CN104085926B - The preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder - Google Patents
The preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder, taking soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent as raw material, according to certain mole proportioning, in alcohol water mixed solution, fully dissolve, then after cross-linking reaction, grind it is fully mixed evenly again at a certain temperature, then form predecessor by high-temperature calcination, then, by predecessor nitrogenize high-temperature process under ammonia, obtain SLSTON powder. Simple process of the present invention is easily gone, and purity is high, and impurity content is low, and product preparation cost is low, is applicable to batch production; Prepared product can be for fields such as ferroelectric, photoelectricity, photocatalysis and fuel cells.
Description
Technical field
The invention belongs to the preparing technical field of Inorganic Non-metallic Materials, specifically relate to a kind of preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder.
Background technology
Solid solution refers to that solute atoms dissolves in solvent lattice and still keeps the alloy phase of type of solvent. Conventionally be dissolved with the crystal that atom or molecule were formed of other materials with a kind of chemical substance for matrix, more common in alloy and silicate system, in polyatom material, also exist. Can stable existence after the crystal structure of solvent adds solute and keep homogeneous phase, this kind of mixture can be considered solid solution. Perovskite refers to that a class has the oxide of specific crystal structure, and its general molecular formula is ABX3, this compounds is found to be the calcium titanate (CaTiO being present in perovskite stone the earliest3) compound, therefore gain the name. Owing to having numerous characteristics on this type of compound structure, aspect Condensed Matter Physics and chemical industry catalysis, application and research are very wide, A position is generally rare earth or alkaline earth element ion, B position is transition element ion, and A position and B position all can be replaced and keep its crystal structure substantially constant by other close metal ion parts of radius.
The nitrogen oxide solid solution (such as the semi-conducting material based on niobium and tantalum) with perovskite structure has obtained considerable concern in nearly decades because of their attracting character and potential application. Tantalum base nitrogen oxides solid solution also more and more obtains people's attention as a kind of novel high efficiency photocatalyst. Sr0.5La0.5Sc0.5Ta0.5O2.5N0.5(A position is Sr0.5La0.5; B position is Sc0.5Ta0.5; X position is O2.5N0.5, be abbreviated as SLSTON) and be a kind of important unleaded perovskite-like Ferroelectric material. Be mainly used in the applications such as photocatalysis, dye pigment, magnetoresistance material and battery material. Because SLSTON is the photochemical catalyst of responding to visible light spectrum (wavelength is greater than 500nm), be more and more subject to people's attention in recent years. The solid phase reaction technology of traditional preparation SLSTON powder is consuming time long and need hot conditions, and reaction is normally carried out at 1000～1300 DEG C, thereby has limited the production of SLSTON powder.
Summary of the invention
Goal of the invention:
In order to overcome the deficiencies in the prior art part, the invention provides a kind of technique simple, object product yield is high, and preparation cost is low, and operating procedure is simple, the preparation method of the SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder of good dispersion.
Technical scheme:
The present invention implements by the following technical programs:
A preparation method for SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder, is characterized in that: step is as follows: after soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent are fully dissolved in alcohol water mixed solution, cross-linking reaction occurs in heating; Then grinding crosslinked product makes to be fully mixed evenly; Be cross-linked product by high-temperature calcination again, make it form predecessor; Predecessor is nitrogenize high-temperature process under ammonia atmosphere, obtains SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder.
The mol ratio of described soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent is 1: 1: 1: 1: 10～200.
Described soluble strontium salt is strontium chloride (SrCl2·6H2And strontium nitrate (Sr (NO O)3)2·4H2O) one in.
Described solubility lanthanum salt is lanthanum chloride (LaCl3·7H2And lanthanum nitrate (La (NO O)3)3·6H2O) one in.
Described solubility scandium salts is scandium chloride (ScCl3) and scandium nitrate (Sc (NO3)3·4H2O) one in.
Described solubility tantalum salt is tantalic chloride (TaCl5) and five ethoxy-tantalum (Ta (C2H5O)5) in one.
Described combustion assisting agent is the one in urea, citric acid, oxalic acid or hexamethylenetetramine.
Described alcohol water mixed solution is the mixed solution of a kind of and water in methyl alcohol, ethanol or ethylene glycol.
The alcohol and water of described alcohol water mixed solution is that 1:1～1:100 mixes according to volume ratio; Described cross-linking reaction temperature is at 50～400 DEG C, and cross-linking reaction time is 1～10h.
The reaction temperature of described high-temperature calcination cross-linking products is at 400～800 DEG C, and the reaction time is 4～24h; Described nitrogenize high-temperature process temperature is at 600～900 DEG C, and the reaction time is 4～48h.
Advantage and effect:
The preparation method who the invention provides a kind of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder, tool has the following advantages and beneficial effect:
(1) process route of the present invention is simple, and preparation cost is low, easy to control, has higher production efficiency.
(2) the object product S LSTON powder that prepared by the present invention, its purity is high, and impurity content is low, and good dispersion can meet the requirement of modern industry to SLSTON powder-product.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the prepared SLSTON powder of the present invention;
Fig. 2 is the ultraviolet-visible spectrogram of the prepared SLSTON powder of the present invention;
Fig. 3 is the energy gap figure of the prepared SLSTON powder of the present invention;
Fig. 4 is the catalytic activity phenogram of the prepared SLSTON powder of the present invention as visible light catalyst.
Detailed description of the invention
The invention provides a kind of preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder, taking soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent as raw material, raw material is according to certain mole proportioning, in alcohol water mixed solution, fully dissolve, then at a certain temperature after cross-linking reaction, grinding is fully mixed evenly it, then form predecessor by high-temperature calcination cross-linking products, then by predecessor nitrogenize high-temperature process under ammonia, obtain SLSTON powder (Ca-Ti ore type nitrogen oxide solid solution Sr0.5La0.5Sc0.5Ta0.5O2.5N0.5, be abbreviated as SLSTON), its preparation process is:
(1) by soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent according to certain molar ratio weighing after, be placed in alcohol water mixed solution fully and dissolve, the time is greater than 30 minutes.
(2) by above-mentioned solution, at 50～400 DEG C, cross-linking reaction 1～10h, put into mortar again grind careful, milling time 30 minutes.
(3) after above-mentioned cross-linking products mixture being packed in crucible, put into chamber type electric resistance furnace, high-temperature calcination reaction, 400～800 DEG C of reaction temperatures, the reaction time is 4～12h.
(4) after reaction, naturally cool to room temperature, carried out high-temperature ammonolysis processing in ammonia atmosphere, nitriding temperature is 600～900 DEG C, and the time is 4～48 hours, makes SLSTON powder.
Above-mentioned soluble strontium salt is strontium chloride (SrCl2·6H2And strontium nitrate (Sr (NO O)3)2·4H2O) a kind of or its mixture in.
Above-mentioned solubility lanthanum salt is lanthanum chloride (LaCl3·7H2And lanthanum nitrate (La (NO O)3)3·6H2O) a kind of or its mixture in.
Above-mentioned solubility scandium salts is scandium chloride (ScCl3) and scandium nitrate (Sc (NO3)3·4H2O) a kind of or its mixture in.
Above-mentioned solubility tantalum salt is tantalic chloride (TaCl5) and five ethoxy-tantalum (Ta (C2H5O)5) in a kind of or its mixture.
Above-mentioned combustion assisting agent is a kind of or its mixture in urea, citric acid, oxalic acid or hexamethylenetetramine.
Above-mentioned alcohol water mixed solution is the mixed solution of a kind of and water in methyl alcohol, ethanol or ethylene glycol or the mixed solution of its mixture and water.
The alcohol and water of above-mentioned alcohol water mixed solution is that 1:1～1:100 mixes according to volume ratio.
As shown in Figures 1 to 4, the SLSTON powder of preparing gained is carried out XRD and ultraviolet-visible analysis of spectrum by the present invention, and consequently, the color of products obtained therefrom SLSTON powder is orange colour (picture sees reference). Products obtained therefrom SLSTON powder X-ray RD diffraction pattern is ABX3The very strong (see figure 1) of type perovskite structure and degree of crystallinity. The ABSORPTION EDGE of products obtained therefrom SLSTON powder is in 550nm left and right (see figure 2), and the about 2.15eV(of energy gap is shown in Fig. 3). And under visible ray condition, in certain catalysis adjuvant and the aqueous solution of finite concentration sacrifice agent, in the reaction model of photochemical catalytic oxidation aquatic products oxygen, there is very high catalytic activity (see figure 4).
Below in conjunction with specific embodiment, the present invention is specifically described, but protection scope of the present invention is not subject to the restriction of embodiment:
Embodiment 1
Be 1:1:1:1:10 by strontium nitrate, lanthanum nitrate, scandium nitrate, tantalic chloride and urea according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 50 DEG C, cross-linking reaction 10h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 24h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 900 DEG C, and the time is 48 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.72%, impurity content: carbon is less than 0.19%; Chlorine is less than 0.04%.
Embodiment 2
Be 1:1:1:1:10 by strontium nitrate, lanthanum nitrate, scandium nitrate, tantalic chloride and urea according to mol ratio, after accurately weighing, put into ethanol water (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 50 DEG C, cross-linking reaction 10h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 24h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 900 DEG C, and the time is 48 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.79%, impurity content: carbon is less than 0.19%; Chlorine is less than 0.03%.
Embodiment 3
Be 1:1:1:1:200 by strontium nitrate, lanthanum nitrate, scandium nitrate, tantalic chloride and urea according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:100) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 50 DEG C, cross-linking reaction 10h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 24h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 600 DEG C, and the time is 48 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.78%, impurity content: carbon is less than 0.17%; Chlorine is less than 0.03%.
Embodiment 4
Be 1:1:1:1:20 by strontium nitrate, lanthanum nitrate, scandium nitrate, tantalic chloride and citric acid according to mol ratio, after accurately weighing, put into glycol water (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 200 DEG C, cross-linking reaction 5h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 24h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 850 DEG C, and the time is 10 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.81%, impurity content: carbon is less than 0.10%; Chlorine is less than 0.01%.
Embodiment 5
Be 1:1:1:1:10 by strontium nitrate, lanthanum nitrate, scandium nitrate, tantalic chloride and oxalic acid according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 400 DEG C, cross-linking reaction 1h, other conditions are with embodiment 1, i.e. SLSTON powder processed. Its product purity is not less than 99.72%, impurity content: carbon is less than 0.19%; Chlorine is less than 0.04%.
Embodiment 6
Be 1:1:1:1:10 by strontium chloride, lanthanum chloride, scandium chloride, tantalic chloride and hexamethylenetetramine according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 200 DEG C, cross-linking reaction 1h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 24h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 900 DEG C, and the time is 48 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.01%, impurity content: carbon is less than 0.19%; Chlorine is less than 0.14%.
Embodiment 7
Be 1:1:1:1:20 by strontium nitrate, lanthanum nitrate, scandium nitrate, five ethoxy-tantalum and citric acid according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 200 DEG C, cross-linking reaction 1h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 8h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 850 DEG C, and the time is 10 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.92%, impurity content: carbon is less than 0.05%; Chlorine is less than 0.01%.
Embodiment 8
Be 1:1:1:1:30 by strontium nitrate, lanthanum nitrate, scandium nitrate, five ethoxy-tantalum and citric acid according to mol ratio, after accurately weighing, put into methanol aqueous solution (volume ratio 1:1) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 400 DEG C, cross-linking reaction 1h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 4h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 900 DEG C, and the time is 10 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.88%, impurity content: carbon is less than 0.09%; Chlorine is less than 0.01%.
Embodiment 9
Be 1:1:1:1:10 by strontium nitrate, lanthanum nitrate, scandium nitrate, five ethoxy-tantalum and urea according to mol ratio, after accurately weighing, put into ethanol water (volume ratio 1:2) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 300 DEG C, cross-linking reaction 5h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 800 DEG C of reaction temperatures, the reaction time is 10h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 850 DEG C, and the time is 12 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 99.82%, impurity content: carbon is less than 0.09%; Chlorine is less than 0.02%.
Embodiment 10
Be 1:1:1:1:50 by strontium chloride, lanthanum chloride, scandium chloride, five ethoxy-tantalum and hexamethylenetetramine according to mol ratio, after accurately weighing, put into ethanol water (volume ratio 1:10) stirring and dissolving, the time is greater than 30 minutes. By this solution, at 100 DEG C, cross-linking reaction 8h, puts into mortar and grinds carefully, and milling time is 30 minutes. After being packed in crucible, above-mentioned cross-linking products mixture puts into chamber type electric resistance furnace, calcination reaction, and 400 DEG C of reaction temperatures, the reaction time is 20h. After reaction, naturally cool to room temperature, by product nitrogen treatment under ammonia atmosphere, nitriding temperature is 600 DEG C, and the time is 30 hours, cooling after, i.e. SLSTON powder processed. Its product purity is not less than 98.91%, impurity content: carbon is less than 0.23%; Chlorine is less than 0.15%.
Conclusion: the present invention, by utilizing combustion assisting agent, has realized Low Temperature Solid-Phase and calcined the technical process of producing pure phase SLSTON powder. By many groups contrast test, find that combustion assisting agent plays an important role in reaction, utilize its fusing in reaction and burning heat release successfully to generate the SLSTON powder with good crystallinity. Preparation method of the present invention can be applied to the chemical synthesis research of other functional material similar with SLSTON equally, and has broad application prospects.
Claims (10)
1. a preparation method for SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder, is characterized in that: step is as follows: after soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent are fully dissolved in alcohol water mixed solution, cross-linking reaction occurs in heating; Then grinding crosslinked product makes to be fully mixed evenly; Be cross-linked product by high-temperature calcination again, make it form predecessor; Predecessor is nitrogenize high-temperature process under ammonia atmosphere, obtains SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder.
2. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: the mol ratio of described soluble strontium salt, lanthanum salt, scandium salts, tantalum salt and combustion assisting agent is 1: 1: 1: 1: 10～200.
3. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described soluble strontium salt is strontium chloride SrCl2·6H2O and strontium nitrate Sr (NO3)2·4H2One in O.
4. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described solubility lanthanum salt is lanthanum chloride LaCl3·7H2O and lanthanum nitrate La (NO3)3·6H2One in O.
5. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described solubility scandium salts is scandium chloride ScCl3With scandium nitrate Sc (NO3)3·4H2One in O.
6. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described solubility tantalum salt is tantalic chloride TaCl5With five ethoxy-tantalum Ta (C2H5O)5In one.
7. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described combustion assisting agent is the one in urea, citric acid, oxalic acid or hexamethylenetetramine.
8. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: described alcohol water mixed solution is the mixed solution of a kind of and water in methyl alcohol, ethanol or ethylene glycol.
9. according to the preparation method of the SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder described in claim 1 or 8, it is characterized in that: the alcohol and water of described alcohol water mixed solution is that 1:1～1:100 mixes according to volume ratio; Described cross-linking reaction temperature is at 50～400 DEG C, and cross-linking reaction time is 1～10h.
10. the preparation method of SLSTON Ca-Ti ore type nitrogen oxide solid-solution powder according to claim 1, is characterized in that: the reaction temperature of described high-temperature calcination cross-linking products is at 400～800 DEG C, and the reaction time is 4～24h; Described nitrogenize high-temperature process temperature is at 600～900 DEG C, and the reaction time is 4～48h.
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