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CN102974793A - Method and equipment for continuously producing high-purity single crystal copper - Google Patents

Method and equipment for continuously producing high-purity single crystal copper Download PDF

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Publication number
CN102974793A
CN102974793A CN2012105266820A CN201210526682A CN102974793A CN 102974793 A CN102974793 A CN 102974793A CN 2012105266820 A CN2012105266820 A CN 2012105266820A CN 201210526682 A CN201210526682 A CN 201210526682A CN 102974793 A CN102974793 A CN 102974793A
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copper
furnace
equipment
purity
raw material
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黄圆圆
付亚波
崔静
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Taizhou University
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Taizhou University
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Abstract

一种连续制备高纯单晶铜的设备与方法,属于新材料制备技术领域。本制备高纯单晶铜的设备包括电子束熔炼炉、水平连铸设备、液位控制块、保温结晶器、牵引设备等。方法是剪切后的4N铜阴极板通过原料运输辊道运入电子束熔炼炉,在石墨舟上进行熔炼和提纯;提纯后的铜熔体通过导流管直接流入水平连铸炉的保温炉,炉内通入保护气体氮气,防止氧化;铜熔体经过保温结晶器和冷却设备,形成具有定向凝固组织的单晶铜线坯;线坯经过牵引设备的牵引,实现了连续生产。本发明所涉及的设备及方法,可实现连续制备高纯单晶铜线坯,具有成本低廉、无污染、易自动控制等优点,所制备的铜线坯既具有高纯又具有单晶的性能,适用于制备IC封装材料的键合丝等材料。

A device and method for continuously preparing high-purity single-crystal copper belong to the technical field of new material preparation. The equipment for preparing high-purity single crystal copper includes electron beam melting furnace, horizontal continuous casting equipment, liquid level control block, heat preservation crystallizer, traction equipment and so on. The method is that the sheared 4N copper cathode plate is transported into the electron beam melting furnace through the raw material transport roller table, and then smelted and purified on the graphite boat; the purified copper melt flows directly into the holding furnace of the horizontal continuous casting furnace through the draft tube , The protective gas nitrogen is introduced into the furnace to prevent oxidation; the copper melt passes through the heat preservation crystallizer and cooling equipment to form a single crystal copper wire blank with directional solidification structure; the wire blank is pulled by the traction equipment to realize continuous production. The equipment and method involved in the present invention can realize the continuous preparation of high-purity single-crystal copper wire blanks, and has the advantages of low cost, no pollution, easy automatic control, etc., and the prepared copper wire blanks have both high-purity and single-crystal properties , suitable for the preparation of bonding wire and other materials for IC packaging materials.

Description

The method and apparatus of the high-purity single crystal Cu of a kind of continuous production
Technical field
The invention belongs to technical field of new material preparation, relate to the method and apparatus of the high-purity single crystal Cu of a kind of continuous production.
Background technology
The contained impurity of high purity copper (purity that refers to copper is 5N-6N, i.e. 99.999%-99.9999%) is considerably less, thereby has good electric conductivity, thermal conductivity, ductility and good processing characteristics.
The characteristic of the existing high purity copper of high-purity single crystal Cu, the characteristic that has again single crystal Cu, various tie lines and the used for electronic packaging that can apply to endurance cable, high conductive cable and electric wire, flexible cable, electronics industry are good for zygonema, high-fidelity acoustics wire rod, ultra tiny enamel-covered wire, miniature coils, high frequency coil etc.Be used as the endurance cable such as high-purity single crystal Cu, has the well performance of anti-repeatedly bend tension, can guarantee millwork people's normal operation, the service life that simultaneously can greatly improve robot, because industrial robot will be finished exercises, need to carry out a large amount of repeating motions, and transmit instruction, a large amount of cable transmission signal of control needs, the some of them cable will rotate along with the rotation of mechanical arm, and this just needs these cables that very high fatigue performance is arranged.Simultaneously, it also can be used as the transmission cable of miniature sniffing robot.
At present, the production of domestic many gold bonding silks and encapsulation enterprise begin to attempt carrying out the production of copper bonding wire one after another, and the main preparation technology who adopts the preparation single crystal Cu is such as the gloomy lattice in Jiaozhuo, Changshu China one microelectronics, the long electricity in Jiangyin, day wawter bloom sky etc.Copper bonding wire quality or the quantity of producing at present all can not satisfy domestic market demand, and particularly the low ultra-fine bonding wire of radian mainly depends on import, and its finished product is mainly from developed country's imports such as the U.S., Japan.
The enterprise of domestic production high purity copper such as Jinchuan Non-ferrous Metals Company can production purity 6N high purity coppers, because carry out die casting after adopting electronic beam vacuum smelting, can only produce short ingot casting again, can not produce continuously.And the companies such as Jiaozhuo Sen Ge adopt horizontal continuous casting technology produce single crystal copper cash, can produce continuously, but can not produce the above high purity copper wire rod of 5N.For this reason, researcher both domestic and external begins one's study and can prepare continuously existing high-purity characteristic, again preparation method and the equipment of high-purity single crystal copper wires of monocrystalline performance arranged.
Chinese patent " a kind of method for preparing ultrapure copper ", publication number 101280430 is that Chinese Jinchuan Non-ferrous Metals Company adopts nitric acid system electrolysis, electronic torch melting to combine and prepare the method for 6N high purity copper.Be characterized in take 6N electrolysis copper coin as raw material, obtain the high-purity copper ingot of 6N through electronic torch melting, satisfy the requirement of copper sputtering target material.Glow discharge spectrometry--GDMS analyzes 18 kinds of impurity elements in employing, adopts the decrement percentage composition to calculate the purity of high purity copper.The shortcoming of this technology is to realize continous way production.
Chinese patent " a kind of device and method for preparing high purity copper ", publication number 102031394A is that Dalian University of Technology adopts the direct directional solidification of electronic torch melting to prepare the device and method of high purity copper.Be characterized in adopting that electronic torch melting and directional solidification are integrated, the electromagnetic purification technology, after repeatedly purifying, high-purity copper ingot of preparation can reach 6N.The shortcoming of this technology is to realize continous way production, is only suitable for adopting die casting to prepare high-purity copper ingot.
Japan Patent " manufacture method of high-purity copper, Unexamined Patent 4-365888 " and Japan Patent " manufacture method of high-purity copper, Unexamined Patent 6-173063 ", the method for employing electrolytic preparation 6N cathode copper.Its anode is cathode copper, and the cathode sheath diaphragm bag adopts the method for ion-exchange to remove impurity element in the electrolyte, obtains the high pure electrolytic copper plate of 6N (99.9999%).
Calendar year 2001, in the Master's thesis that Gansu Polytechnical Univ's fourth ancestor richness is write " experimental study of the standby copper single crystal body of continuous casting of single crystal legal system ", be developed into voluntarily a horizontal continuous casting of single crystal equipment, the appearance that successfully produces diameter of phi 6mm, long 9-30m is the monocrystalline wire rod of minute surface; Grasp and progressively solved the key technology of this technology in device design and technological operation by engineer testing.
2008, the Master's thesis that Lanzhou University of Science ﹠ Technology's Cao Wen brightness is write " single crystal Cu prepares the performance study of bonding wire ", the performance that adopts single crystal Cu to prepare bonding wire is studied, by the single crystal Cu of traditional handicraft preparation is produced the finishing analysis that broken string carries out system drawing the ultra-fine bonding silk, improve the preparation technology of single crystal Cu bar and its quality is tested.Having studied the preparation wire diameter is the high-quality single crystal Cu bar of Φ 8mm microstructure change in orientation and performance variation law under different cold drawing states.It is the bonding wire of Φ 0.050mm that the high-quality single crystal Cu that adopts test to prepare has prepared wire diameter.
In present existing technology of preparing, Main Problems is: can adopt the method for discontinuous formula to prepare high purity copper, but can not prepare single crystal Cu; And when adopting continuation method to prepare single crystal Cu, then can not prepare high purity copper.Therefore, the needs exploitation is a kind of can prepare high-purity method and apparatus that can prepare again the continous way of single crystal Cu.
Summary of the invention
The present invention is directed to the deficiency that exists in the above-mentioned prior art, provide a kind of 4N copper cathode sheets take market sale as raw material, the processing technology of solidifying, draw through sealing charging, transportation, electronic torch melting, electron beam melting purification, horizontal orientation can continuous production has the method and apparatus of the copper blank of high-purity and monocrystalline performance.
The technical solution adopted in the present invention is:
With the 4N copper cathode sheets of selling on the market, because impurity and oxygen content are higher, poor-performing needs to purify and is prepared into the tissue of monocrystalline.The 4N copper cathode sheets is cut into strip, through the position of roller transport to electron beam work, through electronic torch melting and two operations of electron beam purification, copper melts is by high purity graphite boat and mozzle, flow in the holding furnace, be provided with temperature, liquid level automatic checkout equipment in the holding furnace, can automatically control the temperature of melt and the height of liquid level.Through insulation crystallizer and cooling device, blank is solidified with oriented approach, form the blank with oriented freezing organization.Pulling equipment involves the blank that solidifies, and can realize continuously and steady production.This technology will prepare high pure metal and obtain single crystal organization to be combined, and develops a kind ofly can prepare high-purity Apparatus and method for that can prepare again the continous way of single crystal Cu.
The equipment that the present invention prepares high-purity single crystal Cu comprises that holding furnace, liquid level controll block, insulation crystallizer, cooling device, pulling equipment and the raw material conveyor roller of electron beam furnace, horizontal continuous casting furnace consist of.Have friction feeding, laser heating, quantity-produced characteristics, automaticity is higher.
The method of the high-purity single crystal Cu of manufacturing that the present invention relates to may further comprise the steps:
Step 1: the 4N copper cathode sheets after the shearing is transported into electron beam furnace by the raw material conveyor roller, is evacuated to 10 -2-10 -3During Pa, start electron gun bombardment copper billet, carry out melting and purification at graphite boat;
Step 2: the copper melts after the purification flows directly into the holding furnace of horizontal continuous casting furnace by mozzle, passes into protective gas nitrogen in the stove, anti-oxidation;
Step 3: copper melts forms the monocrystalline copper cash base with oriented freezing organization through insulation crystallizer and cooling device;
Step 4: the line base has been realized continuous production through the traction of pulling equipment;
Step 5: above-mentioned steps combined to realize serialization production, can obtain the copper cash base of endless, not only have high-purity but also have the performance of monocrystalline.
Advantage of the present invention is with electronic torch melting and purification, directional solidification are purified and horizontal casting is combined, the copper cash base of preparation has the low characteristics of high-purity, single crystal organization and oxygen content, the pollution to environment can be effectively avoided, low cost, endless and high efficient production can be realized.
Description of drawings
Fig. 1 is the equipment schematic diagram of the high-purity single crystal Cu of preparation.
Among Fig. 1: 1 copper cash base; 2 pulling equipments; 3 cooling devices; 4 insulation crystallizer overcoats; 5 crystallizer heating jackets; 6 insulation crystallizers; The heating jacket of 7 horizontal stoves; The holding furnace of 8 horizontal stoves; 9 level control pieces; 10 electron beam furnaces; 11 feed(raw material)inlets; 12 raw material conveying tracks; 13 raw materials; 14 graphite boats; Liquation behind 15 electron-beam meltings; 16 mozzles; The liquation of 17 holding furnaces
The specific embodiment
Describe specific embodiments of the invention in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
4N copper cathode sheets 13 adds acetone soln with ultrasonic wave and cleans through after shearing, and rinses post-drying with deionized water again; Copper billet is transported to electron beam furnace 10 by feed(raw material)inlet 11 by raw material conveying track 12, and raw material carries out melting and purification at graphite boat 14, forms copper melts 15, and temperature is 1200 ℃; Copper melts flows into mozzle 16 under the effect of 2 degree inclination component, enter the holding furnace 8 of horizontal continuous casting furnace, forms the melt 17 of holding furnace, and the steady temperature of holding furnace is provided in photothermal mode by heating jacket 7; Under the regulating action of level control piece 9, guarantee that liquid level and crystallizer height are more than 300mm; Melt enters insulation crystallizer 6 under the static pressure effect; 4 energisings of insulation crystallizer overcoat, heating jacket 5 are made by graphite, make melt temperature constant about 1100 ℃ by radiation; Cooling device 3 startings make the blank directional solidification, form oriented freezing organization; Pulling equipment 2 startings, the blank 1 that will solidify involves, and realizes producing continuously high line monocrystalline copper cash base.Higher front 22 kinds of impurity elements of content by analysis, the purity of decrement percentage composition is 5N to 6N.
Embodiment 2
4N copper cathode sheets 13 adds acetone soln with ultrasonic wave and cleans through after shearing, and rinses post-drying with deionized water again; Copper billet is transported to electron beam furnace 10 by feed(raw material)inlet 11 by raw material conveying track 12, and raw material carries out melting and purification at graphite boat 14, forms copper melts 15, and temperature is 1250 ℃; Copper melts flows into mozzle 16 under the effect of 3 degree inclination component, enter the holding furnace 8 of horizontal continuous casting furnace, forms the melt 17 of holding furnace, and the steady temperature of holding furnace is provided in photothermal mode by heating jacket 7; Under the regulating action of level control piece 9, guarantee that liquid level and crystallizer height are more than 300mm; Melt enters insulation crystallizer 6 under the static pressure effect; 4 energisings of insulation crystallizer overcoat, heating jacket 5 are made by graphite, make melt temperature constant about 1150 ℃ by radiation; Cooling device 3 startings make the blank directional solidification, form oriented freezing organization; Pulling equipment 2 startings, the blank 1 that will solidify involves, and realizes producing continuously high line monocrystalline copper cash base.Higher front 22 kinds of impurity elements of content by analysis, the purity of decrement percentage composition is 5N to 6N.

Claims (6)

1. the equipment of the high-purity single crystal Cu of continuous production, this equipment comprise holding furnace, liquid level controll block, insulation crystallizer, cooling device, pulling equipment and the raw material conveyor roller etc. of electron beam furnace, horizontal continuous casting furnace, it is characterized in that:
The 4N copper billet is by feed(raw material)inlet (11), be transported to electron beam furnace (10) by raw material conveying track (12), raw material carries out melting and purification at graphite boat (14), copper melts is under the effect of 2 degree inclination component, flow into mozzle (16), enter the holding furnace (8) of horizontal continuous casting furnace, the steady temperature of holding furnace is provided in photothermal mode by heating jacket (7); Under the adjusting of level control piece (9), melt enters insulation crystallizer (6) under the static pressure effect; Insulation crystallizer overcoat (4) energising, heating jacket (5) makes melt temperature constant by radiation; Cooling device (3) starting makes blank form oriented freezing organization; Pulling equipment 2 startings, the blank 1 that will solidify involves, and realizes producing continuously high-purity monocrystalline copper cash base.
2. equipment according to claim 1 is further characterized in that, raw material conveyor roller (12) connects with electron beam furnace (10), is satisfying the continuous adding that has realized raw material under the vacuum condition, is fit to extensive, continous way production.
3. equipment according to claim 1, be further characterized in that, copper melts after electron beam furnace (10) is purified is directly entered the holding furnace (8) of horizontal continuous casting furnace by graphite boat (14) and mozzle (16), graphite boat (14) has certain angle with horizontal plane, the assurance copper melts can be realized abundant purification, can automatically flow into again.
4. equipment according to claim 1 is further characterized in that, the steady temperature of the holding furnace of horizontal continuous casting furnace (8) is provided in photothermal mode by heating jacket (7), guarantees that the temperature of copper melts maintains certain limit, to finish casting.
5. equipment according to claim 1 is further characterized in that, the steady temperature of insulation crystallizer (6) is kept with photothermal form by heating jacket (5), satisfies the requirement of directional solidification.
6. utilize claim 1,2,3,4,5 described equipment to prepare the method for high-purity single crystal Cu, its feature comprises following steps:
Step 1: the 4N copper cathode sheets after the shearing is transported into electron beam furnace by the raw material conveyor roller, is evacuated to 10 -2-10 -3During Pa, start electron gun bombardment copper billet, carry out melting and purification at graphite boat;
Step 2: the copper melts after the purification flows directly into the holding furnace of horizontal continuous casting furnace by mozzle, passes into protective gas nitrogen in the stove, anti-oxidation;
Step 3: copper melts forms the monocrystalline copper cash base with oriented freezing organization through insulation crystallizer and cooling device;
Step 4: the line base has been realized continuous production through the traction of pulling equipment;
Step 5: above-mentioned steps combined to realize serialization production, can obtain the copper cash base of endless, not only have high-purity but also have the performance of monocrystalline; Higher front 22 kinds of impurity elements of content by analysis, the purity of decrement percentage composition is 5N to 6N.
CN2012105266820A 2012-12-10 2012-12-10 Method and equipment for continuously producing high-purity single crystal copper Pending CN102974793A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561865A (en) * 2014-12-31 2015-04-29 安徽森海高新电材有限公司 Preparation method of material for high-strength and high-conductivity copper lead
CN104575874A (en) * 2014-12-31 2015-04-29 安徽森海高新电材有限公司 Method for manufacturing high-conductivity corrosion-resistant pure copper special cable
CN106077535A (en) * 2016-07-14 2016-11-09 深圳市烯世传奇科技有限公司 A kind of method of Graphene modification single crystal Cu
CN106623830A (en) * 2017-03-21 2017-05-10 江苏省冶金设计院有限公司 Single-roll production device and method for copper alloy bar
CN106735032A (en) * 2016-12-14 2017-05-31 江苏亨通精工金属材料有限公司 Nitrogen guard method and its corresponding structure for SCR methods cast copper cash base
CN107460536A (en) * 2017-08-24 2017-12-12 武陟吉铨特种金属材料有限公司 A kind of method of heat type molding V-type continuously casting single crystal Cu
CN107537988A (en) * 2017-08-22 2018-01-05 上海电缆研究所有限公司 Electric wire long length high purity copper rod of metal alloy base horizontally continuously casting device and casting technique
CN108543933A (en) * 2018-04-19 2018-09-18 重庆赛宝工业技术研究院 The method and system of irregular lump material dynamic continuous production magnesium alloy
CN109093088A (en) * 2018-10-12 2018-12-28 兰州理工大学 A kind of monocrystalline copper sheet preparation facilities and preparation method
CN113828744A (en) * 2021-09-08 2021-12-24 湖州金钛导体技术有限公司 Intelligent continuous casting system and continuous casting method
CN113930625A (en) * 2021-11-11 2022-01-14 东莞市单晶电子科技有限公司 Multilayer centrifugal high-purity single crystal copper reduction furnace and smelting method
CN114318001A (en) * 2021-12-16 2022-04-12 虹华科技股份有限公司 Vacuum smelting furnace for purifying high-purity oxygen-free copper

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US6589474B1 (en) * 1999-06-28 2003-07-08 Korea Institute Of Machinery And Materials One-body horizontal continuous casting apparatus and methods of deoxidation, and refining of phosphorized copper using said apparatus
CN1483532A (en) * 2002-09-04 2004-03-24 上海中鑫空调管有限公司 Subcurrent type oxygen-free copper horizontal continuous casting technology and production eguipment thereof
CN102031394A (en) * 2010-12-27 2011-04-27 大连理工大学 Device and method for preparing high-purity copper

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
US6589474B1 (en) * 1999-06-28 2003-07-08 Korea Institute Of Machinery And Materials One-body horizontal continuous casting apparatus and methods of deoxidation, and refining of phosphorized copper using said apparatus
CN2550097Y (en) * 2002-05-31 2003-05-14 广东工业大学 Hot continuous cast furnace
CN1483532A (en) * 2002-09-04 2004-03-24 上海中鑫空调管有限公司 Subcurrent type oxygen-free copper horizontal continuous casting technology and production eguipment thereof
CN102031394A (en) * 2010-12-27 2011-04-27 大连理工大学 Device and method for preparing high-purity copper

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104575874A (en) * 2014-12-31 2015-04-29 安徽森海高新电材有限公司 Method for manufacturing high-conductivity corrosion-resistant pure copper special cable
CN104561865B (en) * 2014-12-31 2017-06-16 安徽森海高新电材有限公司 A kind of preparation method of high-strength highly-conductive pure copper wire material
CN104561865A (en) * 2014-12-31 2015-04-29 安徽森海高新电材有限公司 Preparation method of material for high-strength and high-conductivity copper lead
CN106077535B (en) * 2016-07-14 2018-06-29 深圳市烯世传奇科技有限公司 A kind of method that graphene is modified single crystal Cu
CN106077535A (en) * 2016-07-14 2016-11-09 深圳市烯世传奇科技有限公司 A kind of method of Graphene modification single crystal Cu
CN106735032A (en) * 2016-12-14 2017-05-31 江苏亨通精工金属材料有限公司 Nitrogen guard method and its corresponding structure for SCR methods cast copper cash base
CN106623830A (en) * 2017-03-21 2017-05-10 江苏省冶金设计院有限公司 Single-roll production device and method for copper alloy bar
CN107537988A (en) * 2017-08-22 2018-01-05 上海电缆研究所有限公司 Electric wire long length high purity copper rod of metal alloy base horizontally continuously casting device and casting technique
CN107460536A (en) * 2017-08-24 2017-12-12 武陟吉铨特种金属材料有限公司 A kind of method of heat type molding V-type continuously casting single crystal Cu
CN108543933A (en) * 2018-04-19 2018-09-18 重庆赛宝工业技术研究院 The method and system of irregular lump material dynamic continuous production magnesium alloy
CN108543933B (en) * 2018-04-19 2023-11-03 重庆赛宝工业技术研究院有限公司 Method and system for dynamically and continuously producing magnesium alloy from irregular block materials
CN109093088A (en) * 2018-10-12 2018-12-28 兰州理工大学 A kind of monocrystalline copper sheet preparation facilities and preparation method
CN113828744A (en) * 2021-09-08 2021-12-24 湖州金钛导体技术有限公司 Intelligent continuous casting system and continuous casting method
CN113930625A (en) * 2021-11-11 2022-01-14 东莞市单晶电子科技有限公司 Multilayer centrifugal high-purity single crystal copper reduction furnace and smelting method
CN114318001A (en) * 2021-12-16 2022-04-12 虹华科技股份有限公司 Vacuum smelting furnace for purifying high-purity oxygen-free copper

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Application publication date: 20130320