CN105540677A - Preparation method of yttrium ferrite powder - Google Patents
Preparation method of yttrium ferrite powder Download PDFInfo
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Abstract
The invention discloses a preparation method for combustion synthesis of yttrium ferrite powder. The method comprises steps as follows: firstly, yttrium nitrate and ferric nitrate in the mole ratio being (1-1.5):(1-1.5) are dissolved in deionized water, and a mixed nitrate solution is obtained; then a reducing agent is added, an obtained mixed solution is controlled at the temperature of 200-600 DEG C for a combustion synthesis reaction for 5-30 min, a product is naturally cooled to the room temperature, and the yttrium ferrite powder is obtained. The method is applicable to preparation of the yttrium ferrite powder doped with ions. The yttrium ferrite powder obtained with the preparation method is loose, easy to treat, small in particle and high in purity, the reaction is quick, the efficiency is high, and equipment and the process are simple.
Description
Technical field
The invention belongs to inorganic non-metallic ultrafine powder preparation field, namely relate to a kind of preparation method of ferrous acid yttrium powder, particularly a kind of preparation method of conbustion synthesis ferrous acid yttrium powder.
Background technology
Rare earth orthoferrite ferrous acid yttrium (YFeO
3) orthogonal thereto perovskite structure, be a kind of stable semiconductor material, band gap (Eg) is about 2.58eV, and research discloses, YFeO
3important application prospect is had in blue laser diode, electrode materials, magnetic field sensor, magneto-optic data memory device and photocatalysis field.Ion doping can change ferrous acid yttrium performance, as mixed magnesium and zinc can improve its gas sensing property, mix manganese and can strengthen its multiferroic, mix gadolinium and can change its magnetic property.
Obtain the crystalline material or stupalith with high-performance, the synthesis of powder is committed step wherein.At present, prepare ferrous acid yttrium powder and mainly adopt solid phase method, chemical coprecipitation, sol-gel-spontaneous combustion method synthesis.Due to Y
3feO
12at Y
2o
3-Fe2O
3preferential formation in system, so synthesize single-phase YFeO
3very difficult.
Conventional solid reaction method is often difficult to obtain high-purity single-phase YFeO
3, in product, often can there is binary oxide (as Z 250) and Y
3feO
12deng dephasign, this method also exists that raw material mixing time is long, synthesis reaction temperature is high and product diameter of particle and pattern are difficult to the shortcomings such as control in addition, thus greatly have impact on the performance of material.Although chemical coprecipitation can prepare pure phase powder, also need to calcine 4 hours at 900 DEG C, and powder is easily reunited, and needs later stage milled processed.Sol-gel-spontaneous combustion legal system is for YFeO
3realized by following concrete steps, first prepare the nitrate of rare earth metal or the muriatic aqueous solution, iron nitrate or ferric chloride in aqueous solution, aqueous citric acid solution, subsequently by the aqueous solution of above-mentioned preparation, heat and stir, them are made to form sol-gel precursor, again the sol-gel precursor obtained is inserted in the process furnace of 550-650 DEG C afterwards and carry out spontaneous combustion synthesis, finally again the spontaneous combustion product obtained is calcined 2-4 hour at 600-800 DEG C.The advantage of sol-gel method is that the mixing participating in each component of reacting is carried out in atom, molecule rank, can solve and prepare powder admixtion chemical homogeneous sex chromosome mosaicism, thus other additive in matrix intercrystalline phase and crystallization phases is uniformly distributed.Compared with solid reaction process, the material of sol-gel process synthesis has the advantages such as purity is high, distributed components, particle are little, particle size distribution range is narrow, good dispersity.Secondly adopt the material of sol-gel method synthesis generally without the need to follow-up grinding, and synthesis temperature is lower than traditional high temperature process heat method.As can be seen here, sol-gel-spontaneous combustion method have preparation technology simple, without the need to specific installation, can handling strong, product purity advantages of higher, but the presoma that this method also exists gained be difficult to washing and expensive starting materials, cost higher, be not suitable for the problems such as industrialization.
In sum, above-mentioned at present various preparation YFeO
3all there are some shortcomings in the method for powder, particularly in product purity, powder reuniting, process complexity, industrialization etc., there are some problems, and these become preparation high-quality YFeO
3the bottleneck of material and application thereof.
Low-temperature combustion synthesis (lowcombustionsynthesis, be called for short LCS) mainly using soluble metallic salt (mainly nitrate) and organic-fuel (as urea, citric acid, glycine etc.) as reactant, metal nitrate serves as oxygenant in the reaction, organic-fuel serves as reductive agent in the reaction, reactant system is lighted by extraneous zero energy within very short time, causes violent oxidation-reduction reaction.Reaction system is once light, namely reaction is maintained the carrying out of himself reaction by oxidation-reduction reaction liberated heat, these heats promote mass transport between each reactant and diffusion on the one hand, be conducive to the carrying out reacted, pass to rapidly the unreacted reactant closed on reactant on the other hand, its temperature is raised thus makes reaction be able to from maintaining, whole combustion processes can terminate in several minutes, there is rapidly oxidation-reduction reaction burning at short notice in a large amount of organic compositions, and overflow a large amount of gas, therefore the solid product stayed must contain a large amount of hole, form the distinctive quality of LCS primary product to loosen, the shape characteristic of porous microstructure, easy pulverizing can be formed, the nanometer superfine oxide powder that specific surface area is high.Low-temperature combustion synthesis has following superiority:
(1) low igniting decomposition temperature, once light, decomposition or Automatic Combustion are carried out;
(2) a large amount of gas is formed as NH
3, H
2o, CO
2and N
2, loose being easy to of the powder of synthesis is like this pulverized, and can form the superfine oxide powder that specific surface area is high;
(3) stoichiometric ratio is accurate, and uniformity coefficient is high, can reach molecule or atom level to its uniformity coefficient of multicomponent system, can synthesize and be difficult to containing the new oxide of multiple doped element and traditional method the sintering metal etc. prepared;
(4) these superfine powders have higher sintering activity, and the firing temperature of the product that the firing temperature of target product obtains than conventional solid reaction method is low.
Because low-temperature combustion synthesis has series of advantages, therefore paid close attention to widely, this kind of method becomes the important means of superfine powder synthesis.
Reference:
[1] Ge Xiutao, Chu Xiangfeng, Liu Xingqin, mixes magnesium YFeO
3the conductance of sosoloid and air-sensitive performance research, Chinese Journal of Chemical Physics, 2000,13 (3): 349-353.
[2]HuiShen,JiayueXu,MinJin,GuojianJiang,InfluenceofmanganeseonthestructureandmagneticpropertiesofYFeO
3nanocrystal,CeramicsInternational,2012,38:1473-1477
Summary of the invention
Object of the present invention in order to solve complex process in above-mentioned preparation method, product purity low, be difficult to the technical problems such as industrialization, and proposing a kind of preparation method of ferrous acid yttrium powder, the method has that technique is simple, product purity is high, be easy to the advantages such as industrialization.
Technical scheme of the present invention
A preparation method for ferrous acid yttrium powder, specifically comprises the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1-1.5:1-1.5, Yttrium trinitrate and iron nitrate are added in deionized water and dissolve, obtain mixed nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 250-1000ml:1mol;
(2), by reductive agent join in step (1) gained mixed nitrate solution, stir 30-50 minute, reductive agent is dissolved, obtains mixing solutions;
The add-on of described reductive agent changes because of the kind difference of reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 0.75-10:1;
Described reductive agent is urea, citric acid, ethylenediamine tetraacetic acid (EDTA) or hydrazine; Or be the mixture of urea and hydrazine composition; Or be the mixture of citric acid and ethylenediamine tetraacetic acid (EDTA) composition;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5-30 minute at control temperature is 200-600 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
The preparation method of above-mentioned a kind of ferrous acid yttrium powder is applicable to the preparation of the ferrous acid yttrium powder of ion doping, described dopant ion is a kind of or two or more arbitrarily mixture in mn ion, magnesium ion, gadolinium ion, zine ion, and its preparation process concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: the ratio of dopant ion is the ratio of 0.85-1.45:0.85-1.45:0.05-0.3, the nitrate of Yttrium trinitrate, iron nitrate and dopant ion is joined in deionized water and dissolves, obtain mixed nitrate solution;
The nitrate of described dopant ion is a kind of or two or more arbitrarily mixture in manganous nitrate, magnesium nitrate, Gadolinium trinitrate, zinc nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 450-675ml:1mol;
(2), by reductive agent join in step (1) gained mixed nitrate solution, stir and reductive agent was dissolved in 30-50 minute, obtain mixing solutions;
The add-on of described reductive agent changes because of the kind difference of reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 1-13:1;
Described reductive agent is urea or citric acid;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5-30 minute at control temperature is 200-600 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of ion doping.
Advantageous Effects of the present invention
The preparation method of a kind of ferrous acid yttrium powder of the present invention and ion doping ferrous acid yttrium powder, because combustion synthesis technology overcomes the shortcoming existed in current synthetic method, and has following beneficial effect:
(1) the present invention carries out conbustion synthesis at 200-600 DEG C, and indirect heating temperature is low, and energy consumption is low, is conducive to the production cost reducing ferrous acid yttrium powder;
(2) present invention process is simple, and efficiency is high, is easy to industrialization;
(3) product purity of the present invention's acquisition is high, and particle is tiny, does not need later stage milled processed.
(4) utilize the present invention to carry out the doping of ferrous acid yttrium, stoichiometric ratio is accurate, and uniformity coefficient is high, can reach molecule or atom level, can synthesize the new oxide containing multiple doped element to its uniformity coefficient of multicomponent system.
Accompanying drawing explanation
The thing phase composite figure of the ferrous acid yttrium powder of Fig. 1, embodiment 1 gained;
The shape appearance figure of the ferrous acid yttrium powder of Fig. 2, embodiment 1 gained.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
embodiment 1
A preparation method for ferrous acid yttrium powder, specifically comprises the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1:1,1mol Yttrium trinitrate and 1mol iron nitrate are joined in 1000ml deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 500ml:1mol;
(2), the reductive agent urea of 20mol is joined in the mixed nitrate solution of step (1) gained, stir 30 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium and metal ion iron is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 200 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
The ferrous acid yttrium powder of above-mentioned gained measures through Rigaku D/max2200PC type X-ray diffractometer, and as shown in Figure 1, as can be seen from Figure 1 the XRD figure of products obtained therefrom is composed and standard YFeO in the thing phase composite of gained
3orthorhombic phase collection of illustrative plates (JCPDS73-1345) conforms to, and indicating the product obtained thus is ferrous acid yttrium powder, and feature three strongest ones peak is sharp-pointed, and complete crystallization is described.
The ferrous acid yttrium powder of above-mentioned gained scans through tungsten lamp S-3400N scanning electronic microscope, the product morphology figure of gained as shown in Figure 2, as can be seen from Figure 2 ferrous acid yttrium powder granule shape approximation is spherical, size is comparatively even, median size is about 190nm, show that this preparation method particle diameter that is easy to get is less thus, and homogeneous ferrous acid yttrium powder.
embodiment 2
A preparation method for ferrous acid yttrium powder, specifically comprises the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1:1.1,1mol Yttrium trinitrate and 1.1mol iron nitrate are joined in 1100mL deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 523.8ml:1mol;
(2), the reductive agent urea of 21mol is joined in the mixed nitrate solution of step (1) gained, stir 40 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium and metal ion iron is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 250 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
The ferrous acid yttrium powder of above-mentioned gained, its powder median size is 198nm after measured.
embodiment 3
A preparation method for ferrous acid yttrium powder, specifically comprises the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1.1:1,1.1mol Yttrium trinitrate and 1mol iron nitrate are joined in 1100mL deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 523.8ml:1mol;
(2), the reductive agent urea of 21mol is joined in the mixed nitrate solution of step (1) gained, stir 40 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium and metal ion iron is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 250 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
The ferrous acid yttrium powder of above-mentioned gained, its powder median size is 198nm after measured.
embodiment 4
A preparation method for ferrous acid yttrium powder, specifically comprises the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1.5:1.5,1.5mol Yttrium trinitrate and 1.5mol iron nitrate are joined in 1500mL deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 500ml:1mol;
(2), the reductive agent urea of 30mol is joined in the mixed nitrate solution of step (1) gained, stir 50 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium and metal ion iron is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 30 minutes at temperature is 600 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
The ferrous acid yttrium powder of above-mentioned gained, its powder median size is 205nm after measured.
embodiment 5
A preparation method for ferrous acid yttrium powder, joins in 500ml deionized water by 1mol Yttrium trinitrate and 1mol iron nitrate and dissolves, obtain mixed nitrate solution; The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 250ml:1mol;
And then the reductive agent citric acid adding 2mol obtains mixing solutions, all the other are with embodiment 1, finally obtain the ferrous acid yttrium powder that median size is 110nm;
The add-on of described reductive agent citric acid, calculates in molar ratio, reductive agent citric acid: the total amount of metal ion yttrium and metal ion iron is 1:1.
embodiment 6
A preparation method for ferrous acid yttrium powder, joins in 2000ml deionized water by 1mol Yttrium trinitrate and 1mol iron nitrate and dissolves, obtain mixed nitrate solution; The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 1000ml:1mol;
And then the reductive agent ethylenediamine tetraacetic acid (EDTA) adding 1.5mol obtains mixing solutions, all the other are with embodiment 1, finally obtain the ferrous acid yttrium powder that median size is about 60nm;
The add-on of described reductive agent ethylenediamine tetraacetic acid (EDTA), calculates in molar ratio, reductive agent ethylenediamine tetraacetic acid (EDTA): the total amount of metal ion yttrium and metal ion iron is 0.75:1.
embodiment 7
A preparation method for ferrous acid yttrium powder, joins in 650ml deionized water by 1mol Yttrium trinitrate and 1mol iron nitrate and dissolves, obtain mixed nitrate solution; The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 325ml:1mol;
And then the hydrazine reducing agent adding 7.5mol obtains mixing solutions, all the other are with embodiment 1, finally obtain the ferrous acid yttrium powder that median size is about 55nm;
The add-on of above-mentioned hydrazine reducing agent, calculates in molar ratio, hydrazine reducing agent: the total amount of metal ion yttrium and metal ion iron is 3.75:1.
embodiment 8
A preparation method for ferrous acid yttrium powder, joins in 750ml deionized water by 1mol Yttrium trinitrate and 1mol iron nitrate and dissolves, obtain mixed nitrate solution; The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 475ml:1mol;
And then add reductive agent and 10mol urea and 1mol hydrazine and obtain mixing solutions, at temperature is 200 DEG C, carry out combustion synthesis reaction 8 minutes, all the other are with embodiment 1, finally obtain the ferrous acid yttrium powder that median size is about 85nm;
Above-mentioned reductive agent urea and the add-on of hydrazine, calculate, reductive agent urea and hydrazine in molar ratio: the total amount of metal ion yttrium and metal ion iron is 9:1.
embodiment 9
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 1:1.05:0.05,1mol Yttrium trinitrate and 1.05mol iron nitrate and 0.05mol magnesium nitrate are joined in the deionized water of 1000mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 523.8ml:1mol;
(2), the reductive agent urea of 20.5mol is joined in the mixed nitrate solution of step (1) gained, stir 30 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron and dopant ion is 9.76:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 200 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of magnesium-doped ion.
The ferrous acid yttrium powder of the magnesium-doped ion of above-mentioned gained, its powder median size is 179nm after measured.
embodiment 10
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 0.85:1:0.15,0.85mol Yttrium trinitrate and 1mol iron nitrate and 0.15mol zinc nitrate are joined in the deionized water of 900mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and doped metal ion zinc is the ratio calculating of 450ml:1mol;
(2), the reductive agent urea of 18mol is joined in the mixed nitrate solution of step (1) gained, stir 30 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, iron and doped metal ion zinc is 9:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 200 DEG C, naturally cools to room temperature, the ferrous acid yttrium powder of the zine ion that must adulterate.
The ferrous acid yttrium powder of the doping zine ion of above-mentioned gained, its powder median size is 182nm after measured.
embodiment 11
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 1:1.1:0.1,1mol Yttrium trinitrate and 1.1mol iron nitrate and 0.1mol Gadolinium trinitrate are joined in the deionized water of 1200mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and doped metal ion gadolinium is the ratio calculating of 545.45ml:1mol;
(2), the reductive agent urea of 22mol is joined in the mixed nitrate solution of step (1) gained, stir 40 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron and doped metal ion gadolinium is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 15 minutes at temperature is 350 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of gadolinium-doped ion.
The ferrous acid yttrium powder of the gadolinium-doped ion of above-mentioned gained, its powder median size is 195nm after measured.
embodiment 12
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 1.45:1.35:0.05,1.45mol Yttrium trinitrate and 1.35mol iron nitrate and 0.05mol manganous nitrate are mixed to join in 1450mL deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and doped metal ion manganese is the ratio calculating of 508.77ml:1mol;
(2), the reductive agent urea of 28.5mol is joined in the mixed nitrate solution of step (1) gained, stir 50 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron and doped metal ion manganese is 10:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 20 minutes at temperature is 550 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of doped with manganese ion.
The ferrous acid yttrium powder of the doped with manganese ion of above-mentioned gained, its diameter of particle is 210nm after measured.
embodiment 13
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 0.85:0.85:0.3 (0.15+0.15), 0.85mol Yttrium trinitrate and 0.85mol iron nitrate and magnesium nitrate and each 0.15mol of manganous nitrate are joined in 1350mL deionized water and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron, doped metal ion magnesium and doped metal ion manganese is the ratio calculating of 675ml:1mol;
(2), the reductive agent urea of 26mol is joined in the mixed nitrate solution of step (1) gained, stir 40 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron, doped metal ion magnesium and doped metal ion manganese is 13:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 20 minutes at temperature is 550 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder that is magnesium-doped, mn ion.
The ferrous acid yttrium powder of magnesium-doped, the mn ion of above-mentioned gained, its powder median size is 180nm after measured.
embodiment 14
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: the dopant ion in the nitrate of dopant ion is the ratio of 1:1:0.2 (0.1+0.1), 1mol Yttrium trinitrate and 1mol iron nitrate and Gadolinium trinitrate and each 0.1mol of manganous nitrate are joined in the deionized water of 1100mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron, doped metal ion gadolinium and doped metal ion manganese is the ratio calculating of 500ml:1mol;
(2), the reductive agent urea of 21mol is joined in the mixed nitrate solution of step (1) gained, stir 30 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron, doped metal ion gadolinium and doped metal ion manganese is 9.55:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5 minutes at temperature is 250 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of gadolinium-doped, mn ion.
The gadolinium-doped of above-mentioned gained, the ferrous acid yttrium powder of mn ion, its powder median size is 200nm after measured.
embodiment 15
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: the dopant ion in the nitrate of dopant ion is the ratio of 1.45:1.45:0.1 (0.05+0.05), 1.45mol Yttrium trinitrate and 1.45mol iron nitrate and zinc nitrate and each 0.05mol of manganous nitrate are joined in the deionized water of 1480mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron, doped metal ion zinc and doped metal ion manganese is the ratio calculating of 493ml:1mol;
(2), the reductive agent urea of 29mol is joined in the mixed nitrate solution of step (1) gained, stir 50 minutes, obtain mixing solutions;
The add-on of described reductive agent urea, calculates in molar ratio, reductive agent urea: the total amount of metal ion yttrium, metal ion iron, doped metal ion zinc and doped metal ion manganese is 9.67:1;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 30 minutes at temperature is 600 DEG C, naturally cools to room temperature, the ferrous acid yttrium powder of the zinc that must adulterate, mn ion.
The doping zinc of above-mentioned gained, the ferrous acid yttrium powder of mn ion, its powder median size is 208nm after measured.
embodiment 16
A preparation method for the ferrous acid yttrium powder of dopant ion, concrete steps are as follows:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is the ratio of 1:1.05:0.05,1mol Yttrium trinitrate and 1.05mol iron nitrate and 0.05mol magnesium nitrate are joined in the deionized water of 1000mL and dissolves, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron, doped metal ion magnesium is the ratio calculating of 523.8ml:1mol;
(2), the reductive agent citric acid of 2.2mol is joined in the mixed nitrate solution of step (1) gained, stir 30 minutes, obtain mixing solutions;
The add-on of described reductive agent citric acid, calculates in molar ratio, reductive agent citric acid: the total amount of metal ion yttrium, metal ion iron, doped metal ion magnesium is 1:1.
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 8 minutes at temperature is 200 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of magnesium-doped ion.
The ferrous acid yttrium powder of the magnesium-doped ion of above-mentioned gained, its powder median size is 122nm after measured.
In sum, the preparation method of a kind of conbustion synthesis ferrous acid yttrium powder of the present invention, can synthesize the ferrous acid yttrium of pure phase and the ferrous acid yttrium powder of dopant ion thereof by the method, and the powder complete crystallization obtained, particle diameter ratio is comparatively even, and particle shape is similar to spherical.
Foregoing be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (19)
1. a preparation method for ferrous acid yttrium powder, is characterized in that specifically comprising the steps:
(1), in molar ratio calculate, i.e. Yttrium trinitrate: iron nitrate is the ratio of 1-1.5:1-1.5, Yttrium trinitrate and iron nitrate are added in deionized water and dissolve, obtain mixed nitrate solution;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 250-1000ml:1mol;
(2), by reductive agent join in step (1) gained mixed nitrate solution, stir 30-50 minute, reductive agent is dissolved, obtains mixing solutions;
The add-on of described reductive agent changes because of the kind difference of reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 0.75-10:1;
Described reductive agent is urea, citric acid, ethylenediamine tetraacetic acid (EDTA) or hydrazine; Or be the mixture of urea and hydrazine composition; Or be the mixture of citric acid and ethylenediamine tetraacetic acid (EDTA) composition;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5-30 minute at control temperature is 200-600 DEG C, naturally cools to room temperature, obtains ferrous acid yttrium powder.
2. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 500ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 10:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
3. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1.1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 523.8ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 10:1;
At temperature is 250 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
4. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1.1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 523.8ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 10:1;
At temperature is 250 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
5. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1.5:1.5;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 500ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 10:1;
At temperature is 600 DEG C, combustion synthesis reaction is carried out 30 minutes in step (3).
6. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 250ml:1mol;
Reductive agent used in step (2) is citric acid;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 1:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
7. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 1000ml:1mol;
Reductive agent used in step (2) is ethylenediamine tetraacetic acid (EDTA);
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 0.75:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
8. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 325ml:1mol;
Reductive agent used in step (2) is hydrazine;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 3.75:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
9. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate is 1:1;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium and metal ion iron is the ratio calculating of 475ml:1mol;
Reductive agent used in step (2) is that urea and hydrazine calculate in molar ratio, i.e. urea: hydrazine is the mixture of 10:1 composition;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium and metal ion iron is 9:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 8 minutes in step (3).
10. the preparation method of a kind of ferrous acid yttrium powder as claimed in claim 1 is applicable to the ferrous acid yttrium powder preparing ion doping, and described dopant ion is a kind of or two or more arbitrarily mixture in mn ion, magnesium ion, gadolinium ion, zine ion.
The preparation method of the ferrous acid yttrium powder of 11. ion dopings as claimed in claim 10, is characterized in that specifically comprising the steps:
(1), calculate in molar ratio, i.e. Yttrium trinitrate: iron nitrate: the ratio of dopant ion is the ratio of 0.85-1.45:0.85-1.45:0.05-0.3, the nitrate of Yttrium trinitrate, iron nitrate and dopant ion is joined in deionized water and dissolves, obtain mixed nitrate solution;
The nitrate of described dopant ion is a kind of or two or more arbitrarily mixture in manganous nitrate, magnesium nitrate, Gadolinium trinitrate, zinc nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 450-675ml:1mol;
(2), by reductive agent join in step (1) gained mixed nitrate solution, stir and reductive agent was dissolved in 30-50 minute, obtain mixing solutions;
The add-on of described reductive agent changes because of the kind difference of reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 1-13:1;
Described reductive agent is urea or citric acid;
(3), step (2) gained mixing solutions carries out combustion synthesis reaction 5-30 minute at control temperature is 200-600 DEG C, naturally cools to room temperature, obtains the ferrous acid yttrium powder of ion doping.
The preparation method of the ferrous acid yttrium powder of 12. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1:1.05:0.05;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 523.8ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 9.76:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 13. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 0.85:1:0.15;
The nitrate of described dopant ion is zinc nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 450ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 9:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 14. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1:1.1:0.1;
The nitrate of described dopant ion is Gadolinium trinitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 545.45ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 10:1;
At temperature is 350 DEG C, combustion synthesis reaction is carried out 15 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 15. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1.45:1.35:0.05;
The nitrate of described dopant ion is manganous nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 508.77ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 10:1;
At temperature is 550 DEG C, combustion synthesis reaction is carried out 20 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 16. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 0.85:0.85:0.3;
The nitrate of described dopant ion is the mixture that magnesium nitrate and manganous nitrate calculate in molar ratio as 1:1 forms;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 675ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 13:1;
At temperature is 550 DEG C, combustion synthesis reaction is carried out 20 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 17. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1:1:0.2;
The nitrate of described dopant ion is the mixture that Gadolinium trinitrate and manganous nitrate calculate in molar ratio as 1:1 forms;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 500ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 9.55:1;
At temperature is 250 DEG C, combustion synthesis reaction is carried out 5 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 18. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1.45:1.45:0.1;
The nitrate of described dopant ion is the mixture that zinc nitrate and manganous nitrate calculate in molar ratio as 1:1 forms;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 493ml:1mol;
Reductive agent used in step (2) is urea;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 9.67:1;
At temperature is 600 DEG C, combustion synthesis reaction is carried out 30 minutes in step (3).
The preparation method of the ferrous acid yttrium powder of 19. a kind of dopant ions as claimed in claim 11, is characterized in that calculating in molar ratio in step (1), i.e. Yttrium trinitrate: iron nitrate: in the nitrate of dopant ion, dopant ion is 1:1.05:0.05;
The nitrate of described dopant ion is magnesium nitrate;
The amount of deionized water used, in deionized water: the total amount of metal ion yttrium, metal ion iron and dopant ion is the ratio calculating of 523.8ml:1mol;
Reductive agent used in step (2) is citric acid;
The add-on of described reductive agent, calculates in molar ratio, reductive agent: the total amount of metal ion yttrium, metal ion iron and dopant ion is 1:1;
At temperature is 200 DEG C, combustion synthesis reaction is carried out 8 minutes in step (3).
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| CN109133182A (en) * | 2018-09-30 | 2019-01-04 | 江苏理工学院 | A kind of preparation method of macropore Manganese Ferrite |
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| CN106277065A (en) * | 2015-06-05 | 2017-01-04 | 颜笑天 | A kind of preparation method of nano ferrite |
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