CN106024244A - High-heat-stability nanocrystal rare-earth permanent-magnet material and preparation method thereof - Google Patents
High-heat-stability nanocrystal rare-earth permanent-magnet material and preparation method thereof Download PDFInfo
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- CN106024244A CN106024244A CN201610579015.7A CN201610579015A CN106024244A CN 106024244 A CN106024244 A CN 106024244A CN 201610579015 A CN201610579015 A CN 201610579015A CN 106024244 A CN106024244 A CN 106024244A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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Abstract
The invention relates to a high-heat-stability nanocrystal rare-earth permanent-magnet material, belonging to the technical field of magnetic materials. The basic expression of the permanent-magnet material is RxFe[100-x-y-z]ByMz, wherein R is one or more of light rare-earth elements neodymium, praseodymium and cerium, Fe is iron, B is boron, and M is one or more of zirconium and hafnium; and x, y and z represent atomic percents, 12<=x<=14.9, 5<=y<=10, and 0.1<=z<=4. The invention also relates to a preparation method of the rare-earth permanent-magnet material. The high-heat-stability nanocrystal rare-earth permanent-magnet material is free of the heavy rare-earth element Dy or Tb, has low total rare-earth content, and is free of the element Co; and the high-heat-stability nanocrystal rare-earth permanent-magnet material has the advantages of low coercivity temperature coefficient, high heat stability and fine and uniform grain size. The preparation process does not need annealing technique treatment, has the advantages of simple technique and lower cost, and thus, is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of permanent magnet material, especially relate to the nanocrystalline rare-earth permanent magnetic material of a kind of high thermal stability
Become to be grouped into and preparation method, belong to technical field of magnetic materials.
Background technology
Nd2Fe14B class rare earth permanent-magnetic material, since the eighties in 19th century invents, has been widely used in wind-power electricity generation, has disappeared
Take the fields such as electron-like, white domestic appliances, new-energy automobile, medical apparatus and instruments.But, such material Curie temperature is low, coercivity temperature
Degree poor stability.Along with the rising of operating temperature, coercivity drastically declines, this phenomenon in ternary Nd-Fe-B alloy particularly
Substantially.This latent defect seriously limits such material under high-temperature work environment in terms of electric motor of automobile, sensor etc.
Application.At present, many researchs are main replaces Fe by Co part, and heavy rare earth (Dy, Tb) part replaces the side of light rare earth (Pr, Nd)
Method improves Curie temperature and the high-temp magnetic performance of magnet.But Co belongs to strategic resource, heavy rare earth (Dy, Tb) reserves are few, valency
Lattice are high.Therefore, research and development are one without heavy rare earth (Dy, Tb), low content of rare earth and the high thermal stability rare earth permanent-magnetic material without Co
Main trend.
The method preparing nanocrystalline rare-earth permanent magnetic material at present is mainly melt-quenching method, and first the method prepares foundry alloy
Ingot casting, then uses rotation technique fast quenching of quenching to obtain alloy strip steel rolled stock.
Chinese patent literature of being correlated with discloses high thermal stability nanocrystalline rare-earth permanent magnetic material, but its composition or containing war
Slightly Elements C o, or (Dy, Tb) Han heavy rare earth, or total amount of rare earth is higher, causes relatively costly.
Summary of the invention
It is an object of the invention to provide the nanocrystalline rare-earth permanent magnetic material of a kind of high thermal stability, this material is dilute without weight
Soil Dy or Tb, without strategic resource Co, rare earth total content is low, and Heat stability is good.
The technical scheme is that
The nanocrystalline rare-earth permanent magnetic material of a kind of high thermal stability, its composition and content are formulated as RxFe100-x-y- zByMz, wherein, R is one or more (preferably one or more in neodymium, praseodymium) in LREE neodymium, praseodymium, cerium, and Fe is
Ferrum element, B is boron element, and M is one or more (preferably hafnium elements) in zirconium, two kinds of elements of hafnium;X, y and z represent atom
Percent, 12≤x≤14.9,5≤y≤10,0.1≤z≤4 (preferably 12.9≤x≤14.5,6≤y≤9,0.2≤z≤2).
Wherein, the purity of R, Fe, B and M element is all not less than 99.9% (percentage by weight).
Compared with prior art, the advantage of permanent magnet material of the present invention is: without heavy rare earth Dy or Tb, without strategy
Resource Co, rare earth total content is low, by adding one or more elements in Zr and Hf element in raw material R, Fe, B,
And control the content of these elements, improve the internal microstructure of nanocrystalline rare-earth permanent magnetic material, crystal grain thinning, make crystallite dimension equal
Even unanimously.
Present invention firstly discovers that appropriate Hf element adds and can highly desirable suppress principal phase Nd2Fe14Growing up of B crystal grain,
Significantly refining main phase grain, keep sheet metal strip patch roll surface and scope of freedom main phase grain the most tiny, grain size distribution is narrow,
And make crystal grain in rule spherical, substantially increase the high-temp magnetic performance of rare earth permanent-magnetic material, the heat stability of material obtains
It is obviously improved.
Present invention also offers the preparation method of the nanocrystalline rare-earth permanent magnetic material of described offer high thermal stability, by pressing
Described atomic percent configuration raw material, controls that nozzle and roll surface distance, argon pressure be poor, mother alloy melt is ejected into copper simultaneously
The parameters such as the speed on wheel adjust rate of cooling, thus control the crystallization rate of nanocrystalline rare-earth permanent magnetic material, make preparation
The internal microstructure of permanent magnet material is improved, and high-temp magnetic performance and heat stability get a promotion.Specifically comprise the following steps that
1. proportioning raw material: by element R, Fe, B and M according to RxFe100-x-y-zByMzProportioning, wherein, R is LREE
One or more in neodymium, praseodymium, cerium, Fe is ferrum element, and B is boron element, and M is one or more in zirconium, two kinds of elements of hafnium;x、
Y and z represents atomic percentage, 12≤x≤14.9,5≤y≤10,0.1≤z≤4;(wherein, R, Fe, B and the raw material of M element
Purity is all not less than 99.9wt%.)
2. mother alloy ingot is prepared: being put into by raw material and carry out melting in electric arc furnace under an argon atmosphere, melting electric current is close
Degree is 100~350A/cm2, melting 4-6 time, mix homogeneously, obtain mother alloy ingot after cooling;
3. rotation is quenched: mother alloy ingot is broken into the cobbing of 3~6g, loads in quartz ampoule, and quartz ampoule nozzle diameter is
0.6~1.2mm, nozzle and roll surface distance are 1~6mm, and argon pressure difference is 0.8 × 105~1.5 × 105Pa, uses metal to melt
The method of body fast quenching, the alloy cast ingot refuse that 2. step is prepared, obtain alloy melt;Alloy melt is ejected into rotating speed
Be 10~35m/s copper wheel on, obtain a width of 0.8-2mm, the melt spun alloy band of thick 20-40 μm, this melt spun alloy band is
Nanocrystalline rare-earth permanent magnetic material.
As preferred technical scheme, step 3. described in quartz ampoule nozzle diameter be 0.8mm, nozzle with roll surface distance is
2mm, argon pressure difference is 1.0 × 105Pa, the method using metal bath fast quenching, alloy cast ingot step 2. prepared is again
Fusing, obtains alloy melt;Alloy melt is ejected on the copper wheel that rotating speed is 20m/s, obtains melt spun alloy band.
Compared with prior art, it is an advantage of the current invention that by adding in Zr and Hf element in raw material
Kind or multiple element, control the speed etc. that nozzle and roll surface distance, argon pressure be poor, mother alloy melt is ejected on copper wheel simultaneously
Parameter adjusts rate of cooling, thus controls the crystallization rate of nanocrystalline rare-earth permanent magnetic material, it is thus achieved that less and uniformity divides
The crystallite dimension of cloth, high-temp magnetic performance and heat stability get a promotion;And the preparation method of the present invention need not annealing process
Processing, technique is simple and cost is relatively low, is suitable to large-scale production.
The shortcoming that the present invention solves prior art middle rare earth permanent magnet material poor heat stability, high-temp magnetic performance is low, in nothing
Heavy rare earth Dy or Tb, without strategic resource Co and rare earth total content relatively low in the case of, it is thus achieved that there is high thermal stability, low temperature
The nanocrystalline rare-earth permanent-magnet alloy of coefficient.The rare earth permanent-magnetic material of the present invention under conditions of temperature is 450K, rare earth permanent magnet material
Material HCJ HciStill reach more than 500kA/m, be better than the Sintered NdFeB magnet containing 4wt% heavy rare earth Dy, 300-450K
Temperature range, coercive force temperature coefficient is better than-0.35%/K, substantially increases material at high temperature performance, improves material thermally-stabilised
Property.
Accompanying drawing explanation
Fig. 1 is the Nd of the embodiment of the present invention 1 preparation13Fe80.5B6Hf0.5Melt spun alloy band moving back when temperature T=450K
Magnetic curve chart (VSM);
Fig. 2 is the Nd of the embodiment of the present invention 1 preparation13Fe80.5B6Hf0.5The transmission electron microscope picture (TEM) of melt spun alloy band;
Fig. 3 is Nd prepared by comparative example of the present invention13Fe81B6The melt spun alloy band demagnetizing curve when temperature T=450K
Figure (VSM);
Fig. 4 is Nd prepared by comparative example of the present invention13Fe81B6The transmission electron microscope picture (TEM) of melt spun alloy band.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail, but the invention is not restricted to these embodiments,
Following example the most for the purpose of illustration, should not be taken to limit the scope of the present invention and claim.
In the embodiment of the present invention, the material purity of each element is more than 99.9wt%.
Embodiment 1
The nanocrystalline rare-earth permanent magnetic material of a kind of high thermal stability, its nominal composition and content are formulated as
Nd13Fe80.5B6Hf0.5, its preparation method is as follows:
1., proportioning raw material: be that 13:80.5:6:0.5 prepares by atomic ratio by tetra-kinds of elements of raw material Nd, Fe, B and Hf;
2. mother alloy ingot, is prepared: being put into by raw material and carry out melting in electric arc furnace under an argon atmosphere, melting electric current is close
Degree is 100~350A/cm2, melting 5 times, mix homogeneously, obtain mother alloy ingot after cooling;
3. rotation is quenched: step 2. gained mother alloy ingot is broken into the cobbing of 3~6g, loads in quartz ampoule, quartz ampoule
Nozzle diameter is 0.8mm, and nozzle and roll surface distance are 2mm, and argon pressure difference is 1.0 × 105Pa, uses metal bath fast quenching
Method, the alloy cast ingot refuse that 2. step is prepared, obtain alloy melt;It is 20m/s that alloy melt is ejected into rotating speed
Copper wheel on, obtain a width of 0.8-2mm, the melt spun alloy band of thick 20-40 μm, this melt spun alloy band be nanocrystalline rare-earth forever
Magnetic material.
In the present embodiment, quench in technique in step rotation 3., use the foundry furnace with spray to cast device,
Nd13Fe80.5B6Hf0.5Mother alloy ingot after refuse, utilizes the spray to cast device in foundry furnace, by foundry alloy in foundry furnace
Melt jet is on copper wheel.
To gained Nd13Fe80.5B6Hf0.5Melt spun alloy band detects, hysteresis curve (VSM) when temperature T=450K
As it is shown in figure 1, transmission electron microscope picture (TEM) is as shown in Figure 2.
Analysis chart 1 understands, the Nd of the present embodiment13Fe80.5B6Hf0.5Melt spun alloy band hysteresis curve show as single forever
Magnetic property, when temperature T=450K, band magnetic property is: Br=0.58T, Hci=505kA/m, (BH)max=59kJ/m3。
The Nd of the present embodiment13Fe80.5B6Hf0.5The magnetic parameter recorded under melt spun alloy band different temperatures such as table 1 institute
Show.
Nd under table 1 different temperatures13Fe80.5B6Hf0.5Melt spun alloy band magnetic parameter
Analysis chart 2 understands, the Nd of the present embodiment13Fe80.5B6Hf0.5Melt spun alloy band internal grain size is tiny, averagely
In 15-30nm, regular shape, in the most spherical, and crystal grain is evenly distributed.
Can draw by calculating, the nanocrystalline rare-earth permanent magnetic material in the present embodiment is in 300~400K temperature ranges, surplus
Magnetic temperature coefficient α=-0.13%/K, coercive force temperature coefficient β=-0.41%/K, in 300~450K temperature ranges, remanent magnetism temperature
Degree factor alpha=-0.17%/K, coercive force temperature coefficient β=-0.34%/K.
In sum, the Nd of the present embodiment13Fe80.5B6Hf0.5Melt spun alloy band has the microstructure of excellence, good
High-temp magnetic performance and heat stability.
Comparative example
A kind of nanocrystalline rare-earth permanent magnetic material, its nominal composition and content are formulated as Nd13Fe81B6, without Hf unit
Element, its preparation method is as follows:
1., proportioning raw material: be that 13:81:6 prepares by atomic ratio by raw material Nd, Fe, B;
2. mother alloy ingot, is prepared: being put into by raw material and carry out melting in electric arc furnace under an argon atmosphere, melting electric current is close
Degree is 100~350A/cm2, melting 5 times, mix homogeneously, obtain mother alloy ingot after cooling;
3. rotation is quenched: step 2. gained mother alloy ingot is broken into the cobbing of 3~6g, loads in quartz ampoule, quartz ampoule
Nozzle diameter is 0.8mm, and nozzle and roll surface distance are 2mm, and argon pressure difference is 1.0 × 105Pa, uses metal bath fast quenching
Method, the alloy cast ingot refuse that 2. step is prepared, obtain alloy melt;It is 20m/s that alloy melt is ejected into rotating speed
Copper wheel on, obtain a width of 0.8-2mm, the melt spun alloy band of thick 20-40 μm, this melt spun alloy band be nanocrystalline rare-earth forever
Magnetic material.
In this comparative example, quench in technique in step rotation 3., use the foundry furnace with spray to cast device, Nd13Fe81B6Female conjunction
Gold ingot casting after refuse, utilizes the spray to cast device in foundry furnace, mother alloy melt is ejected on copper wheel in foundry furnace.
To gained Nd13Fe81B6Melt spun alloy band detects, and when temperature T=450K, hysteresis curve (VSM) is such as Fig. 3
Shown in, transmission electron microscope picture (TEM) is as shown in Figure 4.
Analysis chart 3 understands, the Nd of this comparative example13Fe81B6Melt spun alloy band hysteresis curve also shows as single permanent magnetism
Can, when temperature T=450K, band magnetic property is only: Br=0.58T, Hci=289kA/m, (BH)max=49kJ/m3。
Analysis chart 4 understands, the Nd of the present embodiment13Fe81B6Melt spun alloy band internal grain size is thick, 25-180nm,
Distributed more widely, and exist in irregularly shaped crystal grain such as rod shape, polygons.
Can draw by calculating, the nanocrystalline rare-earth permanent magnetic material in this comparative example is in 300~400K temperature ranges, surplus
Magnetic temperature coefficient α=-0.13%/K, coercive force temperature coefficient β=-0.53%/K, in 300~450K temperature ranges, remanent magnetism temperature
Degree factor alpha=-0.20%/K, coercive force temperature coefficient β=-0.48%/K.
In sum, Nd13Fe81B6Melt spun alloy band, because being not added with Hf, high-temp magnetic performance is substantially deteriorated, temperature coefficient
Absolute value becomes big, and crystallite dimension is thick, and distribution is wide, in irregular shape.
Embodiment 2
The nanocrystalline rare-earth permanent magnetic material of a kind of high thermal stability, its nominal composition and content are formulated as
Pr14Fe80.25B5Hf0.75, its preparation method is as follows:
1., proportioning raw material: be that 14:80.25:5:0.75 prepares by atomic ratio by tetra-kinds of elements of raw material Pr, Fe, B and Hf;
2. mother alloy ingot, is prepared: being put into by raw material and carry out melting in electric arc furnace under an argon atmosphere, melting electric current is close
Degree is 100~350A/cm2, melting 4 times, mix homogeneously, obtain mother alloy ingot after cooling;
3., rotation is quenched: step 2. gained mother alloy ingot is broken into the cobbing of 3~6g, loads in quartz ampoule, quartz ampoule
Nozzle diameter is 0.7mm, and nozzle and roll surface distance are 3mm, and argon pressure difference is 1.0 × 105Pa, uses metal bath fast quenching
Method, the alloy cast ingot refuse that 2. step is prepared, obtain alloy melt;It is 18m/s that alloy melt is ejected into rotating speed
Copper wheel on, obtain a width of 0.8-2mm, the melt spun alloy band of thick 20-40 μm, this melt spun alloy band be nanocrystalline rare-earth forever
Magnetic material.
In the present embodiment, quench in technique in step rotation 3., use the foundry furnace with spray to cast device,
Pr14Fe80.25B5Hf0.75Mother alloy ingot after refuse, utilizes the spray to cast device in foundry furnace, by foundry alloy in foundry furnace
Melt jet is on copper wheel.
To gained Pr14Fe80.25B5Hf0.75Melt spun alloy band detects, the hysteresis curve performance when temperature T=450K
For single permanent magnetism performance, its internal grain size is tiny, regular shape, and crystal grain is evenly distributed.The present embodiment
Pr14Fe80.25B5Hf0.75Melt spun alloy band has microstructure, good high-temp magnetic performance and the heat stability of excellence.
Embodiment 3
Being with the difference of embodiment 1, its nominal composition of nanocrystalline rare-earth permanent magnetic material prepared and content are public
Formula is expressed as (Nd0.8Ce0.2)14Fe78B6Hf0.5Zr1.5, gained (Nd0.8Ce0.2)14Fe78B6Hf0.5Zr1.5Melt spun alloy band has
There are microstructure, good high-temp magnetic performance and the heat stability of excellence.
Embodiment 4
Being with the difference of embodiment 1, its nominal composition of nanocrystalline rare-earth permanent magnetic material prepared and content are public
Formula is expressed as Nd14.5Fe76B9Hf0.5, gained Nd14.5Fe76B9Hf0.5Melt spun alloy band has the microstructure, good of excellence
High-temp magnetic performance and heat stability.
Embodiment 5
Being with the difference of embodiment 1, its nominal composition of nanocrystalline rare-earth permanent magnetic material prepared and content are public
Formula is expressed as Nd13.5Fe80.5B5Hf0.5Zr0.5, gained Nd13.5Fe80.5B5Hf0.5Zr0.5Melt spun alloy band has the microcosmic of excellence
Structure, good high-temp magnetic performance and heat stability.
Above-described embodiment, only for technology design and the feature of the explanation present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implements according to this, can not limit the scope of the invention with this.All according to the present invention
The equivalence that spirit is made changes or modifies, and all should contain within protection scope of the present invention.
Claims (7)
1. the nanocrystalline rare-earth permanent magnetic material of a high thermal stability, it is characterised in that: its composition and content are formulated as:
RxFe100-x-y-zByMz, wherein, R is one or more in neodymium, praseodymium, cerium, and Fe is ferrum element, and B is boron element, and M is zirconium, hafnium two
Plant one or more in element;X, y and z represent atomic percentage, 12≤x≤14.9,5≤y≤10,0.1≤z≤4.
2. according to the nanocrystalline rare-earth permanent magnetic material of high thermal stability described in claim 1, it is characterised in that: R, Fe, B and M unit
The purity of element is all not less than 99.9wt%.
3. according to the nanocrystalline rare-earth permanent magnetic material of high thermal stability described in claim 1, it is characterised in that described x, y and z's
Span is: 12.9≤x≤14.5,6≤y≤9,0.2≤z≤2.
4. according to the nanocrystalline rare-earth permanent magnetic material of high thermal stability described in claim 1, it is characterised in that: described R element is
One or more in neodymium, praseodymium, M element is hafnium.
5. the preparation method of the nanocrystalline rare-earth permanent magnetic material of high thermal stability described in a claim 1, it is characterised in that bag
Include following steps:
1. proportioning raw material: by element R, Fe, B and M according to RxFe100-x-y-zByMzProportioning, wherein, R is in neodymium, praseodymium, cerium
Planting or multiple, Fe is ferrum element, and B is boron element, and M is one or more in zirconium, two kinds of elements of hafnium;X, y and z represent atom hundred
Mark, 12≤x≤14.9,5≤y≤10,0.1≤z≤4;
2. mother alloy ingot is prepared: being put into by raw material and carry out melting in electric arc furnace under an argon atmosphere, melting electric current density is
100~350A/cm2, melting 4-6 time, mix homogeneously, obtain mother alloy ingot after cooling;
3. rotation is quenched: mother alloy ingot is broken into the cobbing of 3~6g, loads in quartz ampoule, quartz ampoule nozzle diameter be 0.6~
1.2mm, nozzle and roll surface distance are 1~6mm, and argon pressure difference is 0.8 × 105~1.5 × 105Pa, uses metal bath fast quenching
Method, the alloy cast ingot refuse that 2. step is prepared, obtain alloy melt;Alloy melt is ejected into rotating speed be 10~
On the copper wheel of 35m/s, obtaining a width of 0.8-2mm, the melt spun alloy band of thick 20-40 μm, this melt spun alloy band is nanocrystalline
Rare earth permanent-magnetic material.
6. according to the preparation method of nanocrystalline rare-earth permanent magnetic material of high thermal stability described in claim 5, it is characterised in that: R,
The purity of Fe, B and M element is all not less than 99.9wt%.
7. according to the preparation method of nanocrystalline rare-earth permanent magnetic material of high thermal stability described in claim 5, it is characterised in that: step
The most 3. described in, quartz ampoule nozzle diameter is 0.8mm, and nozzle and roll surface distance are 2mm, and argon pressure difference is 1.0 × 105Pa, makes
With the method for metal bath fast quenching, alloy cast ingot refuse step 2. prepared, obtain alloy melt;Alloy melt is sprayed
It is mapped on the copper wheel that rotating speed is 20m/s, obtains melt spun alloy band.
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