WO2010083632A1 - 钽电容器阳极引线用钽丝及其制造方法 - Google Patents

钽电容器阳极引线用钽丝及其制造方法 Download PDF

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Publication number
WO2010083632A1
WO2010083632A1 PCT/CN2009/000556 CN2009000556W WO2010083632A1 WO 2010083632 A1 WO2010083632 A1 WO 2010083632A1 CN 2009000556 W CN2009000556 W CN 2009000556W WO 2010083632 A1 WO2010083632 A1 WO 2010083632A1
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Prior art keywords
wire
less
ccmm
tantalum
rolling
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PCT/CN2009/000556
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English (en)
French (fr)
Inventor
赵兵
杜领会
解永旭
万庆丰
王慧峰
仇国华
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宁夏东方钽业股份有限公司
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Priority to MX2011007734A priority Critical patent/MX2011007734A/es
Priority to JP2011545609A priority patent/JP5711668B2/ja
Priority to KR1020117019413A priority patent/KR101321938B1/ko
Priority to US13/145,209 priority patent/US20120300362A1/en
Priority to EP09838599.0A priority patent/EP2390886B1/en
Publication of WO2010083632A1 publication Critical patent/WO2010083632A1/zh
Priority to US14/882,249 priority patent/US10121597B2/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/08—Housing; Encapsulation
    • H01G9/12—Vents or other means allowing expansion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/0029—Processes of manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/16—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling wire rods, bars, merchant bars, rounds wire or material of like small cross-section
    • B21B1/18—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling wire rods, bars, merchant bars, rounds wire or material of like small cross-section in a continuous process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/12—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
    • 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
    • C22C1/045—Alloys based on refractory metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/008—Terminals
    • H01G9/012—Terminals specially adapted for solid capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/16—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling wire rods, bars, merchant bars, rounds wire or material of like small cross-section
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052—Sintered electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49117—Conductor or circuit manufacturing
    • Y10T29/49204—Contact or terminal manufacturing

Definitions

  • the present invention relates to a tantalum wire for a tantalum capacitor anode lead and a method of manufacturing the same. Background technique
  • Tantalum capacitors are widely used in communications, computers, automobiles, home appliances, aerospace and other fields. Tantalum electrolytic capacitors made of tantalum powder as anode and tantalum wire as anode lead have the characteristics of small volume, large capacity, high degree of chip formation, good reliability and long service life, so they can be used in many other Capacitors (such as ceramics, aluminum film and other capacitors) can not work properly under the harsh conditions.
  • tantalum wire for tantalum capacitor anode lead As a tantalum wire for tantalum capacitor anode lead, it requires high chemical purity, good surface finish, accurate size, mechanical and electrical properties to meet the stringent requirements of capacitors.
  • the specific requirements for the surface finish of the silk are: No obvious defects such as grooves, burrs, pits, etc. under the microscope of 60 times or more; the specific requirements of electrical performance are leakage current, and the smaller the leakage current, the better the performance.
  • Tantalum capacitors are gradually being developed in the direction of miniaturization, chip formation, and high specific volume, and the specific volume of tantalum powder used is also increasing, which correspondingly limits the sintering temperature of the tantalum capacitor anode block. If the sintering temperature is too high, the porosity of the tantalum powder will be greatly reduced, thereby reducing the specific volume of the tantalum capacitor.
  • the anode lead made of a round tantalum wire has a small contact area with the tantalum anode block due to its small surface area, resulting in a small contact area.
  • the contact strength is not enough, and it is easy to cause the leakage current of the tantalum capacitor to be too large. In severe cases, the silk wire even falls off from the anode block, which directly causes the tantalum capacitor to fail.
  • the above-mentioned problem of low extraction strength of tantalum capacitor leads is reliable for the electrical performance and quality of tantalum capacitors. Sex has a growing negative impact.
  • the present invention provides a profiled wire which satisfies the demanding requirements of tantalum capacitor anode leads and a method of manufacturing the same.
  • the present invention provides a twisted wire for a tantalum capacitor anode lead, characterized in that the cross section of the tantalum wire is approximately rectangular or regular rectangular.
  • the present invention provides a process for producing the above-described twisted wire, the process comprising the steps of:
  • Figure 1 is a cross-sectional photograph of a twisted yarn according to the present invention (magnification of 100 times);
  • Figure 2 is a schematic view of rolling of a twisted yarn according to the present invention. detailed description
  • test method for electrical properties is carried out in accordance with the method specified in the National Standard of the People's Republic of China "GB3463-1995 Reeling".
  • the pull-out strength performance is formed after the following parameters are formed, and then the mechanical properties are tested in accordance with the national standard GB3463-1995 Reeling of the People's Republic of China.
  • Anode block size 5. 7 X 4. 1 X 2. 9mm
  • the leakage current of the present invention is 0. 95 ⁇ A/cm 2 or less, preferably 0. 90 ⁇ A/cm 2 or less, more preferably 0. 80.
  • ⁇ A / cm 2 or less more preferably 2 or less in a 0. 60 ⁇ A / cm, and further preferably 2 or less in a 0. 50 ⁇ A / cm, particularly preferably 2 or less in a 0. 30 ⁇ A / cm, more particularly preferably 0 ⁇ Below 0. 20 ⁇ A / cm 2 or less, more preferably 0. 15 ⁇ A / cm 2 or less, especially 0. 10 ⁇ A / cm 2 or less.
  • the tensile strength of the twisted yarn of the present invention is 150 MPa or more, preferably 160 MPa or more, more preferably 170 MPa or more, more preferably 175 MPa or more, still more preferably 180 MPa or more with respect to mechanical properties. Further, it is preferably 185 MPa or more, particularly preferably 190 MPa or more, and most preferably 195 MPa or more.
  • the cross-sectional dimension of the cross-section is 0. 5-4 legs, preferably l-3 mm, width 0. 015-1 mm, preferably 0. 02-0. 5 mm, and two sides in the width direction With a curvature.
  • the cross-sectional dimension of the cross-section is 0.5- 4 mm, preferably 1-3 mm, and the width is 0. 015- 1 mm, preferably 0. 02-0. 5 mm.
  • the heat treatment of the raw material filament is heated above the recrystallization temperature, preferably from 1000 to 1450, preferably from 1200 to 1400 Torr, and the holding time is from 30 to 60 minutes, preferably from 40 to 60 minutes. .
  • the raw material filament is circular in cross section.
  • vacuum annealing in order to prevent oxidation of the wire and facilitate the escape of impurities from the raw material, vacuum annealing may be employed.
  • the vacuum is less than 5. 0 X 1 0— 2 Pa, and the gas leakage rate is less than 0.5 Pa/min.
  • the round wire in order to prevent the sticking phenomenon from occurring during the rolling of the base metal, affecting the surface quality of the finished profiled wire, the round wire is subjected to surface pretreatment in a high temperature oxygen atmosphere.
  • the circular strands are rolled using a multi-roll precision mill.
  • the pass processing is 30-95% (thickness reduction) and may be rolled once or several times up to the desired size.
  • the surface quality of the finished profiled wire is affected, and the lubricant is lubricated during rolling.
  • the lubricating oil is a fluorochloroorganic lubricating oil.
  • the work rolls may be grooved or flat in a preferred embodiment of the invention.
  • profiled rolls such as curved rolls and raised rolls may also be used.
  • the rolled profiled filaments are cleaned with a degreaser and rinsed with water. At the same time, ultrasonic waves can be applied if necessary.
  • the rolled finished shaped filaments are heated above the recrystallization temperature during annealing, using continuous wire annealing.
  • an inert gas such as argon.
  • the finished profiled filaments are rolled to an annealing temperature of 1600-20001 C and a speed of 5-10 m/min.
  • the curvature of the reel according to the present invention is not too large, and the finished product of the special-shaped twisted wire will be greatly bent on the reel, which cannot meet the requirements for use.
  • the diameter of the reel used is ⁇ 200 mm - (t > 300 mm.
  • a circular twisted wire having a diameter of 0.97 mm is placed in a roll having a diameter of 300 mm, placed in an annealing furnace, and evacuated by a vacuum pump. When the vacuum in the furnace reaches 5. O x I f) - 2 Pa, the power is raised. , Increase to 1380 X, keep warm for 60 minutes, stop heating, cool naturally. When cooling to 180, in order to accelerate cooling and improve efficiency, it can be filled with inert gas such as argon.
  • the annealed circular strands were surface pretreated using a muffle furnace.
  • the annealed circular twisted wire was first placed in a muffle furnace, and high-purity oxygen having a purity of 99% was introduced, and the temperature was raised to 600 C, and the temperature was maintained for 10 minutes, and the surface of the round twisted wire was pretreated.
  • the pre-treated round crepe is straightened and wound around the plate, requiring the entire crepe to be bent.
  • the wire wound around the plate was placed on a tensioning take-up stand, rolled using a twelve-roll precision rolling mill, and lubricated with a fluorochlorine organic lubricating oil during the rolling process.
  • the first pass is rolled at a reduction ratio of 38%, and the rolled size is 0. 60 1. 11mm
  • the second pass is rolled at a reduction ratio of 43%, and the rolled size is 0.34.
  • ⁇ 1. 36 legs, after rolling, the surface of the silk is required to be smooth and flat, without defects such as rolling marks, cracks, grooves and pits.
  • the raw material (circular twisted wire) has a diameter of 0.78 mm, rolled 3 passes, and the rest of the process is the same as in Example 1.
  • the size of each pass changes as follows:
  • the raw material (circular twisted wire) has a diameter of 0.65 mm, rolled 3 passes, and the rest of the process is the same as in Example 1.
  • the size of each pass changes as follows:
  • the raw material (circular twisted wire) has a diameter of 0.97 mm, no surface pretreatment, and the rolling process uses rolling white oil for lubrication cooling, and the rest of the process is the same as in the first embodiment.
  • Comparative example 2
  • the raw material (circular twisted wire) has a diameter of 0.78 mm, no surface pretreatment, and the rolling process uses rolling white oil for lubrication cooling, and the rest of the process is the same as in Example 2.
  • the raw material (circular twisted wire) has a diameter of 0.65 mm, no surface pretreatment, and the rolling process uses rolling white oil for lubrication cooling, and the rest of the process is the same as in Example 3.
  • Comparative example 4

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Description

钽电容器阳极引线用钽丝及其制造方法 技术领域
本发明涉及钽电容器阳极引线用钽丝及其制造方法。 背景技术
钽电容器当今被广泛用于通讯、 计算机、 汽车、 家电、 航空 航天等领域。 用钽粉作阳极， 钽丝作阳极引线制造的钽电解电容 器， 具有体积小、 电容量大、 片式化程度高、 可靠性好、 使用寿 命长等综合性能优异的特点， 因而能在许多其它电容器（如陶瓷、 铝薄膜等电容器）无法胜任的苛刻条件下正常工作。
作为钽电容器阳极引线用的钽丝， 要求化学纯度高， 表面光 洁度好， 尺寸精确， 机械性能、 电学性能满足电容器的严格要求。 例如，对钽丝表面光洁度的具体要求是： 在 60倍以上显微镜下观 察表面无明显沟槽、 毛刺、 坑点等缺陷； 电学性能的具体要求是 漏电流， 漏电流越小， 性能越好。
随着电子技术的发展， 对钽电容器的要求越来越高。 钽电容 器逐渐向小型化、 片式化、 高比容的方向发展， 使用的钽粉比容 也越来越高， 这相应的限制了钽电容器阳极块的烧结温度。 如果 烧结温度过高， 将使钽粉的孔隙度大幅度降低， 进而降低钽电容 器的比容。
但是， 使用常规的圆形阳极引线在低温烧结的钽电容器上， 存在的问题是： 圆形钽丝做成的阳极引线由于其相对表面积小， 与钽阳极块接触面积也就较小， 从而导致接触强度不够， 容易造 成钽电容器漏电流过大， 严重时钽丝甚至从阳极块上脱落， 直接 导致钽电容器失效。 随着钽电容器小型化的进一步发展， 上述的 钽电容器引线拔出强度低的问题对钽电容器的电性能和质量可靠 性产生越来越大的不良影响。
虽然在本世纪初曾提出用采用非圆形截面的钽丝替代现有圆 形截面钽丝以解决上述问题。 但是， 直到今天， 在现有钽电容器 制造技术中， 基本上全部采用圆形截面的钽丝。 其中的原因是， 一直没有一家钽丝制造商可以生产出化学纯度、 表面光洁度、 机 械性能和电学性能全部满足钽电容器使用要求的异形钽丝来。 其 中，很多情况都是在表面光洁度、机械性能和 /或电学性能上不能 满足钽电容器使用的苛刻要求。 发明内容
针对现有技术中存在的一个或多个问题，本发明提供了一种满 足钽电容器阳极引线苛刻使用要求的异形钽丝及其制造方法。
具体的， 本发明提供了一种用于钽电容器阳极引线的钽丝， 其 特征在于， 该钽丝的截面为近似矩形或规则矩形。
另外，本发明还提供了制造上述的钽丝的工艺， 所述工艺包括 如下步骤：
( 1 ) 提供原料钽丝；
( 2 ) 对原料钽丝进行热处理；
( 3 ) 对热处理后的钽丝进行表面预处理，使得处理后的钽丝 表面生成氧化膜；
( 4 ) 采用润滑油进行润滑， 轧制表面预处理后的钽丝， 使得 轧制后的钽丝的截面为近似矩形或规则矩形；
( 5 ) 对钽丝进行最终退火。 附图说明
图 1 根据本发明的钽丝的截面照片 （放大倍数 100倍） ； 图 2 根据本发明的钽丝的轧制示意图。 具体实施方式
可以理解， 以上描述和以下实施方案只是示范性的说明， 可 由本领域的某些技术人员对这些技术方案做各种改进、 改良或变 化而不脱离本发明的实质和范围。
在本发明中，电性能的测试方法按照中华人民共和国国家标 准 《GB3463- 1995 钽丝》规定的方法进行。 拔出强度性能是按以 下参数成型后， 再按照中华人民共和国国家标准 《GB3463-1995 钽丝》规定中测试力学性能的方法进行。
. 成型设备： 钽电解电容器自动成型机
. 壳型： E
. 粉量： 381 - 392mg
. 阳极块尺寸： 5. 7 X 4. 1 X 2. 9mm
. 钽丝埋入量： 1. 6 - 1. 9mm
. 成型后密度： 5. 5 - 5. 6g/cm3
在本发明一个优选实施方案中， 对于电性能， 本发明的钽丝 的漏电流在 0. 95 μ A/cm2以下、 优选在 0. 90 μ A/cm2以下、 更优选 在 0. 80 μ A/cm2以下、 进一步优选在 0. 60 μ A/cm2以下、 再进一步 优选在 0. 50 μ A/cm2以下、 特别优选在 0. 30 μ A/cm2以下， 更特别 优选在 0. 20 μ A/cm2以下、 再优选在 0. 15 μ A/cm2以下、 特别是在 0. 10 μ A/cm2以下。
在本发明的另一个优选实施方案中， 对于力学性能， 本发明 的钽丝的拔出强度在 150MPa以上、 优选在 160MPa以上、 更优选 在 170MPa 以上、 更优选在 175MPa 以上、 进一步优选在 180MPa 以上、 再优选在 185MPa以上、 特别优选在 190MPa以上、 最优选 在 195MPa以上。
在本发明的另一个优选实施方案中， 当所述钽丝的截面为近似 矩形时， 所述截面的截面尺寸为长 0. 5-4 腿， 优选为 l-3 mm， 宽 0. 015-1 mm, 优选为 0. 02-0. 5 mm, 且宽度方向上的两边带有弧 度。
在本发明的另一个优选实施方案中， 当所述钽丝的截面为规则 矩形时， 所述截面的截面尺寸为长 0. 5- 4 mm, 优选为 1-3 mm, 宽 0. 015-1 mm, 优选为 0. 02-0. 5 mm。
在本发明的一个优选实施方案中， 原料钽丝的热处理是在再 结晶温度以上加热， 优选为 1000-1450 ， 优选为 1200- 1400Ό ， 且保温时间为 30-60分钟， 优选为 40- 60分钟。
在本发明的一个实施方案中， 原料钽丝的截面为圆形。
同时， 在本发明的一个优选实施方案中， 为了防止丝材氧化 并利于原料钽丝逸出杂质， 可以采用真空退火。 在本发明的一个 优选实施方案中， 真空退火步骤的真空度大于 5. 0 X 1 0—2 Pa, 漏 气率小于 0. 5 Pa/min。
在本发明的一个优选实施方案中， 为了防止钽金属轧制过程 中发生粘辊现象， 影响成品异形钽丝表面质量， 圆形钽丝在高温 氧气气氛中进行表面预处理。
在本发明的一个优选实施方案中， 圆形钽丝用多辊精密轧机 轧制。在进一步优选的实施方案中，道次加工量 30-95%(减厚率）， 并可以经过一次或数次轧制直至需要的尺寸。
在本发明的一个优选实施方案中， 为了防止轧制中润滑不均 匀， 影响成品异形钽丝表面质量， 轧制时釆用润滑油润滑。
在本发明的一个优选实施方案中， 所述润滑油为氟氯有机润 滑油。 在本发明的另一个实施方案中， 工作辊可以釆用槽辊或平 在本发明的一个优选实施方案中， 为了增强轧制效果， 也可 以使用异形轧辊， 如弧形轧辊和凸辊。 在本发明的一个优选实施方案中， 轧制出的成品异形钽丝采 用除油剂清洗， 采用清水漂洗。 同时， 如果需要， 可以施加超声 波。
在本发明的一个优选实施方案中， 轧制出的成品异形钽丝退 火时在再结晶温度以上加热， 采用连续走线式退火。 在进一步优 选的实施方案中， 为了防止丝材氧化， 可以釆用惰性气体保护， 如氩气。
在本发明的一个优选实施方案中， 轧制出的成品异形钽丝的 退火温度为 1600-20001C , 速度为 5-10m/min。
本发明涉及的绕线盘曲率不能太大， 否则异形钽丝成品在绕 线盘上将发生大幅度弯曲， 无法满足使用要求。 在本发明的一个 优选实施方案中， 使用的绕线盘直径为 φ 200mm— (t> 300mm。 实施例 1
取直径为 0. 97mm的圆形钽丝， 盘成直径 300mm的卷， 放置在 退火炉内， 用真空泵抽空， 当炉内真空度达到 5. O x I f)—2 Pa时， 送电升温， 升至 1380 X， 保温 60分钟， 停止加热， 自然冷却， 当冷却至 180 时， 为了加速冷却， 提高效率， 可以充惰性气体， 如氩气。
退火后的圆形钽丝使用马弗炉进行表面预处理。 先将退火后 的圆形钽丝放置在马弗炉中， 通入纯度为 99%的高纯氧气， 升温 至 600 C， 保温 10分钟， 对圆形钽丝进行表面预处理。 预处理后 的圆形钽丝经过矫直， 绕在盘子上， 要求整根钽丝无弯折。
将绕在盘子上的钽丝放置在带张力的放线架上， 使用十二辊 精密轧机轧制， 轧制过程中加氟氯有机润滑油润滑。
轧制时， 第一道次按减厚率 38%进行轧制， 轧后尺寸为 0. 60 1. 11mm, 第二道次按减厚率 43%进行轧制， 轧后尺寸为 0. 34 χ 1. 36腿， 轧后钽丝表面要求光洁平整， 无轧痕、 裂边、 沟槽、 坑 点等缺陷。
将轧制完成的异形钽丝放置在带张力的放线架上， 通过稀释 到合适浓度的除油剂及清水、 同时施加超声波， 清洗掉异形钽丝 表面的油污及其它杂质， 收在绕线盘上。 清洗干净的异形钽丝， 放在带张力的放线架上，进行连续走线式退火。退火温度 1750 ， 速度 5m/min， 收在绕线盘上， 直到放线架上的整根异形钽丝全部 收到收线盘上， 完成异形钽丝的制备。 实施例 2
原料（圆形钽丝 ) 直径为 0. 78mm, 轧制 3个道次， 其余过程 同实施例 1。 各道次尺寸变化如下：
φ 0. 78— 0. 43 1. 19—0. 27 1. 22—0. 23 χ 1. 24 实施例 3
原料（圆形钽丝） 直径为 0. 65mm, 轧制 3个道次， 其余过程 同实施例 1。 各道次尺寸变化如下：
φ 0. 65— 0. 37 1. 09—0. 20 χ 1. 11— 0. 15 χ 1. 12 比较例 1
原料（圆形钽丝）直径为 0. 97mm, 不进行表面预处理， 轧制 过程使用轧制白油进行润滑冷却， 其余过程同实施例 1。 比较例 2
原料（圆形钽丝） 直径为 0. 78mm， 不进行表面预处理， 轧制 过程使用轧制白油进行润滑冷却， 其余过程同实施例 2。 比较例 3
原料（圆形钽丝）直径为 0. 65mm， 不进行表面预处理， 轧制 过程使用轧制白油进行润滑冷却， 其余过程同实施例 3。 比较例 4
直接取与异形钽丝 0. 34 x l. 36mm、 0. 23 x 1. 24 mm、 0. 15 x 1. 12 麵相同横截面积的合格钽电容器阳极引线用圆形钽丝， 其 直径分另 'J为 Φ 0. 767mm 、 Φ 0. 603mm和 Φ 0. 463mme
检测
以上各例中圆形钽丝和异形钽丝的各项性能检测如下： 表 1 各例中圆形钽丝和异形钽丝拔出强度
Figure imgf000009_0001
各例中圆形钽丝和异形钽丝电性能
序号 规格 (mm) 漏电流 (uA/cm2) 备注
1 0. 34 X 1. 36 0. 10 实施例 1
2 0. 34 X 1. 36 1. 26 比较例 1
3 0. 23 X 1. 24 0. 09 实施例 2
4 0. 23 X 1. 24 0. 98 比较例 2
5 0. 15 X 1. 12 0. 11 实施例 3
6 0. 15 X 1. 12 1. 26 比较例 3

Claims

权 利 要 求
11.. 一一种种用用于于钽钽电电容容器器阳阳极极引引线线的的钽钽丝丝，， 其其特特征征在在于于，， 该该钽钽丝丝 的的截截面面为为近近似似矩矩形形或或规规则则矩矩形形。。
22.. 根根据据权权利利要要求求 11 的的钽钽丝丝，， 其其中中该该钽钽丝丝的的漏漏电电流流在在 00.. 9955 μμ AA//ccmm22以以下下、、 优优选选在在 00.. 9900 μμ AA//ccmm22以以下下、、 更更优优选选在在 00.. 8800 μμ AA//ccmm22以以 下下、、进进一一步步优优选选在在 00.. 6600 μμ AA//ccmm22以以下下、、再再进进一一步步优优选选在在 00.. 5500 μμ AA//ccmm22 以以下下、、 特特别别优优选选在在 00.. 3300 μμ AA//ccmm22以以下下，， 更更特特别别优优选选在在 00.. 2200 μμ AA//ccmm22 以以下下、、 最最优优选选在在 00.. 1155 μμ AA//ccmm22以以下下、、 还还优优选选在在 00.. 1133 μμ AA//ccmm22以以下下。。
33.. 根根据据权权利利要要求求 11或或 22的的钽钽丝丝，，其其中中钽钽丝丝的的拔拔出出强强度度在在 1155 OOMMPPaa 以以上上、、 优优选选在在 116600MMPPaa 以以上上、、 更更优优选选在在 117700MMPPaa 以以上上、、 更更优优选选在在 117755MMPPaa以以上上、、进进一一步步优优选选在在 118800MMPPaa以以上上、、再再优优选选在在 118855MMPPaa以以上上。。
44.. 制制造造权权利利要要求求 11 -- 33中中任任何何一一项项所所述述的的钽钽丝丝的的工工艺艺，，所所述述工工 艺艺包包括括如如下下步步骤骤：：
(( 11 )) 提提供供原原料料钽钽丝丝；；
(( 22 )) 对对原原料料钽钽丝丝进进行行热热处处理理；；
(( 33 )) 对对热热处处理理后后的的钽钽丝丝进进行行表表面面预预处处理理，，使使得得预预处处理理后后的的 钽钽丝丝表表面面生生成成氧氧化化膜膜；；
(( 44 )) 采采用用润润滑滑油油进进行行润润滑滑，， 轧轧制制表表面面预预处处理理后后的的钽钽丝丝，， 使使 得得轧轧制制后后的的钽钽丝丝的的截截面面为为近近似似矩矩形形或或规规则则矩矩形形；；
(( 55 )) 对对钽钽丝丝进进行行最最终终退退火火。。
55.. 根根据据权权利利要要求求 44 的的工工艺艺，， 其其中中，，
Figure imgf000010_0001
lOOO-HSO , 优选为 1200- 1400Π , 且保温时间为 30-60分钟， 优选为 40-60分钟的真空退火。
6. 根据权利要求 4或 5的工艺， 其中， 该表面预处理步骤在 高温氧气气氛中进行，优选在 500 - 700 的温度在下、在 99 %纯 度的氧气中进行， 处理时间为 1分钟到 1小时， 优选为 5分钟到 30分钟。
7. 根据权利要求 4 - 6中任意一项的工艺， 其中， 轧制步骤为 多道次轧制， 且每道次的减厚率为 20-95%, 优选为 20-90%, 更优 选为 22-85%。
8. 根据权利要求 4 - 7中任意一项的工艺， 其中， 在轧制步骤 中插入退火步骤以消除应力。
9. 根据权利要求 4 - 8中任意一项的工艺， 其中， 所述退火步 骤为 1000-1450 ，优选为 1200- 14001C且保温时间为 30- 60分钟， 优选为 40-60分钟的真空退火。
10. 根据权利要求 4 - 9中任意一项的工艺， 其中， 在轧制步骤 之后且在最终退火步骤之前对钽丝进行清洗。
11. 根据权利要求 4 - 10 中任意一项的工艺， 其中， 最终退火 步骤是退火温度为 1600- 2000Ό，优选为 1700-18001C且走线速度 为 5-10m/min的连续走线式退火。
12. 根据权利要求 4 - 11 中任意一项的工艺， 其中， 所述润滑 油为氟氯有机润滑油。
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