CN103274765A - Co-Zn-Cr-Al composite spinel type blue ceramic pigment and preparation method thereof - Google Patents
Co-Zn-Cr-Al composite spinel type blue ceramic pigment and preparation method thereof Download PDFInfo
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- CN103274765A CN103274765A CN2013102139067A CN201310213906A CN103274765A CN 103274765 A CN103274765 A CN 103274765A CN 2013102139067 A CN2013102139067 A CN 2013102139067A CN 201310213906 A CN201310213906 A CN 201310213906A CN 103274765 A CN103274765 A CN 103274765A
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Abstract
The invention discloses a Co-Zn-Cr-Al composite spinel type blue ceramic pigment which is expressed by a general formula (CoxZn1-x)(CryAl1-y)2O4, wherein x and y represents mole fractions; x is 0-1; y is 0-1; and when x and y are different in value, the products are different in color. Besides, the invention also discloses a preparation method of the Co-Zn-Cr-Al composite spinel type blue ceramic pigment. The ceramic pigment disclosed by the invention is small in particle size and uniform in distribution, has high coloration capability in glaze, and is high in coloration stability. Besides, the ceramic pigment is simple in preparation process and controllable in color and shape, and can meet different application requirements; and the whole process is easy to control and realize, and the product quality is stable, thereby being beneficial to large-scale popularization and application.
Description
Technical field
The present invention relates to ceramic pigment glaze technical field, relate in particular to a kind of Co-Zn-Cr-Al composite spinelle type blue ceramic colorant and preparation method thereof.
Background technology
Ceramic pigment refers to " coloured material " that use in Production of Ceramics, contained multiple concepts such as toner (tinting material), color base, pigment, colorant and color material, in order to decorating ceramic articles.Through thing mutually and structural analysis, these coloured materials all are to be the color development element with some transition metal, rare earth metal or other metals, with some mineral crystal formation for carrying the painted mineral of look parent.Common ceramic pigment type mainly contains: simple compounds type, Solid solution-oxide type, spinel type, silicate-type and mixing xenocryst type.
The use of ceramic pigment just begins far away from China's period of late Neolithic, the redness above the faience at that time, and the ground hematite that will contain the red clay of a large amount of ferric oxide or earthy directly is coated in pottery biscuit surface and burns till.The color of merchant Zhou Yihou ceramic ware is more various: the green glaze that has occurred dodging silver-colored light on the Chinese of Han dynasty is made pottery; Famous tri-coloured glazed pottery has not only used iron, copper compound to be coloured to yellow and green, also utilized to contain the cobalt material and obtain blueness, Song Hongcai, Wanli year the five colours, Kangxu's five colours and Doucai contrasting colors etc. redness etc.Rise along with development of modern science and technology and chemical industry, ceramic pigment has also had breakthrough progress, many novel synthetic colorants have been developed, for example spinel type, trichroite type, celsian-felspar type, mullite-type and diopside type etc., and having dropped into batch process, prospect is very wide.Wherein, the spinel type colorant has higher thermostability, chemical stability with it, and tinting strength strong, can be mixed and made into compound colorant with most of ceramic pigments, and be considered to a kind of good ceramic pigment.At present, ceramic pigment mainly be towards improve quality, improve tinting strength and stability, direction such as increase varieties and designs develops.
The raising of the colour generation of ceramic pigment and quality and performance, not only relevant with its prescription composition, and also relevant with the preparation method of colorant.At present, the preparation method of prior art ceramic pigment mainly contains: solid sintering technology, sol-gel method, the precipitator method.Wherein, sol-gel and precipitator method complicated operation, preparation cycle is long, productive rate is low, is difficult to mass production; Solid sintering technology preparation technology is simple relatively, but gained colorant granularity is big, can not be applied to technology such as ceramic ink jet printing decoration, is difficult to satisfy the demand that ceramic pigment is used and developed.How to obtain being ceramic pigment colour-stable, excellent performance, and realize easily that in preparation technology colour generation, form are controlled, thereby satisfy different application demands, remain problem that those skilled in the art are devoted to solve and the direction of researchdevelopment.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of color development stable, the controlled Co-Zn-Cr-Al composite spinelle type blue ceramic colorant of colour generation.Another object of the present invention is to provide the preparation method of above-mentioned ceramic pigment, improving the quality of products, and realize the simple and easy controlled of prescription, thereby satisfy different application demands.
Purpose of the present invention is achieved by the following technical programs:
A kind of Co-Zn-Cr-Al composite spinelle type blue ceramic colorant provided by the invention is by general formula (Co
xZn
1-x) (Cr
yAl
1-y)
2O
4Express, wherein x, y represent molar fraction, x=0～1, y=0～1.Preferably, x=0.25～0.75, y=0.25～0.75.The value difference of ceramic pigment x of the present invention, y, the colour generation of product are then different.
Further, ceramic pigment of the present invention adopts salt hydrotropy liquid combustion method synthetic, is oxygenant with Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate, and dissolved organic matter is fuel and reductive agent, and the inertia soluble salt is auxiliary agent; Particularly, described dissolved organic matter is sucrose, citric acid or ethylene glycol.Be example with sucrose, its chemical equation is as follows:
6xCo(NO
3)
2+6(1-x)Zn(NO
3)
2+12yAl(NO
3)
3+12(1-y)Cr(NO
3)
3+5C
12H
22O
11
→6(Co
xZn
1-x)(Al
yCr
1-y)
2O
4+24N
2+60CO
2+55H
2O
In the such scheme, Xiao Suangu of the present invention, zinc nitrate, chromium nitrate, aluminum nitrate are introduced by stoichiometric ratio separately respectively, and dissolved organic matter is introduced by 100～150wt% of its stoichiometric ratio, and the inertia soluble salt is by (Co
xZn
1-x) (Cr
yAl
1-y)
2O
430～50wt% of theoretical resultant quantity introduces.The inertia soluble salt adopts the muriate of water-soluble basic metal or alkaline-earth metal, as sodium-chlor etc.
Another object of the present invention is achieved by the following technical programs:
The preparation method of above-mentioned Co-Zn-Cr-Al composite spinelle type blue ceramic colorant provided by the invention may further comprise the steps:
(1) take by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio, dissolved organic matter is sucrose, and citric acid or ethylene glycol are introduced by 100～150wt% of its stoichiometric ratio, and the inertia soluble salt is by (Co
xZn
1-x) (Cr
yAl
1-y)
2O
430～50wt% of theoretical resultant quantity introduces; Described each raw material is dissolved in the distilled water, mixes and obtain mixing solutions;
(2) with described mixing solutions in retort furnace under 400～600 ℃ of temperature ignition combustion, burning back insulation 5～15min obtains the product presoma;
(3) with described product presoma at 1100～1200 ℃ of temperature lower calcinations, the insulation 30～60min obtain product;
(4) will get product after described product washing, the drying.
Further, Co in the described step of preparation method of the present invention (1) mixing solutions
2++ Zn
2+Ionic concn is 0.3～0.5mol/L.
The present invention has following beneficial effect:
(1) the present invention passes through to regulate the amount (changing the value of y) of amount (changing the value of x), aluminum ion and the chromium ion of zine ion and cobalt ion, the colour generation of adjustable product, thus satisfy different application demands.
(2) (the Co of the present invention's preparation
xZn
1-x) (Cr
yAl
1-y)
2O
4Composite spinelle type colorant, granularity is little and be uniformly dispersed, colour generation is bright-coloured; Color development power is strong in glaze, and color development is stable.
(3) preparation technology of the present invention is simple, and colour generation, form are controlled, and whole process is easy to control and realizes, is conducive to large-scale promotion and application.
The present invention is described in further detail below in conjunction with embodiment.
Embodiment
The embodiment of the invention is oxygenant with Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate, and sucrose is fuel and reductive agent, and sodium-chlor is auxiliary agent; Carry out according to following chemical equation and obtain (Co
xZn
1-x) (Cr
yAl
1-y)
2O
4Product:
6xCo(NO
3)
2+6(1-x)Zn(NO
3)
2+12yAl(NO
3)
3+12(1-y)Cr(NO
3)
3+5C
12H
22O
11
→6(Co
xZn
1-x)(Al
yCr
1-y)
2O
4+24N
2+60CO
2+55H
2O
X, the y value of various embodiments of the present invention general formula (or reaction formula) are as shown in table 1.
The formulation parameter of table 1 various embodiments of the present invention composite spinelle type ceramic pigment
| Embodiment | x | y |
| Embodiment one | 0.5 | 0.5 |
| Embodiment two | 0.25 | 0.5 |
| Embodiment three | 1/3 | 0.5 |
| Embodiment four | 2/3 | 0.5 |
| Embodiment five | 0.75 | 0.5 |
| Embodiment six | 0.5 | 0.25 |
| Embodiment seven | 0.5 | 1/3 |
| Embodiment eight | 0.5 | 2/3 |
| Embodiment nine | 0.5 | 0.75 |
Embodiment one:
Present embodiment (Co
0.5Zn
0.5) (Cr
0.5Al
0.5)
2O
4The preparation method of composite spinelle type blue ceramic colorant, its step is as follows:
(1) according to the parameter in above-mentioned chemical equation and the table 1, take by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio, sucrose is by the 150wt% weighing of its stoichiometric ratio, and sodium-chlor is by (Co
0.5Zn
0.5) (Cr
0.5Al
0.5)
2O
4The 50wt% weighing of theoretical resultant quantity; Each raw material is dissolved in the distilled water, and magnetic agitation 60min mixes, Co in the mixing solutions
2++ Zn
2+Ionic concn is 0.3mol/L;
(2) above-mentioned mixing solutions is placed heat-resisting crucible, in retort furnace under 500 ℃ of temperature ignition combustion, burning back insulation 10min obtains the product presoma;
(3) above-mentioned product presoma is incubated 30min at 1200 ℃ of temperature lower calcinations, and furnace cooling obtains product;
(4) above-mentioned product is used distilled water, washing with alcohol successively, namely gets product after the drying.
Embodiment two:
Present embodiment (Co
0.25Zn
0.75) (Cr
0.5Al
0.5)
2O
4The preparation method of composite spinelle type blue ceramic colorant, its step is as follows:
(1) according to the parameter in above-mentioned chemical equation and the table 1, take by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio, sucrose is by its 125wt% weighing by stoichiometric ratio, and sodium-chlor is by (Co
0.25Zn
0.75) (Cr
0.5Al
0.5)
2O
4The 30wt% weighing of theoretical resultant quantity; Each raw material is dissolved in the distilled water, and magnetic agitation 45min mixes, Co in the mixing solutions
2++ Zn
2+Ionic concn is 0.4mol/L;
(2) above-mentioned mixing solutions is placed heat-resisting crucible, in retort furnace under 400 ℃ of temperature ignition combustion, burning back insulation 15min obtains the product presoma;
(3) above-mentioned product presoma is incubated 45min at 1200 ℃ of temperature lower calcinations, and furnace cooling obtains product;
(4) above-mentioned product is used distilled water, washing with alcohol successively, namely gets product after the drying.
Embodiment three:
Present embodiment (Co
1/3Zn
2/3) (Cr
0.5Al
0.5)
2O
4The preparation method of composite spinelle type blue ceramic colorant is with embodiment one difference:
In the step (1), each raw material is dissolved in the distilled water, magnetic agitation 30min mixes, in the mixing solutions
Co
2++ Zn
2+Ionic concn is at the 0.5mol/L constant volume;
In the step (3), the product presoma is incubated 60min at 1150 ℃ of temperature lower calcinations, and furnace cooling obtains product.
Embodiment four:
Present embodiment (Co
2/3Zn
1/3) (Cr
0.5Al
0.5)
2O
4The preparation method of composite spinelle type blue ceramic colorant, its step is as follows:
(1) according to the parameter in above-mentioned chemical equation and the table 1, take by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio, sucrose is by its 100 wt% weighings by stoichiometric ratio, and sodium-chlor is by (Co
2/3Zn
1/3) (Cr
0.5Al
0.5)
2O
440 wt% weighings of theoretical resultant quantity; Each raw material is dissolved in the distilled water, and magnetic agitation 30min mixes, Co in the mixing solutions
2++ Zn
2+Ionic concn is 0.3mol/L;
(2) above-mentioned mixing solutions is placed heat-resisting crucible, in retort furnace under 600 ℃ of temperature ignition combustion, burning back insulation 5min obtains the product presoma;
(3) above-mentioned product presoma is incubated 60min at 1100 ℃ of temperature lower calcinations, and furnace cooling obtains product;
(4) above-mentioned product is used distilled water, washing with alcohol successively, namely gets product after the drying.
Embodiment five:
Present embodiment (Co
0.75Zn
0.25) (Cr
0.5Al
0.5)
2O
4The preparation method of composite spinelle type blue ceramic colorant is with embodiment two differences:
In the step (3), the product presoma is at 1150 ℃ of temperature lower calcinations.
Embodiment six:
Present embodiment (Co
0.5Zn
0.5) (Cr
0.25Al
0.75)
2O
4The preparation method of composite spinelle type blue ceramic colorant, its step is as follows:
(1) according to the parameter in above-mentioned chemical equation and the table 1, take by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio, sucrose is by its 150 wt% weighings by stoichiometric ratio, and sodium-chlor is by (Co
0.5Zn
0.5) (Cr
0.25Al
0.75)
2O
450 wt% weighings of theoretical resultant quantity; Each raw material is dissolved in the distilled water, and magnetic agitation 45min mixes, Co in the mixing solutions
2++ Zn
2+Ionic concn is 0.4mol/L;
(2) above-mentioned mixing solutions is placed heat-resisting crucible, in retort furnace under 500 ℃ of temperature ignition combustion, burning back insulation 10min obtains the product presoma;
(3) above-mentioned product presoma is incubated 30min at 1100 ℃ of temperature lower calcinations, and furnace cooling obtains product;
(4) above-mentioned product is used distilled water, washing with alcohol successively, namely gets product after the drying.
Embodiment seven:
Present embodiment (Co
0.5Zn
0.5) (Cr
1/3Al
2/3)
2O
4The preparation method of composite spinelle type blue ceramic colorant is with reality
Executing example six differences is:
In the step (3), the product presoma is at 1150 ℃ of temperature lower calcinations.
Embodiment eight:
Present embodiment (Co
0.5Zn
0.5) (Cr
2/3Al
1/3)
2O
4The preparation method of composite spinelle type blue ceramic colorant is with reality
Executing example six differences is:
In the step (3), the product presoma is incubated 60min at 1200 ℃ of temperature lower calcinations.
Embodiment nine:
Present embodiment (Co
0.5Zn
0.5) (Cr
0.75Al
0.25)
2O
4The preparation method of composite spinelle type blue ceramic colorant, with
Embodiment one difference is:
In the step (3), the product presoma is incubated 45min at 1100 ℃ of temperature lower calcinations.
(the Co that the embodiment of the invention one～nine makes
xZn
1-x) (Cr
yAl
1-y)
2O
4Composite spinelle type blue ceramic colorant
Performance index as shown in table 2.
(the Co that table 2 embodiment of the invention one～nine makes
xZn
1-x) (Cr
yAl
1-y)
2O
4The performance index of composite spinelle blue ceramic colorant
Annotate: L*: expression light and shade (brightness)
A*: represent red green
B*: expression champac
A kind of Co-Zn-Cr-Al composite spinelle of the present invention type blue ceramic colorant and preparation method thereof, the consumption of each component and processing parameter are not limited to above-mentioned listed examples.
Claims (7)
1. a Co-Zn-Cr-Al composite spinelle type blue ceramic colorant is characterized in that: by general formula (Co
xZn
1-x) (Cr
yAl
1-y)
2O
4Express, wherein x, y represent molar fraction, x=0～1, y=0～1.
2. Co-Zn-Cr-Al composite spinelle type blue ceramic colorant according to claim 1 is characterized in that: described x=0.25～0.75, y=0.25～0.75.
3. Co-Zn-Cr-Al composite spinelle type blue ceramic colorant according to claim 1, it is characterized in that: adopt salt hydrotropy liquid combustion method synthetic, be oxygenant with Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate, dissolved organic matter is fuel and reductive agent, and the inertia soluble salt is auxiliary agent.
4. Co-Zn-Cr-Al composite spinelle type blue ceramic colorant according to claim 3, it is characterized in that: described dissolved organic matter is sucrose, citric acid or ethylene glycol.
5. according to claim 3 or 4 described Co-Zn-Cr-Al composite spinelle type blue ceramic colorants, it is characterized in that: described Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate are introduced by stoichiometric ratio separately respectively, dissolved organic matter is introduced by 100～150wt% of its stoichiometric ratio, and the inertia soluble salt is by (Co
xZn
1-x) (Cr
yAl
1-y)
2O
430～50wt% of theoretical resultant quantity introduces.
6. the preparation method of the described Co-Zn-Cr-Al composite spinelle of one of claim 1-5 type blue ceramic colorant is characterized in that may further comprise the steps:
(1) takes by weighing Xiao Suangu, zinc nitrate, chromium nitrate, aluminum nitrate respectively by separately stoichiometric ratio; Dissolved organic matter is sucrose, citric acid or ethylene glycol, by 100～150wt% introducing of its stoichiometric ratio; The inertia soluble salt is by (Co
xZn
1-x) (Cr
yAl
1-y)
2O
430～50wt% of theoretical resultant quantity introduces; Described each raw material is dissolved in the distilled water, mixes and obtain mixing solutions;
(2) with described mixing solutions in retort furnace under 400～600 ℃ of temperature ignition combustion, burning back insulation 5～15min obtains the product presoma;
(3) with described product presoma at 1100～1200 ℃ of temperature lower calcinations, the insulation 30～60min obtain product;
(4) will get product after described product washing, the drying.
7. the preparation method of Co-Zn-Cr-Al composite spinelle type blue ceramic colorant according to claim 6 is characterized in that: Co in described step (1) mixing solutions
2++ Zn
2+Ionic concn is 0.3～0.5mol/L.
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Cited By (7)
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|---|---|---|---|---|
| CN104276850A (en) * | 2014-08-29 | 2015-01-14 | 华北水利水电大学 | Spinel ultrafine blue ceramic pigment and preparation method thereof |
| US9850161B2 (en) | 2016-03-29 | 2017-12-26 | Applied Materials, Inc. | Fluoride glazes from fluorine ion treatment |
| CN108529686A (en) * | 2018-04-13 | 2018-09-14 | 山东国瓷康立泰新材料科技有限公司 | A kind of ceramic ink jet printing low cobalt blue colorant and preparation method thereof |
| CN108821351A (en) * | 2018-07-25 | 2018-11-16 | 安徽工业大学 | A kind of preparation method of the porous high entropy oxide material of spinel-type |
| CN109052491A (en) * | 2018-07-23 | 2018-12-21 | 安徽工业大学 | A kind of preparation method of the porous high entropy oxide material of lithium ion battery negative material spinel-type |
| CN111690282A (en) * | 2020-07-31 | 2020-09-22 | 江西金环颜料有限公司 | Preparation method of blue pigment for coating/ink-jet printing/nano zirconia ceramic |
| CN112500720A (en) * | 2020-12-07 | 2021-03-16 | 武汉理工大学 | Turquoise ceramic pigment synthesized by solid phase method and preparation method thereof |
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| CN108821351A (en) * | 2018-07-25 | 2018-11-16 | 安徽工业大学 | A kind of preparation method of the porous high entropy oxide material of spinel-type |
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| CN111690282A (en) * | 2020-07-31 | 2020-09-22 | 江西金环颜料有限公司 | Preparation method of blue pigment for coating/ink-jet printing/nano zirconia ceramic |
| CN112500720A (en) * | 2020-12-07 | 2021-03-16 | 武汉理工大学 | Turquoise ceramic pigment synthesized by solid phase method and preparation method thereof |
| CN112500720B (en) * | 2020-12-07 | 2022-02-15 | 武汉理工大学 | Turquoise ceramic pigment synthesized by solid phase method and preparation method thereof |
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Application publication date: 20130904 |