of employing is air, avoids the pollution of industrial reduction kiln to environment and the waste of the energy.
embodiment 1
1. variable color powder preparation: adopt original position solid reaction process preparative chemistry formula to be Ca
2nd
8(SiO
4)
6o
2silicon neodymium acid calcium powder.Weigh calcium carbonate, Neodymium trioxide and silicon-dioxide respectively according to stoichiometric ratio, the raw material after weighing put into agate mortar, adds a small amount of dehydrated alcohol, clockwise with alternately grind 30min counterclockwise, make it fully mix; Put into air dry oven, design temperature is 120 DEG C, dry 3h; Take out dried powder, again adopt aforesaid way to grind one time, for subsequent use after dry.Mixed raw material is loaded corundum crucible and puts into retort furnace, temperature rise rate 5 DEG C/min, sintering temperature 1350 DEG C, insulation 30min, then furnace cooling, prepare required variable color silicon neodymate powder.The variable color silicon neodymium acid calcium powder color changeable effect figure prepared under this condition is shown in Fig. 1-1; Silicon neodymium acid calcium powder XRD analysis figure is shown in Fig. 1-2; Silicon neodymium acid calcium powder SEM microscopic appearance figure is shown in Fig. 1-3.
2. variable color pottery preparation process: according to account for glaze mass ratio be 20% silicon neodymate powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1300 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.The variable color pottery test piece color changeable effect prepared under this condition is shown in Fig. 1-4; Fig. 1-5 is shown in glaze layer section SEM microanalysis; Glaze layer powder XRD analysis is shown in Fig. 1-6.
3. this case summary: from Fig. 1-1, the silicon neodymium acid calcium powder prepared under this example condition has obvious color changeable effect, for blue under indoor do not have sunlit condition, having in sunlit situation for purple, XRD and the SEM microanalysis of combining powder is known, and the powder prepared under this condition is Ca
2nd
8(SiO
4)
6o
2, particle diameter is at 0.5-2 micron; From Fig. 1-4, the variable color pottery prepared under this example condition has obvious color changeable effect, under indoor do not have sunlit condition, glaze layer is for blue, having for glaze layer is purple in sunlit situation, scheming from the SEM of glaze layer section, there is particle diameter in glaze layer is the large small-crystalline of 0.5-2 micron, analyze known in conjunction with EDX, having, the site neodymium content of tiny crystals is high, and from the XRD of glaze layer analysis, the crystalline component in glaze layer is Ca
2nd
8(SiO
4)
6o
2; Comprehensive analysis is known, the variable color powder adopting this condition to prepare can after glaze firing stable existence in an ancient unit of weight enamel layer, color changeable effect is mainly by being add prepared variable color powder to cause.
embodiment 2
1. variable color powder preparation: with embodiment 1.
2. variable color pottery preparation process: according to account for glaze mass ratio be 15% silicon neodymium acid calcium powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1280 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.The variable color pottery test piece color changeable effect prepared under this condition is shown in Fig. 2-1.
3. this case summary: from Fig. 2-1, the pottery product color changeable effect prepared under this example condition is obvious.
implement profit 3
1. variable color powder preparation: with embodiment 1.
2. variable color pottery preparation process: according to account for glaze mass ratio be 25% silicon neodymate powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1280 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.The variable color pottery product color changeable effect prepared under this condition is shown in Fig. 3-1.
3. this case summary: from Fig. 3-1, the pottery product color changeable effect prepared under this example condition is obvious.
implement profit 4
1. variable color powder preparation: adopt original position solid reaction process preparative chemistry formula to be Sr
2nd
8(SiO
4)
6o
2silicon neodymium acid strontium powder.Weigh Strontium carbonate powder, Neodymium trioxide and silicon-dioxide respectively according to stoichiometric ratio, the raw material after weighing put into agate mortar, adds a small amount of dehydrated alcohol, clockwise with alternately grind 30min counterclockwise, make it fully mix; Put into air dry oven, design temperature is 120 DEG C, dry 3h; Take out dried powder, again adopt aforesaid way to grind one time, for subsequent use after dry.Mixed raw material loaded corundum crucible and puts into retort furnace, temperature rise rate 5 DEG C/min, sintering temperature 1350 DEG C, insulation 30min, then furnace cooling, preparing required variable color silicon neodymium acid strontium powder.The variable color silicon neodymium acid strontium powder color changeable effect figure prepared under this condition is shown in Fig. 4-1; Silicon neodymium acid strontium powder XRD analysis figure is shown in Fig. 4-2.
2. variable color pottery preparation process: according to account for glaze mass ratio be 20% silicon neodymium acid strontium powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stirs 60min and makes it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1280 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.The variable color pottery test piece color changeable effect prepared under this condition is shown in Fig. 4-3.
3. this case summary: from Fig. 4-1, the silicon neodymium prepared under this example condition acid strontium powder has obvious color changeable effect, for blue under indoor do not have sunlit condition, is purple having in sunlit situation; From Fig. 4-3, the variable color pottery prepared under this example condition has obvious color changeable effect, and under indoor do not have sunlit condition, glaze layer is for blue, is purple there being glaze layer in sunlit situation.
implement profit 5
1. variable color powder preparation: with embodiment 4.
2. variable color pottery preparation process: according to account for glaze mass ratio be 30% silicon neodymate powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1280 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.The variable color pottery product color changeable effect prepared under this condition is shown in Fig. 5-1.
3. this case summary: from Fig. 5-1, the pottery product color changeable effect prepared under this example condition is obvious, and bubble appears in surface.
Claims (5)
1. fire a method for photochromic pottery, it is characterized in that, additional a kind of micro Nano material makes additive, fires the pottery with photochromic effect under oxidizing atmosphere.
2. a kind of method firing variable color pottery as claimed in claim 1, it is characterized in that, described additive is a kind of micro nanometer silicon hydrochlorate, and micro nanometer silicon hydrochlorate amount accounts for the 5%-30% of glaze layer quality proportion.
3. a kind of method firing variable color pottery as claimed in claim 2, is characterized in that, micro nanometer silicon hydrochlorate used, and adopt the preparation of original position solid reaction process, preparation temperature is 1300-1400 DEG C, and its particle diameter is at 0.5-5 micron.
4. a kind of method firing variable color pottery as claimed in claim 2, it is characterized in that, micro nanometer silicon hydrochlorate used is a kind of silicon neodymate, and chemical formula is M
2nd
8(SiO
4)
6o
2, wherein M is calcium, strontium and barium element.
5. a kind of method firing variable color pottery as claimed in claim 1, is characterized in that, variable color powder preparation: adopt original position solid reaction process preparative chemistry formula to be Ca
2nd
8(SiO
4)
6o
2silicon neodymium acid calcium powder; Weigh calcium carbonate, Neodymium trioxide and silicon-dioxide respectively according to stoichiometric ratio, the raw material after weighing put into agate mortar, adds a small amount of dehydrated alcohol, clockwise with alternately grind 30min counterclockwise, make it fully mix; Put into air dry oven, design temperature is 120 DEG C, dry 3h; Take out dried powder, again adopt aforesaid way to grind one time, for subsequent use after dry; Mixed raw material is loaded corundum crucible and puts into retort furnace, temperature rise rate 5 DEG C/min, sintering temperature 1350 DEG C, insulation 30min, then furnace cooling, prepare required variable color silicon neodymate powder; Variable color pottery preparation process: according to account for glaze mass ratio be 20% silicon neodymate powder join in pottery matrix glaze, adopt constant-temperature heating magnetic stirring apparatus, setting speed is 500r/min, stir 60min make it be uniformly distributed in glaze; By leaching glaze mode, the glaze mixed is coated on biscuit; Spent the night by natural air drying after glazing completes, moisture in glaze layer is fully evaporated; Put into retort furnace, setting temperature rise rate 3 DEG C/min, temperature of glaze firing is at 1300 DEG C, and insulation 20min, then furnace cooling, obtain variable color pottery product.
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Cited By (5)
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| CN106396388A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Lead and cadmium free low temperature frit and preparation method thereof |
| CN106396394A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Ecological ceramic tile and preparation method thereof |
| CN106396391A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Photochromic lead and cadmium free low temperature frit and preparation method thereof |
| CN109052950A (en) * | 2018-09-30 | 2018-12-21 | 李文文 | A kind of pottery sky blue glaze and preparation method thereof |
| CN112299717A (en) * | 2020-12-02 | 2021-02-02 | 禹州市华艺钧瓷文化传媒有限公司 | Photochromic jun porcelain glaze and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106396388A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Lead and cadmium free low temperature frit and preparation method thereof |
| CN106396394A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Ecological ceramic tile and preparation method thereof |
| CN106396391A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区诚睿基科技有限公司 | Photochromic lead and cadmium free low temperature frit and preparation method thereof |
| CN109052950A (en) * | 2018-09-30 | 2018-12-21 | 李文文 | A kind of pottery sky blue glaze and preparation method thereof |
| CN112299717A (en) * | 2020-12-02 | 2021-02-02 | 禹州市华艺钧瓷文化传媒有限公司 | Photochromic jun porcelain glaze and preparation method thereof |
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