CN102674898B - Cerium oxide/ aluminium oxide micro-nanostructure ceramic pigment and preparation method thereof - Google Patents
Cerium oxide/ aluminium oxide micro-nanostructure ceramic pigment and preparation method thereof Download PDFInfo
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- CN102674898B CN102674898B CN201210186512.2A CN201210186512A CN102674898B CN 102674898 B CN102674898 B CN 102674898B CN 201210186512 A CN201210186512 A CN 201210186512A CN 102674898 B CN102674898 B CN 102674898B
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Abstract
The invention discloses a cerium oxide/ aluminium oxide micro-nanostructure ceramic pigment and a preparation method of the ceramic pigment. The ceramic pigment is composed of alumina fibers and cerium oxide particles according to a molar ratio of 1:20-3:10 and has uniform size and good dispersity; the lengths of the alumina fibers are 3-4mum; the sizes of the cerium oxide particles are 80-100nm; the dispersion concentration of the cerium oxide particles and the chromatic performance of the final product are controlled by adjusting the concentration of the cerium oxide; and the product is pink after being calcined for 2 hours at the temperature of 1200 DEG C. The cerium oxide/ aluminium oxide micro-nanostructure ceramic pigment and the preparation method provided by the invention have the advantages of simple process, safety in operation and low cost.
Description
Technical field
The invention belongs to micro-nanometer structural material preparing technical field, relate to a kind of cerium oxide/aluminum oxide micro-nanometer structural material, be specifically related to a kind of cerium oxide/aluminum oxide micro nano structure beramic color, the invention still further relates to the preparation method of above-mentioned cerium oxide/aluminum oxide micro nano structure beramic color.
Background technology
Micro-nanometer structural material due to have the special physics and chemistry performance relevant to its unique texture be subject in recent years can people extensive concern, now formed the several different methods of preparing micro-nanometer structural material, as sol-gel processing, coprecipitation method, hydrothermal method, solvent-thermal method, physical vaporous deposition and chemical Vapor deposition process etc.Zinc oxide, aluminum oxide and the multiple micro-nano composite powder material of different-shape by these methods, have successfully been prepared.These micro-nanometer structural materials with unique microscopic appearance have shown many special optical, electrical, magnetic and other excellent performance.
Aluminum oxide micro-nanometer structural material has high specific surface area, stable chemical property, compared with features such as high wear resistance and fusing points, be widely used in the fields such as beramic color, support of the catalyst, sorbent material, luminescent material, high-abrasive material and new texture material be synthetic.Cerium oxide is many in aspect purposes such as electrolyte, high-index material and the silicon substrate insulation layers of catalyzer, solid-oxide fuel cell, in addition because rare earth ion electricity price is high, radius is large, specific refractory power is high, there is unique optical property, make the tinting material of the rare earth compounds such as cerium oxide for environmental protection beramic color.Adopt high temperature solid-state method to prepare beramic color, the more difficult morphology control that realizes, and product particle size is larger.Therefore, preparation method's research of cerium oxide/aluminum oxide micro nano structure beramic color is expanded and will be had great importance in application and the performance in beramic color field for aluminum oxide micro-nanometer structural material.
Summary of the invention
The object of this invention is to provide a kind of cerium oxide/aluminum oxide micro nano structure beramic color, can realize morphology control, product size reaches micro/nano level.
Another object of the present invention is to provide a kind of preparation method of above-mentioned cerium oxide/aluminum oxide micro nano structure beramic color.
The technical solution adopted in the present invention is, a kind of cerium oxide/aluminum oxide micro nano structure beramic color, is that 1:20 ~ 3:10 forms by aluminum oxide and cerium oxide according to mol ratio, and the length of sapphire whisker is 3 ~ 4 μ m, and cerium oxide particle size is 80 ~ 100nm.
Another technical scheme of the present invention is, a kind of preparation method of cerium oxide/aluminum oxide micro nano structure beramic color, cerium oxide/aluminum oxide micro nano structure the beramic color preparing, by aluminum oxide and cerium oxide, according to mol ratio, be that 1:20 ~ 3:10 forms, the length of sapphire whisker is 3 ~ 4 μ m, cerium oxide particle size is 80 ~ 100nm, specifically according to following steps, implements:
Step 1: the cerium solution of preparation 0.03 ~ 0.09mol/L, mol ratio according to cerium salt and aluminium salt material is 1:20 ~ 3:20, add aluminium salt, after aluminium salt dissolves completely, according to the mol ratio of aluminium salt and PEG 20000, be that 1:0.15 ~ 1:0.03 adds PEG 20000 to form clear solution, according to the mol ratio of aluminium salt and urea, be that 1:16 ~ 1:17 adds urea again, be stirred to dissolving;
Step 2: get the mixing solutions that step 1 obtains and proceed to in teflon-lined reactor, sealing, puts into 120 ℃ of insulation 22 ~ 26h of baking oven steady temperature by reactor, takes out reactor and naturally cools to room temperature;
Step 3: the product centrifugation that step 2 is obtained, wash respectively three times with deionized water and dehydrated alcohol, then gained solid product is put into dry 24 hours of the vacuum drying oven of 60 ℃, obtain white powder;
Step 4: the white powder obtaining in step 3 is placed in to retort furnace, is warmed up to 1200 ℃ and be incubated 2 hours with the temperature rise rate of 2 ℃/min in air atmosphere, naturally cool to subsequently room temperature, make cerium oxide/aluminum oxide micro nano structure beramic color.
Feature of the present invention is also,
Beramic color wherein presents pink, and color generation property changes with cerium oxide change in concentration.
Cerium salt wherein adopts six water cerous nitrates or six water Cerium II Chlorides.
Aluminium salt wherein adopts the one in nine water aluminum nitrates, Aluminum Chloride Hexahydrate or 16 water Tai-Ace S 150.
In the present invention, the introduction volume in cerium source is to affect the key factor that cerium oxide particle disperses concentration, the initial molar ratio of cerium salt and aluminium salt has a certain impact to the pattern of the micro nano structure pigment obtaining, in addition calcination time and temperature rise rate can affect its pattern, change He Lv source, cerium source not obvious on the structure and morphology impact of product.1) adopt hydrothermal method to prepare presoma, through 1200 ° of C calcining, obtain cerium oxide/aluminum oxide micro nano structure beramic color, cerium oxide particle is evenly attached to sapphire whisker and carries on look parent and be light yellow.2) by the introduction volume in cerium source, can control cerium oxide particle and disperse concentration, thereby affect color generation property.3) changing He Lv source, cerium source affects not obvious on the structure and morphology of product.
Accompanying drawing explanation
Fig. 1 is the material phase analysis result figure of cerium oxide/aluminum oxide micro nano structure beramic color of making of the embodiment of the present invention 1;
Fig. 2 is the stereoscan photograph of cerium oxide/aluminum oxide micro nano structure beramic color of making of the embodiment of the present invention 1, wherein, is (a) to amplify the stereoscan photograph of 5000 times, is (b) to amplify the stereoscan photograph of 20000 times;
Fig. 3 is the stereoscan photograph of cerium oxide/aluminum oxide micro nano structure beramic color of making of the embodiment of the present invention 2, wherein, is (a) to amplify the stereoscan photograph of 5000 times, is (b) to amplify the stereoscan photograph of 20000 times;
Fig. 4 is the stereoscan photograph of cerium oxide/aluminum oxide micro nano structure beramic color of making of the embodiment of the present invention 5, wherein, is (a) to amplify the stereoscan photograph of 5000 times, is (b) to amplify the stereoscan photograph of 20000 times.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Cerium oxide/aluminum oxide micro nano structure beramic color of the present invention, is comprised of nano level cerium oxide particle and micron-sized sapphire whisker.Sapphire whisker size homogeneous, the length of sapphire whisker is 3 ~ 4 μ m, cerium oxide particle size is 80 ~ 100nm, and the composition that it is characterized by this filamentary material of composition is: the mol ratio of aluminum oxide and cerium oxide is 1:20 ~ 3:20, and the color that product presents is light yellow.
The present invention prepares the method for cerium oxide/aluminum oxide micro nano structure beramic color, specifically according to following steps, carries out:
Step 1: the solution of cerium chloride by oxidation 35mL of preparation 0.03 ~ 0.09mol/L, add nine water aluminum nitrates, the mol ratio of cerium salt and aluminium salt material is 1:20 ~ 3:20, after aluminium salt dissolves completely, according to the mol ratio of aluminium salt and PEG 20000, be that 1:0.15 ~ 1:0.03 adds PEG 20000 to form clear solution, according to the mol ratio of aluminium salt and urea, be that 1:16 ~ 1:17 adds urea again, be stirred to dissolving.
Step 2: the mixing solutions of getting step 1 proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulations of baking oven steady temperature 22 ~ 26 hours, take out reactor and naturally cool to room temperature.
Step 3: by products therefrom centrifugation in step 2, and wash respectively three times with deionized water and dehydrated alcohol, then gained solid product is put into dry 24 hours of the vacuum drying oven of 60 ℃, obtain white powder.
Step 4: the white powder obtaining in step 3 is placed in to retort furnace, in air atmosphere, with the temperature rise rate of 2 ℃/min, be warmed up to 1200 ℃ and be incubated 2 hours, naturally cool to subsequently room temperature, can make cerium oxide/aluminum oxide micro nano structure beramic color.
Wherein in step 1, cerium salt used can be six water cerous nitrates or six water Cerium II Chlorides, and aluminium salt can be nine water aluminum nitrates, Aluminum Chloride Hexahydrate or 16 water Tai-Ace S 150, all can obtain the micro-nano beramic color of cerium oxide/aluminum oxide that structure is identical.
Embodiment 1
The solution of cerium chloride by oxidation 35mL of preparation 0.03mol/L, after being fully uniformly mixed, add 7.5g nine water aluminum nitrates, dissolve completely, the mol ratio of cerium salt and aluminium salt material is 1:20,8g PEG 20000 is dissolved in and in mixing solutions, forms clear solution, then 20g urea is joined in solution, be stirred to dissolving.Mixing solutions proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulations of baking oven steady temperature 22 hours, take out reactor and naturally cool to room temperature.Collect white product in water heating kettle and with deionized water and absolute ethanol washing for several times, then by the vacuum drying oven of product 60 ℃ dry 24 hours, obtain a white powder.Above-mentioned white powder is placed in to retort furnace, calcines and be incubated 2 hours at 1200 ℃, naturally cool to subsequently room temperature, obtained lurid powder and be cerium oxide/aluminum oxide micro nano structure beramic color.Fig. 1 is the material phase analysis result figure of cerium oxide/aluminum oxide micro nano structure beramic color of making, as can be seen from Figure 1 product is the composite granule of aluminum oxide and cerium oxide, Fig. 2 is the stereoscan photograph of prepared cerium oxide/aluminum oxide micro nano structure beramic color, as can be seen from the figure, in prepared micro nano structure beramic color, sapphire whisker size homogeneous, length is 3 ~ 4 μ m, the size of cerium oxide particle is 80 ~ 100nm.
Embodiment 2
The solution of cerium chloride by oxidation 35mL of preparation 0.09mol/L, after being fully uniformly mixed, add 7.5g nine water aluminum nitrates, dissolve completely, the mol ratio of cerium salt and aluminium salt material is 3:20,6g PEG 20000 is dissolved in and in mixing solutions, forms clear solution, then 19.2g urea is joined in solution, be stirred to dissolving.Mixing solutions proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulations of baking oven steady temperature 26 hours, take out reactor and naturally cool to room temperature.Collect white product in water heating kettle and with deionized water and absolute ethanol washing for several times, then by the vacuum drying oven of product 60 ℃ dry 24 hours, obtain a white powder.Above-mentioned white powder is placed in to retort furnace, calcines and be incubated 2 hours at 1200 ℃, naturally cool to subsequently room temperature, obtained lurid powder and be cerium oxide/aluminum oxide micro nano structure beramic color.Fig. 3 is the stereoscan photograph of prepared cerium oxide/aluminum oxide micro nano structure beramic color, and as can be seen from the figure, in prepared micro nano structure beramic color, the dispersion concentration of cerium oxide obviously increases.
Embodiment 3
The solution of cerium chloride by oxidation 35mL of preparation 0.06mol/L, after being fully uniformly mixed, add 7.5g nine water aluminum nitrates, dissolve completely, the mol ratio of cerium salt and aluminium salt material is 1:10,12g PEG 20000 is dissolved in and in mixing solutions, forms clear solution, then 20.4g urea is joined in solution, be stirred to dissolving.Mixing solutions proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulations of baking oven steady temperature 24 hours, take out reactor and naturally cool to room temperature.Collect white product in water heating kettle and with deionized water and absolute ethanol washing for several times, then by the vacuum drying oven of product 60 ℃ dry 24 hours, obtain a white powder.Above-mentioned white powder is placed in to retort furnace, calcines and be incubated 2 hours at 1200 ℃, naturally cool to subsequently room temperature, obtained lurid powder and be cerium oxide/aluminum oxide micro nano structure beramic color.
Embodiment 4
The cerous nitrate solution 35mL of preparation 0.06mol/L, after being fully uniformly mixed, add 7.5g nine water aluminum nitrates, dissolve completely, the mol ratio of cerium salt and aluminium salt material is 1:10,8g PEG 20000 is dissolved in and in mixing solutions, forms clear solution, then 20g urea is joined in solution, be stirred to dissolving.Mixing solutions proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulations of baking oven steady temperature 26 hours, take out reactor and naturally cool to room temperature.Collect white product in water heating kettle and with deionized water and absolute ethanol washing for several times, then by the vacuum drying oven of product 60 ℃ dry 24 hours, obtain a white powder.Above-mentioned white powder is placed in to retort furnace, in air atmosphere, at 1200 ℃, calcines and be incubated 2 hours, naturally cool to subsequently room temperature, obtained lurid powder and be cerium oxide/aluminum oxide micro nano structure beramic color.
Embodiment 5
The cerous nitrate solution 35mL of preparation 0.06mol/L, after being fully uniformly mixed, add 4.8g Aluminum Chloride Hexahydrate, dissolve completely, the mol ratio of cerium salt and aluminium salt material is 3:20,12g PEG 20000 is dissolved in and in mixing solutions, forms clear solution, then 20.4g urea is joined in solution, be stirred to dissolving.Mixing solutions proceeds to in teflon-lined reactor, sealing.Reactor is put into 120 ℃ of insulation 26h of baking oven steady temperature, take out reactor and naturally cool to room temperature.Collect the white product in water heating kettle and use deionized water and absolute ethanol washing several, then, by 60 ℃ of dry 24h in the vacuum drying oven of product, obtain a white powder.Above-mentioned white powder is placed in to retort furnace, calcines and be incubated 2h at 1200 ℃, naturally cool to subsequently room temperature, obtained lurid powder and be cerium oxide/aluminum oxide micro nano structure beramic color.Fig. 4 is the stereoscan photograph of prepared cerium oxide/aluminum oxide micro nano structure beramic color, and as can be seen from the figure, the micro nano structure beramic color structure and morphology prepared as cerium source take cerous nitrate is substantially constant.
Table 1 is the colourimetric number of the cerium oxide/aluminum oxide micro nano structure pottery face that makes of example 1 of the present invention to example 3.As can be seen from the table, along with the increase of cerium aluminum ratio, chromaticity index a
*b
*present increase trend, saturation ratio is relatively low.
Under table 1 cerium proportionings different from aluminium, the colourimetric number of cerium oxide/aluminum oxide micro nano structure beramic color
Claims (4)
1. the preparation method of cerium oxide/aluminum oxide micro nano structure beramic color, it is characterized in that, cerium oxide/aluminum oxide micro nano structure the beramic color preparing, by aluminum oxide and cerium oxide, according to mol ratio, be that 1:20～3:10 forms, the length of sapphire whisker is 3～4 μ m, cerium oxide particle size is 80～100nm, specifically according to following steps, implements:
Step 1: the cerium solution of preparation 0.03～0.09mol/L, mol ratio according to cerium salt and aluminium salt material is 1:20～3:20, add aluminium salt, after aluminium salt dissolves completely, according to the mol ratio of aluminium salt and PEG 20000, be that 1:0.15～1:0.03 adds PEG 20000 to form clear solution, according to the mol ratio of aluminium salt and urea, be that 1:16～1:17 adds urea again, be stirred to dissolving;
Step 2: get the mixing solutions that step 1 obtains and proceed to in teflon-lined reactor, sealing, puts into 120 ℃ of insulations of baking oven steady temperature 22～26 hours by reactor, takes out reactor and naturally cools to room temperature;
Step 3: the product centrifugation that step 2 is obtained, wash respectively three times with deionized water and dehydrated alcohol, then gained solid product is put into dry 24 hours of the vacuum drying oven of 60 ℃, obtain white powder;
Step 4: the white powder obtaining in step 3 is placed in to retort furnace, is warmed up to 1200 ℃ and be incubated 2 hours with the temperature rise rate of 2 ℃/min in air atmosphere, naturally cool to subsequently room temperature, make cerium oxide/aluminum oxide micro nano structure beramic color.
2. the preparation method of cerium oxide/aluminum oxide micro nano structure beramic color according to claim 1, is characterized in that, described beramic color presents pink, and color generation property changes with cerium oxide change in concentration.
3. the preparation method of cerium oxide/aluminum oxide micro nano structure beramic color according to claim 1, is characterized in that, described cerium salt adopts six water cerous nitrates.
4. the preparation method of cerium oxide/aluminum oxide micro nano structure beramic color according to claim 1, is characterized in that, described aluminium salt adopts the one in nine water aluminum nitrates, Aluminum Chloride Hexahydrate or 16 water Tai-Ace S 150.
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| CN108130595B (en) * | 2017-12-22 | 2020-08-07 | 西南交通大学 | Method for preparing alumina whisker by controlling atmosphere |
| CN109338512B (en) * | 2018-10-11 | 2020-11-10 | 厦门大学 | Cerium oxide-aluminum oxide fiber and preparation method thereof |
| CN110105810B (en) * | 2019-07-03 | 2019-10-15 | 佛山市道氏科技有限公司 | Ceramic white seeps flower ink and preparation method thereof, Ceramic Tiles and preparation method thereof |
| CN113198485B (en) * | 2021-05-18 | 2022-08-16 | 贵州大学 | Aluminum cerium composite oxide catalyst, preparation method and application |
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| JP2007511655A (en) * | 2003-11-21 | 2007-05-10 | エッカルト ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフト | Effect pigment having an aluminum core or an aluminum alloy core, and its production method and use |
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| JP2007511655A (en) * | 2003-11-21 | 2007-05-10 | エッカルト ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフト | Effect pigment having an aluminum core or an aluminum alloy core, and its production method and use |
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