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CN103839641B - The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method - Google Patents

The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device and manufacture method Download PDF

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CN103839641B
CN103839641B CN201410107545.2A CN201410107545A CN103839641B CN 103839641 B CN103839641 B CN 103839641B CN 201410107545 A CN201410107545 A CN 201410107545A CN 103839641 B CN103839641 B CN 103839641B
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陈晓东
孙宝玉
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SHENYANG ZHONGBEI VACUUM DEVICE Co Ltd
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Abstract

本发明公开了一种钕铁硼稀土永磁器件的混合镀膜设备及制造方法,镀膜设备设有真空室、圆柱旋转阴极磁控靶、平面阴极磁控靶、多弧离子靶、转架和料筐。工作时转架在真空室内公转,网状料筐两端有转轴安装在转架上即随着转架公转又自转。圆柱旋转磁控靶安装在真空室内转架内部,平面磁控靶、多弧离子靶、阳极层线性离子源和加热装置安装在真空室内转架的周围,真空镀膜共分3层,第一层为磁控溅射镀层,镀层厚度为:0.1‑5μm,第二层为磁控溅射和多弧的混合镀层,镀层厚度为:1‑15μm,第三层为磁控溅射镀层,镀层厚度为:0.1‑5μm。采用混合镀膜作稀土永磁器件的表面处理工序,不仅提高了稀土永磁器件的抗腐蚀能力,同时也提高了稀土永磁器件的磁性能。

The invention discloses a mixed coating equipment and a manufacturing method of a NdFeB rare earth permanent magnet device. The coating equipment is equipped with a vacuum chamber, a cylindrical rotating cathode magnetron target, a planar cathode magnetron target, a multi-arc ion target, a turntable and a material. basket. When working, the turntable revolves in the vacuum chamber, and the rotating shafts at both ends of the mesh basket are installed on the turntable, that is, it revolves and rotates with the turntable. The cylindrical rotating magnetron target is installed inside the turntable in the vacuum chamber. The planar magnetron target, multi-arc ion target, anode layer linear ion source and heating device are installed around the turntable in the vacuum chamber. The vacuum coating is divided into three layers. The first layer It is a magnetron sputtering coating, the coating thickness is: 0.1-5μm, the second layer is a mixed coating of magnetron sputtering and multi-arc, the coating thickness is: 1-15μm, the third layer is a magnetron sputtering coating, the coating thickness For: 0.1-5μm. Using the mixed coating as the surface treatment process of the rare earth permanent magnet device not only improves the corrosion resistance of the rare earth permanent magnet device, but also improves the magnetic performance of the rare earth permanent magnet device.

Description

一种钕铁硼稀土永磁器件的混合镀膜设备及制造方法Hybrid coating equipment and manufacturing method for NdFeB rare earth permanent magnet device

技术领域technical field

本发明属于永磁器件领域,特别是涉及一种钕铁硼稀土永磁器件的混合镀膜设备及制造方法。The invention belongs to the field of permanent magnet devices, and in particular relates to a mixed coating equipment and a manufacturing method for NdFeB rare earth permanent magnet devices.

背景技术Background technique

钕铁硼稀土永磁材料,以其优良的磁性能得到越来越多的应用,被广泛用于医疗的核磁共振成像,计算机硬盘驱动器,音响、手机等;随着节能和低碳经济的要求,钕铁硼稀土永磁材料又开始在汽车零部件、家用电器、节能和控制电机、混合动力汽车,风力发电等领域应用。NdFeB rare earth permanent magnet materials, with their excellent magnetic properties, have been used more and more, and are widely used in medical nuclear magnetic resonance imaging, computer hard drives, audio, mobile phones, etc.; with the requirements of energy saving and low-carbon economy , NdFeB rare earth permanent magnet materials have begun to be used in auto parts, household appliances, energy saving and control motors, hybrid vehicles, wind power generation and other fields.

现有技术的稀土永磁器件的表面处理工艺主要有电镀Ni-Cu-Ni、电镀Zn、电泳、喷涂等技术,也有采用真空镀铝的方法,如中国专利ZL96192129.3,揭示了真空镀Ti和AlN的方法;另一个中国专利ZL01111757.5揭示了采用真空蒸发镀锌、铝、锡、镁的方法。The surface treatment process of rare earth permanent magnet devices in the prior art mainly includes electroplating Ni-Cu-Ni, electroplating Zn, electrophoresis, spraying and other technologies, and there is also a method of vacuum aluminum plating, such as Chinese patent ZL96192129.3, which discloses vacuum Ti plating and AlN methods; another Chinese patent ZL01111757.5 discloses the method of vacuum evaporation zinc, aluminum, tin, magnesium.

现有技术如图1所示,在真空处理腔1内部的上区有两个支撑件7并排设置,可以绕一个水平旋转轴线上的转轴6转动。由不锈钢丝网形成的六个圆筒5装入磁件14,由转轴8在支撑件7的转轴6的外侧圆周方向中并支撑为一个环形,用于绕转轴6旋转。作为用于蒸发的材料铝丝9的蒸发段的多个加热舟2设置在一个在处理腔1下区中的支撑平台3上升起的加热舟支撑基座4上。铝丝9固定和缠绕在支撑平台3之下的一个供给辊子10上。铝丝9的前端由面向加热舟2的一个内表面的热阻保护管11导向达到加热舟2上,一个凹口12 设置在保护管11的一部分中,而进给齿轮13对应于凹口12安装,并直接与铝丝9接触,这样通过进给铝丝9可以恒定地将铝丝供入加热舟2中,加热蒸发沉积到转动的料筒5中的磁件14上完成其表面镀铝。In the prior art, as shown in FIG. 1 , there are two support members 7 arranged side by side in the upper area inside the vacuum processing chamber 1 , which can rotate around a rotating shaft 6 on a horizontal rotation axis. The six cylinders 5 formed by stainless steel wire mesh are loaded into the magnets 14 and supported by the rotating shaft 8 in the outer circumferential direction of the rotating shaft 6 of the supporting member 7 as a ring for rotating around the rotating shaft 6 . A plurality of heating boats 2 serving as evaporation sections of the material aluminum wire 9 for evaporation are arranged on a heating boat support base 4 raised on a support platform 3 in the lower region of the processing chamber 1 . Aluminum wire 9 is fixed and wound on a feed roller 10 under the support platform 3 . The front end of the aluminum wire 9 is guided to the heating boat 2 by a thermal resistance protection tube 11 facing an inner surface of the heating boat 2, a notch 12 is provided in a part of the protection tube 11, and the feed gear 13 corresponds to the notch 12 Installed and directly in contact with the aluminum wire 9, so that the aluminum wire can be constantly fed into the heating boat 2 by feeding the aluminum wire 9, and heated and evaporated to deposit on the magnetic piece 14 in the rotating barrel 5 to complete its surface aluminum plating .

现有技术采用蒸发镀膜,膜层与基体的结合力差,提高稀土永磁器件的抗腐蚀能力存在不足;也有的现有技术采用了磁控溅射镀膜,由于磁控溅射的效率低,不适合低成本大批量生产,也有的没有解决装卡技术,不易装卡,生产麻烦;也有的现有技术采用多弧离子镀膜,由于多弧离子镀膜时存在大颗粒,不能达到稀土永磁器件的耐腐蚀性要求;为了解决多弧离子镀的缺点,现有技术也有人想到了采用多弧离子镀与磁控溅射镀混合镀膜,但都没有解决高效率、低成本、大批量生产技术,设备结构存在不足;特别是现有技术的稀土永磁器件的电镀化学处理工艺,能耗高有污染,要求昂贵的水处理设备,处理不当对生态环境有严重影响,因本发明的生产工艺过程在真空中进行,不使用对环境污染物质,不会给生态环境造成污染,同时还消除在电镀工艺过程中的“电池”作用对磁性能的降低的影响。为此,本发明提供一种新型稀土永磁器件的真空混合镀膜设备弥补了现有技术的不足;另外采用本发明的设备生产的钕铁硼稀土永磁器件不仅提高了稀土永磁器件的抗腐蚀能力,还提高了稀土永磁器件的磁性能,明显提高稀土永磁器件的磁能积和矫顽力,节约稀缺的稀土资源,尤其是节约了更稀缺的重稀土用量。The existing technology uses evaporation coating, the bonding force between the film layer and the substrate is poor, and there are deficiencies in improving the corrosion resistance of rare earth permanent magnet devices; there are also existing technologies that use magnetron sputtering coating, due to the low efficiency of magnetron sputtering, It is not suitable for low-cost mass production, and some have not solved the card installation technology, which is not easy to install, and the production is troublesome; some existing technologies use multi-arc ion coating, because there are large particles in the multi-arc ion coating, it cannot reach rare earth permanent magnet devices Corrosion resistance requirements; In order to solve the shortcomings of multi-arc ion plating, some people in the prior art thought of using multi-arc ion plating and magnetron sputtering mixed coating, but none of them solved the problem of high efficiency, low cost, mass production technology , there are deficiencies in the equipment structure; especially the electroplating chemical treatment process of the rare earth permanent magnet device in the prior art, the energy consumption is high and there is pollution, requiring expensive water treatment equipment, improper treatment has a serious impact on the ecological environment, because the production process of the present invention The process is carried out in a vacuum, without the use of environmental pollutants, and will not cause pollution to the ecological environment. At the same time, it also eliminates the influence of the "battery" effect on the reduction of magnetic properties during the electroplating process. For this reason, the present invention provides a kind of vacuum hybrid coating equipment of novel rare earth permanent magnet device to make up for the deficiencies in the prior art; In addition, the NdFeB rare earth permanent magnet device produced by the equipment of the present invention not only improves the resistance of the rare earth permanent magnet device The corrosion ability also improves the magnetic properties of rare earth permanent magnet devices, significantly improves the magnetic energy product and coercive force of rare earth permanent magnet devices, saves scarce rare earth resources, especially saves the amount of more scarce heavy rare earths.

发明内容Contents of the invention

本发明是提供一种钕铁硼稀土永磁器件混合镀膜设备及制造方法,通过以下技术方案实现提高稀土永磁器件的磁性能和提高的抗腐蚀能力:The present invention provides a mixed coating equipment and manufacturing method for NdFeB rare earth permanent magnet devices, and improves the magnetic properties and corrosion resistance of rare earth permanent magnet devices through the following technical solutions:

一种钕铁硼稀土永磁器件混合镀膜设备,所述的混合镀膜设备包括真空镀膜室、圆柱阴极磁控靶、平面阴极磁控靶、阴极多弧离子靶、转架和料筐;所述的真空镀膜室由卧式真空壳体、前门和后盖组成,前门和真空壳体通过橡胶密封圈密封,后盖或者焊接在真空壳体上或者通过连接件连接,大转架设计在真空镀膜室内,通过转轴支撑在框架上,框架安装在真空壳体上;大转架的轴线与真空壳体的轴线平行,大转架上安装有3个小转架,小转架的轴线与大转架的轴线平行,多个网状料筐两端有转轴安装在小转架上,转轴的轴线与小转架的轴线平行,大转架围绕真空壳体的轴线公转,小转架即围绕大转架的轴线公转又自转,网状料筐即随大转架一起公转也随着小转架公转又自转;所述的圆柱阴极磁控靶安装在真空镀膜室内的后盖上,圆柱阴极磁控靶位于转架的内部,轴线与转架轴线平行,所述的圆柱阴极磁控靶设置一个以上; 所述的平面阴极磁控靶安装在真空壳体上,分布在转架的外围。A hybrid coating equipment for NdFeB rare earth permanent magnet devices, the hybrid coating equipment includes a vacuum coating chamber, a cylindrical cathode magnetron target, a planar cathode magnetron target, a cathode multi-arc ion target, a turntable and a material basket; The vacuum coating chamber is composed of a horizontal vacuum shell, a front door and a back cover. The front door and the vacuum shell are sealed by a rubber sealing ring. The back cover is either welded on the vacuum shell or connected by a connecting piece. In the room, it is supported on the frame by the rotating shaft, and the frame is installed on the vacuum shell; the axis of the large turntable is parallel to the axis of the vacuum shell, and three small turntables are installed on the large turntable, and the axis of the small turntable is parallel to the axis of the large turntable. The axes of the frame are parallel, and the rotating shafts at both ends of the multiple mesh baskets are installed on the small rotating frame. The axis of the rotating shaft is parallel to the axis of the small rotating frame. The large rotating frame revolves around the axis of the vacuum shell. The axis of the turret revolves and rotates, and the mesh basket revolves with the large turret and also revolves and rotates with the small turret; the cylindrical cathode magnetron target is installed on the back cover of the vacuum coating chamber, and the cylindrical cathode magnetron The control target is located inside the turret, and the axis is parallel to the axis of the turret. There is more than one cylindrical cathode magnetron target; the planar cathode magnetron target is installed on the vacuum shell and distributed on the periphery of the turret.

圆柱阴极磁控靶安装在真空镀膜室内的后盖上,电源、冷却水和传动装置由外部引入,圆柱阴极磁控靶位于大转架的内部,轴线与转架轴线平行。The cylindrical cathode magnetron target is installed on the back cover of the vacuum coating chamber, and the power supply, cooling water and transmission device are introduced from the outside. The cylindrical cathode magnetron target is located inside the large turret, and the axis is parallel to the axis of the turret.

所述的圆柱阴极磁控靶设置为一个。There is one cylindrical cathode magnetron target.

所述的圆柱阴极磁控靶内装有多个轴向充磁的磁环,磁环间有导磁环,磁环相对于圆柱阴极磁控靶轴向往复移动。The cylindrical cathode magnetron target is equipped with a plurality of axially magnetized magnetic rings, and there are magnetic conduction rings between the magnetic rings, and the magnetic rings move back and forth axially relative to the cylindrical cathode magnetron target.

所述的圆柱阴极磁控靶内或者装有多条径向充磁的磁条,磁条在圆柱阴极磁控靶内沿着圆周分布,磁条间有间隔,磁条的数量为3条或者3条以上,磁条相对于圆柱阴极磁控靶同轴转动。The cylindrical cathode magnetron target may be equipped with a plurality of radially magnetized magnetic strips, the magnetic strips are distributed along the circumference in the cylindrical cathode magnetron target, there are intervals between the magnetic strips, and the number of magnetic strips is 3 or More than 3, the magnetic strips rotate coaxially with respect to the cylindrical cathode magnetron target.

所述的磁环或者磁条由钕铁硼稀土永磁制造。The magnetic ring or magnetic strip is made of NdFeB rare earth permanent magnets.

平面阴极磁控靶安装在真空壳体上,分布在大转架的外围,所述的平面阴极磁控靶内设置有跑道形状的环状磁条,磁条由钕铁硼稀土永磁制造,用冷却水冷却,数量为一个或一个以上。The planar cathode magnetron target is installed on the vacuum shell and distributed on the periphery of the large turntable. The planar cathode magnetron target is provided with a racetrack-shaped annular magnetic strip, which is made of NdFeB rare earth permanent magnet. Cool with cooling water, the number is one or more.

阴极多弧离子靶安装在真空壳体上,分布在大转架的外围,所述的阴极多弧离子靶为矩形或圆形,内部设置有磁铁,磁铁由钕铁硼稀土永磁制造,用冷却水冷却,数量为一个以上。The cathode multi-arc ion target is installed on the vacuum shell and distributed on the periphery of the large turntable. The cathode multi-arc ion target is rectangular or circular, and a magnet is arranged inside. The magnet is made of NdFeB rare earth permanent magnet. Cooling water cooling, the number is more than one.

阳极层线性离子源安装在真空壳体上,分布在转架的外围。The anode layer linear ion source is installed on the vacuum shell and distributed on the periphery of the turntable.

所述的真空镀膜室内设置有加热器,加热温度范围在100-600℃。The vacuum coating chamber is provided with a heater, and the heating temperature range is 100-600°C.

所述的镀膜靶材为Al、Dy-Al、Tb-Al、Dy-Fe、Tb-Fe、Ni-Cr、Ti、Mo、Si、Al2O3、ZrO2、AZO中的一种以上。The coating target material is more than one of Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Ni-Cr, Ti, Mo, Si, Al 2 O 3 , ZrO 2 , and AZO.

所述的钕铁硼稀土永磁器件镀膜膜系为Al、Dy-Al、Tb-Al、Dy-Fe、Tb-Fe中的一种以上。The coating film of the NdFeB rare earth permanent magnet device is more than one of Al, Dy-Al, Tb-Al, Dy-Fe and Tb-Fe.

所述的钕铁硼稀土永磁器件镀膜膜系为Al、Ni-Cr、Ti、Mo、Si、Al2O3、ZrO2、AZO中的一种以上。The coating film of the NdFeB rare earth permanent magnet device is more than one of Al, Ni-Cr, Ti, Mo, Si, Al 2 O 3 , ZrO 2 and AZO.

所述的钕铁硼稀土永磁器件镀膜膜系为Al。The coating film system of the NdFeB rare earth permanent magnet device is Al.

所述的充气系统或者充入一种气体或者充入一种以上的气体。The inflation system is either filled with one type of gas or filled with more than one type of gas.

所述的充气系统充入的气体为氩气、氮气、氧气、氢气中的一种以上。The gas charged into the inflation system is more than one of argon, nitrogen, oxygen and hydrogen.

所述的充气系统充入的气体为氩气。The gas charged into the inflation system is argon.

所述的真空泵中为机械真空泵、罗茨真空泵、油扩散真空泵、分子泵中的一种以上。The vacuum pump is more than one of mechanical vacuum pump, Roots vacuum pump, oil diffusion vacuum pump and molecular pump.

所述的磁控溅射镀膜条件为,温度30~600℃,沉积压强为氩气条件下0.1~1Pa,功率密度为1~20w/cm2;线性离子源的放电电压100~3000V,离子能量100~2000eV,氩气条件下工作气压0.01~1Pa。所述的镀膜工序中采用磁控溅射镀膜和多弧离子镀膜,磁控溅射镀膜和多弧离子镀膜单独、交替或同时进行工作。The magnetron sputtering coating conditions are: temperature 30-600°C, deposition pressure 0.1-1Pa under argon gas, power density 1-20w/cm 2 ; linear ion source discharge voltage 100-3000V, ion energy 100~2000eV, the working pressure is 0.01~1Pa under the condition of argon. In the coating process, magnetron sputtering coating and multi-arc ion coating are adopted, and magnetron sputtering coating and multi-arc ion coating work independently, alternately or simultaneously.

一种钕铁硼稀土永磁器件的制造方法,首先进行合金熔炼,在熔融状态下将合金浇铸到带水冷却的旋转铜辊上冷却形成合金片,接着对合金片进行氢破碎、混料和气流磨,气流磨后在氮气保护下用混料机混料后送到氮气保护磁场取向压机成型,成形后在保护箱内封装后进行等静压,之后送入烧结设备烧结和时效制成钕铁硼稀土永磁磁体,之后进行机械加工制成钕铁硼稀土永磁器件,之后对钕铁硼稀土永磁器件进行镀膜,镀膜共分3层,第一层为磁控溅射镀层,镀层厚度为:0.02-5μm,第二层为磁控溅射和多弧离子镀的混合镀层,镀层厚度为:1-10μm,第三层为磁控溅射镀层,镀层厚度为: 0.1-5μm。A method for manufacturing NdFeB rare earth permanent magnet devices. First, the alloy is smelted, and the alloy is cast in a molten state on a rotating copper roller with water cooling to cool to form an alloy sheet, and then the alloy sheet is subjected to hydrogen crushing, material mixing and Jet mill, after the jet mill, mix the materials with a mixer under the protection of nitrogen, and then send them to a nitrogen-protected magnetic field orientation press for molding. After forming, they are packaged in a protective box and then subjected to isostatic pressing, and then sent to sintering equipment for sintering and aging. NdFeB rare earth permanent magnets are then machined to make NdFeB rare earth permanent magnet devices, and then the NdFeB rare earth permanent magnet devices are coated. The coating is divided into 3 layers. The first layer is magnetron sputtering coating, Coating thickness: 0.02-5μm, the second layer is a mixed coating of magnetron sputtering and multi-arc ion plating, the coating thickness is: 1-10μm, the third layer is magnetron sputtering coating, the coating thickness is: 0.1-5μm .

所述的混合镀膜工序,镀膜共分3层,第一层为磁控溅射镀层,镀层为Al、Dy-Al、Tb-Al、Dy-Fe、Tb-Fe中的一种,第二层为磁控溅射和多弧离子镀的混合镀层,镀层为Al、Ni-Cr、Ti、Mo、Si、Al2O3、ZrO2、AZO中的一种以上,第三层为磁控溅射镀层,镀层为Al、Ni-Cr、Ti、Mo、Si、Al2O3、ZrO2、AZO中的一种以上。In the mixed coating process, the coating is divided into 3 layers, the first layer is a magnetron sputtering coating, and the coating is one of Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, and the second layer It is a mixed coating of magnetron sputtering and multi-arc ion plating, and the coating is more than one of Al, Ni-Cr, Ti, Mo, Si, Al 2 O 3 , ZrO 2 , AZO, and the third layer is magnetron sputtering Spray coating, the coating is more than one of Al, Ni-Cr, Ti, Mo, Si, Al 2 O 3 , ZrO 2 and AZO.

所述的混合镀膜工序,镀膜共分3层,第一层为磁控溅射镀层,镀层为Dy-Al、Tb-Al、Dy-Fe、Tb-Fe中的一种,第二层为磁控溅射和多弧离子镀的混合镀层,镀层为Al、Ni-Cr、Al2O3、ZrO2、AZO中的一种以上,第三层为磁控溅射镀层,镀层为Al、Ni-Cr、Al2O3、ZrO2、AZO中的一种以上。In the mixed coating process, the coating is divided into 3 layers, the first layer is a magnetron sputtering coating, the coating is one of Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, and the second layer is a magnetron sputtering coating. The hybrid coating of controlled sputtering and multi-arc ion plating, the coating is more than one of Al, Ni-Cr, Al 2 O 3 , ZrO 2 , AZO, the third layer is magnetron sputtering coating, and the coating is Al, Ni - one or more of Cr, Al 2 O 3 , ZrO 2 , and AZO.

所述的混合镀膜工序,镀膜共分3层,第一层为磁控溅射镀层,镀层为Al、Ni-Cr中的一种以上,第二层为磁控溅射和多弧离子镀的混合镀层,镀层为Al、Ni-Cr中的一种以上,第三层为磁控溅射镀层,镀层为Al、Ni-Cr中的一种以上。In the mixed coating process, the coating is divided into 3 layers. The first layer is magnetron sputtering coating, and the coating is more than one of Al and Ni-Cr. The second layer is magnetron sputtering and multi-arc ion plating. Mixed coating, the coating is more than one of Al and Ni-Cr, and the third layer is magnetron sputtering coating, and the coating is more than one of Al and Ni-Cr.

镀膜工序前稀土永磁器件要进行喷砂工序,喷砂采用的材料是石英、玻璃微珠、氧化铝、氧化铈、氧化镧、氧化铈和氧化镧的混合物、氧化锆的一种以上。Before the coating process, the rare earth permanent magnet device needs to undergo a sandblasting process. The materials used for sandblasting are more than one of quartz, glass beads, aluminum oxide, cerium oxide, lanthanum oxide, a mixture of cerium oxide and lanthanum oxide, and zirconia.

镀膜工序前或者有喷涂工序,喷涂材料为铝或含铝的化合物、电泳漆中的一种。Before the coating process or there is a spraying process, the spraying material is one of aluminum or aluminum-containing compounds and electrophoretic paint.

镀膜工序中或者有控制镀膜过程的器件加热工序,温度范围在100-600℃。In the coating process or there is a device heating process to control the coating process, the temperature range is 100-600 ° C.

镀膜工序后或者有热处理工序。After the coating process or there is a heat treatment process.

所述的热处理工序的热处理温度在110-890℃。The heat treatment temperature in the heat treatment process is 110-890°C.

所述的热处理工序的热处理在真空或保护气氛下进行。The heat treatment in the heat treatment process is carried out under vacuum or protective atmosphere.

钕铁硼稀土永磁器件混合镀膜设备或者安装在洁净厂房中,厂房的洁净度在10,000级以上。The hybrid coating equipment for NdFeB rare earth permanent magnet devices may be installed in clean workshops with a cleanliness level above 10,000.

金相分析显示,所述的一种钕铁硼稀土永磁器件从器件表面向内延伸1mm范围内,主相晶粒中重稀土的含量高于器件主相晶粒重稀土的含量,含量高的重稀土分布在主相R2T14B的外围,形成RH2T14B包围R2T14B的新主相结构,RH2T14B相与R2T14B相间无晶界相;其中,R代表在钕铁硼稀土永磁体金相结构中主相中的稀土,T代表元素Fe和Co,RH表示主相中重稀土的含量高于平均值的稀土。Metallographic analysis shows that the NdFeB rare earth permanent magnet device extends within 1 mm from the surface of the device, and the content of heavy rare earths in the main phase grains is higher than that of the main phase grains of the device, and the content is high. The heavy rare earths are distributed in the periphery of the main phase R 2 T 14 B, forming a new main phase structure in which RH 2 T 14 B surrounds R 2 T 14 B, and there is no grain boundary phase between the RH 2 T 14 B phase and the R 2 T 14 B phase ; Wherein, R represents the rare earth in the main phase in the metallographic structure of the NdFeB rare earth permanent magnet, T represents the elements Fe and Co, and RH represents the rare earth whose content of heavy rare earth in the main phase is higher than the average value.

本发明的有益效果:找到了一种钕铁硼稀土永磁器件大批量生产的真空镀膜设备及制造方法,明显提高钕铁硼稀土永磁器件的耐腐蚀性能,使钕铁硼稀土永磁器件能用于海上风电、混合动力汽车等高耐蚀性要求的领域,扩大了钕铁硼稀土永磁的用途;一般情况下,钕铁硼稀土永磁的表面涂层都会降低磁性能,本发明发现采用本发明的设备和工艺生产的钕铁硼稀土永磁器件的磁性能,尤其是磁能积和矫顽力得到明显提高,为提高钕铁硼稀土永磁的磁性能找到了新方法,对减少稀土用量,保护稀缺的自然资源具有重要意义。Beneficial effects of the present invention: find a vacuum coating equipment and manufacturing method for mass production of NdFeB rare earth permanent magnet devices, significantly improve the corrosion resistance of NdFeB rare earth permanent magnet devices, and make NdFeB rare earth permanent magnet devices It can be used in fields with high corrosion resistance requirements such as offshore wind power and hybrid vehicles, expanding the use of NdFeB rare earth permanent magnets; generally, the surface coating of NdFeB rare earth permanent magnets will reduce the magnetic properties. It is found that the magnetic properties of the NdFeB rare earth permanent magnet devices produced by the equipment and process of the present invention, especially the magnetic energy product and the coercive force, are significantly improved, and a new method has been found for improving the magnetic properties of the NdFeB rare earth permanent magnets. It is of great significance to reduce the amount of rare earth and protect scarce natural resources.

附图说明Description of drawings

下面通过附图进一步说明本发明:Further illustrate the present invention by accompanying drawing below:

图1 为现有技术的的真空镀膜示意图Figure 1 is a schematic diagram of vacuum coating in the prior art

图2 为本发明的的真空镀膜示意图Fig. 2 is the vacuum coating schematic diagram of the present invention

图中:1、真空处理腔;2、加热舟;3、支撑平台;4、加热舟支撑基座;5、装料圆筒;6、绕转轴;7、支撑件;8、转轴;9、铝丝;10、辊子;11、热阻保护管;12、凹口;13、进给齿轮;14、磁件;15、真空壳体;16、阳极层线性离子源;17、多弧离子源;18、真空泵;19、平面磁控靶;20、加热装置;21、Ⅰ级自动齿轮;22、Ⅰ级从动齿轮;23、Ⅱ级主动齿轮;24、Ⅱ级从动齿轮;25、大转架;26、料筐;27、永磁器件;28、圆柱磁控靶;29、Ⅲ级主动齿轮;30、Ⅲ级从动齿轮; 31、抽真空管路;32、小转架;33、转轴Ⅰ;34、转轴Ⅱ。In the figure: 1. Vacuum processing chamber; 2. Heating boat; 3. Supporting platform; 4. Heating boat supporting base; Aluminum wire; 10. Roller; 11. Thermal resistance protection tube; 12. Notch; 13. Feed gear; 14. Magnetic parts; 15. Vacuum housing; 16. Anode layer linear ion source; ;18. Vacuum pump; 19. Plane magnetron target; 20. Heating device; 21. Level I automatic gear; 22. Level I driven gear; 23. Level II driving gear; 24. Level II driven gear; 25. Large 26. Material basket; 27. Permanent magnet device; 28. Cylindrical magnetron target; 29. Level III driving gear; 30. Level III driven gear; 31. Vacuumizing pipeline; 32. Small turntable; 33. Revolving shaft I; 34, revolving shaft II.

如图2所示,本发明为磁控溅射镀膜和多弧离子镀膜组合工作的混合镀膜设备。在一个连接有真空泵18的卧式真空壳体15的中心线上设有一个圆柱型磁控靶28,在大转架25的圆周上布置有多个(图中为3个)小转架32,每个小转架32的圆周上布置有多个(图中为6个)不锈钢网制成的料筐26,料筐26内装有永磁器件27。真空室外的驱动电机(未标出)通过动密封传动轴连接Ⅰ级主动齿轮21,带动固定在大转架25上的Ⅰ级从动齿轮22完成大转架25绕圆柱磁控靶28公转。固定在大转架25上的Ⅱ级主动齿轮23通过大转架25的公转带动固定在小转架32上的Ⅱ级从动齿轮24绕转轴Ⅰ33自转;固定在小转架32上的Ⅲ级主动齿轮29带动Ⅲ级从动齿轮30绕转轴Ⅱ34转动,料筐26的两端设有转轴与转轴Ⅱ34和Ⅲ级从动齿轮30联接,因此料筐26可以达到太阳行星轮系公转加自转目的,使永磁器件27在料筐26内翻炒被均匀沉积上靶材材料。在圆形真空壳体15外部设有阳极层线性离子源16,1个以上多弧离子源17,一个以上平面磁控靶19,连接真空泵18的抽真空管路31和加热装置20。As shown in Fig. 2, the present invention is a hybrid coating device that combines magnetron sputtering coating and multi-arc ion coating. A cylindrical magnetron target 28 is arranged on the center line of a horizontal vacuum housing 15 connected with a vacuum pump 18, and a plurality of (three in the figure) small turntables 32 are arranged on the circumference of the large turntable 25 , the circumference of each small turret 32 is arranged with a plurality of (6 in the figure) material baskets 26 made of stainless steel mesh, and permanent magnet devices 27 are housed in the material baskets 26 . The driving motor (not shown) outside the vacuum chamber is connected to the first-stage driving gear 21 through a dynamic seal transmission shaft, and drives the first-stage driven gear 22 fixed on the large turntable 25 to complete the revolution of the large turntable 25 around the cylindrical magnetron target 28. The second-stage driving gear 23 fixed on the large turntable 25 drives the second-stage driven gear 24 fixed on the small turntable 32 to rotate around the rotation axis I33 through the revolution of the large turntable 25; the third-stage driven gear fixed on the small turntable 32 The driving gear 29 drives the third-stage driven gear 30 to rotate around the rotating shaft II34, and the two ends of the material basket 26 are provided with a rotating shaft to connect the rotating shaft II34 and the third-stage driven gear 30, so the material basket 26 can achieve the purpose of revolution and rotation of the sun planetary gear system , so that the permanent magnet device 27 is stirred in the material basket 26 to evenly deposit the target material. An anode layer linear ion source 16 , more than one multi-arc ion source 17 , more than one planar magnetron target 19 , and a vacuuming pipeline 31 connected to a vacuum pump 18 and a heating device 20 are arranged outside the circular vacuum shell 15 .

镀膜工序前真空室抽真空达到E-4Pa量级,回充氩气,工作气压0.01~1Pa,料筐26公转加自转,启动阳极层线性离子源,放电电压100~3000V,离子轰击永磁器件27,经过5~10分钟停止轰击。料筐26是绝缘的,也可以接负压-50~-200V。先期离子轰击清洗的目的,是清洗永磁器件27表面的氧化物、含碳氢化物,使其表面粗化增加表面能和离子辅助沉积等作用。加热装置20对料筐26和料筐26内永磁器件27加热到120~600℃,起到除去水汽,提高膜层附着力作用。镀膜工序是在加热到200℃时,料筐26公转加自转并经高压离子清洗后,真空室15再次抽真空达到E-4Pa量级,回充氩气,工作气压0.1~1Pa,分别或同时启动平面磁控靶19、圆柱型磁控溅射靶28和多弧离子源17,使其分别单独工作或交替工作或同时工作,将靶材材料沉积到永磁器件27上形成单质膜和介质膜的涂层。Before the coating process, the vacuum chamber is evacuated to the level of E-4Pa, backfilled with argon, the working pressure is 0.01~1Pa, the basket rotates 26 revolutions plus rotation, the linear ion source of the anode layer is started, the discharge voltage is 100~3000V, and the ion bombards the permanent magnet device 27. Stop the bombardment after 5-10 minutes. The material basket 26 is insulated, and can also be connected to a negative voltage of -50~-200V. The purpose of the ion bombardment cleaning in the early stage is to clean the oxides and hydrocarbons on the surface of the permanent magnet device 27, so as to roughen the surface and increase the surface energy and ion-assisted deposition. The heating device 20 heats the material basket 26 and the permanent magnet device 27 in the material basket 26 to 120-600°C to remove water vapor and improve the film adhesion. The coating process is when heating to 200°C, the basket rotates at 26 revolutions and rotates, and after high-pressure ion cleaning, the vacuum chamber 15 is evacuated again to reach the level of E-4Pa, and then refilled with argon, with a working pressure of 0.1-1Pa, respectively or at the same time Start the planar magnetron target 19, the cylindrical magnetron sputtering target 28 and the multi-arc ion source 17 to make them work individually or alternately or simultaneously, and deposit the target material on the permanent magnet device 27 to form a simple film and medium film coating.

具体实施方式detailed description

下面通过实施例的对比进一步说明本发明的显著效果。The remarkable effect of the present invention is further illustrated below by comparison of the examples.

实施例1Example 1

按如下工艺制造:Manufactured as follows:

1、分别按表一A1、A2、A3、A4成分选取合金600Kg熔炼,在熔融状态下将合金浇铸到带水冷却的旋转铜辊上冷却形成合金片,接着进行氢破碎,氢破碎后进行混料,混料后进行气流磨,之后在氮气保护下用混料机混料后送到氮气保护磁场取向压机成型,保护箱内的氧含量150ppm,取向磁场强度1.8T,模腔内温度2℃,磁块尺寸62×52×42mm,取向方向为42尺寸方向,成形后在保护箱内封装,然后取出进行等静压,等静压压力200MPa,之后送入烧结设备烧结和时效。1. Select 600Kg of alloys according to the composition of A1, A2, A3, and A4 in Table 1 for smelting. In the molten state, cast the alloy on a rotating copper roller with water cooling to cool to form alloy flakes, then carry out hydrogen crushing, and then carry out mixing after hydrogen crushing. After mixing the materials, jet milling is carried out, and then the materials are mixed with a mixer under the protection of nitrogen, and then sent to the nitrogen protection magnetic field orientation press for molding. The oxygen content in the protection box is 150ppm, the orientation magnetic field strength is 1.8T, and the temperature in the mold cavity is 2 ℃, the size of the magnetic block is 62×52×42mm, and the orientation direction is the 42-dimensional direction. After forming, it is packaged in a protective box, and then taken out for isostatic pressing. The isostatic pressing pressure is 200MPa, and then sent to the sintering equipment for sintering and aging.

2、时效后进行机械加工,加工成方片30×20×10 mm尺寸,将工件选择性进行倒角、喷砂、喷铝、电泳、喷涂、之后进行真空镀膜,第一层采用磁控溅射镀膜,第二层为磁控溅射和多弧离子镀的混合镀层,第三层为磁控溅射镀层,镀层厚度分别为:0.02-5μm,0.1-15μm,1-5μm;有的实验还进行了镀第四层,第四层为磁控溅射镀层,厚度0.1-5μm,第四层未标注元素符号的为只有三层镀膜,各层选用的材料、磁性能和耐腐蚀性能的测量结果列入表二。2. After aging, mechanical processing is carried out, and it is processed into a square piece with a size of 30×20×10 mm. The workpiece is selectively chamfered, sandblasted, aluminum sprayed, electrophoresis, sprayed, and then vacuum coated. The first layer is magnetron sputtering Sputtering coating, the second layer is a mixed coating of magnetron sputtering and multi-arc ion plating, the third layer is magnetron sputtering coating, the coating thickness is: 0.02-5μm, 0.1-15μm, 1-5μm; some experiments The fourth layer was also plated. The fourth layer is a magnetron sputtering coating with a thickness of 0.1-5μm. The fourth layer is not marked with element symbols because there are only three layers of coatings. The materials, magnetic properties and corrosion resistance of each layer are selected. The measurement results are listed in Table 2.

表一、实施例和对比例的稀土永磁合金的成分The composition of the rare earth permanent magnet alloy of table one, embodiment and comparative example

编号Numbering 成分Element A1A1 Nd30Dy1Fe67.90.9Al0.2 Nd 30 Dy 1 Fe 67.9 B 0.9 A l0.2 A2A2 Nd30Dy1Fe67.5Co1.2Cu0.10.9Al0.1 Nd 30 Dy 1 Fe 67.5 Co 1.2 Cu 0.1 B 0.9 Al 0.1 A3A3 (Pr0.2Nd0.8)25Dy5Fe67.4Co1.2Cu0.30.9Al0.2 (Pr 0.2 Nd 0.8 ) 25 Dy 5 Fe 67.4 Co 1.2 Cu 0.3 B 0.9 Al 0.2 A4A4 (Pr0.2Nd0.8)25Dy5Tb1Fe65Co2.4Cu0.30.9Al0.2Ga0.1Zr0.1 (Pr 0.2 Nd 0.8 ) 25 Dy 5 Tb 1 Fe 65 Co 2.4 Cu 0.3 B 0.9 Al 0.2 Ga 0.1 Zr 0.1

表二、本发明的镀层材料、磁性能和耐腐蚀性能的测量结果Table two, the measurement result of coating material of the present invention, magnetic property and corrosion resistance

对比例1Comparative example 1

分别按表一的A1、A2、A3、A4成分选取合金600Kg熔炼,在熔融状态下将合金浇铸到带水冷却的旋转的冷却辊上冷却形成合金片,然后使用真空氢碎炉对合金片进行粗破碎,氢破碎后进行气流磨,在氮气保护下用混料机混料后送到氮气保护磁场取向压机成型,取向磁场强度1.8T,磁块尺寸62×52×42mm,取向方向为42尺寸方向,成形后在保护箱内封装,然后取出进行等静压,等静压压力200MPa,之后送入真空烧结炉烧结和时效,再进行机械加工,加工成方片30×20×10 mm尺寸,将工件选择性进行倒角或喷砂,之后进行电镀Ni-Cu-Ni,磁性能和耐腐蚀性能的测量结果列入表三。According to the A1, A2, A3, and A4 components in Table 1, select 600Kg of the alloy for melting, and cast the alloy in the molten state onto a rotating cooling roll with water cooling to form alloy flakes, and then use a vacuum hydrogen crushing furnace to crush the alloy flakes. Coarse crushing, hydrogen crushing, jet milling, mixing with a mixer under nitrogen protection, and then sending to a nitrogen protection magnetic field orientation press for molding, the orientation magnetic field strength is 1.8T, the size of the magnetic block is 62×52×42mm, and the orientation direction is 42 Dimensional direction, sealed in a protective box after forming, and then taken out for isostatic pressing, the isostatic pressing pressure is 200MPa, and then sent to a vacuum sintering furnace for sintering and aging, and then mechanically processed into a square piece with a size of 30×20×10 mm , the workpiece is selectively chamfered or sandblasted, and then Ni-Cu-Ni is electroplated. The measurement results of magnetic properties and corrosion resistance are listed in Table 3.

表三、对比例的磁性能和耐腐蚀性能的测量结果Table 3. Measurement results of magnetic properties and corrosion resistance of comparative examples

实施例2Example 2

选取实施例1中的成分制作钕铁硼稀土永磁器件,镀层选择第一层镀Dy-Al合金,第二层镀Al+ Al,第三层镀Al的镀层作温度实验,结果列入表四,序号1为镀膜时未加热也没有进行热处理的对比例,通过表四可以看出,镀膜温度和镀膜后的热处理温度对材料的磁性能有影响,明显提高了磁体的矫顽力,也就是提高了磁体的使用温度,在同等使用温度下,可以减少重稀土的用量,节约了稀缺资源。Select the composition in embodiment 1 to make NdFeB rare earth permanent magnet device, the coating selects the first layer of Dy-Al alloy plating, the second layer of Al+Al plating, and the third layer of Al plating for temperature experiments, and the results are listed in Table 4 , No. 1 is the comparative example without heating or heat treatment during coating. It can be seen from Table 4 that the coating temperature and the heat treatment temperature after coating have an impact on the magnetic properties of the material, which significantly improves the coercive force of the magnet, that is, The use temperature of the magnet is increased, and at the same use temperature, the amount of heavy rare earths can be reduced, saving scarce resources.

表四、镀膜温度和热处理温度对磁性能和耐腐蚀性能的影响Table 4. Effect of coating temperature and heat treatment temperature on magnetic properties and corrosion resistance

注:1、耐蚀性(PCT试验)Note: 1. Corrosion resistance (PCT test)

实验条件:样品10X10X10mm,2个标准大气压,120℃,100%湿度,48小时,失重<5mg/cm2Experimental conditions: sample 10X10X10mm, 2 standard atmospheric pressure, 120°C, 100% humidity, 48 hours, weight loss <5mg/cm 2 .

2、盐雾试验:2. Salt spray test:

实验条件:5%NaCl 溶液,25℃≥48小时验,表面没有变化。Experimental conditions: 5% NaCl solution, 25 ℃ ≥ 48 hours test, the surface does not change.

实施例中,真空镀膜工序前要有喷砂工序:因为稀土永磁器件在加工过程中,在其表面都会存在一定量的油脂和脏污,而这些污物对真空镀膜工艺稳定性及镀膜产品的耐腐蚀性能有很大的影响,因此配置合理的清洗设备及工艺是稀土永磁器件真空镀膜质量性能的基本保证,只有合理的清洗工艺才能保证涂层具有良好的附着力。喷砂工序采用的材料是石英、玻璃微珠、氧化铝、氧化铈、氧化镧、氧化铈和氧化镧的混合物、氧化锆的一种以上。真空镀膜工序前或者还有喷涂工序,喷涂材料为铝或含铝的化合物、电泳漆中的一种。In the embodiment, there must be a sandblasting process before the vacuum coating process: because the rare earth permanent magnet device will have a certain amount of grease and dirt on its surface during the processing process, and these dirt will affect the stability of the vacuum coating process and the coating product. Therefore, a reasonable configuration of cleaning equipment and process is the basic guarantee for the quality and performance of rare earth permanent magnet device vacuum coating. Only a reasonable cleaning process can ensure that the coating has good adhesion. The materials used in the blasting process are more than one of quartz, glass beads, aluminum oxide, cerium oxide, lanthanum oxide, a mixture of cerium oxide and lanthanum oxide, and zirconia. Before the vacuum coating process or there is a spraying process, the spraying material is one of aluminum or aluminum-containing compounds and electrophoretic paint.

实施例中,在镀膜工序中高压离子清洗工序:真空室抽真空高于E-4Pa数量级,充氩气,工作气压0.01~1Pa,料筐公转加自转,启动阳极层线性离子源,放电电压100~3000V,离子轰击稀土永磁器件5~10分钟。料筐是绝缘的,也可以接负压-50~-200V。In the embodiment, in the coating process, the high-voltage ion cleaning process: the vacuum chamber is evacuated to an order of magnitude higher than E-4Pa, filled with argon, the working pressure is 0.01-1Pa, the material basket is revolutionized and rotated, the anode layer linear ion source is started, and the discharge voltage is 100 ~3000V, ions bombard the rare earth permanent magnet device for 5~10 minutes. The material basket is insulated, and it can also be connected to a negative voltage of -50~-200V.

实施例中,镀膜工艺配置:合理的工艺配置包括单、双磁控阴极配置(包括平面、圆柱旋转磁控阴极配置),多弧阴极配置,阳极层线性离子源、加热装置和真空泵等。不同镀膜工艺配置导致生产速率、离子能量等变化,对镀膜产品性能有重要影响。真空室抽真空高于E-4Pa数量级,回充氩气,工作气压3E-1Pa,料筐公转加自转,磁控溅射沉积和电弧蒸发沉积分别单独工作或单独交替工作或同时工作;磁控溅射沉积和电弧蒸发沉积分别与离子轰击单独工作或单独交替工作。In the embodiment, coating process configuration: reasonable process configurations include single and double magnetron cathode configurations (including planar and cylindrical rotating magnetron cathode configurations), multi-arc cathode configurations, linear ion sources for the anode layer, heating devices, and vacuum pumps. Different coating process configurations lead to changes in production rate, ion energy, etc., which have an important impact on the performance of coating products. The vacuum chamber is evacuated to an order of magnitude higher than E-4Pa, backfilled with argon, the working pressure is 3E-1Pa, the basket rotates and rotates, and the magnetron sputtering deposition and arc evaporation deposition work separately or alternately or simultaneously; magnetron Sputtering deposition and arc evaporation deposition work alone or alternately with ion bombardment, respectively.

实施例中,镀膜工艺装料:料筐的结构对镀膜产品外观及涂层质量有较大影响,应避免出现表面划伤及其他物理损伤。料筐为不锈钢网制成的圆筒型或多边形柱状结构,中间有隔板形成多个隔离空间,每个空间放置一块或几块永磁器件。In the embodiment, coating process loading: the structure of the material basket has a great influence on the appearance and coating quality of the coating product, and surface scratches and other physical damage should be avoided. The material basket is a cylindrical or polygonal columnar structure made of stainless steel mesh. There are partitions in the middle to form multiple isolated spaces, and one or several permanent magnetic devices are placed in each space.

实施例中,真空镀膜工序后或者有热处理工序,热处理温度100-900℃。In the embodiment, after the vacuum coating process or there is a heat treatment process, the heat treatment temperature is 100-900°C.

通过实施例和对比例的比较进一步说明,采用本发明的技术明显提高磁体的磁性能和耐腐蚀性能,是非常有发展的工艺和设备技术。It is further illustrated by the comparison of the examples and the comparative examples that the magnetic properties and corrosion resistance of the magnets are obviously improved by adopting the technology of the present invention, which is a very developed process and equipment technology.

Claims (13)

1. the admixture plates the film equipment of a neodymium iron boron rare earth permanent magnet device, it is characterised in that: described the admixture plates the film equipment includes Vacuum film coating chamber, cylinder negative electrode magnetic control target, planar cathode magnetic control target, cathodic multi arc ion plating target, anode-layer-linear ion source, pivoted frame And charging basket;Described vacuum film coating chamber is made up of horizontal vacuum housing, Qianmen and bonnet, and Qianmen and vaccum case are close by rubber Seal seals, bonnet or be welded on vaccum case or connect by connector, the design of big pivoted frame in vacuum coating indoor, By rotating shaft support on framework, framework is arranged on vaccum case;The axis of big pivoted frame is parallel with the axis of vaccum case, greatly Being provided with 3 little pivoted frames on pivoted frame, the axis of little pivoted frame is parallel with the axis of big pivoted frame, and multiple netted charging basket two ends have rotating shaft to pacify Being contained on little pivoted frame, the axis of rotating shaft is parallel with the axis of little pivoted frame, and big pivoted frame revolves round the sun around the axis of vaccum case, little pivoted frame The i.e. axis around big pivoted frame revolves round the sun and rotation, and netted charging basket i.e. revolves round the sun also with the revolution of little pivoted frame again certainly with big pivoted frame Turn;Described cylinder negative electrode magnetic control target is arranged on the bonnet that vacuum coating is indoor, and cylinder negative electrode magnetic control target is positioned at pivoted frame Portion, axis is parallel with pivoted frame axis, and described cylinder negative electrode magnetic control target arranges more than one;Described planar cathode magnetic control target It is arranged on vaccum case, is distributed in the periphery of pivoted frame;Described cylinder negative electrode magnetic control target and the target of planar cathode magnetic control target It is respectively the one in Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Al, Ni-Cr, Ti, Mo, Si, Al2O3, ZrO2, AZO, and cylinder In the target of negative electrode magnetic control target or planar cathode magnetic control target, at least a kind of target is selected from Dy-Al, Tb-Al, Dy-Fe, Tb-Fe; Described vacuum coating indoor are provided with heater, and heating temperature range is at 100-600 DEG C.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cylinder negative electrode magnetic control target built with the magnet ring of multiple axial chargings, have magnetic guiding loop between magnet ring, magnet ring is relative to cylinder negative electrode magnetic Control target axial reciprocating moves, and described magnet ring is manufactured by Nd-Fe-B rare-earth permanent magnet.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cylinder negative electrode magnetic control target built with the magnetic stripe of a plurality of radial magnetizing, magnetic stripe is circumferentially distributed in cylinder negative electrode magnetic control target, Having interval between magnetic stripe, the quantity of magnetic stripe is 3 or more than 3, and magnetic stripe coaxially turns relative to cylinder negative electrode magnetic control target sleeve pipe Dynamic, described magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Planar cathode magnetic control target in be provided with run-track shaped annular magnetic stripe, magnetic stripe is manufactured by Nd-Fe-B rare-earth permanent magnet, with cooling water Cooling, quantity is more than one.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Cathodic multi arc ion plating target be arranged on vaccum case, be distributed in the periphery of pivoted frame, described cathodic multi arc ion plating target is rectangle Or circular, it is internally provided with Magnet, Magnet is manufactured by Nd-Fe-B rare-earth permanent magnet, and by cooling water cooling, quantity is more than one.
The admixture plates the film equipment of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 1, it is characterised in that: described Anode-layer-linear ion source be arranged on vaccum case, be distributed in the periphery of pivoted frame.
7. the manufacture of the neodymium iron boron rare earth permanent magnet device of the admixture plates the film equipment used as described in any one of claim 1-6 Method, it is characterised in that: first carry out alloy melting, in the molten state by alloy casting to the rotary copper roller of band water cooling It is cooled into alloy sheet, then alloy sheet is carried out hydrogen is broken, batch mixing and airflow milling, after airflow milling, use batch mixing under nitrogen protection Deliver to nitrogen protection magnetic field orientating press-molding after machine batch mixing, in guard box, carry out isostatic pressed after encapsulation after shaping, send afterwards Enter agglomerating plant sintering and timeliness makes Nd-Fe-B rare-earth permanent magnet magnet, carry out machining afterwards and make Nd-Fe-B rare-earth permanent magnet Device, afterwards in the indoor mixing that neodymium iron boron rare earth permanent magnet device carries out magnetron sputtering plating and multi-arc ion coating of vacuum coating Plated film, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is the one in Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Thickness of coating is: 0.02-5 μm, and the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, and thickness of coating is: 1-10 μm, Third layer is magnetron sputtering coating, and thickness of coating is: 0.1-5 μm;Heat treatment step is also had after described the admixture plates the film operation, Heat treatment temperature 60-900 DEG C.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described is mixed Closing plated film and belong to physical vapour deposition (PVD), magnetic control film coating material is Al, Dy-Al, Tb-Al, Dy-Fe, Tb-Fe, Ti, Mo, Si, stainless Steel, Al2O3, one in ZrO, AZO, the mixing coating of described magnetron sputtering and arc evaporation, Coating Materials is Al, Ti, Mo, Si, rustless steel, Al2O3, more than one in ZrO, ITO, AZO.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described is true Being provided with anode-layer-linear ion source in empty coating chamber, described magnetron sputtering plating condition is, temperature 30 ~ 600 DEG C, deposition pressure Strong is 0.1 ~ 1Pa under the conditions of argon, and power density is 1 ~ 20w/cm2, the discharge voltage 100 ~ 3000V of linear ion source, ion Energy 100 ~ 2000eV, operating air pressure 0.01 ~ 1Pa under the conditions of argon, in described filming process use magnetron sputtering plating and Multi-arc ion plating film is individually, be either alternatively or simultaneously operated.
The manufacture method of a kind of neodymium iron boron rare earth permanent magnet device the most according to claim 7, it is characterised in that: described Also having sandblasting operation before filming process, the material that sandblasting uses is quartz, glass microballoon, aluminium oxide, cerium oxide, lanthana, oxygen Change cerium and the mixture of lanthana, zirconic more than one, before filming process or also spraying process, sprayed on material is aluminum Or containing the one in the compound of aluminum, electrophoretic paint.
The manufacture method of 11. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described Also having the device heating process controlling coating process in filming process, temperature range is at 100-600 DEG C.
The manufacture method of 12. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described The admixture plates the film operation, plated film is divided into 3 layers, and ground floor is magnetron sputtering coating, and coating is Al, Dy-Al, Tb-Al, Dy-Fe, Tb- One in Fe, the second layer is the mixing coating of magnetron sputtering and multi-arc ion coating, coating is Al, Ni-Cr, Ti, Mo, Si, Al2O3、ZrO2, more than one in AZO, third layer is magnetron sputtering coating, and coating is Al, Ni-Cr, Ti, Mo, Si, Al2O3、 ZrO2, more than one in AZO.
The manufacture method of 13. a kind of neodymium iron boron rare earth permanent magnet device according to claim 7, it is characterised in that: described A kind of neodymium iron boron rare earth permanent magnet device in the range of device surface extends internally 1mm main phase grain the content of heavy rare earth higher than crystalline substance The content of heavy rare earth in grain principal phase, the heavy rare earth that content is high is distributed in principal phase R2T14The periphery of B, forms RH2T14B surrounds R2T14B New principal phase structure, RH2T14B phase and R2T14B is alternate without Grain-Boundary Phase;Wherein, R represents at Fe-B rare-earth permanent magnet structure Rare earth in middle principal phase, T representative element Fe and Co, RH represent that in principal phase, the content of heavy rare earth is higher than the rare earth of meansigma methods.
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CN106198366A (en) * 2016-06-23 2016-12-07 宁波国际材料基因工程研究院有限公司 A kind of screening technique of high flux soft magnetic materials surface anticorrosion layer
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CN113838660A (en) * 2021-11-25 2021-12-24 天津三环乐喜新材料有限公司 Vacuum coating equipment and method for surface protection of neodymium iron boron rare earth permanent magnet device

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Denomination of invention: A mixed coating equipment and manufacturing method for neodymium iron boron rare earth permanent magnet devices

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