CN106710767B - The corrosion-resistant more coating neodymium iron borons of one kind and preparation process - Google Patents
The corrosion-resistant more coating neodymium iron borons of one kind and preparation process Download PDFInfo
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- CN106710767B CN106710767B CN201611157661.0A CN201611157661A CN106710767B CN 106710767 B CN106710767 B CN 106710767B CN 201611157661 A CN201611157661 A CN 201611157661A CN 106710767 B CN106710767 B CN 106710767B
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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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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- 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
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
Abstract
The corrosion-resistant more coating neodymium iron borons of one kind provided by the invention and preparation process, it is made of Nd-Fe-B permanent magnet and more coating, more coating are set to the outer surface of the Nd-Fe-B permanent magnet, more coating include nickel coating successively from the inside to the outside, plate dysprosium aluminum alloy thin film layer and nickel chromium triangle composite deposite, wherein, the nickel plating layer thick is 10~15 μm, the thickness of the plating dysprosium aluminum alloy thin film layer is 10~20 μm, the thickness of the nickel chromium triangle composite deposite is 6~10 μm, more coating modifications may be implemented in permanent magnet surfaces, on the basis of ensureing coating with permanent magnet bond matrix intensity, coating is relatively thin caused by overcoming single technique, corrosion resistance and the shortcomings that wearing no resistance, so that the corrosion-resistant more coating neodymium iron borons prepared have good corrosion resistance and wear-resisting property.
Description
Technical field
The present invention relates to permanent-magnet material fields, specifically, be a kind of corrosion resistant more coating Nd-Fe-B permanent magnet materials and
Its preparation process.
Background technology
Neodymium iron boron as third generation permanent-magnet material due to excellent magnetic property and cheap price, microwave technology,
The fields such as audio-visual technology, electrical engineering, instrumental technique, computer technology, magnetic separation technique, auto industry have obtained answering extensively
With.As sintered NdFeB is in the defrosting of the patented technologies such as Japan, Germany, European Union, the concerted effort of major sintering producer of China,
The grade of sintered NdFeB product also greatly improves.Further genralrlization with neodymium iron boron as high-tech applications simultaneously,
The comprehensive performance of its product is required also to be continuously improved, especially its corrosion resistance is required higher and higher.Therefore, to neodymium iron boron
Permanent magnet carries out overlay coating processing, can further increase its rotproofness performance.
But Nd-Fe-B permanent magnet prepared by single chemical plating or electroplating technology only has single coating, thickness of coating
It is limited, generally at 10 μm hereinafter, and coating adhesion it is bad, compactness is also poor, cause its it is corrosion-resistant with wear-resisting property still
The needs of technology development cannot be met.
Invention content
The main purpose of the present invention is to provide a kind of corrosion-resistant more coating neodymium iron borons and preparation processes, for existing
The problem of NbFeB sintered permanent magnet corrosion resistance and oxidation resistance difference, it is more to prepare that a kind of corrosion resistance is strong, wearability is good
Coating Nd-Fe-B permanent magnet, while the preparation process of more coating neodymium iron borons being provided.
To achieve the above objectives, the technical solution adopted by the present invention is：The corrosion-resistant more coating neodymium iron borons of one kind are by neodymium iron boron
Permanent magnet and more coating composition, more coating are set to the outer surface of the Nd-Fe-B permanent magnet, more coating by it is inner extremely
Include nickel coating, plating dysprosium aluminum alloy thin film layer and nickel chromium triangle composite deposite successively outside, wherein the nickel plating layer thick is 10~15
μm, the thickness of the plating dysprosium aluminum alloy thin film layer is 10~20 μm, and the thickness of the nickel chromium triangle composite deposite is 6~10 μm.
A kind of preparation process of corrosion-resistant more coating neodymium iron borons comprising step：
S100 pre-processes Nd-Fe-B permanent magnet, and acid is carried out to Nd-Fe-B permanent magnet with the mixing pickle of dust technology and thiocarbamide
It washes down clean, then is cleaned by ultrasonic with absolute ethyl alcohol, completion, which is placed in sulfosalicylic acid and ammonium acid fluoride mixed liquor, lives
Change；
S200 chemical nickel platings are in the outer surface of Nd-Fe-B permanent magnet, by six hydration nickel sulfate solution, sodium hypophosphite solution, boron
Sand solution, sodium citrate solution, ammonium fluoride solution, succinic acid solution are configured to chemical plating fluid, forever by pretreated neodymium iron boron
Magnet is placed in chemical plating fluid, carries out nickel plating under default chemical plating temperature, default electroless plating time, the nickel coating is made；
S300 magnetron sputterings dysprosium aluminum alloy thin film layer is in the nickel coating outer surface, in the neodymium iron boron magnetic body of chemical nickel plating
Surface carries out magnetron sputtering plating, combines sputtering system progress with ion beam using superhigh vacuum magnetron sputtering, and sputtering target material is
Dysprosium aluminium alloy, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity argon
Gas, carries out magnetron sputtering plating in preset time, and after plated film, Vacuum Heat diffusion penetration, system are used under preset temperature
Obtain the plating dysprosium aluminum alloy thin film layer；And
The surfaces S400 pulse plating nickel chromium triangle composite deposite is hydrated sulphur in the outer surface of the plating dysprosium aluminum alloy thin film layer by six
Sour nickel, ammonium chloride, boric acid are added to the water and dissolve by heating, and lauryl sodium sulfate are added in above-mentioned solution, magnetic agitation
Nanometer chromium powder is added in above-mentioned solution in 30min, increases temperature to 65 DEG C, vibration of ultrasonic wave 30min, which is uniformly mixed, prepares plating
Liquid adjusts acid plating liquid basicity and is saved backup in preset temperature, using nickel plate as anode, using neodymium iron boron as cathode, uses number
It controls Double-pulse Plating Power Source and carries out electroplating surface, corrosion-resistant more coating neodymium iron borons are made.
An embodiment according to the present invention, the step S100 specifically include step：The 0.5-1.0mol/L of 500mL is added
Dust technology and the thiocarbamide of 0.5g/L of 500mL prepare pickle, Nd-Fe-B permanent magnet is placed in acid solution and cleans 2-3min, so
Be placed in the absolute ethyl alcohol of 500mL and carry out 1~2min of ultrasonic cleaning, complete be placed on 500mL 20g/L sulfosalicylic acids and
It is activated in the 10g/L ammonium acid fluoride mixed liquors of 500mL, soak time 1min, 25 DEG C of activation temperature.
An embodiment according to the present invention, the step S200 specifically include step：By six hydrations of the 26g/L of 300mL
Nickel sulfate solution, the sodium hypophosphite solution of 30g/L of 300mL, the borax soln of 30g/L of 100mL, 100mL 30g/L lemon
Lemon acid sodium solution, the ammonium fluoride solution of 30g/L of 100mL, 100mL the succinic acid solution of 3g/L prepare chemical plating fluid, will be pre-
Processed Nd-Fe-B permanent magnet is placed in chemical plating fluid, is 80~85 DEG C in chemical plating temperature, 30~40min of electroless plating time
Under the conditions of carry out nickel plating.
An embodiment according to the present invention, the step S300 specifically include step：In the neodymium iron boron magnetic body of chemical nickel plating
Surface carries out magnetron sputtering plating, combines sputtering system progress with ion beam using superhigh vacuum magnetron sputtering, and sputtering target material is
Dysprosium aluminium alloy, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity argon
Gas, 1~2h of magnetron sputtering plating after plated film, use Vacuum Heat diffusion penetration 6h at a temperature of 750~850 DEG C, institute are made
State plating dysprosium aluminum alloy thin film layer.
An embodiment according to the present invention, the step S400 specifically include step：Weigh 150g six hydration nickel sulfate,
The ammonium chloride of 15g, the boric acid of 15g are added 1000ml distilled water, are placed in 50 DEG C of thermostat water baths heat and make it dissolve, then plus
Entering the lauryl sodium sulfate of 1g in above-mentioned solution, the nanometer chromium powder of 50g is added in above-mentioned solution in magnetic agitation 30min,
Temperature is increased to 65 DEG C, vibration of ultrasonic wave 30min, which is uniformly mixed, prepares electroplate liquid, adjusts bath pH values, is preserved at 65 DEG C
Spare, the nickel plate for being 99% using purity is anode, using neodymium iron boron as cathode, is electroplated using numerical control Double-pulse Plating Power Source,
Electroplating current density in a certain range, under pulse duty factor, it is compound that the nickel chromium triangle is made in surface pulse plating certain time
Coating.
The pH value of an embodiment according to the present invention, the pulse plating liquid in the step S400 is 6.5~7.0.
An embodiment according to the present invention, the pulsed electroplating current density in the step S400 are 2.5~3.5A/dm2。
An embodiment according to the present invention, pulse duty factor is 0.3,0.4 when pulse plating in the step S400,
0.5。
An embodiment according to the present invention, 30~50min of pulse plating time in the step S400.
The present invention compared with the existing technology, mainly has the following advantages and beneficial effect：
1, a kind of preparation process of corrosion-resistant more coating neodymium iron borons provided by the invention uses pre-treating technology to neodymium iron boron
Permanent magnet is activated, and the binding force for improving matrix and coating is conducive to；Using chemical plating, magnetically controlled DC sputtering, surface pulse
The technique that is combined is electroplated, more coating moditied processings are carried out in surface of Nd-Fe-B permanent magnet, may be implemented each thickness of coating with
More coating modifications may be implemented in permanent magnet surfaces, in the base for ensureing coating and permanent magnet bond matrix intensity in the regulation and control of evenness
On plinth, overcome that coating caused by single technique is relatively thin, corrosion resistance and the shortcomings that wear no resistance so that preparation it is corrosion-resistant more
Coating neodymium iron boron has good corrosion resistance and wear-resisting property；
2, the uniformity and flatness of permanent magnet surfaces nickel coating can be effectively ensured in chemical nickel plating, be conducive to raising second
The cohesive force of coating ensures the thickness of the second coating；
3, magnetically controlled DC sputtering plating DyAl alloy firms can ooze temperature regulation and control by adjusting plated film time and vacuum thermal expansion
The thickness and the uniformity of coating, use rare earth element for coating, further increase the wear-resisting property of coating；
4, surface pulse plating Ni-Cr composite deposites can control plating by adjusting the technical data of pulse plating
The thickness of layer is conducive to the corrosion resistance for improving coating using Ni-Cr composite deposites.
Specific implementation mode
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1
A kind of preparation process of corrosion-resistant more coating neodymium iron borons comprising step：
(1) it pre-processes, the thiocarbamide that the dust technology of a concentration of 0.5mol/L of 500ml and the 0.5g/L of 500ml is added prepares acid
Nd-Fe-B permanent magnet is placed in acid solution and cleans 2-3min by washing lotion, is subsequently placed in the absolute ethyl alcohol of 500mL and is cleaned by ultrasonic
1-2min, completion, which is placed in the 20g/L sulfosalicylic acids of 500ml and the 10g/L ammonium acid fluoride mixed liquors of 500ml, lives
Change, soak time 1min, 25 DEG C of activation temperature；
(2) chemical nickel plating weighs the sodium hypophosphite of the six hydration nickel sulfate solution of the 26g/L of 300ml, the 30g/L of 300ml
Solution, the borax soln of 30g/L of 100ml, the sodium citrate solution of 30g/L of 100ml, 100ml 30g/L ammonium fluoride it is molten
Liquid, 100ml 3g/L succinic acid solution prepare chemical plating fluid, pretreated Nd-Fe-B permanent magnet is placed in chemical plating fluid
In, at a temperature of 80 DEG C of chemical platings, chemical nickel plating 30min, gained chemical nickel plating layer thickness is 10 μm；
(3) magnetically controlled DC sputtering plates DyAl alloy firms, and magnetron sputtering is carried out on the neodymium iron boron magnetic body surface of chemical nickel plating
Plated film, sputtering system progress is combined using FJL560CI1 types superhigh vacuum magnetron sputtering with ion beam, and sputtering target material is
Dy35A165 alloys, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity
Argon gas, the magnetron sputtering plating time is 1h, and after plated film, Vacuum Heat diffusion penetration is used at a temperature of 750 DEG C, handles 6h,
The thickness of gained DyAl alloy firm layers is 10 μm；
(4) surface pulse plating weighs the boric acid of the six hydration nickel sulfate of 150g, the ammonium chloride of 15g, 15g, is added
1000ml distilled water, is placed in 50 DEG C of thermostat water baths to heat and makes it dissolve, and the lauryl sodium sulfate of 1g is added in above-mentioned molten
In liquid, the nanometer Cr powder of 50g is added in above-mentioned solution in magnetic agitation 30min, increases temperature to 65 DEG C, vibration of ultrasonic wave
30min, which is uniformly mixed, prepares electroplate liquid, and it is 6.5 to adjust bath pH values, and nickel that is spare, being 99% with purity is kept the temperature at 65 DEG C
Plate is anode, using neodymium iron boron as cathode, is electroplated using SMD-30 type numerical control Double-pulse Plating Power Sources, electroplating current density
2.5/dm2, pulse duty factor 0.3, electroplating time 30min, 6 μm of the thickness of gained Ni-Cr composite deposites.
Embodiment 2
A kind of preparation process of corrosion-resistant more coating neodymium iron borons comprising step：
(1) it pre-processes, the thiocarbamide that the dust technology of a concentration of 1.0mol/L of 500ml and the 0.5g/L of 500ml is added prepares acid
Nd-Fe-B permanent magnet is placed in acid solution and cleans 2-3min by washing lotion, is subsequently placed in the absolute ethyl alcohol of 500mL and is cleaned by ultrasonic
1-2min, completion, which is placed in the 20g/L sulfosalicylic acids of 500ml and the 10g/L ammonium acid fluoride mixed liquors of 500ml, lives
Change, soak time 1min, 25 DEG C of activation temperature；
(2) chemical nickel plating weighs the sodium hypophosphite of the six hydration nickel sulfate solution of the 26g/L of 300ml, the 30g/L of 300ml
Solution, the borax soln of 30g/L of 100ml, the sodium citrate solution of 30g/L of 100ml, 100ml 30g/L ammonium fluoride it is molten
Liquid, 100ml 3g/L succinic acid solution prepare chemical plating fluid, pretreated Nd-Fe-B permanent magnet is placed in chemical plating fluid
In, at a temperature of 85 DEG C of chemical platings, chemical nickel plating 40min, gained chemical nickel plating layer thickness is 15 μm；
(3) magnetically controlled DC sputtering plates DyAl alloy firms, and magnetron sputtering is carried out on the neodymium iron boron magnetic body surface of chemical nickel plating
Plated film, sputtering system progress is combined using FJL560CI1 types superhigh vacuum magnetron sputtering with ion beam, and sputtering target material is
Dy35A165 alloys, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity
Argon gas, the magnetron sputtering plating time is 2h, and after plated film, Vacuum Heat diffusion penetration is used at a temperature of 850 DEG C, handles 6h,
The thickness of gained DyAl alloy firm layers is 20 μm；
(4) surface pulse plating.The boric acid of the six hydration nickel sulfate of 150g, the ammonium chloride of 15g, 15g is weighed, is added
1000ml distilled water, is placed in 50 DEG C of thermostat water baths to heat and makes it dissolve, and the lauryl sodium sulfate of 1g is added in above-mentioned molten
In liquid, the nanometer Cr powder of 50g is added in above-mentioned solution in magnetic agitation 30min, increases temperature to 65 DEG C, vibration of ultrasonic wave
30min, which is uniformly mixed, prepares electroplate liquid, and it is 7.0 to adjust bath pH values, and nickel that is spare, being 99% with purity is kept the temperature at 65 DEG C
Plate is anode, using neodymium iron boron as cathode, is electroplated using SMD-30 type numerical control Double-pulse Plating Power Sources, electroplating current density
3.5A/dm2, pulse duty factor 0.5, electroplating time 50min, 10 μm of the thickness of gained Ni-Cr composite deposites.
Embodiment 3
A kind of preparation process of corrosion-resistant more coating neodymium iron borons comprising step：
(1) it pre-processes, the thiocarbamide that the dust technology of a concentration of 0.8mol/L of 500ml and the 0.5g/L of 500ml is added prepares acid
Nd-Fe-B permanent magnet is placed in acid solution and cleans 2-3min by washing lotion, is subsequently placed in the absolute ethyl alcohol of 500mL and is cleaned by ultrasonic
1-2min, completion, which is placed in the 20g/L sulfosalicylic acids of 500ml and the 10g/L ammonium acid fluoride mixed liquors of 500ml, lives
Change, soak time 1min, 25 DEG C of activation temperature；
(2) chemical nickel plating weighs the sodium hypophosphite of the six hydration nickel sulfate solution of the 26g/L of 300ml, the 30g/L of 300ml
Solution, the borax soln of 30g/L of 100ml, the sodium citrate solution of 30g/L of 100ml, 100ml 30g/L ammonium fluoride it is molten
Liquid, 100ml 3g/L succinic acid solution prepare chemical plating fluid, pretreated Nd-Fe-B permanent magnet is placed in chemical plating fluid
In, at a temperature of 82 DEG C of chemical platings, chemical nickel plating 35min, gained chemical nickel plating layer thickness is 13 μm；
(3) magnetically controlled DC sputtering plates DyAl alloy firms, and magnetron sputtering is carried out on the neodymium iron boron magnetic body surface of chemical nickel plating
Plated film, sputtering system progress is combined using FJL560CI1 types superhigh vacuum magnetron sputtering with ion beam, and sputtering target material is
Dy35A165 alloys, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity
Argon gas, the magnetron sputtering plating time is 1.5h, and after plated film, Vacuum Heat diffusion penetration, processing are used at a temperature of 800 DEG C
The thickness of 6h, gained DyAl alloy firm layers are 15 μm；
(4), surface pulse plating weighs the boric acid of the six hydration nickel sulfate of 150g, the ammonium chloride of 15g, 15g, is added
1000ml distilled water, is placed in 50 DEG C of thermostat water baths to heat and makes it dissolve, and the lauryl sodium sulfate of 1g is added in above-mentioned molten
In liquid, the nanometer Cr powder of 50g is added in above-mentioned solution in magnetic agitation 30min, increases temperature to 65 DEG C, vibration of ultrasonic wave
30min, which is uniformly mixed, prepares electroplate liquid, and it is 6.8 to adjust bath pH values, and nickel that is spare, being 99% with purity is kept the temperature at 65 DEG C
Plate is anode, using neodymium iron boron as cathode, is electroplated using SMD-30 type numerical control Double-pulse Plating Power Sources, electroplating current density
3.0A/dm2, pulse duty factor 0.4, electroplating time 40min, 8 μm of the thickness of gained Ni-Cr composite deposites.
A kind of corrosive nature test of corrosion-resistant more coating neodymium iron borons of the present invention is surveyed according to GB/T10125-1997 standards
Examination, using the Nd-Fe-B permanent magnet of no coating as control sample, each embodiment performance test results are as shown in table 1.
The performance of table 1, each embodiment product
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its
Equivalent defines.
Claims (9)
1. a kind of corrosion-resistant more coating neodymium iron boron preparation processes, which is characterized in that including step：
S100 pre-processes Nd-Fe-B permanent magnet, and it is clear to carry out pickling to Nd-Fe-B permanent magnet with the mixing pickle of dust technology and thiocarbamide
It is clean, then be cleaned by ultrasonic with absolute ethyl alcohol, completion, which is placed in sulfosalicylic acid and ammonium acid fluoride mixed liquor, to be activated；
S200 chemical nickel platings are molten by six hydration nickel sulfate solution, sodium hypophosphite solution, borax in the outer surface of Nd-Fe-B permanent magnet
Liquid, sodium citrate solution, ammonium fluoride solution, succinic acid solution are configured to chemical plating fluid, by pretreated Nd-Fe-B permanent magnet
It is placed in chemical plating fluid, carries out nickel plating under default chemical plating temperature, default electroless plating time, the nickel coating is made, it is described
Nickel plating layer thick is 10~15 μm；
S300 magnetron sputterings dysprosium aluminum alloy thin film layer is in the nickel coating outer surface, on the neodymium iron boron magnetic body surface of chemical nickel plating
Magnetron sputtering plating is carried out, combines sputtering system progress with ion beam using superhigh vacuum magnetron sputtering, sputtering target material is dysprosium aluminium
Alloy, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power 300W, atmosphere are high-purity argon gas,
It carries out magnetron sputtering plating in preset time, after plated film, Vacuum Heat diffusion penetration is used under preset temperature, is made described
Dysprosium aluminum alloy thin film layer is plated, the thickness of the plating dysprosium aluminum alloy thin film layer is 10~20 μm；And
The surfaces S400 pulse plating nickel chromium triangle composite deposite is in the outer surface of the plating dysprosium aluminum alloy thin film layer, by six hydrated sulfuric acids
Nickel, ammonium chloride, boric acid are added to the water and dissolve by heating, and lauryl sodium sulfate are added in above-mentioned solution, magnetic agitation
Nanometer chromium powder is added in above-mentioned solution in 30min, increases temperature to 65 DEG C, vibration of ultrasonic wave 30min, which is uniformly mixed, prepares plating
Liquid adjusts acid plating liquid basicity and is saved backup in preset temperature, using nickel plate as anode, using neodymium iron boron as cathode, uses number
It controls Double-pulse Plating Power Source and carries out electroplating surface, corrosion-resistant more coating neodymium iron borons are made.
2. preparation process according to claim 1, which is characterized in that the step S100 specifically includes step：It is added
The thiocarbamide of the dust technology of the 0.5-1.0mol/L of 500mL and the 0.5g/L of 500mL prepare pickle, and Nd-Fe-B permanent magnet is placed in
2-3min is cleaned in acid solution, is subsequently placed in the absolute ethyl alcohol of 500mL and carries out 1~2min of ultrasonic cleaning, and completion is placed on 500mL
20g/L sulfosalicylic acids and 500mL 10g/L ammonium acid fluoride mixed liquors in activated, soak time 1min, activation temperature
25℃。
3. preparation process according to claim 2, which is characterized in that the step S200 specifically includes step：By 300mL
The six hydration nickel sulfate solution of 26g/L, the sodium hypophosphite solution of 30g/L of 300mL, 100mL 30g/L borax soln,
The sodium citrate solution of the 30g/L of 100mL, the ammonium fluoride solution of the 30g/L of 100mL, 100mL the succinic acid solution of 3g/L match
Pretreated Nd-Fe-B permanent magnet is placed in chemical plating fluid by chemical plating fluid processed, is 80~85 DEG C in chemical plating temperature, chemistry
Nickel plating is carried out under the conditions of plating 30~40min of time.
4. preparation process according to claim 3, which is characterized in that the step S300 specifically includes step：In chemistry
The neodymium iron boron magnetic body surface of nickel plating carries out magnetron sputtering plating, combines sputtering system with ion beam using superhigh vacuum magnetron sputtering
It carries out, sputtering target material is dysprosium aluminium alloy, working vacuum degree 1.0Pa, DC power supply plated film, sputtering current 0.67A, power
300W, atmosphere are high-purity argon gas, 1~2h of magnetron sputtering plating, and after plated film, Vacuum Heat is used at a temperature of 750~850 DEG C
The plating dysprosium aluminum alloy thin film layer is made in diffusion penetration 6h.
5. preparation process according to claim 4, which is characterized in that the step S400 specifically includes step：It weighs
The boric acid of the six hydration nickel sulfate of 150g, the ammonium chloride of 15g, 15g is added 1000ml distilled water, is placed in 50 DEG C of thermostat water baths
Middle heating makes it dissolve, and adds the lauryl sodium sulfate of 1g in above-mentioned solution, receiving for 50g is added in magnetic agitation 30min
Rice chromium powder increases temperature to 65 DEG C, vibration of ultrasonic wave 30min, which is uniformly mixed, prepares electroplate liquid, adjusts plating in above-mentioned solution
Liquid pH value saves backup at 65 DEG C, and the nickel plate for being 99% using purity is anode, using neodymium iron boron as cathode, uses the double arteries and veins of numerical control
It rushes electroplating power supply to be electroplated, electroplating current density in a certain range, under pulse duty factor, one timing of surface pulse plating
Between, the nickel chromium triangle composite deposite is made, the thickness of the nickel chromium triangle composite deposite is 6~10 μm.
6. preparation process according to claim 5, which is characterized in that the pH value of the pulse plating liquid in the step S400
It is 6.5~7.0.
7. preparation process according to claim 6, which is characterized in that the pulsed electroplating current density in the step S400
For 2.5~3.5A/dm2。
8. preparation process according to claim 7, which is characterized in that pulse accounts for when pulse plating in the step S400
Sky is than being 0.3 or 0.4 or 0.5.
9. preparation process according to claim 8, which is characterized in that pulse plating time 30 in the step S400~
50min。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611157661.0A CN106710767B (en) | 2016-12-09 | 2016-12-09 | The corrosion-resistant more coating neodymium iron borons of one kind and preparation process |
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| WO2019014095A1 (en) * | 2017-07-10 | 2019-01-17 | Xtalic Corporation | Magnets comprising a coating including an aluminum layer |
| CN107419231B (en) * | 2017-07-26 | 2019-11-15 | 沈阳广泰真空科技有限公司 | The preparation method of Nd-Fe-B permanent magnetic anti-corrosion insulation coating and Nd-Fe-B permanent magnet with the coating |
| CN108015293B (en) * | 2017-12-21 | 2021-04-13 | 宁波金轮磁材技术有限公司 | Double-alloy neodymium iron boron rare earth permanent magnet and manufacturing method thereof |
| CN108251810B (en) * | 2018-01-22 | 2020-12-04 | 安徽大地熊新材料股份有限公司 | Preparation method of corrosion-resistant sintered neodymium-iron-boron magnet |
| CN108597840B (en) * | 2018-04-04 | 2020-07-03 | 北京工业大学 | Surface diffusion method and device for nano particles |
| KR102045400B1 (en) * | 2018-04-30 | 2019-11-15 | 성림첨단산업(주) | Manufacturing method of rare earth sintered magnet |
| CN108950503B (en) * | 2018-07-30 | 2020-03-31 | 山西金山磁材有限公司 | Sintered neodymium iron boron coating film and vacuum coating process thereof |
| CN109692963B (en) * | 2018-12-18 | 2022-06-10 | 宁波中杭磁材有限公司 | Preparation method of neodymium iron boron magnet with corrosion-resistant coating attached to surface |
| CN110983333A (en) * | 2019-12-06 | 2020-04-10 | 东莞中探探针有限公司 | Neodymium-iron-boron composite coating and preparation method and application thereof |
| CN110983395A (en) * | 2019-12-17 | 2020-04-10 | 广东小天才科技有限公司 | Magnet, preparation method and wearable device |
| CN111128503B (en) * | 2019-12-19 | 2021-07-23 | 安徽大地熊新材料股份有限公司 | High-strength neodymium iron boron magnet and preparation method thereof |
| CN111243846B (en) * | 2020-01-19 | 2021-12-24 | 北京工业大学 | Method capable of simultaneously improving oxidation corrosion resistance of NdFeB powder and magnet |
| CN113005440A (en) * | 2020-12-30 | 2021-06-22 | 昆明狴犴人力资源服务有限公司 | Neodymium-iron-boron permanent magnet surface coating and preparation method thereof |
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Address after: 315812 No. 83 Nanhu Road, Xiexi Industrial Zone, Daxie Development Zone, Ningbo City, Zhejiang Province Patentee after: Ningbo Yuanchen New Materials Co., Ltd. Address before: 315812 No. 83 Nanhu Road, Xiexi Industrial Zone, Daxie Development Zone, Ningbo City, Zhejiang Province Patentee before: Ningbo Daxie Development Zone Xin silver Magnetic Industry Co Ltd |