CN1443811A - Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method - Google Patents
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- CN1443811A CN1443811A CN 03116190 CN03116190A CN1443811A CN 1443811 A CN1443811 A CN 1443811A CN 03116190 CN03116190 CN 03116190 CN 03116190 A CN03116190 A CN 03116190A CN 1443811 A CN1443811 A CN 1443811A
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Abstract
The present invention relates to a method for preparing nano crystal cobalt aluminium spinella (CoAl2O4) pigment by utilizing low-temp. combustion synthesis process. Said invention includes the following steps: using soluble aluminium salt (aluminium nitrate, aluminium acetate and aluminium sulfate), soluble cobalt salt (cobalt nitrate, cobalt acetate and cobalt sulfate), citric acid or urea as initiation raw material, after the solutions are mixed, forming complex, using citric acid or urea as complexing agent and fuel, electrically-heating or microwave heating mixed solution, lighting and self-combusting to obtain puff powder, then heat treatment at 500-1000 deg.C so as to obtain the invented nano crystal CoAl2O4 whose grain size is 10-100 nm.
Description
Technical field
The present invention relates to nanocrystalline CoAl
2O
4The synthetic method of powder is particularly with electrically heated or microwave heating inducing solution burning synthesizing nanocrystalline CoAl
2O
4Method, belong to nanocrystalline pigment prepared field.
Background technology
CoAl with spinel structure
2O
4Blue pigments has excellent thermostability and chemical stability, painted (the P.A.Lewis that has been widely used in plastics, rubber, coating, pottery, enamel, glass, glaze, colour TV blue light fluorescent powder etc., Pigment handbook, John Wiley and Sons, New York, Vol.1,1998).CoAl
2O
4The traditional preparation process method of spinel is a solid reaction process, generally be to utilize cobaltous carbonate and aluminum oxide to be raw material, with the two mix according to a certain percentage, ball milling, under～1300 ℃ high temperature, calcine then, and, reach designated size through further pulverizing.Because solid state reaction needs the diffusion of the long distance of metal ion to finish, thereby the reaction required time is long, product is formed inhomogeneous, granularity big (μ m level) and wider distribution.In the high-temperature calcination process, cause local sintering inevitably, thereby the powder specific surface area is descended.Generally the specific surface area of the powder that obtains with this method is 1～5m
2g
-1(C.Otero Are à n, M.
Mentruit, et al., Mater.Lett.39 (1999) 22-27), though opacifying power is better, can only be as the ceramic grade pigment applications.Since the eighties, nanocrystalline CoAl
2O
4Research active day by day, the nanocrystalline CoAl of multiple preparation has appearred
2O
4The method of spinel powder, as chemical coprecipitation (Japanese Patent, flat 4-55322,1992), sol-gel method (S.Chemlala, A.Larbotb, et al., Mater.Res.Bull., 35 (2000) 2515-2523), polymer precursor method (W.-S.Cho, M.Kakihana, J.Alloys Comp., 287 (1999) 87-90) etc.Prepare CoAl with wet chemical method
2O
4Advantage be to be easy to control chemical constitution, the product purity height, fine size, even particle size distribution, tone saturation ratio height can be applicable in the fields such as senior plastics, fiber, coating, rubber.Nanocrystalline CoAl
2O
4Pigment is the most outstanding to be characterised in that it can produce transparent coloring effect, and wherein pigment granularity and the pigment dispersiveness in matrix is the key factor of decision tinctorial property.Though aforesaid method can both prepare nanocrystalline CoAl
2O
4, but common drawback is the technological process more complicated, the building-up process required time is longer.As the refine big day a kind of preparation technology of ultra-fine transparent cobalt blue dye of (strain) exploitation of Japan be: aluminium salt, cobalt salt, aqueous solution of urea are mixed stir, the heating back forms Al (OH)
3And Co (OH)
2Co-precipitation, more than the dry 12h of 120, then at 1000 ℃ of thermal treatment 1h, obtaining specific surface area is 80m behind the filtration washing throw out
2g
-1Ultra-fine transparent cobalt blue dye (Japanese Patent, flat 2-283771,1990).
Low-temperature burning synthetic technology (LCS) is that saturated aqueous solution-the organic-fuel mixture is a raw material to the employing metal-salt, synthesizing superfine powder under lower ignition temperature and burning exothermic temperature, its appearance is the important expansion to SHS, for new way has been opened up in the preparation of nanocrystalline powder.The liquid phase batching has guaranteed the homogeneity of component, ignition temperature lower (200～500 ℃), and combustion processes is rapid, and energy consumption is low.This oxidation-reduction reaction has autocatalytic characteristics, and promptly the combustion reactions liberated heat makes reaction spontaneously carry out synthetic product.Discharge a large amount of gases in the reaction process, cause products of combustion to expand into loose bubble end, avoid the generation of hard aggregation, be beneficial to powder and disperse, thereby synthetic powder specific surface area is big.Since the nineties, particularly in the later stage nineties, the research of the nanocrystalline powder of employing cryogenic fluid combustion method synthesis oxide has been subjected to scientist and has more and more paid close attention to, and it is carried out in a lot of fields, as be used for Al
2O
3, ZrO
2, ZnO, ZnAl
2O
4Deng synthesizing of powder.But cryogenic fluid combustion method synthesizing nanocrystalline CoAl is not arranged as yet at present
2O
4Report.
Summary of the invention
The objective of the invention is to wet chemistry method and self-propagating combustion synthesis method are combined, a kind of quick, easy, energy-conservation nanocrystalline CoAl is provided
2O
4The preparation method of powder.Preparation flow figure as shown in Figure 1.
Main implementation process of the present invention is:
(1) be starting raw material with aluminum soluble salt (a kind of in aluminum nitrate, Burow Solution or the Tai-Ace S 150), solubility cobalt salt (a kind of in Xiao Suangu, Cobaltous diacetate or the rose vitriol), citric acid or urea, Co
2+: Al
3+: citric acid three's mixing mol ratio is 1: 2～3: 1～6, perhaps Co
2+: Al
3+: urea three's mixing mol ratio is 1: 2～3: 3～15.Solution mixes the back and forms complex compound, twists lemon acid or urea as complexing agent, and double as fuel is used.
(2) earlier aluminium salt, cobalt salt, citric acid are dissolved in the deionized water, make solution in ratio described in (1) then, mix the back and constantly stir, adjusting pH value with ammoniacal liquor is 4～8, electrically heated or microwave heating then.Microwave frequency is 2.45GHz, power input 500W; Retort furnace is in advance 300 ℃ of insulations.Along with the water vapor volatilization, solution concentration forms gel.When reaching certain temperature, gel auto-combustion on fire, the time is no more than 15min, obtains fluffy spumescence powder.
(3) or earlier aluminium salt, cobalt salt, urea are dissolved in the deionized water, make solution in ratio described in (1) then, mix constantly stirring of back, electrically heated or microwave heating then.Microwave frequency is 2.45GHz, power input 500W; Retort furnace is in advance 300 ℃ of insulations.Along with the water vapor volatilization, solution concentration forms gel.When reaching certain temperature, gel auto-combustion on fire, the time is no more than 15min, obtains fluffy spumescence powder.
(4), obtain the CoAl of different-grain diameter, different specific surface areas with above-mentioned (2), the resulting powder of (3) step thermal treatment 0.3～5h in 500～1000 ℃ of air
2O
4Powder.
(5) in the mixing solutions of aluminum soluble salt, solubility cobalt salt and stubborn lemon acid, the preferential Co that recommends
2+: Al
3+=1: 2～2.5 (mol ratios); Co
2+And Al
3+Metal ion and citric acid mol ratio are 1: 0.5～2.5.
(6) in the mixed solution of aluminum soluble salt, solubility cobalt salt and urea, preferential recommendation; Co
2+: Al
3+=1: 2～2.5 (mol ratios); Co
2+And Al
3+Metal ion and urea mol ratio are 1: 1～5.
Equipment used of the present invention is simple, with existing nanocrystalline CoAl
2O
4Powder preparation method is compared and is had the following advantages:
(1) reactant mixes with atomic level, helps reaction and carries out fast.Reaction process is easy, need not high-tension apparatus, and combustion reactions can be finished in 15min, and the subsequent heat treatment temperature is no more than 1000 ℃, and heat treatment time is less than 5h.
(2) by the add-on of control citric acid or urea, regulate the subsequent heat treatment temperature and time, thereby can control CoAl
2O
4Size of microcrystal (10～100nm) and specific surface area (12～87m
2g
-1).
(3) product purity height, controllable granularity, narrow particle size distribution.
Description of drawings
Fig. 1 is preparation flow figure provided by the invention.
Fig. 2 is the XRD figure spectrum of products of combustion and thermal treatment product among the embodiment 1.
Fig. 3 is the XRD figure spectrum of products of combustion and thermal treatment product among the embodiment 2.
Fig. 4 is the XRD figure spectrum of products of combustion and thermal treatment product among the embodiment 3.
Fig. 5 is the TEM photo of thermal treatment product among the embodiment 1.
Fig. 6 is the TEM photo of thermal treatment product among the embodiment 2.
Fig. 7 is the TEM photo of thermal treatment product among the embodiment 3.
Embodiment
Further illustrate characteristics of the present invention by the following examples, but be not limited to embodiment.
Embodiment 1
With aluminum nitrate, Cobaltous diacetate and citric acid is raw material, presses Co
2+: Al
3+: citric acid mol ratio=1: 2: 2 batching, method is as follows: respectively aluminum nitrate, Cobaltous diacetate and citric acid are dissolved in the deionized water, make solution, mix the back and constantly stir, adjust PH with ammoniacal liquor and equal 7, after fully stirring, place the microwave cavity internal heating.Microwave frequency is 2.45GHz, power input 500W.Along with the water vapor volatilization, solution takes place to concentrate, and forms gel.When reaching certain temperature, gel auto-combustion on fire, the time is about 5min, obtains fluffy spumescence powder.With above-mentioned powder thermal treatment 2h in 700 ℃ of air, obtain the finished product, its XRD figure is composed as Fig. 2, TEM photo such as Fig. 5.The CoAl that makes
2O
4The median size of powder (by the Scherrer Equation for Calculating) is 19nm, and specific surface area is 59m
2/ g.
With Tai-Ace S 150, Xiao Suangu and citric acid is raw material, presses Co
2+: Al
3+: citric acid mol ratio=1: 2: 3 batching, method is as follows: respectively Tai-Ace S 150, Xiao Suangu and citric acid are dissolved in the deionized water, make solution, mix the back and constantly stir, adjust PH with ammoniacal liquor and equal 7, after fully stirring, place on the electric furnace and heat.Along with the continuous evaporation of moisture, form gel.Then gel is placed retort furnace, when arriving 300 ℃ of temperature, gel auto-combustion on fire, the time is about 15min, obtains fluffy spumescence powder.With above-mentioned powder thermal treatment 1h in 900 ℃ of air, obtain the finished product, its XRD figure is composed as Fig. 3, TEM photo such as Fig. 6.The CoAl that obtains
2O
4The median size of powder (by the Scherrer Equation for Calculating) is 31nm, and specific surface area is 43m
2/ g.
Embodiment 3
With aluminum nitrate, Xiao Suangu, urea is raw material, presses Co
2+: Al
3+: urea mol ratio=1: 2: 10 batching, method is as follows: respectively aluminum nitrate and Xiao Suangu, urea are dissolved in the deionized water, make solution, mix the back and constantly stir, place the microwave cavity internal heating.Microwave frequency is 2.45GHz, power input 500W.Along with the water vapor volatilization, solution takes place to concentrate, and forms gel.When reaching certain temperature, gel auto-combustion on fire, the time is about 2min, obtains fluffy spumescence powder.With above-mentioned powder thermal treatment 3h in 500 ℃ of air, obtain the finished product, its XRD figure is composed as Fig. 4, TEM photo such as Fig. 7.The CoAl that obtains
2O
4The median size of powder (by the Scherrer Equation for Calculating) is 42nm, and specific surface area is 37m
2/ g.
Claims (10)
1. solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder comprises batching, mixing and high-temperature heat treatment.It is characterized in that concrete synthesis step is:
(1) earlier aluminum soluble salt, solubility cobalt salt, citric acid are dissolved in deionized water, make solution, press Co again
2+: Al
3+: citric acid=1: 2～3: 1～6 (mol ratio) mixes;
(2) mix the back and constantly stir, adjusting pH value with ammoniacal liquor is 4～8, heating then, and solution concentration forms gel and catching fire, obtains the spumescence powder;
(3) with spumescence powder high-temperature heat treatment in 500～1000 ℃ of air, time 0.3～5h makes CoAl
2O
4Manocrystalline powders.
2. by the described solution combustion synthesizing nanocrystalline of claim 1 CoAl
2O
4The method of powder is characterized in that aluminum soluble salt is a kind of in aluminum nitrate, Burow Solution or the Tai-Ace S 150; The solubility cobalt salt is a kind of in Xiao Suangu, Cobaltous diacetate or the rose vitriol; Co
2+: Al
3+=1: 2～2.5 (mol ratios).
3. by claim 1 or 2 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that burning by electrically heated or microwave induced lighting, is no more than 15min combustion time.
4. by claim 1 or 2 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that Co
2+And Al
3+Metal ion and citric acid mol ratio are 1: 0.5～2.5.
5. by claim 1,2 or 4 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that CoAl
2O
4Size of microcrystal is between between 10～100nm.
6. solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder comprises batching, mixing and high-temperature heat treatment.It is characterized in that concrete synthesis step is:
(1) earlier aluminum soluble salt, solubility cobalt salt, urea are dissolved in deionized water, make solution, press Co again
2+: Al
3+: urea=1: 2～3: 3～15 (mol ratio) mixes;
(2) mix the back and constantly stir, heating then, solution concentration forms gel and catching fire, obtains the spumescence powder;
(3) with the spumescence powder, high-temperature heat treatment in 500～1000 ℃ of air, time 0.3～5h makes CoAl
2O
4Manocrystalline powders.
7. by the described solution combustion synthesizing nanocrystalline of claim 6 CoAl
2O
4The method of powder is characterized in that Co
2+: Al
3+=1: 2～2.5 (mol ratios).
8. by claim 6 or 7 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that burning by electrically heated or microwave induced lighting, is no more than 15min combustion time.
9. by claim 6 or 7 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that Co
2+And Al
3+Metal ion and urea mol ratio are 1: 1～5.
10. by claim 6,7 or 9 described solution combustion synthesizing nanocrystalline CoAl
2O
4The method of powder is characterized in that CoAl
2O
4Size of microcrystal is between between 10～100nm.
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| CN100439254C (en) * | 2004-11-12 | 2008-12-03 | 南京大学 | Preparation for nanometer cobalt compound |
| CN101559982B (en) * | 2009-05-27 | 2011-08-31 | 南京工业大学 | Method of one-step synthesis of hexagonal barium ferrite nanometer crystal by microwave-assistant sol-gel spontaneous combustion |
| CN102198395A (en) * | 2011-04-15 | 2011-09-28 | 河北科技大学 | Visible light photocatalyst containing amorphous MgAl2O4 and preparation method thereof |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD293568A5 (en) * | 1985-10-30 | 1991-09-05 | Adw,Zi F. Kernforschung,De | METHOD FOR PRODUCING POWDER-FORMED COBALT ALUMINATE |
-
2003
- 2003-04-04 CN CNB031161901A patent/CN100523094C/en not_active Expired - Fee Related
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| CN112811457A (en) * | 2021-03-03 | 2021-05-18 | 甘肃农业大学 | Preparation method of loose porous nano cerium oxide |
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