CN105293585B - A kind of iron titanate nano-powder of zinc-nickel doping and preparation method thereof - Google Patents
A kind of iron titanate nano-powder of zinc-nickel doping and preparation method thereof Download PDFInfo
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- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000011858 nanopowder Substances 0.000 title claims abstract description 36
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011701 zinc Substances 0.000 claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 13
- 239000013081 microcrystal Substances 0.000 claims abstract description 10
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims abstract description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 9
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000003380 propellant Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 34
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 20
- 229930195725 Mannitol Natural products 0.000 claims description 20
- 235000010355 mannitol Nutrition 0.000 claims description 20
- 239000000594 mannitol Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 16
- 150000001455 metallic ions Chemical class 0.000 claims description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 229910021645 metal ion Inorganic materials 0.000 claims description 9
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract 1
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 20
- 239000000203 mixture Substances 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention discloses iron titanate nano-powder of a kind of zinc-nickel doping and preparation method thereof, it is specifically with iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride as raw material, blended, evaporate, be dried, twice heat treatment prepares described iron titanate nano-powder, the formula of gained iron titanate nano-powder is Fe1‑xZnx‑yNiyTiO3, wherein, 0.1≤x≤0.3,0 < y < x；Its size of microcrystal is 20 50nm.The iron titanate nano-powder of gained zinc-nickel of the present invention doping has different-grain diameter and different specific surface area, can be used as improving the catalytic additive of Properties of propellant.
Description
Technical field
The invention belongs to metal oxide functional field of material technology, be specifically related to iron titanate nano-powder of a kind of zinc-nickel doping and preparation method thereof.
Background technology
Iron titanate composite oxides are a kind of metal oxide functional materials, and it all has a wide range of applications in fields such as magnetic, catalysis, energy storage.The iron titanate powder body of high-quality is the basis preparing performance function material, and it usually requires that powder body composition uniformly, and size of microcrystal is little, soilless sticking or few reunion, to improve the performance of material.The method preparing iron titanate composite oxides at present mainly has solid reaction process, hydro-thermal method and chemical coprecipitation etc..Although solid reaction process has, technology of preparing is simple, low cost and other advantages, but the powder grain particle diameter that this method is prepared is big, and chemical uniformity is poor, it is not easy to obtain pure phase；Hydro-thermal method can prepare the crystal grain that crystallite dimension is less, but hydro-thermal method equipment and instrument is expensive, and operation with high pressure is not easily accomplished industrial scale and produces；Chemical coprecipitation technique is simple, operating aspect, it is easy to industrialized production, but shortcoming is the washing difficulty of the sedimentation method.
Summary of the invention
It is an object of the invention to provide iron titanate nano-powder of a kind of zinc-nickel doping and preparation method thereof, gained iron titanate nano-powder has different-grain diameter and different specific surface area, make it be catalyzed activity there are differences, and can be used as to improve the catalytic additive of Properties of propellant as required.
For achieving the above object, the present invention adopts the following technical scheme that
The iron titanate nano-powder of a kind of zinc-nickel doping, its formula is Fe1-xZnx-yNiyTiO3, wherein, 0.1≤x≤0.3,0 < y < x；
The size of microcrystal of gained iron titanate nano-powder is 20-50nm.
The preparation method of the iron titanate nano-powder of described zinc-nickel doping comprises the following steps:
1) weigh iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride by required ferrum, zinc, nickel, the mol ratio of titanium ion, be dissolved in ethanol, be made into metallic ion mixed liquor；Then in gained metallic ion mixed liquor, add mannitol mixing；
2) solvent evaporative removal solvent step 1) obtained, obtains gel；
3) by step 2) the heated dry formation xerogel of gel that obtains；
4), after xerogel step 3) obtained grinds, carry out heat treatment under an argon atmosphere, obtain black powder；
5) black powder step 4) obtained carries out secondary heat treatment in atmosphere, thus obtains the iron titanate nano-powder of described zinc-nickel doping.
In step 1), mannitol is 1-3:1 with the mol ratio of total metal ion.
In step 3), the temperature of heat drying is 120 DEG C, and drying time is 6 hours.
In step 4), the temperature of heat treatment is 500-900 DEG C, and heat treatment time is 0.5-3 hour.
In step 5), the temperature of secondary heat treatment is 600-900 DEG C, and heat treatment time is 0.5-3 hour.
The iron titanate nano-powder of zinc-nickel of the present invention doping can be used as improving the catalytic additive of Properties of propellant.
The method of the iron titanate nano-powder that the present invention prepares zinc-nickel doping is the sol-gal process of a kind of improvement, and it is based on oxidation-reduction reaction principle, and wherein nitrate ion used is as oxidant, and mannitol is as chelating agent and fuel.Mannitol and zinc, nickel, ferrum plasma effect, form complex, and therefore reactant mixes with atomic level, can effectively shorten diffusion length, reduces reaction temperature, is conducive to reaction quickly to carry out.
The present invention is by the adjustment of mannitol with metal ion mixed proportion, and obtain the composite mixed iron titanate presoma of zinc, nickel and the mixture of carbon template being decomposed to form by mannitol by calcining in an inert atmosphere, the effect of suppression iron titanate crystal grain fast growth can be played；Afterwards by calcining this mixture under different temperatures in atmosphere, to go de-carbon template acquisition to have different-grain diameter and the different zinc of specific surface area, nickel composite mixed iron titanate nano-powder, its course of reaction is easy, without high pressure equipment, subsequent heat treatment temperature is less than 900 DEG C, and product purity is high, granularity is controlled, narrow particle size distribution.
Detailed description of the invention
A kind of iron titanate nano-powder of zinc-nickel doping, its preparation method comprises the following steps:
1) it is that 1-x:x-y:y:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride by ferrum, zinc, nickel, the mol ratio of titanium ion, is dissolved in ethanol, is made into metallic ion mixed liquor, wherein, 0.1≤x≤0.3,0 < y < x；Then adding mannitol mixing in gained metallic ion mixed liquor, mannitol is 1-3:1 with the mol ratio of total metal ion；
2) solvent step 1) obtained is in 60 DEG C of evaporative removal solvents, obtains gel；
3) by step 2) gel that obtains is dried 6 hours through 120 DEG C and forms xerogel；
4), after the xerogel that step 3) obtained grinds, in argon gas atmosphere, heat treatment 0.5-3 hour at 500-900 DEG C, black powder is obtained；
5) black powder that step 4) is obtained in atmosphere, secondary heat treatment 0.5-3 hour at 600-900 DEG C, thus obtain the iron titanate nano-powder with the zinc-nickel doping of different-grain diameter, different specific surface area, its size of microcrystal is 20-50nm.
In order to make content of the present invention easily facilitate understanding, below in conjunction with detailed description of the invention, technical solutions according to the invention are described further, but the present invention is not limited only to this.
Embodiment 1, prepare formula and meet Fe0.9Zn0.05Ni0.05TiO3Zinc-nickel doping iron titanate nano-powder
It is that 0.9:0.05:0.05:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride according to the mol ratio of ferrum, zinc, nickel and titanium ion, it is dissolved in ethanol, it is stirred continuously and makes it fully dissolve, after forming limpid metallic ion mixed liquor, adding mannitol mixing in gained metallic ion mixed liquor, making mannitol is 1:1 with the mol ratio of total metal ion；Then at 60 DEG C, heating evaporation removes solvent, forms gel；Move to gained gel constant temperature oven heats 6 hours at 120 DEG C, obtain fluffy xerogel；By xerogel in mortar finely ground after, be placed in tube furnace, calcine 0.5 hour in argon gas atmosphere, at 500 DEG C, obtain black powder；The black powder obtained is calcined 0.5 hour in air atmosphere, at 900 DEG C, obtains formula and meet Fe0.9Zn0.05Ni0.05TiO3Zinc-nickel doping iron titanate nano-powder.
Observing gained powder under JEM2010 transmission electron microscope, its size of microcrystal is 20-30nm.
Take 5mg and add the ammonium perchlorate mixture of this powder of 2wt%, it is placed in differential scanning calorimeter and is analyzed, result shows, contrast with pure ammonium perchlorate, the heat decomposition temperature that with the addition of the ammonium perchlorate mixture's hot stage after this powder of 2wt% reduces 90 DEG C, illustrates that it can be effectively improved the thermal decomposition performance of ammonium perchlorate.
Embodiment 2, prepare formula and meet Fe0.7Zn0.2Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder
It is that 0.7:0.2:0.1:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride according to the mol ratio of ferrum, zinc, nickel and titanium ion, it is dissolved in ethanol, it is stirred continuously and makes it fully dissolve, after forming limpid metallic ion mixed liquor, adding mannitol mixing in gained metallic ion mixed liquor, making mannitol is 3:1 with the mol ratio of total metal ion；Then at 60 DEG C, heating evaporation removes solvent, forms gel；Move to gained gel constant temperature oven heats 6 hours at 120 DEG C, obtain fluffy xerogel；By xerogel in mortar finely ground after, be placed in tube furnace, calcine 3 hours in argon gas atmosphere, at 900 DEG C, obtain black powder；The black powder obtained is calcined 3 hours in air atmosphere, at 900 DEG C, obtains described formula and meet Fe0.7Zn0.2Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder.
Observing gained powder under JEM2010 transmission electron microscope, its size of microcrystal is 30-50nm.
Take 5mg and add the ammonium perchlorate mixture of this powder of 2wt%, it is placed in differential scanning calorimeter and is analyzed, result shows, contrast with pure ammonium perchlorate, the heat decomposition temperature that with the addition of the ammonium perchlorate mixture's hot stage after this powder of 2wt% reduces 50 DEG C, illustrates that it can be effectively improved the thermal decomposition performance of ammonium perchlorate.
Embodiment 3, prepare formula and meet Fe0.8Zn0.1Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder
It is that 0.8:0.1:0.1:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride according to the mol ratio of ferrum, zinc, nickel and titanium ion, it is dissolved in ethanol, it is stirred continuously and makes it fully dissolve, after forming limpid metallic ion mixed liquor, adding mannitol mixing in gained metallic ion mixed liquor, making mannitol is 2:1 with the mol ratio of total metal ion；Then at 60 DEG C, heating evaporation removes solvent, forms gel；Move to gained gel constant temperature oven heats 6 hours at 120 DEG C, obtain fluffy xerogel；By xerogel in mortar finely ground after, be placed in tube furnace, calcine 2 hours in argon gas atmosphere, at 700 DEG C, obtain black powder；The black powder obtained is calcined 1.5 hours in air atmosphere, at 800 DEG C, obtains described formula and meet Fe0.8Zn0.1Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder.
Observing gained powder under JEM2010 transmission electron microscope, its size of microcrystal is 25-40nm.
Take 5mg and add the ammonium perchlorate mixture of this powder of 2wt%, it is placed in differential scanning calorimeter and is analyzed, result shows, contrast with pure ammonium perchlorate, the heat decomposition temperature that with the addition of the ammonium perchlorate mixture's hot stage after this powder of 2wt% reduces 60 DEG C, illustrates that it can be effectively improved the thermal decomposition performance of ammonium perchlorate.
Embodiment 4, prepare formula and meet Fe0.85Zn0.1Ni0.05TiO3Zinc-nickel doping iron titanate nano-powder
It is that 0.85:0.1:0.05:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride according to the mol ratio of ferrum, zinc, nickel and titanium ion, it is dissolved in ethanol, it is stirred continuously and makes it fully dissolve, after forming limpid metallic ion mixed liquor, adding mannitol mixing in gained metallic ion mixed liquor, making mannitol is 1.5:1 with the mol ratio of total metal ion；Then at 60 DEG C, heating evaporation removes solvent, forms gel；Move to gained gel constant temperature oven heats 6 hours at 120 DEG C, obtain fluffy xerogel；By xerogel in mortar finely ground after, be placed in tube furnace, calcine 2.5 hours in argon gas atmosphere, at 800 DEG C, obtain black powder；The black powder obtained is calcined 1.5 hours in air atmosphere, at 800 DEG C, obtains described formula and meet Fe0.85Zn0.1Ni0.05TiO3Zinc-nickel doping iron titanate nano-powder.
Observing gained powder under JEM2010 transmission electron microscope, its size of microcrystal is 25-40nm.
Take 5mg and add the ammonium perchlorate mixture of this powder of 2wt%, it is placed in differential scanning calorimeter and is analyzed, result shows, contrast with pure ammonium perchlorate, the heat decomposition temperature that with the addition of the ammonium perchlorate mixture's hot stage after this powder of 2wt% reduces 70 DEG C, illustrates that it can be effectively improved the thermal decomposition performance of ammonium perchlorate.
Embodiment 5, prepare formula and meet Fe0.75Zn0.15Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder
It is that 0.75:0.15:0.1:1 weighs iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride according to the mol ratio of ferrum, zinc, nickel and titanium ion, it is dissolved in ethanol, it is stirred continuously and makes it fully dissolve, after forming limpid metallic ion mixed liquor, adding mannitol mixing in gained metallic ion mixed liquor, making mannitol is 2.5:1 with the mol ratio of total metal ion；Then at 60 DEG C, heating evaporation removes solvent, forms gel；Move to gained gel constant temperature oven heats 6 hours at 120 DEG C, obtain fluffy xerogel；By xerogel in mortar finely ground after, be placed in tube furnace, calcine 1 hour in argon gas atmosphere, at 750 DEG C, obtain black powder；The black powder obtained is calcined 1 hour in air atmosphere, at 900 DEG C, obtains described formula and meet Fe0.75Zn0.15Ni0.1TiO3Zinc-nickel doping iron titanate nano-powder.
Observing gained powder under JEM2010 transmission electron microscope, its size of microcrystal is 35-25nm.
Take 5mg and add the ammonium perchlorate mixture of this powder of 2wt%, it is placed in differential scanning calorimeter and is analyzed, result shows, contrast with pure ammonium perchlorate, the heat decomposition temperature that with the addition of the ammonium perchlorate mixture's hot stage after this powder of 2wt% reduces 65 DEG C, illustrates that it can be effectively improved the thermal decomposition performance of ammonium perchlorate.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.
Claims (6)
1. the preparation method of the iron titanate nano-powder of a zinc-nickel doping, it is characterised in that: comprise the following steps:
1) weigh iron chloride, zinc nitrate, nickel nitrate and titanium tetrachloride by required ferrum, zinc, nickel, the mol ratio of titanium ion, be dissolved in ethanol, be made into metallic ion mixed liquor；Then in gained metallic ion mixed liquor, add mannitol mixing；
2) solution evaporation step 1) obtained removes solvent, obtains gel；
3) by step 2) the heated dry formation xerogel of gel that obtains；
4), after xerogel step 3) obtained grinds, carry out heat treatment under an argon atmosphere, obtain black powder；
5) black powder step 4) obtained carries out secondary heat treatment in atmosphere, thus obtains the iron titanate nano-powder of described zinc-nickel doping；Its formula is Fe1-xZnx-yNiyTiO3, wherein, 0.1≤x≤0.3,0 < y < x；
The size of microcrystal of described iron titanate nano-powder is 20-50nm.
The preparation method of the iron titanate nano-powder of zinc-nickel doping the most according to claim 1, it is characterised in that: in step 1), mannitol is 1-3:1 with the mol ratio of total metal ion.
The preparation method of the iron titanate nano-powder of zinc-nickel doping the most according to claim 1, it is characterised in that: in step 3), the temperature of heat drying is 120 DEG C, and drying time is 6 hours.
The preparation method of the iron titanate nano-powder of zinc-nickel doping the most according to claim 1, it is characterised in that: in step 4), the temperature of heat treatment is 500-900 DEG C, and heat treatment time is 0.5-3 hour.
The preparation method of the iron titanate nano-powder of zinc-nickel doping the most according to claim 1, it is characterised in that: in step 5), the temperature of secondary heat treatment is 600-900 DEG C, and heat treatment time is 0.5-3 hour.
6. the application of the iron titanate nano-powder of the zinc-nickel doping that a method as claimed in claim 1 prepares, it is characterised in that: for the catalytic additive as raising Properties of propellant.
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