US20060144485A1 - Metal structure and method for production thereof - Google Patents

Metal structure and method for production thereof Download PDF

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Publication number
US20060144485A1
US20060144485A1 US10/546,824 US54682405A US2006144485A1 US 20060144485 A1 US20060144485 A1 US 20060144485A1 US 54682405 A US54682405 A US 54682405A US 2006144485 A1 US2006144485 A1 US 2006144485A1
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US
United States
Prior art keywords
temperature
annealing
crystals
metal structure
contact probe
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US10/546,824
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English (en)
Inventor
Kazunori Okada
Yoshihiro Hirata
Shinji Inazawa
Masao Sakuta
Yoshiaki Tani
Teruhisa Sakata
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Assigned to SUMITOMO ELECTRIC INDUSTRIES, LTD. reassignment SUMITOMO ELECTRIC INDUSTRIES, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HIRATA, YOSHIHIRO, INAZAWA, SHINJI, OKADA, KAZUNORI, SAKATA, TERUHISA, SAKUTA, MASAO, TANI, YOSHIAKI
Publication of US20060144485A1 publication Critical patent/US20060144485A1/en
Assigned to SUMITOMO ELECTRIC INDUSTRIES, LTD. reassignment SUMITOMO ELECTRIC INDUSTRIES, LTD. RE-RECORD TO CORRECT THE ASSIGNEE'S ADDRESS ON A DOCUMENT PREVIOUSLY RECORDED AT REEL 017689, FRAME 0133. (ASSIGNMENT OF ASSIGNOR'S INTEREST) Assignors: HIRATA, YOSHIHIRO, INAZAWA, SHINJI, OKADA, KAZUNORI, SAKATA, TERUHISA, SAKUTA, MASAO, TANI, YOSHIAKI
Priority to US12/399,589 priority Critical patent/US8052810B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R1/00—Details of instruments or arrangements of the types included in groups G01R5/00 - G01R13/00 and G01R31/00
    • G01R1/02—General constructional details
    • G01R1/06—Measuring leads; Measuring probes
    • G01R1/067—Measuring probes
    • G01R1/06711—Probe needles; Cantilever beams; "Bump" contacts; Replaceable probe pins
    • G01R1/06755—Material aspects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R1/00—Details of instruments or arrangements of the types included in groups G01R5/00 - G01R13/00 and G01R31/00
    • G01R1/02—General constructional details
    • G01R1/06—Measuring leads; Measuring probes
    • G01R1/067—Measuring probes
    • G01R1/06711—Probe needles; Cantilever beams; "Bump" contacts; Replaceable probe pins
    • G01R1/06733—Geometry aspects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R1/00—Details of instruments or arrangements of the types included in groups G01R5/00 - G01R13/00 and G01R31/00
    • G01R1/02—General constructional details
    • G01R1/06—Measuring leads; Measuring probes
    • G01R1/067—Measuring probes
    • G01R1/06711—Probe needles; Cantilever beams; "Bump" contacts; Replaceable probe pins
    • G01R1/06733—Geometry aspects
    • G01R1/0675—Needle-like

Definitions

  • the present invention relates to a method of modifying a metal structure, and more particularly, to a method of annealing for fabricating a metal structure unlikely to become brittle and having excellent hardness and creep resistance.
  • Annealing is a process to heat a metal structure and the like, hold it at a temperature and then cool the same to lower temperature. It is a heat treatment intended for improvement of plastic working properties, removal of residual internal stress, adjustment of crystal grain and the like.
  • a metal structure formed of nickel (Ni) the structure is generally heated to around 700-900° C. and held for 1-2 hours, and then cooled down slowly. With this heat treatment, since nickel (Ni) is recrystallized, nanocrystal material of a crystal size of around 10 nm, or amorphous material of a further smaller crystal size, will have a larger crystal size of several ⁇ m —a several ten ⁇ m.
  • the relatively unordered initial structure is reconfigured by annealing, to arrive at a more stable state of equilibrium, and is essentially removed of all residual internal stress.
  • Japanese Patent National Publication No. 2001-516812 discloses a method of heat treatment to obtain stable machinability under load.
  • a wire coated with metal such as nickel (Ni) and cobalt (Co) using saccharine and 2-butyne-1,4-diol and the like is relatively mildly heat-treated to fabricate an elastic metal structure.
  • a heat treatment temperature of this method effective is a temperature 0-150° C. higher than the transformation temperature at which crystals of a metal material on the wire become larger.
  • the effective temperature for heat treatment is 266-416° C. since the transformation temperature of the metal material is 266° C. (refer to FIG. 6 ). Therefore, in this method, the structure is heat treated at a temperature lower than the normal annealing temperature for nickel (Ni) of 700-900° C.
  • nanocrystal material or amorphous material having an average grain diameter of 16 nm will have larger crystals to become crystal material with an average grain diameter of 78 nm. Consequently, due to annealing, yield strength, elastic modulus and temperature stability of the metal structure are modified.
  • the contact probe Since the contact probe is pressed against a circuit of a semiconductor substrate or the like for usage, it has a spring capability to increase the reliability of connection with the circuit as well as not to damage the circuit. Therefore, the contact probe is required to have the property of being unlikely to become brittle and damaged while having high hardness. Further, since the contact probe is repeatedly used, it is required to have a property to return to its original shape when load is removed after the test.
  • creep amount the amount remaining as deformation after load is removed
  • spring load which occurs when the spring achieves a predetermined stroke does not change with loading time. Therefore, it is necessary to use a metal structure having superior creep resistance. More specifically, it is required to maintain creep resistance even when a semiconductor substrate to be tested is at a temperature of around 50-125° C. or higher.
  • One object of the present invention is to provide a method of annealing to fabricate a metal structure unlikely to become brittle and having excellent creep resistance while maintaining hardness.
  • a metal structure according to the present invention is a metal structure unlikely to become brittle and having excellent hardness and creep resistance, characterized in that annealing has been applied at a temperature not more than the temperature at which crystals of the metal material start to become larger.
  • This metal structure is formed of at least two kinds of metal material, and annealing can be applied at a temperature not more than the temperature at which crystals of the metal material start to become larger.
  • the present invention is more advantageous in the manner of a microstructure for a contact probe or the like.
  • a method of fabricating a metal structure according to the present invention is a method of fabricating a metal structure unlikely to become brittle and having excellent hardness and creep resistance, characterized in that a step of applying annealing at a temperature not more than the temperature at which crystals of the metal material start to become larger is included.
  • FIG. 1 shows a perspective view of a contact probe according to the present invention.
  • FIGS. 2A-2D show steps in a method of fabricating a contact probe according to the present invention.
  • FIG. 3 shows a plan view of a mask having a pattern of a contact probe.
  • FIGS. 4 and 5 show a deformation amount of a contact probe over time.
  • FIG. 6 shows the relationship between annealing temperature and metal crystal size.
  • the method of fabricating a metal structure according to the present invention is characterized in that a step of applying annealing at a temperature not more than the temperature at which crystals of the metal material start to become larger is included.
  • Methods to increase creep resistance of the metal material include a method to reduce residual internal stress within crystals and a method to enlarge the crystal grain size.
  • Annealing is applied at a temperature not more than the temperature at which crystals of the metal material start to become larger. At a temperature higher than this temperature, decrease in hardness or embrittlement of the metal material is likely to occur. More specifically, if the metal structure includes nickel-manganese (Ni—Mn) alloy, annealing is applied at a temperature not more than 260° C. since the temperature at which crystals start to become larger is 260° C. In this case, since the range of 250-260° C. is a transitional region where some of the crystals start to become larger, the annealing temperature is preferably 150-250° C., and more preferably 200-230° C.
  • the annealing temperature When the annealing temperature is lower than 150° C., it is difficult to sufficiently reduce the residual stress within crystals. On the other hand, when the annealing temperature is higher than 250° C., it is possible to reduce internal stress of crystals and increase creep resistance, but decrease in hardness or embrittlement tends to occur.
  • the annealing period of time varies depending on the metal material and annealing temperatures, in general, when annealing is applied at a lower temperature, embrittlement of crystals is depressed and longer annealing time is preferable to reduce residual stress within crystals sufficiently and to prevent crystals from enlarging. Meanwhile, when annealing is applied at a higher temperature, shorter annealing time is preferable to depress enlargement of crystals since it is possible to efficiently reduce residual stress within crystals.
  • the metal structure is formed of nickel-manganese (Ni—Mn) alloy and the annealing temperature is 150° C., annealing of 10-30 hours is preferable. When the annealing temperature is 250° C., annealing of 0.5-2 hours is preferable.
  • the metal material to be subjected to annealing is preferably at least one material selected from the group consisting of nickel (Ni), cobalt (Co), iron (Fe), rhodium (Rh), palladium (Pd), tungsten (W), copper (Cu), manganese (Mn), chromium (Cr), titanium (Ti), aluminum (Al), gold (Au) and platinum (Pt).
  • nickel (Ni), cobalt (Co) or iron (Fe) are more preferable.
  • nickel-cobalt (Ni—Co), cobalt-manganese (Co—Mn), nickel-manganese (Ni—Mn), nickel-iron (Ni—Fe), cobalt-iron (Co—Fe), titanium-tungsten (Ti—W) or nickel-cobalt-manganese (Ni—Co—Mn) are more preferable.
  • the metal structure according to the present invention is characterized in that annealing has been at a temperature not more than the temperature at which crystals of the metal material start to become larger.
  • the metal structure according to the present invention includes at least two kinds of metal material, and annealing can be applied at a temperature not more than the temperature at which crystals of the metal material start to become larger. These metal structures are unlikely to cause decrease in hardness and embrittlement, and have excellent creep resistance.
  • Coating with the metal material can be effected by any of commonly known methods such as electroplating, chemical vapor deposition (CVD), physical vapor deposition (PVD), or electrolytic plating or electroless plating of metal.
  • CVD chemical vapor deposition
  • PVD physical vapor deposition
  • electrolytic plating or electroless plating of metal for example, for physical vapor deposition, vacuum deposition, sputtering or ion plating can be used, and a metal material layer with a thickness of 250-600 nm can be formed by sputter
  • the present invention is more effective for a microstructure.
  • the present invention is also effective for a metal structure which is not a microstructure.
  • the effect of making the material itself homogeneous by preventing crystals from enlarging according to the invention is outstanding for a microstructure with a minimum machinable dimension of several ⁇ m—several hundred ⁇ m. Therefore, the metal structure according to the present invention can be preferably used as a contact probe, since the contact probe needs to have a microstructure of several ⁇ m—several hundred ⁇ m in its spring portion and the like, and it is necessary to use a material unlikely to become brittle and having excellent hardness and creep resistance.
  • the contact probe includes a plunger portion 1 in contact with a circuit to be tested, a spring portion 2 supporting plunger portion 1 at one end, and a lead line connection portion 3 electrically connecting the other end of spring portion 2 to the lead line.
  • the contact probe is arranged within a probe card. When test is conducted, the contact probe is used with plunger portion 1 pressed against a circuit to be tested.
  • FIG. 2 An example of the method of fabricating a contact probe is shown in FIG. 2 .
  • a resist layer 22 is formed on a surface of a conductive substrate 21 .
  • a conductive substrate of SUS, Cu or Al can be used.
  • a non-conductive substrate can be used which includes Si or glass and the like and has a conductive layer formed thereon of Ti, Al, Cu or alloys thereof by sputtering and the like.
  • a metal layer 25 is formed on resin mold 22 b .
  • Metal layer 25 can be formed by electroforming. Electroforming means to form a metal layer including nickel (Ni) and the like on a conductive substrate using a metal solution.
  • resin mold 22 b on substrate 21 is removed by ashing with oxygen plasma and the like, followed by removal of substrate 21 by dry etching and the like. Finally, annealing is applied at a temperature not more than the temperature at which crystals of the metal material start to become larger to obtain a contact probe according to the present invention as shown in FIG. 2D .
  • a contact probe unlikely to become brittle and having excellent hardness and creep resistance can be fabricated.
  • a contact probe with its plunger portion, spring portion and lead line connection portion integrated can be easily fabricated, adaptable to micro miniaturization or complexation of the contact probe. Furthermore, assembling work is eliminated.
  • X-ray resist layer 22 was formed on a surface of SUS substrate 21 . Then, exposed to X-ray 24 through mask 23 having a pattern of the contact probe, the pattern was transformed to X-ray resist layer 22 .
  • the mask corresponding to the pattern of the contact probe had a shape as shown in FIG. 3 , with L of 1550 ⁇ m, W of 1000 ⁇ m, T 1 of 82 ⁇ m and T 2 of 65 ⁇ m.
  • Exposed region 22 a of resist layer 22 was removed by development to obtain resin mold 22 b as shown in FIG. 2B . Then, as shown in FIG. 2C , metal layer 25 of nickel-manganese alloy was formed on resin mold 22 b .
  • Formation of metal layer 25 was performed by electroforming.
  • electroforming a plating bath having nickel sulfamate solution blended with manganese sulfamate, boric acid, saccharine sodium, 2-butyne-1,4-diol and sodium lauryl sulfate was used.
  • Creep resistance of the contact probe was evaluated by a micro load test machine (H-100 produced by Fischer). Evaluation of creep resistance was performed by measuring the deformation amount when the contact probe was subjected to a constant load of 50 mN for 1 hour (3600 seconds) at 85° C. The result is shown in FIG. 4 .
  • the deformation amount of the contact probe not subjected to annealing gradually increased over time, and after 1 hour of loading, it reached 45 ⁇ m.
  • the initial deformation amount was comparable, but the delayed deformation amount after 1 hour of loading was about 2 ⁇ m. Therefore, it was found that the contact probe subjected to annealing according to the present invention did not have enlargement of crystals and showed higher creep resistance than the contact probe not subjected to annealing.
  • annealing time was fixed to 1 hour, and annealing was applied at various temperatures of 150° C., 200° C., 230° C., 250° C. and 300 ° C. Then creep resistance was measured respectively. Evaluation method of creep resistance was the same as in Example 1, and deformation amount after the contact probe was subjected to a constant load of 50 mN for 1 hour (3600 seconds) at 85° C., was measured. The result is shown in FIG. 5 .
  • deformation amount (108-132 ⁇ m) ⁇ 10% of the initial deformation amount (120 ⁇ m) of the contact probe not subjected to annealing was evaluated as the tolerable range for a product.
  • the contact probe subjected to annealing at 150-250° C. for 1 hour was within that tolerable range.
  • the contact probe subjected to annealing at the range of 200-230° C. for 1 hour exhibited extremely superior creep resistance.
  • the annealing temperature was 300° C., although creep resistance was apparently good, the initial deformation amount decreased considerably, and the metal became hard and brittle. Therefore, the contact probe unpreferably often broke when installed or used repeatedly.
  • annealing was applied at temperatures of 150° C., 200° C., 250° C., 260° C. and 300° C., and the metal crystal size was measured. The result is shown in FIG. 6 .
  • annealing at 250° C., crystals slightly began to grow, and at 260° C., the crystal size became about ten times larger.
  • crystal size reached about 600 nm, showing that crystals completely enlarged.
  • the temperature at which crystals enlarge was 260° C.
  • the annealing temperature to effectively exhibit the effects of the present invention was a temperature at which crystals of the metal material start to enlarge, or lower.
  • a metal structure unlikely to become brittle and having good creep resistance can be fabricated while maintaining hardness.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Geometry (AREA)
  • Measuring Leads Or Probes (AREA)
  • Heat Treatment Of Articles (AREA)
  • Manufacture Of Switches (AREA)
US10/546,824 2003-04-16 2004-04-12 Metal structure and method for production thereof Abandoned US20060144485A1 (en)

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Application Number Priority Date Filing Date Title
US12/399,589 US8052810B2 (en) 2003-04-16 2009-03-06 Metal structure and fabrication method thereof

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2003-111710 2003-04-16
JP2003111710A JP3745744B2 (ja) 2003-04-16 2003-04-16 金属構造体の製造方法およびその方法により製造した金属構造体
PCT/JP2004/005228 WO2004092435A1 (ja) 2003-04-16 2004-04-12 金属構造体およびその製造方法

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US12/399,589 Expired - Fee Related US8052810B2 (en) 2003-04-16 2009-03-06 Metal structure and fabrication method thereof

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US (2) US20060144485A1 (zh)
JP (1) JP3745744B2 (zh)
KR (1) KR101034828B1 (zh)
CN (1) CN100430513C (zh)
DE (1) DE112004000610B4 (zh)
TW (1) TWI318648B (zh)
WO (1) WO2004092435A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140269228A1 (en) * 2013-03-14 2014-09-18 Seiko Instruments Inc. Metal structure, method of manufacturing metal structure, spring component, chronograph coupling lever for timepiece, and timepiece

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US7957119B2 (en) * 2005-08-29 2011-06-07 Kyocera Corporation Metal films, methods for production thereof, methods for production of laminated electronic components, and laminated electronic components
JP2008078061A (ja) * 2006-09-25 2008-04-03 Alps Electric Co Ltd 弾性接触子及びその製造方法、ならびに前記弾性接触子を用いた接続装置及びその製造方法
US8826529B2 (en) * 2009-09-23 2014-09-09 General Electric Company Method of forming a micro-electromechanical system device
JP6137725B2 (ja) * 2012-12-04 2017-05-31 日本電産リード株式会社 搬送装置及び接触子組立装置
RU2616742C2 (ru) * 2015-09-29 2017-04-18 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Сибирский государственный индустриальный университет" Способ повышения долговечности изделия из меди, работающего в условиях ползучести
US11807929B2 (en) * 2019-03-14 2023-11-07 Unison Industries, Llc Thermally stabilized nickel-cobalt materials and methods of thermally stabilizing the same

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US5306414A (en) * 1993-05-17 1994-04-26 Regents Of The University Of California Corrosion sensor
US20040104739A1 (en) * 2001-04-13 2004-06-03 Tsuyoshi Haga Contact probe
US20050028900A1 (en) * 2003-08-04 2005-02-10 National Taiwan Ocean University Annealing-induced extensive solid-state amorphization in metallic films

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US3310389A (en) * 1963-10-02 1967-03-21 High Duty Alloys Ltd Sheets of aluminum alloy and methods of manufacturing same
US4021271A (en) * 1975-07-07 1977-05-03 Kaiser Aluminum & Chemical Corporation Ultrafine grain Al-Mg alloy product
US4247326A (en) * 1979-08-29 1981-01-27 Inland Steel Company Free machining steel with bismuth
US4507180A (en) * 1983-03-14 1985-03-26 U.S. Philips Corporation Method of electrodepositing a homogeneously thick metal layer, metal layer thus obtained and the use of the metal layer thus obtained, device for carrying out the method and resulting matrix
US5306414A (en) * 1993-05-17 1994-04-26 Regents Of The University Of California Corrosion sensor
US20040104739A1 (en) * 2001-04-13 2004-06-03 Tsuyoshi Haga Contact probe
US20050028900A1 (en) * 2003-08-04 2005-02-10 National Taiwan Ocean University Annealing-induced extensive solid-state amorphization in metallic films

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140269228A1 (en) * 2013-03-14 2014-09-18 Seiko Instruments Inc. Metal structure, method of manufacturing metal structure, spring component, chronograph coupling lever for timepiece, and timepiece
US9310772B2 (en) * 2013-03-14 2016-04-12 Seiko Instruments Inc. Metal structure, method of manufacturing metal structure, spring component, chronograph coupling lever for timepiece, and timepiece

Also Published As

Publication number Publication date
DE112004000610B4 (de) 2014-08-14
JP2004315892A (ja) 2004-11-11
TW200508405A (en) 2005-03-01
KR101034828B1 (ko) 2011-05-16
KR20050121213A (ko) 2005-12-26
WO2004092435A1 (ja) 2004-10-28
CN1774522A (zh) 2006-05-17
TWI318648B (en) 2009-12-21
US20090176027A1 (en) 2009-07-09
JP3745744B2 (ja) 2006-02-15
DE112004000610T5 (de) 2006-03-09
US8052810B2 (en) 2011-11-08
CN100430513C (zh) 2008-11-05

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