CN103111487B - Preparation method of platinum-coated palladium wire for hot resistance lead - Google Patents

Preparation method of platinum-coated palladium wire for hot resistance lead Download PDF

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Publication number
CN103111487B
CN103111487B CN201310065550.7A CN201310065550A CN103111487B CN 103111487 B CN103111487 B CN 103111487B CN 201310065550 A CN201310065550 A CN 201310065550A CN 103111487 B CN103111487 B CN 103111487B
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platinum
palladium
wire
silk
platinotron
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CN103111487A (en
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李国纲
唐会毅
刘庆宾
吴保安
汪建胜
陈德茂
潘勇
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Chongqing Materials Research Institute Co Ltd
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Chongqing Materials Research Institute Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/42Wire connectors; Manufacturing methods related thereto
    • H01L24/43Manufacturing methods
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42Wire connectors; Manufacturing methods related thereto
    • H01L2224/43Manufacturing methods
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42Wire connectors; Manufacturing methods related thereto
    • H01L2224/44Structure, shape, material or disposition of the wire connectors prior to the connecting process
    • H01L2224/45Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Measuring Temperature Or Quantity Of Heat (AREA)
  • Wire Processing (AREA)

Abstract

The invention relates to a preparation method of a platinum-coated palladium wire for a hot resistance lead. According to the method, through a drawing process of thermal treatment and thermal lamination, a pre-smelted and processed platinum tube and palladium bar are assembled, and in combination with a sufficient annealing heat treatment process and through uniform deformation processing, the assembly is made into the platinum-coated palladium wire which replaces an expensive pure platinum wire as a hot resistance thermometer lead applied to a platinum hot resistance thermometer. An envelope layer of the platinum palladium wire prepared by the method is compact, uniform and continuous, is not prone to crack and is high in bonding strength; and when replacing the expensive pure platinum wire as the hot resistance thermometer lead applied to the platinum hot resistance thermometer, the platinum palladium wire is free from any influence on thermoelectric properties. The platinum palladium wire has good overall characteristics of wide use temperature zone, high temperature measurement accuracy, high stability, good reproducibility and the like, thus becoming a most important resistance temperature measuring element with a highest use level in current industry. The method has the advantages of simple process and low production cost.

Description

A kind of thermal resistance lead-in wire is with covering platinum palladium silk preparation method
Technical field
The present invention relates to a kind of preparation method of thermal resistance lead material, particularly a kind of thermal resistance lead-in wire preparation method covering platinum palladium silk.
Background technology
Along with continuous progress and the upgrading of China's industrial technology, as therm-param method technology and the high new information industry sustained and rapid development of one of the key technology of all fields of national economy, increasing to the demand of platinum-group noble metals material.Platinum is as the thermal resistance lead material of extensive use the most in the world, its physics, chemical property are good, there is use wide temperature region, temperature measurement accuracy is high, thermoelectricity capability is stable and antioxygenic property is good, repdocutbility is good, long service life, be applicable in oxidisability and inert atmosphere, the temperature being widely used in the fields such as metallurgy, petrochemical industry, Aeronautics and Astronautics, metering controls and measures.But the shortcomings such as platinum is expensive, resource scarcity make it apply to be restricted.Therefore in the urgent need to a kind of performance meeting the requirement of platinum resistance thermometer sensor, element, the pure platinum filament lead-in wire of material substitution platinum resistance thermometer sensor, cheap compared with platinum in price.
Cover the instead expensive pure platinum filament of platinum palladium silk (FPT) and make thermal resistance thermometer lead-in wire, its platinum thermal resistance thermometer performance is not affected, and the consumption of platinum accounts for about 12% of total amount, serve the consumption saving platinum, thus greatly reduce the cost of platinum thermal resistance thermometer.
Cover platinum palladium silk be on palladium silk evenly, parcel one deck alloy platinum material continuously, form a complete entirety.In real work, adopt as method preparations such as powder metallurgic method, chemical plating, plating, magnetron sputtering method, machinery parcels, these method complex process, cost are high, and due to the defect such as not fine and close, the easy cracking of its binder course, bond strength be low, cause product quality to decline.
Summary of the invention
The object of this invention is to provide a kind of thermal resistance lead-in wire preparation method covering platinum palladium silk, the integument of the platinum palladium silk adopting the method to prepare is fine and close, even, continuous, not easy to crack and bond strength is high, instead expensive pure platinum filament makes thermal resistance thermometer lead-in wire for platinum thermal resistance thermometer, its thermoelectricity capability is not affected, have use wide temperature region, the good overall characteristic such as temperature measurement accuracy is high, stability is high, repdocutbility is good and become current industrial most important, resistance temperature measurement element that consumption is maximum.The method has the advantage that technique is simple, production cost is low.
Technical scheme of the present invention is as follows:
The thermal resistance lead-in wire preparation method covering platinum palladium silk, described thermal resistance lead-in wire is made up of the pure platinum of skin, middle continuous, uniform transition zone platinum palladium and the pure palladium of internal layer with covering platinum palladium silk, and its preparation method has following steps:
1) get platinum ingot, through forge hot with cold rolling become thickness be the platinum plate of 0.6 ~ 1.0mm, roll into platinotron 1 under annealed state, shaping;
2) the pipe seam oxygen-hydrogen welding welding of step 1) gained platinotron 1, weld seam shaping, drawbench is drawn into the regular platinotron of shape 2, and cleans;
3) get palladium ingot, through forge hot with cold rolling become palladium rod, be drawn into palladium silk, cleaning;
4) by described in step 3) palladium silk load step 2) gained platinotron 2 in, obtain assembly, according to the passage machining deformation amount homogeneous deformation drawing of 10% ~ 35%, the diameter to assembly be φ 2mm ~ 4.5mm platinum palladium rod;
5) the platinum palladium rod described in step 4) is placed in high-temperature annealing furnace and heat-treats, and being the even drawing of 10% ~ 20% passage machining deformation amount according to deflection, is φ 0.05mm ~ 0.2mm to its diameter, obtains thermal resistance lead-in wire with covering platinum palladium silk.
Described platinum material purity >=99.95%, palladium material purity >=99.95%.
The consumption of the palladium silk described in step 3) is 85% ~ 90% of platinum palladium silk gross weight.
Heat treatment described in step 5) is in the lehr, and under argon atmosphere, temperature is 1450 DEG C ~ 1550 DEG C, the abundant annealing in process of insulation 1 ~ 2h.
The method of the invention by heat treatment, the laminating drawing process of heat by melting in advance, the platinotron processed and the assembling of palladium rod with in conjunction with abundant annealing heat treatment process, processed by homogeneous deformation, make and replace expensive pure platinum filament to make thermal resistance thermometer lead-in wire covering platinum palladium silk on platinum thermal resistance thermometer, greatly save the consumption of platinum, reduce the cost of platinum thermal resistance thermometer.The method of the invention is adopted to obtain thermal resistance lead-in wire with covering platinum palladium silk, intermediate layer is by heat treatment, hot laminating technique, form a floor height densification, continuous uniform, transition zone that bond strength is high, therefore, described its thermoelectricity capability of platinum palladium silk that covers is not affected, and has the overall characteristic that such as to use that wide temperature region, temperature measurement accuracy are high, stability is high, repdocutbility is good etc. good.
Method production technology described in this patent is simple, and cost is low.
Thermal resistance lead-in wire of the present invention is with covering platinum palladium silk, its structure is outer is pure platinum, and intermediate layer is continuously, uniform transition zone platinum palladium, and internal layer is pure palladium, namely pure platinum, platinum palladium, pure palladium is arranged as successively from outside to inside, its outer layer covers intermediate layer, intermediate layer wrapping inner layer.
Below in conjunction with embodiment, the present invention is further illustrated, but therefore do not limit the present invention among described scope of embodiments.
Detailed description of the invention
embodiment 1
Get spongy platinum (purity >=99.95%), platinum ingot is prepared in high-frequency induction melting, forge hot under 1300 DEG C of annealing temperatures, more cold rolling one-tenth 1.0mm platinum plate, finishing platinum plate surface, remove the defects such as burr, carry out rolling into internal diameter φ 10.0mm platinotron 1 after annealing, pipe seam adopts oxygen-hydrogen welding welding, carries out commissure finishing, the platinotron 2 that the shape of φ 7.0mm is regular is drawn to subsequently on drawbench, stand-by after clean;
Palladium powder (purity >=99.95%) is pressed into palladium block, carries out Medium frequency induction melting and prepare palladium ingot, forge hot under 1200 DEG C of annealing temperatures, and cold rolling one-tenth palladium is excellent, palladium rod is drawn into the palladium silk of φ 6.0mm size on drawbench.Alignment palladium silk, according to platinotron weight portion 10 parts, palladium silk weight portion 90 parts of proportionings, an assembly is become by loading in above-mentioned platinotron through the palladium silk of cleaning, rope type drawbench carries out distortion drawing processing according to the even machining deformation amount of the passage of 35%, until the platinum palladium rod of φ 4.5mm size is made in drawing, platinum palladium rod is placed in high-temperature annealing furnace, abundant annealing in process is carried out under argon atmosphere, temperature is 1550 DEG C, insulation 1h, be that 20% passage machining deformation amount carries out homogeneous deformation drawing processing to platinum palladium rod according to deflection again, to the diameter phi 0.2mm of platinum palladium rod, namely binder course fine and close is continuously obtained, the thermal resistance lead-in wire of excellent combination property is with covering platinum palladium silk.
embodiment 2
Except following content, the other the same as in Example 1.
Carry out high frequency melting to spongy platinum and prepare platinum ingot, cold rolling one-tenth 0.8mm platinum plate, rolls into internal diameter φ 8.0mm platinotron, drawbench is drawn to the platinotron that the shape of φ 5.0mm is regular; Palladium rod after cold rolling, drawbench is drawn into the palladium silk of φ 4.0mm size.Platinum palladium assembly carries out homogeneous deformation drawing processing according to platinotron weight portion 15 parts, the passage machining deformation amount of palladium silk weight portion 85 parts of proportional quantities according to 10% on rope type drawbench, until drawing makes closely knit assembly to obtain the platinum palladium rod of φ 2.0mm size, platinum palladium rod is at 1450 DEG C, insulation 2h carries out abundant annealing in process, be that 10% passage machining deformation amount is carried out homogeneous deformation drawing and is machined to required φ 0.05mm size to platinum palladium rod according to deflection again, namely obtain binder course fine and close continuously, excellent combination property thermal resistance lead-in wire with covering platinum palladium silk.
embodiment 3
Except following content, the other the same as in Example 1.
Carry out high frequency melting to spongy platinum and prepare platinum ingot, cold rolling one-tenth 0.6mm platinum plate, rolls into internal diameter φ 6.0mm platinotron, drawbench is drawn to the platinotron that the shape of φ 4.0mm is regular; Palladium rod after cold rolling, drawbench is drawn into the palladium silk of φ 3.0mm size.Platinum palladium assembly carries out homogeneous deformation drawing processing according to platinotron weight portion 12 parts, the passage machining deformation amount of palladium silk weight portion 88 parts of proportional quantities according to 20% on rope type drawbench, until drawing makes closely knit assembly to obtain the platinum palladium rod of φ 3.0mm size, platinum palladium rod is incubated 1.5h and carries out abundant annealing in process at 1500 DEG C, being that 15% passage machining deformation amount is carried out homogeneous deformation drawing and is machined to required φ 0.1mm size to platinum palladium rod according to deflection again, namely obtaining the thermal resistance lead-in wire of excellent combination property with covering platinum palladium silk.
The thermal resistance lead-in wire of Example 1-3 gained carries out electric performance test with covering platinum palladium silk, and the resistance ratio that all can meet GB/T5977-1999 standard pertinent resistances thermometer platinum filament requires and calibration requirement, and its resistance ratio meets R 100/ R 0=1.3850 and tolerance requirements, under annealed state, tensile strength values is 210MPa, and the bending number of times under annealed state is 16 times, and performance all reaches or exceeded the mechanical property of pure platinum lead-in wire, meets the application function of thermal resistance lead-in wire.

Claims (3)

1. thermal resistance lead-in wire is by the preparation method covering platinum palladium silk, it is characterized in that, described thermal resistance lead-in wire is made up of the pure platinum of skin, middle continuous, uniform transition zone platinum palladium and the pure palladium of internal layer with covering platinum palladium silk, and its preparation method has following steps:
1) get platinum ingot, through forge hot with cold rolling become thickness be the platinum plate of 0.6 ~ 1.0mm, roll into platinotron 1 under annealed state, shaping;
2) the pipe seam oxygen-hydrogen welding welding of step 1) gained platinotron 1, weld seam shaping, drawbench is drawn into the regular platinotron of shape 2, cleaning;
3) get palladium ingot, through forge hot with cold rolling become palladium rod, be drawn into palladium silk, cleaning;
4) by described in step 3) palladium silk load step 2) gained platinotron 2 in, obtain assembly, according to the passage machining deformation amount homogeneous deformation drawing of 10% ~ 35%, the diameter to assembly be φ 2mm ~ 4.5mm platinum palladium rod;
5) the platinum palladium rod described in step 4) is placed in high-temperature annealing furnace; under argon atmosphere; temperature is 1450 DEG C ~ 1550 DEG C; insulation 1 ~ 2h heat-treats; be the even drawing of 10% ~ 20% passage machining deformation amount according to deflection; being φ 0.05mm ~ 0.2mm to its diameter, obtaining thermal resistance lead-in wire with covering platinum palladium silk.
2. method according to claim 1, is characterized in that: described platinum ingot purity >=99.95%, palladium ingot purity >=99.95%.
3. method according to claim 1, is characterized in that: the consumption of the palladium silk described in step 3) is 85% ~ 90% of platinum palladium silk gross weight.
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CN107579010B (en) * 2017-07-31 2020-06-30 昆明贵金属研究所 Method for improving binding force of gold-silver composite bonding wire coating and core material
CN114309125A (en) * 2021-12-29 2022-04-12 英特派铂业股份有限公司 Preparation method of platinum-platinum rhodium composite wire

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DE3832342C1 (en) * 1988-09-23 1989-07-20 W.C. Heraeus Gmbh, 6450 Hanau, De Platinum-jacketed wire, method for production of a platinum-jacketed wire and use of a platinum-jacketed wire
CN1504283A (en) * 2002-11-28 2004-06-16 贵研铂业股份有限公司 Method for producing composite silver copper yarn and composite silver zinc paktong yarn
CN1526546A (en) * 2003-09-23 2004-09-08 贵研铂业股份有限公司 Composit Pd-containing material wire and its prepn and use
CN1868049A (en) * 2003-10-20 2006-11-22 住友电气工业株式会社 Bonding wire and integrated circuit device using the same
CN101707083A (en) * 2009-12-15 2010-05-12 中国科学院电工研究所 Iron-based compound superconducting wire or tape prepared from silver sheath

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