CN106756830A - The manufacture method of alumal target - Google Patents

The manufacture method of alumal target Download PDF

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Publication number
CN106756830A
CN106756830A CN201611192961.2A CN201611192961A CN106756830A CN 106756830 A CN106756830 A CN 106756830A CN 201611192961 A CN201611192961 A CN 201611192961A CN 106756830 A CN106756830 A CN 106756830A
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target
alumal
slab
hot
aluminum
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CN106756830B (en
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鲁飞
刘树峰
张志宏
孙良成
刘小鱼
李慧
郑天仓
王峰
李静雅
邢正茂
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Baotou Rare Earth Research Institute
Ruike National Engineering Research Centre of Rare Earth Metallurgy and Functional Materials Co Ltd
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Baotou Rare Earth Research Institute
Ruike National Engineering Research Centre of Rare Earth Metallurgy and Functional Materials Co Ltd
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses a kind of manufacture method of alumal target, including：Slab is produced, the mass ratio of slab chemical constituent is, aluminium：75~95%, manganese：5~25%；Shaping slab is fitted into mould, hot-pressed sintering furnace is put into and is obtained alumal target article through hot pressed sintering；Target product is obtained after alumal target article is machined.More than 99%, internal imporosity, outside flawless, crystallite dimension is tiny homogeneous, distributed components for the alumal target relative density that the present invention is obtained.

Description

铝锰合金靶材的制造方法Manufacturing method of aluminum-manganese alloy target

技术领域technical field

本发明涉及一种材料加工技术，具体说，涉及一种铝锰合金靶材的制造方法。The invention relates to a material processing technology, in particular to a method for manufacturing an aluminum-manganese alloy target.

背景技术Background technique

烧结钕铁硼(NdFeB)永磁材料的表面防护是磁体生产的重要技术环节。目前国内常见的工业规模的表面防护处理方法电镀和化学镀存在膜层附着力低，污染环境等诸多问题。真空镀膜技术作为一种环境友好表面处理工艺，镀膜过程无原料外溢，无污染物排放，生产现场清洁，防护膜层附着力比电镀膜大5-10倍，在NdFeB永磁材料的表面防护领域显示出极大的发展潜力，产业应用前景好。The surface protection of sintered neodymium iron boron (NdFeB) permanent magnet materials is an important technical link in magnet production. At present, electroplating and electroless plating, the common industrial-scale surface protection treatment methods in China, have many problems such as low film adhesion and environmental pollution. Vacuum coating technology is an environmentally friendly surface treatment process. There is no spillage of raw materials, no pollutant discharge during the coating process, and the production site is clean. The adhesion of the protective film layer is 5-10 times greater than that of the electroplating film. It is used in the surface protection field of NdFeB permanent magnet materials. It shows great potential for development, and has good prospects for industrial application.

从成本及耐蚀性能考虑，目前市场上比较认可铝锰合金耐蚀镀层。作为镀膜源，铝锰合金靶材的质量影响着镀膜环境及镀层质量，进而影响着NdFeB磁体的耐蚀性能。制作高质量靶材关键在于提高靶材相对密度。靶材相对密度的提高可以极大地减少靶材组织内部的残留气孔，气孔率的减少甚至消除能够极大地提高成膜速率，降低工业化生产成本。采用常规熔铸工艺制作的铝锰合金靶材相对密度约为94％左右，组织内部存在残留孔洞，无法满足真空镀膜对高质量铝锰靶材的需求。From the consideration of cost and corrosion resistance, the current market is relatively recognized aluminum-manganese alloy corrosion-resistant coating. As a coating source, the quality of the Al-Mn alloy target affects the coating environment and coating quality, which in turn affects the corrosion resistance of the NdFeB magnet. The key to making high-quality targets is to increase the relative density of the targets. The increase in the relative density of the target can greatly reduce the residual pores inside the target structure, and the reduction or even elimination of the porosity can greatly increase the film formation rate and reduce the cost of industrial production. The relative density of the aluminum-manganese alloy target produced by the conventional melting and casting process is about 94%, and there are residual holes in the structure, which cannot meet the needs of vacuum coating for high-quality aluminum-manganese targets.

发明内容Contents of the invention

本发明所解决的技术问题是提供一种铝锰合金靶材的制造方法，获得的铝锰合金靶材相对密度在99％以上，内部无孔隙，外部无裂纹，晶粒尺寸细小均一，成分分布均匀。The technical problem to be solved by the present invention is to provide a method for manufacturing an Al-Mn alloy target. The obtained Al-Mn alloy target has a relative density of more than 99%, no internal pores, no external cracks, fine and uniform grain size, and a distribution of components. uniform.

技术方案如下：The technical solution is as follows:

一种铝锰合金靶材的制造方法，包括：A method for manufacturing an aluminum-manganese alloy target, comprising:

制取板坯，板坯化学组分的质量比为，铝：75～95％，锰：5～25％；Prepare the slab, the mass ratio of the chemical components of the slab is: aluminum: 75-95%, manganese: 5-25%;

将成型板坯装入模具中，放入热压烧结炉经热压烧结得到铝锰合金靶材制品；Put the formed slab into the mold, put it into a hot-press sintering furnace, and obtain an aluminum-manganese alloy target product through hot-press sintering;

铝锰合金靶材制品经机加工后得到靶材产品。Al-Mn alloy target products are machined to obtain target products.

进一步：成型板坯为铝锰合金铸锭，表面粗糙度为1.0～3.0m。Further: the forming slab is an aluminum-manganese alloy ingot, and the surface roughness is 1.0-3.0m.

进一步：热压烧结时，热压炉内真空度高于1×10-2Pa，烧结温度为600～800℃，成型压力为5～20MPa，保温保压1～2小时。Further: during hot-press sintering, the vacuum degree in the hot-press furnace is higher than 1×10 -2 Pa, the sintering temperature is 600-800° C., the forming pressure is 5-20 MPa, and the temperature and pressure are kept for 1-2 hours.

进一步：对铝锰合金靶材制品进行表面磨抛及外形加工处理获得靶材产品。Further step: surface grinding and polishing and shape processing of aluminum-manganese alloy target products to obtain target products.

与现有技术相比，本发明技术效果包括：Compared with the prior art, the technical effects of the present invention include:

1、获得的铝锰合金靶材相对密度在99％以上，内部无孔隙，外部无裂纹；晶粒尺寸细小均一；采用本发明方法制造靶材成品率高，易于规模化生产。1. The relative density of the obtained aluminum-manganese alloy target is above 99%, and there are no pores inside and no cracks outside; the grain size is fine and uniform; the target produced by the method of the present invention has a high yield and is easy for large-scale production.

2、成分分布均匀，可以满足真空镀膜对高质量铝锰靶材的需求。本发明方法可以有效避免采用传统粉末装填模具后热压工艺存在的由于粉料装填不均匀造成的烧结制品在径向(或轴向)密度不一致的弊端。所制造的铝锰靶材成分分布均匀，无偏析，批次一致性好，适合规模化生产。2. The ingredients are evenly distributed, which can meet the needs of vacuum coating for high-quality aluminum-manganese targets. The method of the invention can effectively avoid the drawbacks of inconsistent density of sintered products in the radial direction (or axial direction) caused by uneven powder filling in the hot pressing process after the traditional powder is filled into the mold. The manufactured aluminum-manganese target has uniform composition distribution, no segregation, good batch consistency, and is suitable for large-scale production.

3、经济效益显著。3. Significant economic benefits.

我国NdFeB磁体每年的产量超过10万吨。北方稀土NdFeB磁体年产量约为1.5万吨，镀膜费用按0.08元人民币/cm2计算(每克NdFeB磁体按0.15-0.2cm2计)，产值达2亿元/年左右，经济效益显著。The annual output of NdFeB magnets in my country exceeds 100,000 tons. The annual output of rare earth NdFeB magnets in the North is about 15,000 tons, and the coating cost is calculated at 0.08 yuan/cm2 (calculated at 0.15-0.2cm2 per gram of NdFeB magnet), and the output value is about 200 million yuan/year, with significant economic benefits.

本发明采用环境有好的真空镀膜技术在NdFeB表面制备防护膜层，相对于电镀和化学镀而言，镀膜过程无原料外溢，无污染物排放，生产现场清洁，防护膜层附着力比电镀膜大5-10倍。本发明提高了永磁材料产品档次，加强了产品国际市场竞争力，能够发挥稀土大国的资源优势，对于提升企业技术含量具有重要现实意义。The invention adopts a vacuum coating technology with good environment to prepare a protective film on the surface of NdFeB. Compared with electroplating and chemical plating, the coating process has no overflow of raw materials, no discharge of pollutants, clean production site, and the adhesion of the protective film is higher than that of electroplating. 5-10 times larger. The invention improves the product grade of the permanent magnet material, strengthens the competitiveness of the product in the international market, can give full play to the resource advantages of a large rare earth country, and has important practical significance for improving the technical content of enterprises.

具体实施方式detailed description

下面参考示例实施方式，对本发明技术方案作详细描述。然而，示例实施方式能够以多种形式实施，且不应被理解为限于在此阐述的实施方式；相反，提供这些实施方式使得本发明更全面和完整，并将示例实施方式的构思全面地传达给本领域的技术人员。The technical solutions of the present invention will be described in detail below with reference to example implementations. Example embodiments may, however, be embodied in many forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art.

铝锰合金靶材的制造方法，具体包括以下步骤：A method for manufacturing an aluminum-manganese alloy target, specifically comprising the following steps:

步骤1：制取板坯；Step 1: Prepare the slab;

成型板坯为铝锰合金铸锭，表面粗糙度为1.0～3.0m，板坯化学组分的质量比为，铝：75～95％，锰：5～25％。The formed slab is an aluminum-manganese alloy ingot, the surface roughness is 1.0-3.0m, and the mass ratio of the chemical components of the slab is: aluminum: 75-95%, manganese: 5-25%.

步骤2：热压烧结；Step 2: hot pressing and sintering;

将成型板坯装入模具中，放入热压烧结炉经热压烧结得到铝锰合金靶材制品。热压烧结时，热压炉内真空度高于1×10-2Pa，烧结温度为600～800℃，成型压力为5～20MPa，保温保压1～2小时。Put the formed slab into the mold, put it into a hot-press sintering furnace and perform hot-press sintering to obtain an aluminum-manganese alloy target product. During hot-press sintering, the vacuum degree in the hot-press furnace is higher than 1×10 -2 Pa, the sintering temperature is 600-800°C, the molding pressure is 5-20 MPa, and the heat preservation and pressure are held for 1-2 hours.

将铝锰合金铸锭板坯进行热压烧结，对板坯同时施加力和温度的双重作用。在设定参数范围内，铝会出现液相，提升靶材烧结致密性，所制造靶材相对密度高，组织致密，无孔隙，晶粒尺寸细小均一。The aluminum-manganese alloy ingot slab is hot-pressed and sintered, and the dual effects of force and temperature are applied to the slab at the same time. Within the set parameter range, aluminum will appear in liquid phase, which improves the sintering compactness of the target material. The target material produced has high relative density, compact structure, no pores, and small and uniform grain size.

步骤3：机加工；对铝锰合金制品进行表面磨抛及外形加工处理获得靶材产品。Step 3: Machining; surface grinding and polishing and shape processing of aluminum-manganese alloy products to obtain target products.

实施例1：Example 1:

一种铝锰合金靶材制造方法，具体包括以下步骤：A method for manufacturing an aluminum-manganese alloy target, specifically comprising the following steps:

(1)成型板坯；(1) Formed slab;

准备质量百分比为95％Al、5％Mn的铝锰合金铸锭，经车铣加工至表面粗糙度为2.0m的成型板坯。An aluminum-manganese alloy ingot with a mass percentage of 95% Al and 5% Mn is prepared, and a formed slab with a surface roughness of 2.0 m is processed by turning and milling.

(2)热压烧结；(2) hot pressing sintering;

将成型板坯装入模具中，放入热压烧结炉。关闭炉门开始抽真空，当热压炉内真空度高于1×10-2Pa时，开始升温，温度升到600℃时，增加压力至5MPa，保温保压2小时，随炉冷却得到铝锰合金制品。Put the formed slab into the mold and put it into the hot-press sintering furnace. Close the furnace door and start vacuuming. When the vacuum degree in the hot-press furnace is higher than 1×10 -2 Pa, start to heat up. When the temperature rises to 600°C, increase the pressure to 5MPa, hold the heat for 2 hours, and get aluminum Manganese alloy products.

(3)机加工。(3) Machining.

对铝锰合金制品进行表面磨抛及外形加工处理获得靶材产品。经上述工艺获得的铝锰合金靶材外观质量好，无裂纹和隐裂等宏观缺陷，组织致密无孔隙，相对密度达99.7％。Surface grinding and polishing and shape processing are performed on aluminum-manganese alloy products to obtain target products. The aluminum-manganese alloy target obtained by the above process has good appearance quality, no macroscopic defects such as cracks and hidden cracks, dense structure without pores, and a relative density of 99.7%.

实施例2：Example 2:

一种铝锰合金靶材制造方法，具体包括以下步骤：A method for manufacturing an aluminum-manganese alloy target, specifically comprising the following steps:

(1)成型板坯；(1) Formed slab;

准备质量百分比为80％Al、20％Mn的铝锰合金铸锭，经车铣加工至表面粗糙度为1.0m的成型板坯。An aluminum-manganese alloy ingot with a mass percentage of 80% Al and 20% Mn is prepared, and processed by turning and milling to form a slab with a surface roughness of 1.0 m.

(2)热压烧结：将成型板坯装入模具中，放入热压烧结炉。关闭炉门开始抽真空，当热压炉内真空度高于1×10-2Pa时，开始升温，温度升到780℃时，增加压力至10MPa，保温保压1.5小时，随炉冷却得到铝锰合金制品。(2) Hot-press sintering: put the formed slab into a mold and put it into a hot-press sintering furnace. Close the furnace door and start vacuuming. When the vacuum degree in the hot-press furnace is higher than 1×10 -2 Pa, start to heat up. When the temperature rises to 780°C, increase the pressure to 10MPa, keep the temperature and hold the pressure for 1.5 hours, and cool down with the furnace to obtain aluminum Manganese alloy products.

(3)机加工。(3) Machining.

对铝锰合金制品进行表面磨抛及外形加工处理获得靶材产品。经上述工艺获得的铝锰合金靶材外观质量好，无裂纹和隐裂等宏观缺陷，组织致密无孔隙，相对密度达99.5％。Surface grinding and polishing and shape processing are performed on aluminum-manganese alloy products to obtain target products. The aluminum-manganese alloy target obtained by the above process has good appearance quality, no macroscopic defects such as cracks and hidden cracks, dense structure without pores, and a relative density of 99.5%.

实施例3：Example 3:

一种铝锰合金靶材制造方法，具体包括以下步骤：A method for manufacturing an aluminum-manganese alloy target, specifically comprising the following steps:

(1)成型板坯；(1) Formed slab;

准备质量百分比为75％Al—25％Mn的铝锰合金铸锭，经车铣加工至表面粗糙度为3.0m的成型板坯。Prepare an aluminum-manganese alloy ingot with a mass percentage of 75% Al-25% Mn, and process it into a formed slab with a surface roughness of 3.0 m through turning and milling.

(2)热压烧结；(2) hot pressing sintering;

将成型板坯装入模具中，放入热压烧结炉。关闭炉门开始抽真空，当热压炉内真空度高于1×10-2Pa时，开始升温，温度升到800℃时，增加压力至20MPa，保温保压1小时，随炉冷却得到铝锰合金制品。Put the formed slab into the mold and put it into the hot-press sintering furnace. Close the furnace door and start vacuuming. When the vacuum degree in the hot-press furnace is higher than 1×10 -2 Pa, start to heat up. When the temperature rises to 800°C, increase the pressure to 20MPa, keep the temperature and hold the pressure for 1 hour, and get aluminum alloy with the furnace cooling. Manganese alloy products.

(3)机加工。(3) Machining.

对铝锰合金制品进行表面磨抛及外形加工处理获得靶材产品。经上述工艺获得的铝锰合金靶材外观质量好，无裂纹和隐裂等宏观缺陷，组织致密无孔隙，相对密度达99.2％。Surface grinding and polishing and shape processing are performed on aluminum-manganese alloy products to obtain target products. The aluminum-manganese alloy target obtained by the above process has good appearance quality, no macroscopic defects such as cracks and hidden cracks, dense structure without pores, and a relative density of 99.2%.

本发明所用的术语是说明和示例性、而非限制性的术语。由于本发明能够以多种形式具体实施而不脱离发明的精神或实质，所以应当理解，上述实施例不限于任何前述的细节，而应在随附权利要求所限定的精神和范围内广泛地解释，因此落入权利要求或其等效范围内的全部变化和改型都应为随附权利要求所涵盖。The terms used herein are terms of description and illustration, rather than limitation. Since the present invention can be embodied in many forms without departing from the spirit or essence of the invention, it should be understood that the above-described embodiments are not limited to any of the foregoing details, but should be construed broadly within the spirit and scope of the appended claims. , all changes and modifications falling within the scope of the claims or their equivalents shall be covered by the appended claims.

Claims (4)

1. a kind of manufacture method of alumal target, including：
Slab is produced, the mass ratio of slab chemical constituent is, aluminium：75~95%, manganese：5~25%；
Shaping slab is fitted into mould, hot-pressed sintering furnace is put into and is obtained alumal target article through hot pressed sintering；
Target product is obtained after alumal target article is machined.
2. the manufacture method of alumal target as claimed in claim 1, it is characterised in that：Shaping slab is cast for alumal Ingot, surface roughness is 1.0~3.0m.
3. the manufacture method of alumal target as claimed in claim 1, it is characterised in that：It is true in hot pressing furnace during hot pressed sintering Reciprocal of duty cycle is higher than 1 × 10-2Pa, sintering temperature is 600~800 DEG C, and briquetting pressure is 5~20MPa, heat-insulation pressure keeping 1~2 hour.
4. the manufacture method of alumal target as claimed in claim 1, it is characterised in that：Alumal target article is carried out Surface grinding and polishing and sharp processing treatment obtain target product.
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