CN103117143A - Neodymium iron boron magnet made of neodymium iron boron nickel-plating waste materials in sintered mode - Google Patents
Neodymium iron boron magnet made of neodymium iron boron nickel-plating waste materials in sintered mode Download PDFInfo
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Abstract
The invention discloses a neodymium iron boron magnet made of neodymium iron boron nickel-plating waste materials in a sintered mode. The neodymium iron boron magnet resolves the problems that a neodymium iron boron magnet in the prior art is low in performance, low in utilizing rate of the waste materials and the like. The neodymium iron boron magnet is made of mixed materials through a sintering process, wherein the mixed materials are formed by the neodymium iron boron magnet nickel-plating waste materials and rich rare-earth compound material. For the neodymium iron boron magnet, residual magnetism (Br) of is greater than or equal to 1.2T, intrinsic coercive force (Hcj) is greater than or equal to 13.3 KOe, coercive force (Hcb) is greater than or equal to 11.6 KOe, the magnetic energy product (BH(max)) is greater than or equal to 34.8 MGOe, squareness (HK/Hcj) ranges from 0.97 to 0.98, the weight loss ratio is 0.19-1.10 mg/cm<2>, and the Br temperature coefficient is negative 0.090- negative 0.11% DEG C. The preparation method of the neodymium iron boron magnet comprises roasting the neodymium iron boron nickel-plating waste materials; manufacturing neodymium iron boron nickel-plating waste material powder; preparing the mixed materials; moulding in a compressed mode; and sintering. The preparation method is simple, effective, environment-friendly and low in cost.
Description
Technical field
The present invention relates to a kind of neodymium iron boron magnetic body, be specifically related to a kind of neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering, belong to Rare-Earth Magnetic material technology field.
Technical background
In recent years, along with the rapid expansion of neodymium iron boron magnetic body application, raw-material demand has been become increasing, but higher and along with the increasing of national regulation and control dynamics, its material cost also strengthens gradually because of the cost of rare earth mining.In the situation that the present price amount of increase is excessive, the price endurance of Downstream Market is more limited, portion downstream enterprise has selected to use the materials such as more cheap ferrite or aluminium nickel cobalt, SmCo to replace rare earth in the neodymium iron boron magnetic body raw material, and this brings larger unsteadiness for neodymium iron boron magnetic body market.In addition, Nd-Fe-B magnetic material fragility is high, and specification is assorted, very easily occurs the problems such as unfilled corner and size be bad in electroplating process.And after electroplating, the learies of neodymium iron boron magnetic body is very large, is only that the scrappage of finished product outward appearance and size is just between 2～5%, because the otherwise requirement of client also causes occuring the bad phenomenon of scrapping often.Therefore the cost that reduces Sintered NdFeB magnet is one of problem demanding prompt solution.
In neodymium iron boron nickel plating waste material, 80% for being coated with the plating Ni waste material of Ni or NiCuNi layer, plating Ni waste material can be processed unclean because of coating in utilizing process, cause product surface the problem that pore, oxidation spots etc. affect performance to occur, reduce simultaneously the recovery utilization rate of nickel plating waste material.In prior art, general adopt first carried out strip with acid solution or alkali lye and processed and the nickel plating waste material is recycled again.Yet matrix very easily occurs by the phenomenon of acid solution or alkali liquid corrosion in the strip process, cause the rate of recovery low, in addition, the pollution that meeting brings environment because of problems such as discharge of wastewater in the strip process.Therefore utilize the strip method to recycle neodymium iron boron nickel plating waste material cost higher, waste utilization rate, also easy contaminated environment.
And Chinese patent application (notification number: CN1076853C) disclose a kind of method for preparing Nd-Fe-B series permanent magnet with leftover bits and pieces of material, the method is converted neodymium iron boron magnetic body waste material and neodymium iron boron magnetic body virgin material according to a certain percentage and is mixed after mixing, adopt traditional handicraft and legacy equipment, as intermediate frequency furnace, melting obtains neodymium iron boron magnetic body.Yet in this method, the mass percent of described neodymium iron boron magnetic body waste material in compound is usually below 50%, and the neodymium iron boron waste material utilance is not high, and the poor-performing of resulting neodymium iron boron magnetic body, the application scenario that is difficult to satisfy high request.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of high performance neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material to sinter into is provided.
Purpose of the present invention is achieved through the following technical solutions, a kind of neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering, this neodymium iron boron magnetic body is to be prepared from by sintering process by the compound that neodymium iron boron nickel plating waste material and neodymium iron boron formulation form, and the mass percent of wherein said neodymium iron boron nickel plating waste material and neodymium iron boron formulation is respectively 50%～98% and 2%～50%.Contain mass percent in described neodymium iron boron nickel plating waste material and be 0.01%～0.1% nickel element, when the neodymium iron boron magnetic body probe temperature after making is 20 ℃, performance is as follows: remanent magnetism (Br) 〉=1.2T, HCJ (Hcj) 〉=13.3KOe, coercive force (Hcb) 〉=11.6KOe, magnetic energy product (BHmax) is 〉=34.8MGSOe, squareness (HK/Hcj) is 0.97～0.98, and weight-loss ratio is 0.19～1.10mg/cm
2, the Br temperature coefficient is-0.090～-0.11% ℃.
With respect to prior art, the neodymium iron boron magnetic body in the application mixes with the neodymium iron boron formulation by the suitable neodymium iron boron nickel plating waste material of selection, and can obtain high-performance by sintering process, low weight-loss ratio, the neodymium iron boron magnetic body that temperature stability is good.The main performance of described neodymium iron boron magnetic body all reaches higher level, as common low weightless neodymium iron boron magnetic body at the weight-loss ratio under 132 ℃, 3atm, 168h condition is 〉=5mg/cm
2And in the present invention, the weight-loss ratio of neodymium iron boron magnetic body is≤2mg/cm
2And for example each trade mark maximum operating temperature Br temperature coefficient of former pure material preparation is-0.1～-0.12% ℃, and the temperature coefficient of the neodymium iron boron magnetic body in the present invention is-0.09～-0.11% ℃.And the mass percent of described neodymium iron boron waste material in compound reaches 98%, greatly improved the utilance of neodymium iron boron waste material, greatly reduces the cost of processing the waste material Sintered NdFeB magnet, saves cost and is about 10%～50%.Other elements described in the present invention mean non-rare earth.
In the described neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:28%～30%, B:0.95%～1.05%, Al:0.35%～0.5%, Nb:0.20%～0.25%, Ni:0.05%～0.1%, Cu:0.16%～0.18%, Gd or Dy:2.8%～3.5%, surplus are Fe and inevitable impurity.In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%～28%, B:1.0～1.2%, in Gd, Dy, Co one or both: 4%～40%, Al:0.4%～2.0%, Nb:0.2%～0.3%, Cu:0.18%～0.2%, surplus are Fe and inevitable impurity.
Further, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:28%, and B:0.99%, Gd:3.5%, Al:0.5%, Nb:0.2%, Ni:0.1%, Cu:0.18%, surplus is Fe and inevitable impurity.In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:28%, and B:1%, Gd:4%, Al:0.4%, Nb:0.2%, Cu:0.18%, surplus is Fe and inevitable impurity.When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.249T, HCJ (Hcj) is 13.34KOe, coercive force (Hcb) is 11.82KOe, magnetic energy product (BHmax) is 37.62MGSOe, remanent magnetism when probe temperature is 80 ℃ (Br) is 1.173T, HCJ (Hcj) is 7.17KOe, and coercive force (Hcb) is 7.032KOe, and magnetic energy product (BHmax) is 32.16MGSOe; The squareness of described neodymium iron boron magnetic body (HK/Hcj) is 0.97, and weight-loss ratio is 0.85～1.10mg/cm
2, the Br temperature coefficient is-0.101% ℃.
Further, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:29.1%, and B:0.99%, Dy:2.8%, Al:0.35%, Nb:0.21%, Ni:0.09%, Cu:0.17%, surplus is Fe and inevitable impurity.In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%, and B:1.2%, Dy:40%, Al:2.0%, Nb:0.2%, Cu:0.2%, Co:20%, surplus is Fe and inevitable impurity.When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.203T, HCJ (Hcj) is 21.24KOe, coercive force (Hcb) is 11.76KOe, magnetic energy product (BHmax) is 34.86MGSOe, remanent magnetism when probe temperature is 150 ℃ (Br) is 1.038T, HCJ (Hcj) is 6.131KOe, and coercive force (Hcb) is 5.86KOe, and magnetic energy product (BHmax) is 25.07MGSOe; Described squareness (HK/Hcj) is 0.98, and weight-loss ratio is 0.19～0.25mg/cm
2, the Br temperature coefficient is-0.106% ℃.
Further, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:29.2%, and B:0.99%, Dy:0.8%, Al:0.25%, Nb:0.25%, Ni:0.08%, Cu:0.16%, surplus is Fe and inevitable impurity.In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%, and B:1%, Dy:40%, Al:0.5%, Nb:0.2%, Cu:0.18%, Co:20%, surplus is Fe and inevitable impurity.When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.349T, HCJ (Hcj) is 18.48KOe, coercive force (Hcb) is 12.86KOe, magnetic energy product (BHmax) is 43.06MGSOe, remanent magnetism when probe temperature is 120 ℃ (Br) is 1.203T, HCJ (Hcj) is 7.242KOe, and coercive force (Hcb) is 7.041KOe, and magnetic energy product (BHmax) is 33.22MGSOe; Described squareness (HK/Hcj) is 0.97, and weight-loss ratio is 0.28～0.53mg/cm
2, the Br temperature coefficient is-0.108% ℃.
The present invention also aims to provide a kind of method of using simply, effectively, cheaply the above-mentioned neodymium iron boron magnetic body of neodymium iron boron nickel plating waste material sintering, described method comprises the following steps:
S1, roasting neodymium iron boron nickel plating waste material: neodymium iron boron nickel plating waste material is carried out roasting in sintering furnace, cooling after being filled with nitrogen, come out of the stove.
S2, preparation neodymium iron boron nickel plating waste material powder: the neodymium iron boron nickel plating waste material after roasting is put into the vacuum rapid hardening furnace melting, pour into rejection tablet after waste material melts fully.Rejection tablet is placed in hydrogen crushing furnace, and to carry out hydrogen broken, carries out composition measurement after hydrogen is broken, then rejection tablet is put into the fine grinding of air-flow grinding machine form neodymium iron boron nickel plating waste material powder.
S3, preparation compound: according to rejection tablet composition measurement result, preparation neodymium iron boron formulation mixes described neodymium iron boron nickel plating waste material powder and is stirred to the even compound that forms with the neodymium iron boron formulation powder of being made by the neodymium iron boron formulation.
S4, compressing: described compound is put into the moulding press mould and be pressed into green compact under the protection of nitrogen, green compact are put into the isostatic pressing machine pressurization, pressurize gets blank.
S5, sintering: with described base substrate stripping oil in gloves stripping fuel tank, stripping oil is placed on and carries out high temperature sintering, tempering in vacuum sintering furnace, uses air-cooled the coming out of the stove to normal temperature of nitrogen to make neodymium iron boron magnetic body after tempering.
In described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet, the sintering temperature described in step S1 is 1100～1150 ℃, and roasting time is 1～6 hour, and the low vacuum of baking furnace is in 10
-1Pa, tapping temperature is lower than 80 ℃.Under this sintering temperature, roasting time and vacuum degree, the comprehensive utilization ratio of neodymium iron boron nickel plating waste material will be improved.
As preferably; in described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet; the described smelting temperature of step S2 is 1350～1550 ℃, described air-flow grinding machine oxygen content less than the nitrogen protection of 200ppm under powder process, the powder particle mean size of making is 2～5 μ m.The neodymium iron boron magnetic body that melting neodymium iron boron nickel plating waste material can make sintering form under this smelting temperature obtains performance and higher productive rate preferably.Under this nitrogen protection, neodymium iron boron nickel plating waste material is made the powder that particle mean size is 2～5 μ m; when neodymium iron boron nickel plating waste material powder is mixed with neodymium iron boron formulation powder, contact area increases; more easily mix, thus the comprehensive utilization ratio of raising neodymium iron boron nickel plating waste material.
Further, in described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet, described step S2 concrete steps are put into the vacuum rapid hardening furnace melting after comprising the steps: the neodymium iron boron nickel plating waste material after roasting is mixed, when the air in stove is evacuated to vacuum degree and is 0.4Pa, begin the melting of heating.Material when rubescent, is filled with argon gas in stove, and is warming up to 1450 ℃ and carries out melting, until neodymium iron boron nickel plating waste material melts fully.Refining poured into rejection tablet after 10 minutes, and rejection tablet is carried out the ICP composition measurement, then rejection tablet was placed in hydrogen crushing furnace, led to hydrogen in hydrogen crushing furnace.Carry out hydrogen broken after product is inhaled hydrogen fully, then rejection tablet is put into airflow milling machine fine grinding formation neodymium iron boron nickel plating waste material powder under the nitrogen protection of oxygen content less than 200ppm, the powder particle mean size of making is controlled between 2～5 μ m.
The present invention utilizes the hydrogen absorption characteristic of rare earth intermetallic compound, neodymium iron boron nickel plating waste material alloy is placed under hydrogen environment, hydrogen enters neodymium iron boron nickel plating waste material alloy along rich neodymium phase thin layer, make it expansion explosion and fragmentation, ftracture at a layer place mutually along rich neodymium, thereby make neodymium iron boron nickel plating waste material alloy sheet become neodymium iron boron nickel plating waste material alloy meal.And the meal after stirring with high pressure draught blows afloat, and the collision by each other diminishes dynamics, becomes neodymium iron boron nickel plating waste material alloy fine powder.Broken being combined with airflow milling of hydrogen can be improved milling efficiency 2～3 times, reaches 120～500KG/HR.
As preferably, in described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet, the mixing time described in step S3 is 2～12 hours.
As preferably; in described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet; described step S4 specifically comprises the steps: described compound is put into the moulding press mould under the nitrogen protection of oxygen content less than 5000ppm; the magnetic field that adds 1～10T is orientated, and is pressed into green compact after orientation.Green compact are put into isostatic pressing machine pressurization 100～250Mpa, and pressurize got blank in 1～5 minute, and described green density is 3.5～4.5g/cm
3
In described method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet, described step S5 further comprises the steps: described blank stripping oil in gloves stripping fuel tank, stripping oil is placed in vacuum sintering furnace, be sintering 3～8h under the condition of 1030～1110 ℃ in temperature, the low vacuum of high temperature sintering is in 10
-1Handkerchief.Be to carry out one-level tempering 1～3h under the condition of 850～950 ℃ in temperature, then be cooled to 480～580 ℃ and carry out second annealing 2～4h, adopt the air-cooled neodymium iron boron magnetic body that obtains of nitrogen.
In sum, the present invention has following advantage:
1, the method for the recycling neodymium iron boron nickel plating waste material in the present invention simple, effectively, environmental protection, improved the comprehensive utilization ratio of electroplating waste material, greatly reduce and process the cost of electroplating waste material.
2, the neodymium iron boron magnetic body material combination that forms of sintering of the present invention is reasonable, and the neodymium iron boron magnetic body magnetic property is high, and corrosion resistance is good, and weight-loss ratio is low, and temperature stability is good.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiment.
Embodiment one:
Utilize neodymium iron boron nickel plating waste material to produce the N38 product:
Roasting neodymium iron boron nickel plating waste material: neodymium iron boron nickel plating waste material is placed in sintering furnace, is warming up to 1100 ℃ and carries out roasting.Vacuum degree in sintering furnace is less than 10
-1Pa, roasting time is 4 hours, then is filled with nitrogen, blower fan is cooling, treats that temperature is down to below 80 ℃ to come out of the stove.
Preparation neodymium iron boron nickel plating waste material powder: the neodymium iron boron nickel plating waste material after the 600kg roasting is put into the vacuum rapid hardening furnace melting, when the air in stove is evacuated to vacuum degree and is 0.4Pa, begin the melting of heating.Material when rubescent, is filled with argon gas in stove, and is warming up to 1450 ℃ and carries out melting, until neodymium iron boron nickel plating waste material melts fully.Refining poured into rejection tablet after 10 minutes.Rejection tablet is carried out the ICP composition measurement, and composition measurement the results are shown in Table 1.Again rejection tablet is placed in hydrogen crushing furnace; lead to hydrogen in hydrogen crushing furnace; carry out hydrogen broken after product is inhaled hydrogen fully, the hydrogen flour is put into the fine grinding of airflow milling machine and form neodymium iron boron nickel plating waste material powder under the nitrogen protection of oxygen content lower than 200ppm, the powder particle mean size of making is controlled between 2～5 μ m.
Table 1: neodymium iron boron nickel plating waste material composition measurement result
The preparation compound: according to rejection tablet composition measurement result, preparation neodymium iron boron formulation, the component content of neodymium iron boron formulation sees Table 2.Described neodymium iron boron nickel plating waste material powder is mixed for 50%:50% by mass percentage with the neodymium iron boron formulation powder of being made by the neodymium iron boron formulation and stir 2h to evenly forming compound.
Table 2: the component content of neodymium iron boron formulation
Compressing: described compound is put into the moulding press mould under the nitrogen protection of oxygen content lower than 5000ppm; the magnetic field that adds 1～10T is orientated, and is pressed into green compact after orientation, and green compact are put into isostatic pressing machine pressurization 100Mpa; pressurize got blank in 1 minute, and described green density is 3.5g/cm
3
Sintering: with described blank stripping oil in gloves strippings fuel tank, stripping oil is placed in vacuum sintering furnace, is sintering 4h under the condition of 1075 ℃ in temperature, and the low vacuum of high temperature sintering is in 10
-1Handkerchief.Be to carry out one-level tempering 2h under the condition of 900 ℃ in temperature, then be cooled to 530 ℃ and carry out second annealing 3h, adopt nitrogen air-cooled to obtaining neodymium iron boron magnetic body below 80 ℃.
One, with being cut into D10 * 10mm sample post after the neodymium iron boron magnetic body surface grinding that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment, carry out performance test according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method, the performance test results sees Table 3.
Table 3: neodymium iron boron magnetic body the performance test results
From above-mentioned test result as can be known, the present invention is comparatively desirable with the neodymium iron boron magnetic body performance that neodymium iron boron nickel plating waste material sintering forms, Br temperature coefficient as neodymium iron boron magnetic body of the present invention is-0.097% ℃, and the Br temperature coefficient of the N38 neodymium iron boron magnetic body that the conventional formulation sintering forms is at-0.11% ℃ more than even-0.12% ℃.And the present invention hangs down 15% with the cost of neodymium iron boron nickel plating waste material Sintered NdFeB magnet than preparing Sintered NdFeB magnet with pure material.
Two, the neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment is hanged down weightless test, test condition is 132 ℃, 3atm, 168h, and low weightless test the results are shown in Table 4.
Table 4: neodymium iron boron magnetic body hangs down the weightless test result
From above-mentioned test result as can be known, the present invention is low with the weight-loss ratio of the neodymium iron boron magnetic body that neodymium iron boron nickel plating waste material sintering forms, and is 0.85～1.1mg/cm
2, and the weight-loss ratio of the N38 neodymium iron boron magnetic body that the conventional formulation sintering forms is usually at 10mg/cm
2Above.
Embodiment two:
Produce the 35SH product with neodymium iron boron nickel plating waste material:
Roasting neodymium iron boron nickel plating waste material: neodymium iron boron nickel plating waste material is placed in sintering furnace, is warming up to 1120 ℃ and carries out roasting.Low vacuum in sintering furnace is in 10
-1Pa, roasting time is 4 hours, then is filled with nitrogen, blower fan is cooling, treats that temperature is down to below 80 ℃ to come out of the stove.
Preparation neodymium iron boron nickel plating waste material powder: put into the vacuum rapid hardening furnace melting after will the neodymium iron boron nickel plating waste material after the 600kg roasting mixing, and when the air in stove is evacuated to vacuum degree and is 0.4Pa, begin the melting of heating.Material when rubescent, is filled with argon gas in stove, and is warming up to 1500 ℃ and carries out melting, until neodymium iron boron nickel plating waste material melts fully.Refining poured into rejection tablet after 10 minutes.Rejection tablet is carried out the ICP composition measurement, and the composition measurement result is as shown in table 5.Then rejection tablet is placed in hydrogen crushing furnace; lead to hydrogen in hydrogen crushing furnace; after inhaling hydrogen fully, product carries out hydrogen broken; the hydrogen flour is put into the fine grinding of airflow milling machine again and form neodymium iron boron nickel plating waste material powder under the nitrogen protection of oxygen content less than 200ppm, the powder particle mean size of making is controlled between 2～5 μ m.
Table 5: neodymium iron boron nickel plating waste material composition measurement result
The preparation compound: according to rejection tablet composition measurement result, preparation neodymium iron boron formulation, the component content of neodymium iron boron formulation sees Table 6.Described neodymium iron boron nickel plating waste material powder is mixed for 98%:2% by mass percentage with the neodymium iron boron formulation powder of being made by the neodymium iron boron formulation and stir 12h to evenly forming compound.
Table 6: the component content of neodymium iron boron formulation
Compressing: described compound is put into the moulding press mould under the nitrogen protection of oxygen content lower than 5000ppm; the magnetic field that adds 1～10T is orientated, and is pressed into green compact after orientation, and green compact are put into isostatic pressing machine pressurization 250Mpa; pressurize got blank in 5 minutes, and described green density is 4.5g/cm
3
Sintering: with described blank stripping oil in gloves strippings fuel tank, stripping oil is placed in vacuum sintering furnace, is sintering 4h under the condition of 1060 ℃ in temperature, and the low vacuum of high temperature sintering is in 10
-1Handkerchief.Be to carry out one-level tempering 2h under the condition of 900 ℃ in temperature, then be cooled to 520 ℃ and carry out second annealing 3h, adopt nitrogen air-cooled to obtaining neodymium iron boron magnetic body below 80 ℃.
One, with being cut into D10 * 10mm sample post after the neodymium iron boron magnetic body surface grinding that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment, carry out performance test according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method, the performance test results sees Table 7.
Table 7: neodymium iron boron magnetic body the performance test results
From above-mentioned test result as can be known, the present invention is comparatively desirable with the neodymium iron boron magnetic body performance that neodymium iron boron nickel plating waste material sintering forms, Br temperature coefficient as neodymium iron boron magnetic body of the present invention is-0.106% ℃, and the Br temperature coefficient of the 35SH neodymium iron boron magnetic body that the conventional formulation sintering forms is more than-0.115% ℃, and the present invention with the cost of neodymium iron boron nickel plating waste material Sintered NdFeB magnet than hanging down 35% with pure material preparation Sintered NdFeB magnet.
Two, the neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment is hanged down weightless test, test condition is 132 ℃, 3atm, 168h, and low weightless test the results are shown in Table 8.
Table 8: neodymium iron boron magnetic body hangs down the weightless test result
From above-mentioned test result as can be known, the present invention is low with the weight-loss ratio of the neodymium iron boron magnetic body that neodymium iron boron nickel plating waste material sintering forms, and is 0.85～1.1mg/cm
2, and the weight-loss ratio of the 35SH neodymium iron boron magnetic body that the conventional formulation sintering forms is usually at 10mg/cm
2Above.
Embodiment three:
Produce the 45H product with neodymium iron boron nickel plating waste material:
Roasting neodymium iron boron nickel plating waste material: neodymium iron boron nickel plating waste material is placed in sintering furnace, is warming up to 1130 ℃ and carries out roasting.Low vacuum in sintering furnace is in 10
-1Pa, roasting time is 4 hours, then is filled with nitrogen, blower fan is cooling, treats that temperature is down to below 80 ℃ to come out of the stove.
Preparation neodymium iron boron nickel plating waste material powder: put into the vacuum rapid hardening furnace melting after will the neodymium iron boron nickel plating waste material after the 600kg roasting mixing, and when the air in stove is evacuated to vacuum degree and is 0.4Pa, begin the melting of heating.Material when rubescent, is filled with argon gas in stove, and is warming up to 1500 ℃ and carries out melting, until neodymium iron boron nickel plating waste material melts fully.Refining poured into rejection tablet after 10 minutes.Rejection tablet is carried out the ICP composition measurement, and the composition measurement result is as shown in table 9.Then rejection tablet is placed in hydrogen crushing furnace; lead to hydrogen in hydrogen crushing furnace; after inhaling hydrogen fully, product carries out hydrogen broken; the hydrogen flour is put into the fine grinding of airflow milling machine again and form neodymium iron boron nickel plating waste material powder under the nitrogen protection of oxygen content lower than 200ppm, the powder particle mean size of making is controlled between 2～5 μ m.
Table 9: neodymium iron boron nickel plating waste material composition measurement result
The preparation compound: according to rejection tablet composition measurement result, preparation neodymium iron boron formulation, the component content of neodymium iron boron formulation sees Table 10.Described neodymium iron boron nickel plating waste material powder is mixed for 98%:2% by mass percentage with the neodymium iron boron formulation powder of being made by the neodymium iron boron formulation and stir 12h to evenly forming compound.
Table 10: the component content of neodymium iron boron formulation
Compressing: described compound is put into the moulding press mould under the nitrogen protection of oxygen content lower than 5000ppm; the magnetic field that adds 1～10T is orientated, and is pressed into green compact after orientation, and green compact are put into isostatic pressing machine pressurization 250Mpa; pressurize got blank in 5 minutes, and described green density is 4.5g/cm
3
Sintering: with described blank stripping oil in gloves strippings fuel tank, stripping oil is placed in vacuum sintering furnace, is sintering 4h under the condition of 1060 ℃ in temperature, and the low vacuum of high temperature sintering is in 10
-1Handkerchief.Be to carry out one-level tempering 2h under the condition of 900 ℃ in temperature, then be cooled to 520 ℃ and carry out second annealing 3h, adopt nitrogen air-cooled to obtaining neodymium iron boron magnetic body below 80 ℃.
One, with being cut into D10 * 10mm sample post after the neodymium iron boron magnetic body surface grinding that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment, carry out performance test according to GB/T3217 permanent magnetism (Hard Magnetic) magnetism of material test method, the performance test results sees Table 11.
Table 11: neodymium iron boron magnetic body the performance test results
From above-mentioned test result as can be known, the present invention is comparatively desirable with the neodymium iron boron magnetic body performance that neodymium iron boron nickel plating waste material sintering forms, Br temperature coefficient as neodymium iron boron magnetic body of the present invention is-0.108% ℃, and the Br temperature coefficient of the 45H neodymium iron boron magnetic body that the conventional formulation sintering forms is more than-0.115% ℃, and the present invention with the cost of neodymium iron boron nickel plating waste material Sintered NdFeB magnet than hanging down 30% with pure material preparation Sintered NdFeB magnet.
Two, the neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering in the present embodiment is hanged down weightless test, test condition is 132 ℃, 3atm, 168h, and low weightless test the results are shown in Table 12.
Table 12: neodymium iron boron magnetic body hangs down the weightless test result
From above-mentioned test result as can be known, the weight-loss ratio of the neodymium iron boron magnetic body that forms with neodymium iron boron nickel plating waste material sintering in the present invention is low, is 0.28～0.531mg/cm
2, and the weight-loss ratio of the 45H neodymium iron boron magnetic body that the conventional formulation sintering forms is usually at 5mg/cm
2Above.
In sum, the magnetic property of the neodymium iron boron magnetic body from embodiment one, two, three, high-temperature behavior and low weightless test result, the present invention has higher magnetic property, lower weight-loss ratio, temperature stability preferably with the neodymium iron boron magnetic body that neodymium iron boron nickel plating waste material sintering forms.And described neodymium iron boron magnetic body can use to surpass 50% neodymium iron boron nickel plating waste material over mass percent in sintering process, has reduced the preparation cost of neodymium iron boron magnetic body, method is simple, effectively, environmental protection, cost be low.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (8)
1. neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material sintering to form, it is characterized in that, described neodymium iron boron magnetic body is to be prepared from by sintering process by the compound that neodymium iron boron nickel plating waste material and neodymium iron boron formulation form, and the mass percent of wherein said neodymium iron boron nickel plating waste material and neodymium iron boron formulation is respectively 50%～98% and 2%～50%; Contain mass percent in described neodymium iron boron nickel plating waste material and be 0.01%～0.1% nickel element, when the neodymium iron boron magnetic body probe temperature after making is 20 ℃, performance is as follows: remanent magnetism (Br) 〉=1.2T, HCJ (Hcj) 〉=13.3KOe, coercive force (Hcb) 〉=11.6KOe, magnetic energy product (BHmax) is 〉=34.8MGSOe, squareness (HK/Hcj) is 0.97～0.98, and weight-loss ratio is 0.19～1.10mg/cm
2, the Br temperature coefficient is-0.090～-0.11% ℃.
2. the neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material sintering to form according to claim 1, it is characterized in that, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:28%～30%, B:0.95%～1.05%, Al:0.35%～0.5%, Nb:0.20%～0.25%, Ni:0.05%～0.1%, Cu:0.16%～0.18%, Gd or Dy:2.8%～3.5%, surplus is Fe and inevitable impurity; In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%～28%, B:1.0～1.2%, in Gd, Dy, Co one or both: 4%～40%, Al:0.4%～2.0%, Nb:0.2%～0.3%, Cu:0.18%～0.2%, surplus are Fe and inevitable impurity.
3. the neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material sintering to form according to claim 1 and 2, it is characterized in that, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:28%, B:0.99%, Gd:3.5%, Al:0.5%, Nb:0.2%, Ni:0.1%, Cu:0.18%, surplus is Fe and inevitable impurity; In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:28%, and B:1%, Gd:4%, Al:0.4%, Nb:0.2%, Cu:0.18%, surplus is Fe and inevitable impurity; When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.249T, HCJ (Hcj) is 13.34KOe, coercive force (Hcb) is 11.82KOe, magnetic energy product (BHmax) is 37.62MGSOe, remanent magnetism when probe temperature is 80 ℃ (Br) is 1.173T, HCJ (Hcj) is 7.17KOe, and coercive force (Hcb) is 7.032KOe, and magnetic energy product (BHmax) is 32.16MGSOe; The squareness of described neodymium iron boron magnetic body (HK/Hcj) is 0.97, and weight-loss ratio is 0.85～1.10mg/cm
2, the Br temperature coefficient is-0.101% ℃.
4. the neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material sintering to form according to claim 1 and 2, it is characterized in that, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:29.1%, B:0.99%, Dy:2.8%, Al:0.35%, Nb:0.21%, Ni:0.09%, Cu:0.17%, surplus is Fe and inevitable impurity; In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%, and B:1.2%, Dy:40%, Al:2.0%, Nb:0.2%, Cu:0.2%, Co:20%, surplus is Fe and inevitable impurity; When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.203T, HCJ (Hcj) is 21.24KOe, coercive force (Hcb) is 11.76KOe, magnetic energy product (BHmax) is 34.86MGSOe, remanent magnetism when probe temperature is 150 ℃ (Br) is 1.038T, HCJ (Hcj) is 6.131KOe, and coercive force (Hcb) is 5.86KOe, and magnetic energy product (BHmax) is 25.07MGSOe; Described squareness (HK/Hcj) is 0.98, and weight-loss ratio is 0.19～0.25mg/cm
2, the Br temperature coefficient is-0.106% ℃.
5. the neodymium iron boron magnetic body that utilizes neodymium iron boron nickel plating waste material sintering to form according to claim 1 and 2, it is characterized in that, in described neodymium iron boron nickel plating waste material, each composition and mass percent thereof are: PrNd:29.2%, B:0.99%, Dy:0.8%, Al:0.25%, Nb:0.25%, Ni:0.08%, Cu:0.16%, surplus is Fe and inevitable impurity; In described neodymium iron boron formulation, each composition and mass percent thereof are: PrNd:25%, and B:1%, Dy:40%, Al:0.5%, Nb:0.2%, Cu:0.18%, Co:20%, surplus is Fe and inevitable impurity; When described neodymium iron boron magnetic body probe temperature is 20 ℃, remanent magnetism (Br) is 1.349T, HCJ (Hcj) is 18.48KOe, coercive force (Hcb) is 12.86KOe, magnetic energy product (BHmax) is 43.06MGSOe, remanent magnetism when probe temperature is 120 ℃ (Br) is 1.203T, HCJ (Hcj) is 7.242KOe, and coercive force (Hcb) is 7.041KOe, and magnetic energy product (BHmax) is 33.22MGSOe; Described squareness (HK/Hcj) is 0.97, and weight-loss ratio is 0.28～0.53mg/cm
2, the Br temperature coefficient is-0.108% ℃.
6. one kind prepares the method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet as claimed in claim 1 or 2, it is characterized in that, said method comprising the steps of:
S1, roasting neodymium iron boron nickel plating waste material: neodymium iron boron nickel plating waste material is carried out roasting in sintering furnace, cooling after being filled with nitrogen, come out of the stove;
S2, preparation neodymium iron boron nickel plating waste material powder: the neodymium iron boron nickel plating waste material after roasting is put into the vacuum rapid hardening furnace melting, after melting fully, waste material pours into rejection tablet, rejection tablet is placed in hydrogen crushing furnace, and to carry out hydrogen broken, carry out composition measurement after hydrogen is broken, then rejection tablet is put into air-flow grinding machine fine grinding formation neodymium iron boron nickel plating waste material powder;
S3, preparation compound: according to rejection tablet composition measurement result, preparation neodymium iron boron formulation mixes described neodymium iron boron nickel plating waste material powder and is stirred to the even compound that forms with the neodymium iron boron formulation powder of being made by the neodymium iron boron formulation;
S4, compressing: described compound is put into the moulding press mould and be pressed into green compact under the protection of nitrogen, green compact are put into the isostatic pressing machine pressurization, pressurize gets blank;
S5, sintering: with described base substrate stripping oil in gloves stripping fuel tank, stripping oil is placed on and carries out high temperature sintering in vacuum sintering furnace, and tempering uses air-cooled the coming out of the stove to normal temperature of nitrogen to make neodymium iron boron magnetic body after tempering.
7. the method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet according to claim 6, is characterized in that, the sintering temperature described in step S1 is 1100～1150 ℃, and roasting time is 1～6 hour, and the vacuum degree of baking furnace is less than 10
-1Pa, tapping temperature is less than 80 ℃.
8. the method with neodymium iron boron nickel plating waste material Sintered NdFeB magnet according to claim 6, it is characterized in that, described step S5 further comprises the steps: described blank stripping oil in gloves stripping fuel tank, stripping oil is placed in vacuum sintering furnace, be sintering 3～8h under the condition of 1030～1110 ℃ in temperature, the vacuum degree of high temperature sintering is less than 10
-1Handkerchief is to carry out one-level tempering 1～3h under the condition of 850～950 ℃ in temperature, then is cooled to 480～580 ℃ and carries out second annealing 2～4h, adopts the air-cooled neodymium iron boron magnetic body that obtains of nitrogen.
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