CN106938927A - The method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel - Google Patents

The method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel Download PDF

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CN106938927A
CN106938927A CN201710217182.1A CN201710217182A CN106938927A CN 106938927 A CN106938927 A CN 106938927A CN 201710217182 A CN201710217182 A CN 201710217182A CN 106938927 A CN106938927 A CN 106938927A
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magnetostriction materials
lithium ion
calcining
waste
nickel
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席国喜
张烨
王路
赵婷婷
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Henan Normal University
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Abstract

The invention discloses the method that a kind of utilization waste and old lithium ion battery doping nickel prepares Ni-Co ferrite magnetostriction materials, belong to the preparing technical field of magnetostriction materials.Technical scheme main points are：Using citric acid as gel, nickel doping cobalt ferrite powder is prepared using the method for collosol and gel microwave hydrothermal, the nickel cobalt ferrite powder that adulterates is added mass concentration for 8% 10% polyvinyl alcohol and grinds uniform again, cylinder is pressed under 10MPa pressure, prior to 650 DEG C calcining 6h, then at 1450 DEG C of calcining 6h, Ni is finally madexCo1‑xFe2O4Magnetostriction materials.The synthetic method simple and fast of the present invention, economizes on resources, obtained NixCo1‑xFe2O4Magnetostriction materials pattern is homogeneous and function admirable.

Description

Ni-Co ferrite magnetostriction materials are prepared using waste and old lithium ion battery doping nickel Method
Technical field
The invention belongs to the preparing technical field of magnetostriction materials, and in particular to one kind is mixed using waste and old lithium ion battery The method that miscellaneous nickel prepares Ni-Co ferrite magnetostriction materials.
Background technology
In terms of magnetostriction materials are widely used in pressure sensor and actuator.Commonly rare earth alloy ultra-magnetic telescopic Material, but because its cost is higher and has certain application limitation.Conjugate ferrite magnetostriction materials are preferably mechanical due to it With Magnetostriction, high corrosion resistance, easy processing and low cost advantage and widely paid close attention to.Current Conjugate ferrite Main synthetic method has solid phase method, chemical coprecipitation, sol-gel process and hydro-thermal method etc., and synthesis material is mainly analysis Pure chemicals, the content of research is concentrated mainly on the discussion of synthesis condition.
The fast development of electronic technology in recent years causes the amount of waste and old lithium ion battery constantly to rise, the pollution day to environment It is beneficial serious.But the content of cobalt in waste lithium ion batteries element is than containing for being found in the natural crystal of natural crystal or concentration Amount is taller, therefore, is that raw material prepares ferrite and on the one hand reduces heavy metal element environment is made with waste and old lithium ion battery Into pollution, on the other hand alleviate shortage of resources.And use the synthetic method calcining heat of sol-gel-microwave hydrothermal low, Reaction time is short, process simplification, prepares crystallization rate soon, product cut size is small, purity is high.
And the nickel that adulterated into waste and old lithium ion battery is utilized, a part of cobalt ions in nickel replacing cobalt ferrite, Neng Goucong Inside changes ferritic architectural feature, so as to modify its magnetic and Magnetostriction.
The content of the invention
Present invention solves the technical problem that there is provided one kind prepares nickel cobalt iron oxygen using waste and old lithium ion battery doping nickel The method of body magnetostriction materials, this method is under 2.45GHz microwave condition by controlling the doping of nickel element to adjust The performance of product, and this method shortens the reaction time, saving energy consumption, and operation is simple, and properties of product are excellent.
The present invention adopts the following technical scheme that to solve above-mentioned technical problem, is prepared using waste and old lithium ion battery doping nickel The method of Ni-Co ferrite magnetostriction materials, it is characterised in that concretely comprise the following steps：
（1）With containing H2O2Molar concentration for 3.5mol/L sulfuric acid solution dissolving waste lithium ion cell anode material, regulation PH makes Co2+、Fe3+Fully precipitation, is filtered；
（2）By step（1）Middle filtering products therefrom is redissolved, and Co is measured with atomic absorption spectrophotometer2+、Fe3+Content, is mended Fill addition CoSO4、Fe2(SO4)3And NiSO4Make Co in solution2+、Ni2+With Fe3+Mol ratio be 1-x:x:2, wherein x are 0.1- 0.5；
（3）It is 1 to add with the ratio between total metal ion mole:1 citric acid, adjusts pH=6.5, forms gel in 80 DEG C, obtains To gel in 110 DEG C be dried to obtain xerogel；
（4）By step（3）Middle gained xerogel moves into microwave after being mixed with molar concentration for 2-12mol/L sodium hydroxide solution In hydrothermal reaction kettle, compactedness reacts suction filtration after 1.0-2.5h in 180-240 DEG C, is dried to obtain Ni up to 80%xCo1-xFe2O4Powder End；
（5）By NixCo1-xFe2O4Mass concentration is added in powder uniform for 8%-10% polyvinyl alcohol grinding, in 10MPa pressure Under be pressed into cylinder, prior to 650 DEG C calcining 6h, then at 1450 DEG C calcining 6h, finally be made NixCo1-xFe2O4Magnetostriction material Material.
The present invention has the advantages that compared with prior art：
1st, this method promotes its motion to accelerate by the way of heating using microwave from inside particles, promotes reaction to carry out, greatly shortens The time required to reaction, reaction efficiency is improved, resource consumption is reduced；
2nd, Ni produced by the present inventionxCo1-xFe2O4Magnetostriction materials product cut size is evenly distributed, and scope is narrower, in 10-20nm Between, and soilless sticking phenomenon；
3rd, the present invention is adjusted merely by the performance parameter of the i.e. controllable product of doping of nickel.
Brief description of the drawings
Fig. 1 is Ni made from the embodiment of the present invention 10.1Co0.9Fe2O4The XRD of magnetostriction materials；
Fig. 2 is Ni made from the embodiment of the present invention 10.1Co0.9Fe2O4The magnetostriction coefficient figure of magnetostriction materials；
Fig. 3 is Ni made from the embodiment of the present invention 10.1Co0.9Fe2O4The magnetostrictive strain curve map of magnetostriction materials.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair Bright scope.
Embodiment 1
（1）With containing a small amount of H2O2Molar concentration for 3.5mol/L sulfuric acid solution dissolving waste lithium ion cell anode material, Regulation pH makes Co2+、Fe3+Fully precipitation, is filtered；
（2）By step（1）Middle filtering products therefrom is redissolved, and measures Co2+、Fe3+Content, supplement adds CoSO4、Fe2(SO4)3 And NiSO4Make Co in solution2+、Ni2+And Fe3+Mol ratio be 0.9:0.1:2；
（3）It is 1 to add with the ratio between total metal ion mole:1 citric acid, adjusts pH=6.5, forms gel in 80 DEG C, obtains To gel in 110 DEG C be dried to obtain xerogel；
（4）By step（3）It is micro- that middle gained xerogel moves into 100mL after being mixed with molar concentration for 6mol/L sodium hydroxide solution In ripple hydrothermal reaction kettle, compactedness reacts suction filtration after 1.5h in 220 DEG C, is dried to obtain Ni up to 80%0.1Co0.9Fe2O4Powder；
（5）By Ni0.1Co0.9Fe2O4Mass concentration is added in powder uniform for 8%-10% polyvinyl alcohol grinding, in 10MPa pressures Cylinder is pressed under power, then at 1450 DEG C of calcining 6h, Ni is finally made in prior to 650 DEG C calcining 6h0.1Co0.9Fe2O4Magnetostriction Material.
Obtained Ni as shown in Figure 10.1Co0.9Fe2O4Magnetostriction materials meet the standard diagram of Ni-Co ferrite；Fig. 2 and Fig. 3 is obtained Ni0.1Co0.9Fe2O4The performance parameter of magnetostriction materials, as seen from the figure obtained Ni0.1Co0.9Fe2O4Mangneto Telescopic material magnetostriction coefficient is 120ppm to the maximum, belongs to normal level, but its maximum strain derivative reaches -1.0 × 10- 9A-1More than m, has reached at a relatively high level, and the corresponding magnetic field of this maximum is than relatively low, only 40KA/m or so, right There is certain advantage in the practical application of the magnetostriction materials.
Embodiment 2
（1）With containing a small amount of H2O2Molar concentration for 3.5mol/L sulfuric acid solution dissolving waste lithium ion cell anode material, Regulation pH makes Co2+、Fe3+Fully precipitation, is filtered；
（2）By step（1）Middle filtering products therefrom is redissolved, and measures Co2+、Fe3+Content, supplement adds CoSO4、Fe2(SO4)3 And NiSO4Make Co in solution2+、Ni2+And Fe3+Mol ratio be 0.5:0.5:2；
（3）It is 1 to add with the ratio between total metal ion mole:1 citric acid, adjusts pH=6.5, forms gel in 80 DEG C, obtains To gel in 110 DEG C be dried to obtain xerogel；
（4）By step（3）It is micro- that middle gained xerogel moves into 100mL after being mixed with molar concentration for 2mol/L sodium hydroxide solution In ripple hydrothermal reaction kettle, compactedness reacts suction filtration after 1.0h in 180 DEG C, is dried to obtain Ni up to 80%0.5Co0.5Fe2O4Powder；
（5）By Ni0.5Co0.5Fe2O4Mass concentration is added in powder uniform for 8%-10% polyvinyl alcohol grinding, in 10MPa pressures Cylinder is pressed under power, then at 1450 DEG C of calcining 6h, Ni is finally made in prior to 650 DEG C calcining 6h0.5Co0.5Fe2O4Magnetostriction Material.
Embodiment 3
（1）With containing a small amount of H2O2Molar concentration for 3.5mol/L sulfuric acid solution dissolving waste lithium ion cell anode material, Regulation pH makes Co2+、Fe3+Fully precipitation, is filtered；
（2）By step（1）Middle filtering products therefrom is redissolved, and measures Co2+、Fe3+Content, supplement adds CoSO4、Fe2(SO4)3 And NiSO4Make Co in solution2+、Ni2+And Fe3+Mol ratio be 0.7:0.3:2；
（3）It is 1 to add with the ratio between total metal ion mole:1 citric acid, adjusts pH=6.5, forms gel in 80 DEG C, obtains To gel in 110 DEG C be dried to obtain xerogel；
（4）By step（3）Middle gained xerogel moves into 100mL after being mixed with molar concentration for 12mol/L sodium hydroxide solution In microwave hydrothermal reaction kettle, compactedness reacts suction filtration after 2.5h in 40 DEG C, is dried to obtain Ni up to 80%0.3Co0.7Fe2O4Powder；
（5）By Ni0.3Co0.7Fe2O4Mass concentration is added in powder uniform for 8%-10% polyvinyl alcohol grinding, in 10MPa pressures Cylinder is pressed under power, then at 1450 DEG C of calcining 6h, Ni is finally made in prior to 650 DEG C calcining 6h0.3Co0.7Fe2O4Magnetostriction Material.
Have been shown and described above the general principle of the present invention, principal character and advantage, do not depart from spirit of the invention and On the premise of scope, the present invention also has various changes and modifications, and these changes and improvements both fall within claimed invention Scope.

Claims (1)

1. the method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel, it is characterised in that specific Step is：
（1）With containing H2O2Molar concentration for 3.5mol/L sulfuric acid solution dissolving waste lithium ion cell anode material, adjust pH Make Co2+、Fe3+Fully precipitation, is filtered；
（2）By step（1）Middle filtering products therefrom is redissolved, and Co is measured with atomic absorption spectrophotometer2+、Fe3+Content, supplement Add CoSO4、Fe2(SO4)3And NiSO4Make Co in solution2+、Ni2+With Fe3+Mol ratio be 1-x:x:2, wherein x are 0.1- 0.5；
（3）It is 1 to add with the ratio between total metal ion mole:1 citric acid, adjusts pH=6.5, forms gel in 80 DEG C, obtains To gel in 110 DEG C be dried to obtain xerogel；
（4）By step（3）Middle gained xerogel moves into microwave after being mixed with molar concentration for 2-12mol/L sodium hydroxide solution In hydrothermal reaction kettle, compactedness reacts suction filtration after 1.0-2.5h in 180-240 DEG C, is dried to obtain Ni up to 80%xCo1-xFe2O4Powder End；
（5）By NixCo1-xFe2O4Mass concentration is added in powder uniform for 8%-10% polyvinyl alcohol grinding, in 10MPa pressure Under be pressed into cylinder, prior to 650 DEG C calcining 6h, then at 1450 DEG C calcining 6h, finally be made NixCo1-xFe2O4Magnetostriction material Material.
CN201710217182.1A 2017-04-05 2017-04-05 The method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel Withdrawn CN106938927A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231979A (en) * 2018-11-09 2019-01-18 河南师范大学 A method of Conjugate ferrite magnetostriction materials are prepared by raw material of waste and old lithium ion battery
CN112745115A (en) * 2021-01-11 2021-05-04 电子科技大学 Magnetostrictive material with high strain sensitivity in low magnetic field and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104557006A (en) * 2015-01-19 2015-04-29 河南师范大学 Method for preparing cobalt ferrite magnetostrictive material from waste lithium ion batteries in low magnetic field
CN104600390A (en) * 2015-01-19 2015-05-06 河南师范大学 Method for preparing magnetostriction material by utilizing spent lithium ion batteries
CN104600391A (en) * 2015-01-19 2015-05-06 河南师范大学 Method for preparing manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104557006A (en) * 2015-01-19 2015-04-29 河南师范大学 Method for preparing cobalt ferrite magnetostrictive material from waste lithium ion batteries in low magnetic field
CN104600390A (en) * 2015-01-19 2015-05-06 河南师范大学 Method for preparing magnetostriction material by utilizing spent lithium ion batteries
CN104600391A (en) * 2015-01-19 2015-05-06 河南师范大学 Method for preparing manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231979A (en) * 2018-11-09 2019-01-18 河南师范大学 A method of Conjugate ferrite magnetostriction materials are prepared by raw material of waste and old lithium ion battery
CN112745115A (en) * 2021-01-11 2021-05-04 电子科技大学 Magnetostrictive material with high strain sensitivity in low magnetic field and preparation method thereof

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