CN106356187B - Ooze dysprosium technique in a kind of neodymium iron boron surface - Google Patents
Ooze dysprosium technique in a kind of neodymium iron boron surface Download PDFInfo
- Publication number
- CN106356187B CN106356187B CN201610779496.6A CN201610779496A CN106356187B CN 106356187 B CN106356187 B CN 106356187B CN 201610779496 A CN201610779496 A CN 201610779496A CN 106356187 B CN106356187 B CN 106356187B
- Authority
- CN
- China
- Prior art keywords
- neodymium iron
- iron boron
- dysprosium
- heated
- incubated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention relates to one kind to ooze dysprosium technique, more particularly to dysprosium technique is oozed on a kind of neodymium iron boron surface.The technical problem to be solved in the present invention is to provide it is a kind of can increase ooze dysprosium depth, reduce dysprosium dosage, dysprosium technique is oozed on the neodymium iron boron surface without other metallic element additives.The present invention passes through step a f, creativeness all passes through various conditions, through overaging, cleaning and vacuum ooze the processes such as dysprosium, ooze dysprosium processing in the surface for realizing neodymium iron boron, overcome neodymium iron boron surface under prior art ooze dysprosium technique exist ooze dysprosium depth as shallow, process costs are high, the shortcomings that needing to add additive gallium, enhance the quality of neodymium iron boron, strengthen the magnetic of neodymium iron boron, improve the microstructure and crystals microscopic structure of neodymium iron boron magnetic body, reduce scattered magnetic field to exist, improve the HCJ of neodymium iron boron magnetic body, reach increase and ooze dysprosium depth, reduce dysprosium dosage, effect without other metallic element additives, with very strong practicality and operability, it is adapted to promote the use of.
Description
Technical field
The present invention relates to one kind to ooze dysprosium technique, more particularly to dysprosium technique is oozed on a kind of neodymium iron boron surface.
Background technology
Neodymium iron boron, it is exactly a kind of magnet to be briefly, and our magnet for usually seeing except that, its is excellent
Magnetic property and be referred to as " magnetic king ", neodymium iron boron has high magnetic energy product and coercivity as a kind of of rare earth permanent-magnetic material, can
To realize the mutual conversion between magnetic energy and electric energy, so being widely used in information communication, Medical Devices, Aero-Space, existing
In foundry industry and electronic technology field, simultaneously as the advantages of its high-energy-density, make Nd-Fe-B permanent magnet material in modern industry
With more applications are obtained in electronic technology so that instrument and meter, electroacoustic motor, magnetic separation magnetization etc. the miniaturization of equipment,
Lightweight, slimming are possibly realized.The advantages of neodymium iron boron is cost-effective, has good mechanical property；It is disadvantageous in that work
It is low to make temperature, temperature characterisitic is poor, and is easy to dusting corrosion, it is necessary to by adjusting its chemical composition and taking surface treatment method to make
Improved, can be only achieved the requirement of practical application.
Neodymium iron boron is divided into two kinds of sintered NdFeB and Agglutinate neodymium-iron-boron, and Agglutinate neodymium-iron-boron all directions are all magnetic, corrosion resistant
Erosion；And sintered NdFeB, because perishable, surface needs coating, typically there is zinc-plated, nickel, zinc electroplating bath, environmentally friendly nickel, ambrose alloy nickel, environmentally friendly nickel
Cupro-nickel etc..And sintered NdFeB typically divides axial charging and radial magnetizing, determined according to required working face.With sintering neodymium
Iron boron Japan, Germany and European Union etc. are in the defrosting of patented technology, the concerted effort of major sintering producer of China, sintered NdFeB production
Product grade greatly improves, as the continuous improvement to its combination property of high-tech applications, to its sintered NdFeB surface
The requirement of processing also greatly improves, and traditional processing method can not meet the requirement of industrial chain progress, electronics University of Science and Technology, river
Greatly, the research institutions such as big and Rui Shilaisi are handed over, are started with from micro molecule structure, inherently the principle and work of perfect surface processing
The exploitation of industry technique for applying.
With the rapid development of Chinese industrial technology, scientific and technical development, magnetic material has also widely been dissolved into us and given birth to
Among work, our production and life is greatly facilitated, meanwhile, pollution-free industry and green economy have become social development
Trend, how using nature renewable resource be we develop direction of advance.At present, increasing industry needs neodymium iron boron
Be used as products material, it is also growing day by day to the demand of Sintered NdFeB magnet, but contain substantial amounts of rare earth in neodymium iron boron
Element neodymium and boron element, its chemical quality is harder and crisp, and surface is easily oxidized corrosion, the heat of Sintered NdFeB magnet
Stability is poor, so industrial circle will utilize neodymium iron boron, just must carry out surface coated treatment to it.At common surface
Reason method nanometer chelates film without coating processing, phosphatization, electrophoresis plating, vacuum vapor deposition, plated film, organic plastic-spraying, crystalline substance
Boundary, which expands, the handling process such as oozes.It is industrially that crystal boundary expansion is oozed with more methods must be compared, especially with rare earth element as crystal boundary
Expand the raw material oozed, improve Sintered NdFeB magnet anisotropy field by adding trace element, utilize the increase of anisotropy field
The raising of drive Sintered NdFeB magnet HCJ, microstructure and the crystals for improving Sintered NdFeB magnet are micro-
Tissue, reduce and dissipate magnetic field presence, improve the HCJ of Sintered NdFeB magnet.
Neodymium iron boron surface oozes the presence of dysprosium technique and oozes dysprosium depth as shallow, process costs height, needs to add additive under prior art
The shortcomings that gallium, the process operation of sintered NdFeB is not only have impact on, more had a strong impact on the magnetic and again of sintered NdFeB magnetite
Processing, requirement for neodymium iron boron processing technology and quality also more and more higher more and more extensive with the application of neodymium iron boron, therefore
Need badly research and development it is a kind of can increase ooze dysprosium depth, reduce dysprosium dosage, dysprosium is oozed on the neodymium iron boron surface without other metallic element additives
Technique.
The content of the invention
(1) technical problems to be solved
The present invention oozes that dysprosium depth as shallow, process costs are high, needs to overcome under prior art neodymium iron boron surface to ooze dysprosium technique
The shortcomings that adding additive gallium, can increase the technical problem to be solved in the present invention is to provide one kind ooze dysprosium depth, reduction dysprosium dosage,
Ooze dysprosium technique in neodymium iron boron surface without other metallic element additives.
(2) technical scheme
In order to solve the above-mentioned technical problem, the invention provides such a neodymium iron boron surface to ooze dysprosium technique, specifically includes
Following steps：
A. the neodymium iron boron sintered is taken, places it in 12-16 hours under room temperature condition, is heated to 70-90 DEG C, and
Kept for this temperature 10-20 minutes, place it in and cool down at room temperature, and place 12-16 hours again at room temperature；
B. neodymium iron boron in a is taken, its surface is cleaned using clear water, after cleaning up, neodymium iron boron is taken out and is put into 2-
In 3mol/L hydrochloric acid, pickling is carried out to it, the amount of hydrochloric acid submerged neodymium iron boron, and after pickling, 1-2mol/ is added into pickle
L sodium hydroxide solution, the pH of pickle is neutralized to 6.8-7.2, takes out neodymium iron boron and cleaned again with clear water；
C. neodymium iron boron in b is taken to be encased in rustless steel container, tiling placement not stacked, and rustless steel container is heated to
140-160 DEG C, and kept for this temperature 25-35 minutes, stop thereafter heating and vacuumizing inside rustless steel container, keep
30-40 minutes, the dysprosium fluoride nano dispersion fluid to stir is injected in rustless steel container afterwards, dysprosium fluoride nano dispersion fluid
Amount submerged neodymium iron boron, soaked 10-30 minutes, stopped vacuumizing thereafter, allowed its Temperature fall；
D. when neodymium iron boron temperature drops to 40-50 DEG C in c, the dysprosium fluoride nano-dispersed in rustless steel container is persistently stirred
Liquid, continue 8-10 minutes, take out neodymium iron boron afterwards, and put it into heating furnace, continue to be passed through argon gas into heating furnace, will add
Air in hot stove is completely exhausted out, and the flow velocity that is passed through of argon gas is 60-80m3/h；
E. under the protection of argon gas, neodymium iron boron is heated to 300-400 DEG C, is incubated 0.5-0.7 hours, thereafter, then by neodymium
Iron boron is heated to 400-500 DEG C, is incubated 0.7-0.9 hours, and then neodymium iron boron is heated into 500-600 DEG C, is incubated 0.9-
1.1 hours, thereafter, then neodymium iron boron is heated to 600-700 DEG C, is incubated 2.5-3.5 hours, and then neodymium iron boron is heated to
700-800 DEG C, 1.5-2.5 hours are incubated, finally, then neodymium iron boron 850 DEG C is heated to, is incubated 0.8-1.2 hours；
F. neodymium iron boron Temperature fall in e is made, when neodymium iron boron temperature drops to 180-200 DEG C, stopping passes through argon gas, and after
Continuous Temperature fall, when neodymium iron boron temperature drops to 70-90 DEG C, takes out neodymium iron boron, and place it in room temperature from heating furnace
Under the conditions of cooled down, after neodymium iron boron is cooled to room temperature, then at room temperature place 12-16 hours, obtain neodymium iron boron ooze dysprosium into
Product.
Preferably, in step a, 80 DEG C are heated to, and keeps this temperature 15 minutes.
Preferably, in stepb, the concentration of hydrochloric acid is 2.5mol/L, and the concentration of sodium hydroxide solution is 1.5mol/L, will
The pH of pickle is neutralized to 7.0.
Preferably, it in step c, will vacuumize, kept for 35 minutes, the fluorine that will be stirred afterwards inside rustless steel container
To change in dysprosium nano dispersion fluid injection rustless steel container, the amount of dysprosium fluoride nano dispersion fluid submerged neodymium iron boron, soaked 20 minutes, its
Stop vacuumizing afterwards.
Preferably, in step e, under the protection of argon gas, neodymium iron boron is heated to 350 DEG C, is incubated 0.6 hour, thereafter,
Neodymium iron boron is heated to 450 DEG C again, is incubated 0.8 hour, and then neodymium iron boron is heated to 550 DEG C, is incubated 1 hour, thereafter,
Neodymium iron boron is heated to 650 DEG C again, is incubated 3 hours, and then neodymium iron boron is heated to 750 DEG C, is incubated 2 hours, finally, then
Neodymium iron boron is heated to 850 DEG C, is incubated 1 hour.
Preferably, in step f, when neodymium iron boron temperature drops to 190 DEG C, stopping passes through argon gas, and continues nature drop
Temperature, when neodymium iron boron temperature drops to 80 DEG C, neodymium iron boron is taken out from heating furnace.
(3) beneficial effect
The present invention compared with the prior art, overcome neodymium iron boron surface under prior art ooze dysprosium technique exist ooze dysprosium depth
It is shallow, process costs are high, need add additive gallium the shortcomings that, breakthroughly by the adjustment on process structure, first carry out timeliness
Processing, ensure the stability of neodymium iron boron, then by cleaning and pickling, the impurity on neodymium iron boron surface is removed, then is soaked by heating
Bubble, carry out oozing dysprosium, and the heating of the protection lower leaf time in argon gas under vacuum, finally, then carry out Ageing Treatment, so
Mode of operation the operating cost of technique on the basis of dysprosium dosage is reduced, also without additive gallium to be added, can be reduced, together
When, at splendid temperature and vacuum operation, the depth for oozing dysprosium is further increased, moreover, enhancing the quality of neodymium iron boron, is added
The strong magnetic of neodymium iron boron, improves the microstructure and crystals microscopic structure of neodymium iron boron magnetic body, reduces scattered magnetic field and deposit
The HCJ of neodymium iron boron magnetic body is being improved, dysprosium depth is being oozed so as to reach increase, reduces dysprosium dosage, without other gold
Belong to the effect of element additive, there is very strong practicality and operability, be adapted to promote the use of.
Embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
Dysprosium technique is oozed on a kind of neodymium iron boron surface, is specifically comprised the following steps：
A. the neodymium iron boron sintered is taken, room temperature condition is placed it in lower 12 hours, is heated to 70 DEG C, and keep this
Individual temperature 20 minutes, places it in and cools down at room temperature, and places 16 hours again at room temperature；
B. neodymium iron boron in a is taken, its surface is cleaned using clear water, after cleaning up, neodymium iron boron is taken out and is put into
In 2mol/L hydrochloric acid, pickling is carried out to it, the amount of hydrochloric acid submerged neodymium iron boron, and after pickling, 1mol/L is added into pickle
Sodium hydroxide solution, the pH of pickle is neutralized to 6.8, neodymium iron boron is taken out and is simultaneously cleaned again with clear water；
C. neodymium iron boron in b is taken to be encased in rustless steel container, tiling placement not stacked, and rustless steel container is heated to
140 DEG C, and keep this temperature 35 minutes, stop thereafter heating and vacuumizing inside rustless steel container, kept for 30 minutes, it
The dysprosium fluoride nano dispersion fluid to stir is injected in rustless steel container afterwards, the amount of dysprosium fluoride nano dispersion fluid submerged neodymium iron
Boron, soak 30 minutes, stop vacuumizing thereafter, allow its Temperature fall；
D. when neodymium iron boron temperature drops to 50 DEG C in c, the dysprosium fluoride nano dispersion fluid in rustless steel container is persistently stirred,
Continue 8 minutes, take out neodymium iron boron afterwards, and put it into heating furnace, continue to be passed through argon gas into heating furnace, by heating furnace
Air be completely exhausted out, the flow velocity that is passed through of argon gas is 60m3/h；
E. under the protection of argon gas, neodymium iron boron is heated to 300 DEG C, is incubated 0.7 hour, thereafter, then neodymium iron boron heated
To 400 DEG C, 0.9 hour is incubated, and then neodymium iron boron is heated to 500 DEG C, is incubated 1.1 hours, thereafter, then neodymium iron boron is added
Heat is incubated 3.5 hours to 600 DEG C, and then neodymium iron boron is heated into 700 DEG C, is incubated 2.5 hours, finally, then by neodymium iron boron
850 DEG C are heated to, is incubated 0.8 hour；
F. neodymium iron boron Temperature fall in e is made, when neodymium iron boron temperature drops to 180 DEG C, stopping passes through argon gas, and continues certainly
So cooling, when neodymium iron boron temperature drops to 70 DEG C, takes out neodymium iron boron, and place it under room temperature condition from heating furnace
Row cooling, after neodymium iron boron is cooled to room temperature, then place 16 hours at room temperature, obtain neodymium iron boron and ooze dysprosium finished product.
Embodiment 2
Dysprosium technique is oozed on a kind of neodymium iron boron surface, is specifically comprised the following steps：
A. the neodymium iron boron sintered is taken, room temperature condition is placed it in lower 14 hours, is heated to 80 DEG C, and keep this
Individual temperature 15 minutes, places it in and cools down at room temperature, and places 14 hours again at room temperature；
B. neodymium iron boron in a is taken, its surface is cleaned using clear water, after cleaning up, neodymium iron boron is taken out and is put into
In 2.5mol/L hydrochloric acid, pickling is carried out to it, the amount of hydrochloric acid submerged neodymium iron boron, after pickling, was added into pickle
1.5mol/L sodium hydroxide solution, the pH of pickle is neutralized to 7, takes out neodymium iron boron and cleaned again with clear water；
C. neodymium iron boron in b is taken to be encased in rustless steel container, tiling placement not stacked, and rustless steel container is heated to
150 DEG C, and keep this temperature 30 minutes, stop thereafter heating and vacuumizing inside rustless steel container, kept for 35 minutes, it
The dysprosium fluoride nano dispersion fluid to stir is injected in rustless steel container afterwards, the amount of dysprosium fluoride nano dispersion fluid submerged neodymium iron
Boron, soak 20 minutes, stop vacuumizing thereafter, allow its Temperature fall；
D. when neodymium iron boron temperature drops to 45 DEG C in c, the dysprosium fluoride nano dispersion fluid in rustless steel container is persistently stirred,
Continue 9 minutes, take out neodymium iron boron afterwards, and put it into heating furnace, continue to be passed through argon gas into heating furnace, by heating furnace
Air be completely exhausted out, the flow velocity that is passed through of argon gas is 70m3/h；
E. under the protection of argon gas, neodymium iron boron is heated to 350 DEG C, is incubated 0.6 hour, thereafter, then neodymium iron boron heated
To 450 DEG C, 0.8 hour is incubated, and then neodymium iron boron is heated to 550 DEG C, is incubated 1 hour, thereafter, then neodymium iron boron is heated
To 650 DEG C, 3 hours are incubated, and then neodymium iron boron is heated to 750 DEG C, is incubated 2 hours, finally, then neodymium iron boron is heated to
850 DEG C, it is incubated 1 hour；
F. neodymium iron boron Temperature fall in e is made, when neodymium iron boron temperature drops to 190 DEG C, stopping passes through argon gas, and continues certainly
So cooling, when neodymium iron boron temperature drops to 80 DEG C, takes out neodymium iron boron, and place it under room temperature condition from heating furnace
Row cooling, after neodymium iron boron is cooled to room temperature, then place 14 hours at room temperature, obtain neodymium iron boron and ooze dysprosium finished product.
Embodiment 3
Dysprosium technique is oozed on a kind of neodymium iron boron surface, is specifically comprised the following steps：
A. the neodymium iron boron sintered is taken, room temperature condition is placed it in lower 16 hours, is heated to 90 DEG C, and keep this
Individual temperature 10 minutes, places it in and cools down at room temperature, and places 12 hours again at room temperature；
B. neodymium iron boron in a is taken, its surface is cleaned using clear water, after cleaning up, neodymium iron boron is taken out and is put into
In 3mol/L hydrochloric acid, pickling is carried out to it, the amount of hydrochloric acid submerged neodymium iron boron, and after pickling, 2mol/L is added into pickle
Sodium hydroxide solution, the pH of pickle is neutralized to 7.2, neodymium iron boron is taken out and is simultaneously cleaned again with clear water；
C. neodymium iron boron in b is taken to be encased in rustless steel container, tiling placement not stacked, and rustless steel container is heated to
160 DEG C, and keep this temperature 25 minutes, stop thereafter heating and vacuumizing inside rustless steel container, kept for 40 minutes, it
The dysprosium fluoride nano dispersion fluid to stir is injected in rustless steel container afterwards, the amount of dysprosium fluoride nano dispersion fluid submerged neodymium iron
Boron, soak 10 minutes, stop vacuumizing thereafter, allow its Temperature fall；
D. when neodymium iron boron temperature drops to 40 DEG C in c, the dysprosium fluoride nano dispersion fluid in rustless steel container is persistently stirred,
Continue 10 minutes, take out neodymium iron boron afterwards, and put it into heating furnace, continue to be passed through argon gas into heating furnace, by heating furnace
Interior air is completely exhausted out, and the flow velocity that is passed through of argon gas is 80m3/h；
E. under the protection of argon gas, neodymium iron boron is heated to 400 DEG C, is incubated 0.5 hour, thereafter, then neodymium iron boron heated
To 500 DEG C, 0.7 hour is incubated, and then neodymium iron boron is heated to 600 DEG C, is incubated 0.9 hour, thereafter, then neodymium iron boron is added
Heat is incubated 2.5 hours to 700 DEG C, and then neodymium iron boron is heated into 800 DEG C, is incubated 1.5 hours, finally, then by neodymium iron boron
850 DEG C are heated to, is incubated 1.2 hours；
F. neodymium iron boron Temperature fall in e is made, when neodymium iron boron temperature drops to 200 DEG C, stopping passes through argon gas, and continues certainly
So cooling, when neodymium iron boron temperature drops to 90 DEG C, takes out neodymium iron boron, and place it under room temperature condition from heating furnace
Row cooling, after neodymium iron boron is cooled to room temperature, then place 12 hours at room temperature, obtain neodymium iron boron and ooze dysprosium finished product.
In the present invention, oozed by three kinds of neodymium iron boron surfaces of above-described embodiment 1, embodiment 2 and embodiment 3 at dysprosium technique
Reason, obtains sample 1, sample 2, three neodymium iron borons of sample 3 and oozes dysprosium finished product, and ooze dysprosium work using neodymium iron boron surface under prior art
The neodymium iron boron that skill handles to obtain oozes dysprosium finished product sample 4 and detected, and carries out data comparison：Oozing the neodymium iron of dysprosium processing homogenous quantities
In the case of boron, embodiment 1, embodiment 2 and embodiment 3 descend neodymium iron boron surface to ooze dysprosium technique compared with prior art, and dysprosium element makes
Reduce 3.8%, 4.2% and 3.9% respectively with dosage, meanwhile, by cutting measurement sample 1, sample 2, sample 3 and sample 4,
Sample 1, sample 2 and sample 3 descend neodymium iron boron surface to ooze the sample 4 that dysprosium technique obtains compared with prior art, ooze dysprosium depth and carry respectively
Height knows clearly 1.6%, 1.8% and 1.7%.Therefore deduce that, the present invention significantly enhances neodymium iron while dysprosium dosage is saved
The quality of boron, the magnetic of neodymium iron boron is strengthened, improve the microstructure and crystals microscopic structure of neodymium iron boron magnetic body.
Embodiment described above only expresses the preferred embodiment of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, some deformations can also be made, improves and substitutes, these belong to this hair
Bright protection domain.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. dysprosium technique is oozed on a kind of neodymium iron boron surface, it is characterised in that is specifically comprised the following steps：
A. the neodymium iron boron sintered is taken, places it in 12-16 hours under room temperature condition, is heated to 70-90 DEG C, and keep
This temperature 10-20 minutes, place it in and cool down at room temperature, and place 12-16 hours again at room temperature；
B. neodymium iron boron in a is taken, its surface is cleaned using clear water, after cleaning up, neodymium iron boron is taken out and is put into 2-3mol/
In L hydrochloric acid, pickling is carried out to it, the amount of hydrochloric acid submerged neodymium iron boron, and after pickling, 1-2mol/L hydrogen is added into pickle
Sodium hydroxide solution, the pH of pickle is neutralized to 6.8-7.2, takes out neodymium iron boron and cleaned again with clear water；
C. neodymium iron boron in b is taken to be encased in rustless steel container, tiling placement not stacked, and rustless steel container is heated into 140-
160 DEG C, and kept for this temperature 25-35 minutes, stop thereafter heating and vacuumizing inside rustless steel container, keep 30-40
Minute, the dysprosium fluoride nano dispersion fluid to stir is injected in rustless steel container afterwards, the amount leaching of dysprosium fluoride nano dispersion fluid
Do not cross neodymium iron boron, soak 10-30 minutes, stop vacuumizing thereafter, allow its Temperature fall；
D. when neodymium iron boron temperature drops to 40-50 DEG C in c, the dysprosium fluoride nano dispersion fluid in rustless steel container is persistently stirred,
Continue 8-10 minutes, take out neodymium iron boron afterwards, and put it into heating furnace, continue to be passed through argon gas into heating furnace, will heat
Air in stove is completely exhausted out, and the flow velocity that is passed through of argon gas is 60-80m3/h；
E. under the protection of argon gas, neodymium iron boron is heated to 300-400 DEG C, is incubated 0.5-0.7 hours, thereafter, then by neodymium iron boron
400-500 DEG C is heated to, is incubated 0.7-0.9 hours, and then neodymium iron boron is heated to 500-600 DEG C, insulation 0.9-1.1 is small
When, thereafter, then neodymium iron boron is heated to 600-700 DEG C, is incubated 2.5-3.5 hours, and then neodymium iron boron is heated to 700-
800 DEG C, 1.5-2.5 hours are incubated, finally, then neodymium iron boron 850 DEG C is heated to, is incubated 0.8-1.2 hours；
F. neodymium iron boron Temperature fall in e is made, when neodymium iron boron temperature drops to 180-200 DEG C, stopping passes through argon gas, and continues certainly
So cooling, when neodymium iron boron temperature drops to 70-90 DEG C, takes out neodymium iron boron, and place it in room temperature condition from heating furnace
Under cooled down, after neodymium iron boron is cooled to room temperature, then at room temperature place 12-16 hours, obtain neodymium iron boron and ooze dysprosium finished product.
2. dysprosium technique is oozed on a kind of neodymium iron boron surface according to claim 1, it is characterised in that in step a, is heated
To 80 DEG C, and keep this temperature 15 minutes.
3. dysprosium technique is oozed on a kind of neodymium iron boron surface according to claim 1, it is characterised in that in stepb, hydrochloric acid it is dense
Spend for 2.5mol/L, the concentration of sodium hydroxide solution is 1.5mol/L, and the pH of pickle is neutralized into 7.0.
4. dysprosium technique is oozed on a kind of neodymium iron boron surface according to claim 1, it is characterised in that in step c, by stainless steel
Vacuumized inside container, kept for 35 minutes, afterwards injected the dysprosium fluoride nano dispersion fluid to stir in rustless steel container, fluorine
The amount for changing dysprosium nano dispersion fluid submerged neodymium iron boron, soaked 20 minutes, stopped vacuumizing thereafter.
5. dysprosium technique is oozed on a kind of neodymium iron boron surface according to claim 1, it is characterised in that in step e, in argon gas
Under protection, neodymium iron boron is heated to 350DEG C, 0.6 hour is incubated, thereafter, then neodymium iron boron is heated to 450 DEG C, insulation 0.8 is small
When, and then neodymium iron boron is heated to 550 DEG C, is incubated 1 hour, thereafter, then neodymium iron boron is heated to 650 DEG C, be incubated 3 hours,
And then neodymium iron boron is heated to 750 DEG C, 2 hours are incubated, finally, then neodymium iron boron 850 DEG C is heated to, is incubated 1 hour.
6. dysprosium technique is oozed on a kind of neodymium iron boron surface according to claim 1, it is characterised in that in step f, works as neodymium iron boron
When temperature drops to 190 DEG C, stopping passes through argon gas, and continues Temperature fall, when neodymium iron boron temperature drops to 80 DEG C, from heating
Neodymium iron boron is taken out in stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610779496.6A CN106356187B (en) | 2016-08-30 | 2016-08-30 | Ooze dysprosium technique in a kind of neodymium iron boron surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610779496.6A CN106356187B (en) | 2016-08-30 | 2016-08-30 | Ooze dysprosium technique in a kind of neodymium iron boron surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106356187A CN106356187A (en) | 2017-01-25 |
| CN106356187B true CN106356187B (en) | 2018-03-09 |
Family
ID=57856254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610779496.6A Active CN106356187B (en) | 2016-08-30 | 2016-08-30 | Ooze dysprosium technique in a kind of neodymium iron boron surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106356187B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799294B (en) * | 2017-11-29 | 2019-11-29 | 宁德市星宇科技有限公司 | A kind of method that grain boundary decision prepares neodymium iron boron magnetic body |
| CN108376595A (en) * | 2017-12-31 | 2018-08-07 | 江西荧光磁业有限公司 | A kind of preparation method of heat-resist sintered NdFeB |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4737248A (en) * | 1985-12-19 | 1988-04-12 | Sumitomo Light Metal Industries, Ltd. | Process for producing dysprosium-iron alloy and neodymium-dysprosium-iron alloy |
| CN102930975A (en) * | 2012-10-24 | 2013-02-13 | 烟台正海磁性材料股份有限公司 | Manufacturing method of R-Fe-B series sintered magnets |
| CN103258633A (en) * | 2013-05-30 | 2013-08-21 | 烟台正海磁性材料股份有限公司 | Method for preparing R-Fe-B series sintered magnets |
| CN103757587A (en) * | 2014-01-13 | 2014-04-30 | 赣南师范学院 | Method for penetrating metal penetrant into sintered NdFeB permanent-magnet material |
| CN104164646A (en) * | 2014-08-01 | 2014-11-26 | 浙江英洛华磁业有限公司 | Dysprosium infiltration method on neodymium-iron-boron surface and terbium infiltration method on neodymium-iron-boron surface |
| CN105489336A (en) * | 2016-01-22 | 2016-04-13 | 宁波松科磁材有限公司 | Method for dysprosium infiltration of NdFeB magnets |
-
2016
- 2016-08-30 CN CN201610779496.6A patent/CN106356187B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4737248A (en) * | 1985-12-19 | 1988-04-12 | Sumitomo Light Metal Industries, Ltd. | Process for producing dysprosium-iron alloy and neodymium-dysprosium-iron alloy |
| CN102930975A (en) * | 2012-10-24 | 2013-02-13 | 烟台正海磁性材料股份有限公司 | Manufacturing method of R-Fe-B series sintered magnets |
| CN103258633A (en) * | 2013-05-30 | 2013-08-21 | 烟台正海磁性材料股份有限公司 | Method for preparing R-Fe-B series sintered magnets |
| CN103757587A (en) * | 2014-01-13 | 2014-04-30 | 赣南师范学院 | Method for penetrating metal penetrant into sintered NdFeB permanent-magnet material |
| CN104164646A (en) * | 2014-08-01 | 2014-11-26 | 浙江英洛华磁业有限公司 | Dysprosium infiltration method on neodymium-iron-boron surface and terbium infiltration method on neodymium-iron-boron surface |
| CN105489336A (en) * | 2016-01-22 | 2016-04-13 | 宁波松科磁材有限公司 | Method for dysprosium infiltration of NdFeB magnets |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106356187A (en) | 2017-01-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2017067251A1 (en) | Electrodeposition method, bath and rare earth permanent magnet materials preparation method using same | |
| CN102808210B (en) | Micro-arc oxidation surface treatment method and product prepared by same | |
| CN103839670A (en) | Method for preparing high-coercivity sintered Nd-Fe-B permanent magnet | |
| CN103617884A (en) | Heavy rear earth adhering method of sintered NdFeB magnet | |
| CN106356187B (en) | Ooze dysprosium technique in a kind of neodymium iron boron surface | |
| CN110211797A (en) | A method of promoting Sintered NdFeB magnet magnetic property | |
| CN107653440A (en) | A kind of method that sintered Nd-Fe-B permanent magnet surface prepares aluminium or mock silver coating | |
| CN107564723A (en) | The preparation method of high-coercive force neodymium iron boron magnetic body | |
| CN106876072A (en) | The method for improving neodymium-iron-boron magnetic material magnetic property | |
| CN105513733B (en) | A kind of preparation method of sintering type Nd iron boron permanent magnetic material | |
| CN108335898A (en) | A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique | |
| CN105648487A (en) | Electro-deposition method, electro-deposition liquid and method for preparing rare earth permanent magnetic material in electro-deposition manner | |
| CN102560445B (en) | Process for chemically and compositely plating nickel and phosphorus on sintered neodymium iron boron | |
| CN102925851B (en) | Two-section gas nitridation method for surfaces of aluminum and aluminum alloy | |
| CN100484666C (en) | Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique | |
| CN109692963A (en) | A kind of preparation method of the neodymium iron boron magnetic body of surface with corrosion-resistant finishes | |
| CN105040004B (en) | A kind of Sintered NdFeB magnet surface coating technique | |
| CN115475745B (en) | Preparation process and coating method of vanadium oxide rare earth double-doped ferrite magnetic composite film slurry | |
| CN111748783A (en) | Multi-element heavy rare earth metal target for magnetic material coating | |
| CN106544657A (en) | Improve coating liquid, method and its application of material surface modifying layer performance | |
| CN102703951B (en) | Room-temperature magnetic field assisted sealing method for aluminum alloy anode oxide film | |
| CN103540977A (en) | Method for preparing high-gas tightness nickel-copper alloy for travelling wave tube | |
| CN108565088B (en) | A kind of band coating sintered NdFeB magnet and preparation method thereof | |
| CN102416483B (en) | Method for preparing double-phase composite samarium cobalt-iron powder | |
| CN104911511B (en) | Composite amorphous soft magnetic alloy with excellent alternating current stability |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Process for infiltrating dysprosium in neodymium, iron and boron surfaces Effective date of registration: 20190716 Granted publication date: 20180309 Pledgee: Ganzhou Branch of Bank of Communications Co., Ltd. Pledgor: Jiangxi YG Magnet Industry Co., Lt. Registration number: 2019360000021 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20201014 Granted publication date: 20180309 Pledgee: Ganzhou Branch of Bank of Communications Co.,Ltd. Pledgor: JIANGXI YG MAGNET Co.,Ltd. Registration number: 2019360000021 |