CN106431379A - Method for preparing Sn-Fe spinel material through low-temperature solid-phase reaction - Google Patents

Method for preparing Sn-Fe spinel material through low-temperature solid-phase reaction Download PDF

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CN106431379A
CN106431379A CN201610801363.4A CN201610801363A CN106431379A CN 106431379 A CN106431379 A CN 106431379A CN 201610801363 A CN201610801363 A CN 201610801363A CN 106431379 A CN106431379 A CN 106431379A
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stannum
iron
source
ferrum
spinel
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CN106431379B (en
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姜涛
张元波
苏子键
李光辉
刘兵兵
范晓慧
黄柱成
彭志伟
郭宇峰
杨永斌
李骞
陈许玲
甘敏
徐斌
张鑫
陈迎明
杜明辉
路漫漫
刘继成
欧阳学臻
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Central South University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/636—Polysaccharides or derivatives thereof
    • C04B35/6365—Cellulose or derivatives thereof
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6582—Hydrogen containing atmosphere

Abstract

The invention discloses a method for preparing a Sn-Fe spinel material through a low-temperature solid-phase reaction. The method comprises the following steps: after carrying out mixing and ball milling on an iron source, a stannum source, carbon powder and sodium carboxymethyl cellulose, pelletizing and drying; putting an obtained dried block in a mixed atmosphere containing CO, CO2 and H2, and roasting under a condition that the temperature is below 1000 DEG C, thus obtaining the Sn-Fe spinel material. Compared with a traditional technology for preparing Sn-Fe spinel, the method disclosed by the invention has the advantages that the roasting temperature is reduced, the roasting time is shortened, a used organic additive has no residue after being roasted, the product purity cannot be influenced, and a high-purity Sn-Fe spinel product can be obtained; the method is simple, the cost is low, and the method is beneficial for industrial production.

Description

A kind of method that low-temperature solid phase reaction prepares stannum hercynite material
Technical field
The present invention relates to a kind of preparation method of stannum hercynite material, a kind of more particularly to low-temperature solid phase reaction prepares stannum Hercynite material (Fe3-xSnxO4, x=0.1～0.5) method, belong to stannum hercynite field of material preparation.
Background technology
Stanniferous hercynite material (Fe3-xSnxO4, x=0～1.0) and it is widely used in preparation ferrimagnetic material, electric power Transformer core, gas sensitive, heterogeneous catalyst and magnetic memory material etc..Especially as ferrite magnetic material, It is mainly used in magnetic antenna, inducer, transformator, magnetic head, earphone, relay, ticker, delay line, sensor, microwave absorption Material, electric magnet, accelerator radio-frequency acceleration cavity, magnet field probe, magnetic substrate, magnetic field shielding, high-frequency quenching cumulative, electromagnetism are inhaled Disk, magneto sensor (such as magneto-caloric material is switched) etc..
The preparation method of existing stannum hercynite material mainly includes high temperature solid phase synthesis and wet chemical methods.High Warm solid reaction process is mainly by Fe3O4And SnO2Proportionally dispensing, the height after mix homogeneously, more than high temperature (1300 DEG C) Roasting more than 12 hours under the conditions of temperature, by Fe3O4And SnO2Between solid state reaction, ion diffusion, realize stannum, ferrum binary The synthesis of oxide.High temperature solid phase synthesis low cost, treating capacity are big, relative cost is low, preparation process is simple, are current industry Production main method.Due to sintering temperature height, stannum hercynite minimum fusing point (1000 DEG C) is alreadyd exceed, in roasting process, Unavoidable produce sintering liquid phase, cause to synthesize that stannum hercynite product granularity is thick, physicochemical properties are uneven, and be unfavorable for synthesis Product be processed further utilize.
Wet chemical methods, mainly use co-precipitation and ion exchange, first by the solubility villaumite of ferrum and stannum or After person's nitrate is made into special ratios solution, then add ammonia or NaOH solution adjustment pH, stannum and ferrum co-precipitation is made, is obtained Hydroxyl stannum iron compound precipitate, the filtration repeatedly through organic solvent, washing, after foreign ion eluting, finally will precipitation Thing carries out roasting dehydration at a temperature of 200-600 DEG C, obtains stannum hercynite product, and the major advantage of wet chemical methods is Obtain product grain uniform, controlled, especially prepare the grain products of nanoscale.But wet process is unavoidably used Various organic solvent washing agent, can produce certain environment pollution；In addition Moist chemical synthesis low yield, complicated process of preparation, therefore, wet Method is limited to laboratory preparatory phase.
Therefore, a kind of low temperature, the efficient, process for preparing stannum hercynite material of environmental protection are developed, with very heavy The meaning that wants.
Content of the invention
The deficiency that the technology for stannum hercynite material being prepared for existing high temperature oxidation roasting is present, the purpose of the present invention It is the side for being to propose the stannum hercynite that synthesis purity is high, crystal phase structure is uniform and stable that a kind of sintering temperature is low, the time is short Method, the method is more beneficial for industrialized production.
In order to realize above-mentioned technical purpose, the invention provides a kind of low-temperature solid phase reaction prepares ferrum stannum spinel Method, the method is agglomeration, drying by after source of iron, Xi Yuan, powdered carbon and sodium carboxymethyl cellulose mixing and ball milling, gained dried pieces Material is placed in containing CO, CO2And H2Mixed atmosphere in, in 850～1000 DEG C of roasting temperatures, obtain final product stannum hercynite material.
Technical scheme, it is critical only that organic using special calcination atmosphere and carbon dust and sodium carboxymethyl cellulose Additive, shows through the research of long-term lot of experiments：Containing CO, CO2And H2Powdered carbon and carboxymethyl cellulose is combined in mixed atmosphere Under the common activation of sodium, greatly enhance the activity of Xi Yuan, Xi Yuan be easier to react with source of iron, particularly solid During phase reaction, the migration velocity of each metal ion species is accelerated, it is easier to form uniform and stable ferrum stannum spinel crystal phase.With When, the use of Multimetal oxide is raw material, in roasting process, the metal ion itself of internal multiple valence states can be aoxidized Reduction reaction, is conducive to increasing ion migration speed, improves reaction rate.By the method for the present invention, entirely will can prepare Temperature control in journey below 1000 DEG C, within generated time foreshortens to 300min.
Preferred scheme, in source of iron and stannum source, the mol ratio of stannum and ferrum is 0.1:2.9～0.5:2.5.
Preferred scheme, the mole of powdered carbon is 0.5～0.8% of the integral molar quantity of stannum and ferrum in source of iron and stannum source.
Preferred scheme, the mole of sodium carboxymethyl cellulose is 0.05 of the integral molar quantity of stannum and ferrum in source of iron and stannum source ～0.25%.
More preferably scheme, source of iron is made up of with iron sesquioxide and/or metal iron powder ferroso-ferric oxide；Described source of iron The molar content of middle ferroso-ferric oxide is 10～95%.
More preferably scheme, Xi Yuan is made up of with Tin monoxide and/or metallic tin powder tin ash；Two in described stannum source The mole percent level of stannum oxide is 88～98%.
Preferred scheme, containing CO, CO2And H2Mixed atmosphere include volumes below percent composition：CO 5～12.5%； CO240～87.5%；H20.5～5.5%；N20～50%.
Preferred scheme, the time of the roasting is 30～300min.
Preferred scheme, powdered carbon is activated carbon powder.
Preferred scheme, the granularity 100% of the ball mill pulverizing to mixed material is less than -0.045mm.
Preferred scheme, product of roasting is placed in protective atmosphere and is cooled to room temperature.Described protective atmosphere is typically to nitrogen Or noble gases and combinations thereof.As N2And/or Ar.
Hinge structure, the Advantageous Effects that technical scheme is brought：
1) advantage of technical scheme maximum is that greatly reducing solid state reaction prepares stannum hercynite material During reaction temperature, shorten the response time, so that reaction condition is gently changed, reach the purpose of energy-conservation, reduces cost.Tradition Solid state reaction kinetics stannum hercynite luminescent material method, as tin ash is stable in properties, up to 1630 DEG C of fusing point, low Temperature is lower to be difficult to react with other materials, with Fe3O4And SnO2For raw material, sintering temperature up to more than 1300, and reaction rate Slowly, roasting time is in more than 12h；And technical solution of the present invention, it has suffered temperature control in building-up process and, below 1000 DEG C, synthesizes Within time foreshortens to 300min, be conducive to industrialized production.
2) the stannum hercynite material crystals purity height that prepared by technical scheme, structural homogeneity is good, property is steady Fixed.There is crystal structure is uneven, and physico-chemical property is unstable etc. in the stannum hercynite material for overcoming the synthesis of conventional solid method Problem.
Description of the drawings
【Fig. 1】It is the product XRD spectrum of embodiment 1.
【Fig. 2】It is the product XRD spectrum of comparative example 1.
Specific embodiment
Following examples are intended to further illustrate present invention, rather than limit the protection model of the claims in the present invention Enclose.
Embodiment 1
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, Tin monoxide, metallic tin powder, activated carbon powder, With CMC dispensing mix homogeneously according to a certain percentage, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder be 0mol%:95mol%:5mol%, tin ash, Tin monoxide, the ratio of metallic tin powder are 88mol%:10mol%: 2mol%, stannum ferrum element ratio is 0.5:2.5, activated carbon powder and CMC account for respectively stannum, the 0.5mol% of iron substance total amount and 0.25mol%, is milled to granularity 100% less than -0.045mm after above material is mixed.Then the moisture of interpolation 8.5% is carried out Agglomeration, after its drying, will dry agglomerate and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 5%:40%: 5%:50%, 1000 DEG C of sintering temperature, roasting time 30min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X=0.5) contain Amount accounts for 99.1%, and the stannum hercynite product XRD analysis for obtaining under the conditions of being somebody's turn to do as shown in Figure 1, only exist Fe in collection of illustrative plates3-xSnxO4 (X=0.5) diffraction maximum, illustrates that reaction is abundant, product purity height.
Comparative example 1
By ferroso-ferric oxide, tin ash certain proportion dispensing mix homogeneously, stannum ferrum element ratio is 0.5:2.5, will be with Upper material is milled to granularity 100% less than -0.045mm after mixing.Then the moisture for adding 8.5% carries out agglomeration, treats its drying Afterwards, agglomerate will be dry and is placed in 100%N2Roasting, 1000 DEG C of sintering temperature, roasting time 30min is carried out in atmosphere.Product is through XRD Quantitative analyses, in product, Wuxi hercynite is generated, and under the conditions of being somebody's turn to do, product XRD analysis as shown in Figure 2, only exist four oxygen in collection of illustrative plates Change the diffraction maximum of three-iron and tin ash, illustrate that reaction is not almost carried out.
Comparative example 2
Ferroso-ferric oxide, tin ash, Tin monoxide, metallic tin powder, activated carbon powder and CMC are joined according to a certain percentage Material mix homogeneously, wherein tin ash, Tin monoxide, the ratio of metallic tin powder are 88mol%:10mol%:2mol%, stannum ferrum Element ratio is 0.5:2.5, activated carbon powder and CMC account for stannum, the 0.5mol% of iron substance total amount and 0.25mol% respectively, will be with Upper material is milled to granularity 100% less than -0.045mm after mixing.Then the moisture for adding 8.5% carries out agglomeration, treats its drying Afterwards, agglomerate will be dry and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 5%:40%:5%:50%, roasting temperature 1000 DEG C of degree, roasting time 30min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X=0.5) content accounts for 90.1%.
Comparative example 3
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, activated carbon powder and CMC according to a certain percentage Dispensing mix homogeneously, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder are 0mol%:95mol%:5mol%, Stannum ferrum element ratio is 0.5:2.5, activated carbon powder and CMC account for stannum, the 0.5mol% of iron substance total amount and 0.25mol% respectively, Granularity 100% is milled to after above material is mixed less than -0.045mm.Then the moisture for adding 8.5% carries out agglomeration, treats which After drying, agglomerate will be dry and be placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 5%:40%:5%:50%, roasting Burn 1000 DEG C of temperature, roasting time 30min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X=0.5) content accounts for 87.9%.
Embodiment 2
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, Tin monoxide, metallic tin powder, activated carbon powder, With CMC dispensing mix homogeneously according to a certain percentage, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder be 90mol%:10mol%:0mol%, tin ash, Tin monoxide, the ratio of metallic tin powder are 98mol%:0mol%: 2mol%, stannum ferrum element ratio is 0.4:2.6, activated carbon powder and CMC account for respectively stannum, the 0.8mol% of iron substance total amount and 0.05mol%, is milled to granularity 100% less than -0.045mm after above material is mixed.Then the moisture of interpolation 8.5% is carried out Agglomeration, after its drying, will dry agglomerate and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 12%: 87.5%:0.5%:0%, 900 DEG C of sintering temperature, roasting time 60min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X= 0.4) content accounts for 98.7%.
Embodiment 3
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, Tin monoxide, metallic tin powder, activated carbon powder, With CMC dispensing mix homogeneously according to a certain percentage, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder be 0mol%:95mol%:5mol%, tin ash, Tin monoxide, the ratio of metallic tin powder are 98mol%:1mol%: 1mol%, stannum ferrum element ratio is 0.1:2.9, activated carbon powder and CMC account for respectively stannum, the 0.5mol% of iron substance total amount and 0.05mol%, is milled to granularity 100% less than -0.045mm after above material is mixed.Then the moisture of interpolation 8.5% is carried out Agglomeration, after its drying, will dry agglomerate and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 12.5%: 67.5%:5.5%:14.5%, 850 DEG C of sintering temperature, roasting time 300min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X =0.1) content accounts for 99.3%.
Embodiment 4
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, Tin monoxide, metallic tin powder, activated carbon powder, With CMC dispensing mix homogeneously according to a certain percentage, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder be 90mol%:5mol%:5mol%, tin ash, Tin monoxide, the ratio of metallic tin powder are 98mol%:0mol%: 2mol%, stannum ferrum element ratio is 0.2:2.8, activated carbon powder and CMC account for respectively stannum, the 0.6mol% of iron substance total amount and 0.15mol%, is milled to granularity 100% less than -0.045mm after above material is mixed.Then the moisture of interpolation 8.5% is carried out Agglomeration, after its drying, will dry agglomerate and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 5%:40%: 5%:50%, 975 DEG C of sintering temperature, roasting time 45min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X=0.2) content Account for 99.2%.
Embodiment 5
By iron sesquioxide, ferroso-ferric oxide, metal iron powder, tin ash, Tin monoxide, metallic tin powder, activated carbon powder, With CMC dispensing mix homogeneously according to a certain percentage, wherein iron sesquioxide, ferroso-ferric oxide, the ratio of metal iron powder be 45mol%:50mol%:5mol%, tin ash, Tin monoxide, the ratio of metallic tin powder are 90mol%:8mol%: 2mol%, stannum ferrum element ratio is 0.2:2.8, activated carbon powder and CMC account for respectively stannum, the 0.8mol% of iron substance total amount and 0.05mol%, is milled to granularity 100% less than -0.045mm after above material is mixed.Then the moisture of interpolation 8.5% is carried out Agglomeration, after its drying, will dry agglomerate and is placed in CO-CO2-H2-N2Roasting is carried out in atmosphere, and gas ratio is 12.5%: 70%:0.5%:17%, 915 DEG C of sintering temperature, roasting time 100min.Product is through XRD quantitative analyses, Fe3-xSnxO4(X= 0.2) content accounts for 99.4%.

Claims (7)

1. a kind of method that low-temperature solid phase reaction prepares ferrum stannum spinel, it is characterised in that：By source of iron, Xi Yuan, powdered carbon and After sodium carboxymethyl cellulose mixing and ball milling, agglomeration, drying, gained dries block and is placed in containing CO, CO2And H2Mixed atmosphere in, in 850～1000 DEG C of roasting temperatures, obtain final product stannum hercynite material.
2. the method that solid state reaction according to claim 1 prepares stannum hercynite type ferrite material precursor, which is special Levy and be：
In described source of iron and stannum source, the mol ratio of stannum and ferrum is 0.1:2.9～0.5:2.5；
The mole of the powdered carbon is 0.5～0.8% of the integral molar quantity of stannum and ferrum in source of iron and stannum source；
The mole of the sodium carboxymethyl cellulose is 0.05～0.25% of the integral molar quantity of stannum and ferrum in source of iron and stannum source.
3. the method that solid state reaction according to claim 1 and 2 prepares ferrum stannum spinel, it is characterised in that：Described Source of iron be made up of with iron sesquioxide and/or metal iron powder ferroso-ferric oxide；In described source of iron ferroso-ferric oxide mole Degree is 10～95%.
4. the method that solid state reaction according to claim 1 and 2 prepares ferrum stannum spinel, it is characterised in that：Described Xi Yuan be made up of with Tin monoxide and/or metallic tin powder tin ash；The molar percentage of tin ash in described stannum source Content is 88～98%.
5. the method that solid state reaction according to claim 1 prepares ferrum stannum spinel type materials, it is characterised in that：Described Containing CO, CO2And H2Mixed atmosphere include volumes below percent composition：
CO 5～12.5%；
CO240～87.5%；
H20.5～5.5%；
N2≤ 50%.
6. the method that solid state reaction according to claim 1 prepares ferrum stannum spinel, it is characterised in that：The roasting Time be 30～300min.
7. the method that the solid state reaction according to 1,2,5 or 6 any one of claim prepares ferrum stannum spinel, its feature It is：The granularity 100% of the ball mill pulverizing to mixed material is less than -0.045mm.
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CN111029563A (en) * 2019-12-10 2020-04-17 河南创力新能源科技股份有限公司 Preparation method of alkaline secondary battery iron negative electrode material

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