CN101670521A - Preparation method of metal tantalum belt - Google Patents

Preparation method of metal tantalum belt Download PDF

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Publication number
CN101670521A
CN101670521A CN200910180106A CN200910180106A CN101670521A CN 101670521 A CN101670521 A CN 101670521A CN 200910180106 A CN200910180106 A CN 200910180106A CN 200910180106 A CN200910180106 A CN 200910180106A CN 101670521 A CN101670521 A CN 101670521A
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China
Prior art keywords
tantalum
rolling
preparation
metal
working modulus
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CN200910180106A
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Chinese (zh)
Inventor
王艳
武宇
姚秀楠
宜楠
朱海林
吕雨红
赵鸿磊
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XIBU METAL MATERIAL CO Ltd
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XIBU METAL MATERIAL CO Ltd
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Priority to CN200910180106A priority Critical patent/CN101670521A/en
Publication of CN101670521A publication Critical patent/CN101670521A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a preparation method of metal tantalum belts. The method is characterized in that the preparation method comprises the following steps: adopting high purity smelted tantalum ingots to forge tantalum metal slabs; then rolling, annealing the rolled blanks; welding the annealed blanks and a leading tape by adopting argon arc protective welding, and then performing tension rolling to prepare tantalum belts, wherein in the rolling process, the first pass adopts 35% or more of processing rate, the second pass adopts 30% or more of processing rate and the following passess adopt 15% or more of processing rate. The invention adopts high purity smelted tantalum ingots to perform forging and deformation so as to refine original coarse grains of blanks; the method adopts mechanical milling and chemical acid cleaning to clean blanks, combines large processing rate rolling technology in the early stage of rolling to fully refine the grains of the finished belts and finallyadopts heat treatment technology to control and obtain high purity metal tantalum belts with fine grains and high elongation.

Description

A kind of preparation method of metal tantalum belt
Technical field
A kind of preparation method of metal tantalum belt relates to the preparation method of a kind of superconducting line barrier layer with high purity metal tantalum band.
Background technology
Along with the continuous development of industrial technology, tantalum becomes the development of new developing direction, particularly superconductor technology with the application of ribbon form, and market increases gradually to tantalum band demand.Use the main material of tantalum band during for example superconducting line is produced as the superconducting line barrier layer.The tantalum band requires tantalum band purity height in the application of superconduction production field, and crystal grain is tiny evenly, good extending performance.Tiny and uniform grain structure can improve the deformation uniformity of tantalum band, strengthens deep-draw ductility, makes the tantalum band still can homogeneous deformation under near 100% working modulus, and thickness reaches 2~4 microns and do not break.In the traditional processing technology, tantalum band homogeneous grain size is bad, percentage elongation is low, the tantalum desmorrhexis can appear in superconducting line in process makes metallic copper and alloy spread the generation frangible compounds in hot-working, this compound can bring harm to the multi-core composite superconducting wire performance, influences the final performance of superconducting line.
Summary of the invention
The objective of the invention is deficiency, a kind of preparation method that can effectively guarantee the superconducting line barrier layer of grain size and extension property with high purity metal tantalum band is provided at above-mentioned prior art existence.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of metal tantalum belt is characterized in that the steps in sequence of its preparation process comprises:
(1) adopting diameter is the high-purity melting tantalum ingot of 80~120mm, under 500~800 ℃ of temperature, the tantalum ingot is forged into the tantalum metal slabs, and forging process comprises that jumping-up, pulling and bat are flat; Its jumping-up working modulus is 40%~45%, and the pulling working modulus is 45%~50%, and clapping flat working modulus is 40%~50%;
(2) the tantalum metal slabs are dug mill and pickling, cleaning tantalum metal slabs surface;
(3) be rolled, first passage adopts 〉=35% working modulus when rolling, and second passage adopts 〉=30% working modulus, every time working modulus 〉=15% afterwards; The direction that operation of rolling blank prolongs is the axial of starting ingot all the time;
(4) with behind the rolling blank, at the annealing process that carries out of 900~1100 ℃ of insulation 2~2.5h;
(5) adopt argon arc protection welding manner, after blank after the annealing and leader tape welding connection, carry out tension-rolling, preparation tantalum band.
The preparation method of a kind of metal tantalum belt of the present invention, the purity that it is characterized in that described high-purity melting tantalum ingot is greater than 99.98%.
Method of the present invention adopts purity greater than 99.98% high purity metal tantalum ingot, prepares superconducting line barrier layer metal tantalum belt in conjunction with forging, rolling, annealing process, by forging deformation, makes the original coarse-grain of blank obtain the refinement fragmentation; Adopt big working modulus rolling mill practice in conjunction with the rolling initial stage, make finished product band crystal grain obtain abundant refinement, obtain the high-purity tantalum band of fine grain, high-elongation again by Technology for Heating Processing control.The superconducting line barrier layer of preparation has fine grain, high-elongation with high purity metal tantalum band, and thickness range is at 0.4~0.7mm.
The specific embodiment
A kind of preparation method of metal tantalum belt, adopt the metal tantalum ingot of elegant high-purity (purity is at least more than 99.98%), in conjunction with forge, the method for the metal tantalum belt of rolling preparation fine grain and high-elongation, adopt the high-purity melting tantalum ingot of diameter 80~120mm, obtain slab through the upsetting pull forging, mill and the chemical pickling processing through the machinery plane, prepare the tantalum band in conjunction with rolling, Technology for Heating Processing.Its preparation process comprises following process successively: (1) adopts the high-purity melting tantalum ingot of diameter 80~120mm, is forging after the heating under 500~800 ℃ of temperature, and forging process comprises that jumping-up, pulling and bat are flat.The jumping-up working modulus is 40%~45%, and the pulling working modulus is 45%~50%, and clapping flat working modulus is 40%~50%.
(2) dig by machinery and mill and chemical pickling method cleaning tantalum metal slabs surface, wherein the acid solution proportioning is 20%~30%HNO 3+ 5%~15%HF+H 2The O surplus.(3) rolling first pass reduction 〉=35%, the second pass reduction 〉=30%, every time working modulus 〉=15% afterwards; The direction that operation of rolling blank prolongs is the axial of starting ingot all the time.(4) adopt argon arc protection welding manner, before finished product is rolling, blank is connected with the leader tape postwelding and carries out tension-rolling.(5) adopt 900~1100 ℃ of annealing process that are incubated 2~2.5h, can obtain 7~9 grades of grain sizes, percentage elongation is greater than 45% superconducting line barrier layer high purity metal tantalum band.
Embodiment 1
Diameter 110 * 200mm high-purity melting tantalum ingot, in 600 ℃ electric furnace, heat 80min, upset ratio 40% to length 120mm, pull out 50% to length 180mm again, clap flat one-tenth 50 * 170 * 220mm slab, steel slab surface through machinery dig mill and the chemical pickling cleaning after rolling, first passage 40% to thickness 30mm, second passage 30% is rolled down to 2.0mm thickness again to thickness 21mm and carries out tension-rolling to 0.5mm thickness, 8 grades of 980 ℃ of temperature 2.5h annealing of finished product back band grain sizes, percentage elongation reaches 52%, and mechanical performance is shown in Table 1.
The room-temperature mechanical property of table 1 embodiment 1 tantalum band
Tensile strength (Rm) Yield strength (Rp0.2) Percentage elongation (%) Hardness (HV) Grain size
??270MPa ??160MPa ??52 ??90 8 grades
Embodiment 2
Diameter 120 * 250mm high-purity melting tantalum ingot, in 800 ℃ electric furnace, heat 70min, upset ratio 45% to length 137.5mm, pull out 45% to length 199mm again, clap flat one-tenth 50 * 170 * 330mm slab, steel slab surface through machinery dig mill and the chemical pickling cleaning after rolling, first passage 40% to thickness 30mm, second passage 35% to thickness 19.5mm is rolled down to 2mm thickness again, with the argon arc welding mode blank is welded on the leader tape, carry out tension-rolling again to 0.7mm thickness, 1100 ℃ of temperature 2h annealing of finished product back band percentage elongation reaches 54%, 8 grades of grain sizes, and mechanical performance is shown in Table 2.
The room-temperature mechanical property of table 2 embodiment 2 tantalum bands
Tensile strength (Rm) Yield strength (Rp0.2) Percentage elongation (%) Hardness (HV) Grain size
??290MPa ??175MPa ??54 ??87 8 grades
Embodiment 3
Two on diameter 80 * 200mm high-purity melting tantalum ingot, in 500 ℃ of electric furnaces, heat 80min, upset ratio 40% to 120mm, pull out 50% to 180mm again, clap flat one-tenth 40 * 170 * 148mm, steel slab surface through plane mill and the pickling cleaning after, rolling first passage 35% to thickness 26mm, second passage 30% to thickness 18.2mm is rolled down to 2.0mm thickness again, with the argon arc welding mode two blank butt welding is connected into one, carry out tension-rolling again to 0.45mm thickness, 950 ℃ of 2h annealing of finished product back band percentage elongation reaches 49%, 8 grades of grain sizes, and mechanical performance is shown in Table 3.
The room-temperature mechanical property of table 3 embodiment 3 tantalum bands
Tensile strength (Rm) Yield strength (Rp0.2) Percentage elongation (%) Hardness (HV) Grain size
??275MPa ??160MPa ??49 ??86 8 grades

Claims (2)

1. the preparation method of a metal tantalum belt is characterized in that the steps in sequence of its preparation process comprises:
(1) adopting diameter is the high-purity melting tantalum ingot of 80~120mm, under 500~800 ℃ of temperature, the tantalum ingot is forged into the tantalum metal slabs, and forging process comprises that jumping-up, pulling and bat are flat; Its jumping-up working modulus is 40%~45%, and the pulling working modulus is 45%~50%, and clapping flat working modulus is 40%~50%;
(2) the tantalum metal slabs are dug mill and pickling, cleaning tantalum metal slabs surface;
(3) be rolled, first passage adopts 〉=35% working modulus when rolling, and second passage adopts 〉=30% working modulus, every time working modulus 〉=15% afterwards; The direction that operation of rolling blank prolongs is the axial of starting ingot all the time;
(4) with behind the rolling blank, at the annealing process that carries out of 900~1100 ℃ of insulation 2~2.5h;
(5) adopt argon arc protection welding manner, after blank after the annealing and leader tape welding connection, carry out tension-rolling, preparation tantalum band.
2. the preparation method of a kind of metal tantalum belt according to claim 1, the purity that it is characterized in that described high-purity melting tantalum ingot is greater than 99.98%.
CN200910180106A 2009-09-29 2009-09-29 Preparation method of metal tantalum belt Pending CN101670521A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920436A (en) * 2010-08-20 2010-12-22 宁夏东方钽业股份有限公司 Preparation process of tantalum bar for sputtering tantalum ring
CN102251201A (en) * 2011-07-07 2011-11-23 广东省钢铁研究所 Preparation method of high purity nickel wire
CN103240417A (en) * 2013-05-27 2013-08-14 宁夏东方钽业股份有限公司 Tantalum tape and preparation method thereof
WO2014026639A1 (en) * 2012-08-16 2014-02-20 宁夏东方钽业股份有限公司 Method for preparing high-performance tantalum target
CN109666907A (en) * 2017-10-16 2019-04-23 宁波江丰电子材料股份有限公司 Target manufacturing method
CN112410699A (en) * 2020-11-11 2021-02-26 西安诺博尔稀贵金属材料股份有限公司 Method for optimizing grain size and uniformity of tantalum plate

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920436A (en) * 2010-08-20 2010-12-22 宁夏东方钽业股份有限公司 Preparation process of tantalum bar for sputtering tantalum ring
CN101920436B (en) * 2010-08-20 2011-10-26 宁夏东方钽业股份有限公司 Preparation process of tantalum bar for sputtering tantalum ring
CN102251201A (en) * 2011-07-07 2011-11-23 广东省钢铁研究所 Preparation method of high purity nickel wire
CN102251201B (en) * 2011-07-07 2012-10-31 广东省钢铁研究所 Preparation method of high purity nickel wire
WO2014026639A1 (en) * 2012-08-16 2014-02-20 宁夏东方钽业股份有限公司 Method for preparing high-performance tantalum target
US9957603B2 (en) 2012-08-16 2018-05-01 Ningxia Orient Tantalum Industry Co., Ltd. Method for preparing high-performance tantalum target
CN103240417A (en) * 2013-05-27 2013-08-14 宁夏东方钽业股份有限公司 Tantalum tape and preparation method thereof
CN103240417B (en) * 2013-05-27 2016-02-10 宁夏东方钽业股份有限公司 A kind of tantalum band and preparation method thereof
CN109666907A (en) * 2017-10-16 2019-04-23 宁波江丰电子材料股份有限公司 Target manufacturing method
CN112410699A (en) * 2020-11-11 2021-02-26 西安诺博尔稀贵金属材料股份有限公司 Method for optimizing grain size and uniformity of tantalum plate
CN112410699B (en) * 2020-11-11 2022-05-27 西安诺博尔稀贵金属材料股份有限公司 Method for optimizing grain size and uniformity of tantalum plate

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Open date: 20100317