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 PDFInfo
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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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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 30
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- 239000002699 waste material Substances 0.000 title claims abstract description 16
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 12
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910017709 Ni Co Inorganic materials 0.000 title claims abstract description 7
- 229910003267 Ni-Co Inorganic materials 0.000 title claims abstract description 7
- 229910003262 Ni‐Co Inorganic materials 0.000 title claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000010405 anode material Substances 0.000 claims description 5
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000013589 supplement Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 abstract description 3
- 239000010941 cobalt Substances 0.000 abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 3
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- SJDUYOJYRZSPGP-UHFFFAOYSA-N [Co]=O.[Ni].[Fe] Chemical compound [Co]=O.[Ni].[Fe] SJDUYOJYRZSPGP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
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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
- C04B35/2666—Other ferrites containing nickel, copper or cobalt
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B35/64—Burning or sintering processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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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
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.
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Cited By (2)
| 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)
| 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 |
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2017
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Patent Citations (3)
| 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)
| 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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