WO2021206096A1 - はんだ粒子、はんだ粒子の製造方法及びはんだ粒子付き基体 - Google Patents

はんだ粒子、はんだ粒子の製造方法及びはんだ粒子付き基体 Download PDF

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Publication number
WO2021206096A1
WO2021206096A1 PCT/JP2021/014656 JP2021014656W WO2021206096A1 WO 2021206096 A1 WO2021206096 A1 WO 2021206096A1 JP 2021014656 W JP2021014656 W JP 2021014656W WO 2021206096 A1 WO2021206096 A1 WO 2021206096A1
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Prior art keywords
solder particles
solder
substrate
convex portion
alloy
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.)
Ceased
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PCT/JP2021/014656
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English (en)
French (fr)
Japanese (ja)
Inventor
勝将 宮地
芳則 江尻
邦彦 赤井
純一 畠
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.)
Resonac Corp
Original Assignee
Showa Denko Materials Co Ltd
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Filing date
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Application filed by Showa Denko Materials Co Ltd filed Critical Showa Denko Materials Co Ltd
Priority to CN202180026545.8A priority Critical patent/CN115362044B/zh
Priority to JP2022514090A priority patent/JP7768127B2/ja
Publication of WO2021206096A1 publication Critical patent/WO2021206096A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400°C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550°C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40—Making wire or rods for soldering or welding
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C12/00—Alloys based on antimony or bismuth
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/02—Alloys based on gold

Definitions

  • the present invention relates to solder particles, a method for producing solder particles, and a substrate with solder particles.
  • Patent Document 1 describes a conductive paste containing a thermosetting component and a plurality of solder particles that have been subjected to a specific surface treatment.
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for producing solder particles capable of producing solder particles having both a small average particle size and a narrow particle size distribution. Another object of the present invention is to provide solder particles having both a small average particle size and a narrow particle size distribution by the above manufacturing method.
  • One aspect of the present invention includes a preparatory step of preparing a substrate having a plurality of convex portions, a solder layer forming step of forming a solder layer on the convex portions of at least a part of the substrate, and forming on the convex portions.
  • the present invention relates to a method for producing solder particles, which comprises a fusion step of fusing the said solder layers to form solder particles on the convex portion.
  • solder particles having a desired particle size can be obtained with a narrow particle size distribution by appropriately adjusting the shape of the convex portion and the thickness of the solder layer. That is, according to the above manufacturing method, it is possible to easily manufacture solder particles having both a small average particle size and a narrow particle size distribution, which was difficult to manufacture in the past.
  • the convex portion may be columnar or frustum-shaped.
  • the substrate may have a first surface comprising a plurality of convex portions and a bottom portion formed between the convex portions, and the projection of the bottom portion in the projected area of the first surface.
  • the area ratio may be 8% or more.
  • the manufacturing method according to one aspect may form the solder layer on the convex portion by at least one method selected from the group consisting of plating, vapor deposition, sputtering and spray coating in the solder layer forming step.
  • the manufacturing method according to one aspect may further include a reduction step of exposing the solder layer formed on the convex portion to a reducing atmosphere before the fusion step.
  • the solder layer formed on the convex portion may be fused in a reducing atmosphere.
  • the solder layer may contain at least one selected from the group consisting of tin, tin alloys, indium and indium alloys.
  • the solder layer comprises In—Bi alloy, In—Sn alloy, In—Sn—Ag alloy, Sn—Au alloy, Sn—Bi alloy, Sn—Bi-Ag alloy, Sn—Ag—Cu alloy and It may contain at least one selected from the group consisting of Sn—Cu alloys.
  • the average particle size is 100 nm or more and less than 1 ⁇ m, and C.I. V. For solder particles with a value of 20% or less.
  • solder particles according to one aspect are obtained when a quadrangle circumscribing the projected image of the solder particles is created by two pairs of parallel lines and the distances between the opposing sides are X and Y (however, Y ⁇ X).
  • X and Y may satisfy the following formula. 0.8 ⁇ Y / X ⁇ 1.0
  • the solder particles according to one embodiment may contain at least one selected from the group consisting of tin, tin alloys, indium and indium alloys.
  • solder particles include In—Bi alloy, In—Sn alloy, In—Sn—Ag alloy, Sn—Au alloy, Sn—Bi alloy, Sn—Bi-Ag alloy, Sn—Ag—Cu alloy and Sn.
  • -It may contain at least one selected from the group consisting of Cu alloys.
  • Yet another aspect of the present invention relates to a substrate with solder particles, comprising a substrate having a plurality of convex portions and a plurality of solder particles arranged on the convex portions of the substrate.
  • a substrate with solder particles can be easily manufactured by the fusion step in the above-mentioned manufacturing method.
  • Such a substrate with solder particles facilitates transportation, storage and management of the solder particles.
  • the average particle size of the solder particles may be 100 nm or more and less than 1 ⁇ m, and the C.I. V. The value may be 20% or less.
  • solder particles capable of producing solder particles having both a small average particle size and a narrow particle size distribution. Further, according to the present invention, solder particles having both a small average particle size and a narrow particle size distribution are provided.
  • FIG. 1A is a plan view schematically showing an example of a substrate
  • FIG. 1B is a cross-sectional view taken along the line Ib-Ib shown in FIG. 1A.
  • FIG. 2A is a cross-sectional view schematically showing an example of the convex portion
  • FIG. 2B is a cross-sectional view schematically showing another example of the convex portion.
  • 3A to 3E are diagrams schematically showing an example of the shape of the cross section perpendicular to the height direction of the convex portion.
  • FIG. 4 is a cross-sectional view schematically showing an example of a state in which a solder layer is formed on a convex portion of a substrate.
  • FIG. 5 is a cross-sectional view schematically showing an example of a state in which solder particles are formed on the convex portion of the substrate.
  • FIG. 6 is a cross-sectional view schematically showing another example of a state in which a solder layer is formed on a convex portion of a substrate.
  • FIG. 7 is a cross-sectional view schematically showing another example of a state in which solder particles are formed on the convex portion of the substrate.
  • FIG. 8 is a diagram showing distances X and Y (provided that Y ⁇ X) between opposite sides when a quadrangle circumscribing a projected image of solder particles is created by two pairs of parallel lines.
  • FIG. 9 is an SEM image of the substrate prepared in Example 13.
  • FIG. 9 is an SEM image of the substrate prepared in Example 13.
  • FIG. 10 is an SEM image of the state in which the solder layer is formed on the convex portion of the substrate in Example 13.
  • FIG. 11 is an SEM image of the state in which the solder particles are formed on the convex portion of the substrate in Example 13.
  • FIG. 12 is an SEM image of the solder particles obtained in Example 2.
  • FIG. 13 is an SEM image of the solder particles obtained in Comparative Example 2.
  • each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
  • the numerical range indicated by using "-" indicates a range including the numerical values before and after "-" as the minimum value and the maximum value, respectively.
  • the upper limit value or the lower limit value of the numerical range of one step may be replaced with the upper limit value or the lower limit value of the numerical range of another step.
  • the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the examples.
  • the method for producing solder particles according to the present embodiment includes a preparatory step of preparing a substrate having a plurality of convex portions, a solder layer forming step of forming a solder layer on at least a part of the convex portions of the substrate, and a solder layer forming step on the convex portions. It includes a fusion step of fusing the solder layers formed in the above to form solder particles on the convex portion.
  • solder particles having a desired particle size can be obtained with a narrow particle size distribution by appropriately adjusting the shape of the convex portion and the thickness of the solder layer. That is, according to the above manufacturing method, solder particles having both a small average particle size and a narrow particle size distribution (for example, an average particle size of 100 nm to 30 ⁇ m and a CV value of 20%), which was difficult to manufacture in the past, are achieved. The following solder particles) can be easily manufactured.
  • solder particles that are difficult to manufacture by the conventional method.
  • extremely small solder particles having an average particle diameter of 100 nm or more and less than 1 ⁇ m can be obtained with a narrow particle size distribution (for example, a CV value of 20% or less).
  • FIG. 1A is a diagram schematically showing an example of a substrate
  • FIG. 1B is a cross-sectional view taken along the line Ib-Ib shown in FIG. 1A.
  • the substrate 10 shown in FIG. 1A has a plurality of convex portions 11.
  • the plurality of convex portions 11 may be regularly arranged in a predetermined pattern.
  • the solder particles formed on the convex portion 11 can be transferred to a resin material or the like so that the solder particles can be arranged regularly.
  • the substrate 10 may have a first surface 10a including a plurality of convex portions 11 and a bottom portion 12 formed between the convex portions 11.
  • the first surface 10a may be composed of a top portion 11a of the convex portion 11 and a bottom surface 12a composed of the bottom portion 12.
  • the solder particles on the convex portions 11 may come into contact with each other and fuse with each other to generate solder particles having a large particle size in the fusion step described later.
  • the ratio of the projected area of the bottom 12 to the projected area of the first surface 10a (that is, the area of the bottom surface 12a to the projected area of the first surface 10a).
  • the ratio is preferably 8% or more, more preferably 10% or more, and may be 15% or more.
  • the upper limit of the ratio is not particularly limited. From the viewpoint of further improving the production efficiency of the solder particles, for example, it may be 95% or less, preferably 90% or less, and further preferably 80% or less.
  • the convex portion 11 is formed in a columnar shape, but the shape of the convex portion 11 is not limited to this.
  • the convex portion 11 may have a columnar shape such as a columnar shape, an elliptical columnar shape, a triangular columnar shape, a square columnar shape, or a polygonal columnar shape, and may have a conical frustum shape, an elliptical frustum shape, a triangular frustum shape, or a square frustum shape. , It may be a frustum shape such as a polygonal frustum shape.
  • the top portion 11a of the convex portion 11 is described as a flat surface in FIGS. 1A and 1B, the top portion 11a does not necessarily have to be a flat surface.
  • the top 11a may have a recess or a protrusion. From the viewpoint of improving the retention of the solder particles formed on the top portion 11a, it is preferable that the top portion 11a has a recess in the center.
  • FIG. 2A is a cross-sectional view schematically showing an example of a convex portion
  • FIG. 2B is a cross-sectional view schematically showing an example of a convex portion.
  • the convex portion 11 shown in FIG. 2A is a prismatic convex portion
  • the convex portion 21 shown in FIG. 2B is a frustum-shaped convex portion.
  • the width D 11 and the width D 12 are not particularly limited, and may be, for example, 200 nm or more, preferably 400 nm or more, and more preferably 1.0 ⁇ m or more from the viewpoint of avoiding contact between solder particles on adjacent convex portions. Further, the width D 11 and the width D 12 may be, for example, 10 ⁇ m or less, preferably 4.0 ⁇ m or less, and more preferably 2.0 ⁇ m or less from the viewpoint of producing ultrafine particle size solder particles having a particle size of 800 nm or less.
  • the height H 1 of the convex portion 11 is not particularly limited, and may be, for example, 10% or more of the width D 11 , avoiding contact with the solder on the bottom portion 12, and making it easier to obtain more accurate solder particles. preferably at least 25% of the width D 11 from the viewpoint, more preferably at least 50% of the width D 11.
  • the height H 1 of the convex portion 11, for example, may be less 1000% of the width D 11, avoiding the breakage of the projections 11, 500% of the width D 11 from the viewpoint of enhancing the recovery rate of the solder particles The following is preferable, and 300% or less of the width D 11 is more preferable.
  • the convex portion 11 can be arranged at an arbitrary position on the substrate 10.
  • the distance L 1 between the adjacent convex portions 11 is not particularly limited, but from the viewpoint of suppressing the formation of large particle size particles due to the contact and fusion of the solder particles on the convex portions 11, for example, it is 3% or more of the width D 11. be in a, preferably 8% or more of the width D 11, more preferably at least 15% of the width D 11.
  • the distance L 1 between the convex portions 11 adjacent for example may be up to 1000% of the width D 11, from the viewpoint of further improving the manufacturing efficiency of the solder particles, preferably 500% or less of the width D 11, More preferably, it is 200% or less of the width D 11.
  • the width D 21 at the top 21 a of the convex portion 21 is smaller than the width D 22 at the contact surface with the bottom 22.
  • the width D 21 is not particularly limited, and may be, for example, 200 nm or more, preferably 400 nm or more, and more preferably 1.0 ⁇ m or more from the viewpoint of avoiding contact between solder particles on adjacent convex portions.
  • the width D 21 may be, for example, 10 ⁇ m or less, preferably 4.0 ⁇ m or less, and more preferably 2.0 ⁇ m or less from the viewpoint of producing ultrafine particle size solder particles having a particle size of 800 nm or less.
  • the width D 22 is not particularly limited, and may be, for example, 200 nm or more, preferably 400 nm or more, and more preferably 1.0 ⁇ m or more from the viewpoint of avoiding contact between solder particles on adjacent convex portions.
  • the width D 22 may be, for example, 10 ⁇ m or less, preferably 4.0 ⁇ m or less, and more preferably 2.0 ⁇ m or less, from the viewpoint of producing ultrafine particle size solder particles having a particle size of 800 nm or less.
  • the ratio of the width D 21 to the width D 22 is not particularly limited, and may be, for example, 1.1 or more. From the viewpoint of avoiding contact between solder particles on the adjacent convex portion, 1. 3 or more is preferable, and 1.5 or more is more preferable.
  • the ratio (D 22 / D 21 ) may be, for example, 3.0 or less, preferably 2.0 or less.
  • the difference between the width D 21 and the width D 22 (D 22- D 21 ) is not particularly limited and may be, for example, 2.0 ⁇ m or less, reducing the amount of solder supplied to the side surface and the bottom 22 of the convex portion 21. From the viewpoint that more accurate solder particles can be easily obtained, 1.0 ⁇ m or less is preferable, and 500 nm or less is more preferable.
  • the height H 2 of the convex portion 21 is not particularly limited, and may be, for example, 10% or more of the width D 22 , avoiding contact with the solder on the bottom portion 12, and making it easier to obtain more accurate solder particles. preferably at least 25% of the width D 22 from the viewpoint, more preferably at least 50% of the width D 22.
  • the height H 2 of the convex portion 21, for example, may be less 1000% of the width D 22, avoiding the breakage of the projections 11, 500% of the width D 22 from the viewpoint of enhancing the recovery rate of the solder particles The following is preferable, and 300% or less of the width D 22 is more preferable.
  • the distance L 2 between the adjacent convex portions 21 is not particularly limited, but from the viewpoint of suppressing the formation of large particle size particles due to the contact and fusion of the solder particles on the convex portions 21, for example, it is 3% or more of the width D 22. be in a, preferably 8% or more of the width D 22, more preferably at least 15% of the width D 22.
  • the distance L 2 between adjacent convex portions 21 is, for example may be up to 1000% of the width D 22, from the viewpoint of further improving the manufacturing efficiency of the solder particles, preferably 500% or less of the width D 22, More preferably, it is 200% or less of the width D 22.
  • the shape of the cross section perpendicular to the height direction of the convex portion 11 and the convex portion 21 is not particularly limited, and may be, for example, the shape shown in FIG. 3A to 3E are diagrams schematically showing an example of the shape of the cross section perpendicular to the height direction of the convex portion.
  • the material constituting the substrate 10 is not particularly limited, and a material having heat resistance that does not deteriorate at the melting temperature of the solder layer is preferable.
  • the material constituting the substrate 10 may be, for example, an inorganic material such as silicon, various ceramics, glass, or stainless steel, or an organic material such as various resins.
  • the method for producing the substrate 10 is not particularly limited, and the substrate 10 can be appropriately produced by a known method (for example, a photolithography method) capable of forming the convex portion 11.
  • solder layer forming step a solder layer is formed on at least a part of the convex portion of the substrate (solder layer forming step).
  • solder material for forming the solder layer a commercially available solder material can be used without particular limitation, and can be appropriately selected depending on the desired characteristics of the solder particles, the method for forming the solder layer, and the like.
  • a solder plate that can be used as a target for sputtering is selected.
  • the solder material may include, for example, tin or a tin alloy.
  • tin alloy for example, In—Sn alloy, In—Sn—Ag alloy, Sn—Au alloy, Sn—Bi alloy, Sn—Bi—Ag alloy, Sn—Ag—Cu alloy, Sn—Cu alloy and the like are used. be able to. Specific examples of these tin alloys include the following examples.
  • the solder material may include, for example, indium or an indium alloy.
  • the indium alloy for example, an In—Bi alloy, an In—Ag alloy, or the like can be used. Specific examples of these indium alloys include the following examples. -In-Bi (In66.3% by mass, Bi33.7% by mass, melting point 72 ° C.) -In-Bi (In33.0% by mass, Bi67.0% by mass, melting point 109 ° C) -In-Ag (In97.0% by mass, Ag3.0% by mass, melting point 145 ° C)
  • the tin alloy or indium alloy can be selected as the solder material according to the use of the solder particles (temperature at the time of use) and the like. For example, when it is desired to obtain solder particles used for fusion at a low temperature, an In—Sn alloy or a Sn—Bi alloy may be adopted. In this case, solder particles that can be fused at 150 ° C. or lower can be obtained. When a solder material having a high melting point such as a Sn—Ag—Cu alloy or a Sn—Cu alloy is used, solder particles capable of maintaining high reliability even after being left at a high temperature can be obtained.
  • the solder material may further contain one or more selected from Ag, Cu, Ni, Bi, Zn, Pd, Pb, Au, P and B.
  • Ag or Cu may be contained from the following viewpoints. That is, when the solder material contains Ag or Cu, the melting point of the obtained solder particles can be lowered to about 220 ° C., and the solder particles having excellent bonding strength with the electrode can be obtained, so that better conduction reliability can be obtained. The effect of obtaining sex is achieved.
  • the Cu content of the solder material is, for example, 0.05 to 10% by mass, and may be 0.1 to 5% by mass or 0.2 to 3% by mass.
  • the Cu content is 0.05% by mass or more, it becomes easy to obtain solder particles capable of achieving good solder connection reliability. Further, when the Cu content is 10% by mass or less, solder particles having a low melting point and excellent wettability can be easily obtained, and as a result, the connection reliability of the joint portion by the solder particles tends to be improved.
  • the Ag content of the solder material is, for example, 0.05 to 10% by mass, and may be 0.1 to 5% by mass or 0.2 to 3% by mass.
  • the Ag content is 0.05% by mass or more, it becomes easy to obtain solder particles capable of achieving good solder connection reliability. Further, when the Ag content is 10% by mass or less, solder particles having a low melting point and excellent wettability can be easily obtained, and as a result, the connection reliability of the joint portion by the solder particles tends to be improved.
  • solder layer forming step a solder layer is formed on each of the convex portions of the substrate.
  • the solder layer forming step may be a step of forming a solder layer on all the convex portions of the substrate prepared in the preparation step, and is a step of forming a solder layer on a part of the convex portions of the substrate prepared in the preparation step. May be good.
  • the method of forming the solder layer is not particularly limited.
  • the method for forming the solder layer include plating, vapor deposition, sputtering, and spray coating. Of these, sputtering is preferable from the viewpoint that the thickness of the solder layer can be strictly controlled and solder particles having a smaller particle size distribution can be easily obtained.
  • the amount of the solder layer formed is not particularly limited, and may be appropriately changed according to the desired size of the solder particles. By appropriately changing the amount of the solder layer formed on the convex portion, the size of the solder particles formed on the convex portion can be easily adjusted.
  • the solder layer may be formed only on the convex portion of the substrate, and the solder layer may be formed on a portion other than the convex portion of the substrate.
  • a solder layer may be formed on the convex portion and the bottom portion of the substrate.
  • FIG. 4 is a cross-sectional view schematically showing an example of a state in which the solder layer 50 is formed on the convex portion 11 of the substrate 10.
  • the solder layer is formed only on the convex portion 11 of the substrate 10.
  • the solder layer is formed using the above-mentioned solder materials and may contain at least one selected from the group consisting of tin, tin alloys, indium and indium alloys.
  • the solder layer includes In—Bi alloy, In—Sn alloy, In—Sn—Ag alloy, Sn—Au alloy, Sn—Bi alloy, Sn—Bi-Ag alloy, Sn—Ag—Cu alloy and Sn—Cu. It may include at least one selected from the group consisting of alloys.
  • FIG. 6 is a cross-sectional view schematically showing another example of a state in which the solder layer 50 is formed on the convex portion 11 of the substrate 10.
  • the solder layer 50 is formed on the convex portion 11 of the substrate 10, and the solder layer 51 is also formed on the bottom portion 12 of the substrate 10.
  • the amount of the solder layer 50 formed on the convex portion 11 is, for example, 20% with respect to the total volume of the solder layers formed on the substrate (total volumes of the solder layer 50 and the solder layer 51).
  • the above is preferable, 30% or more is more preferable, 50% or more is further preferable, and 60% or more is further preferable.
  • solder layers formed on the convex portions are fused to form solder particles on the convex portions (fusion step).
  • the solder layer formed on the convex portion is united by melting and spheroidized by surface tension to form solder particles.
  • Examples of the method of melting the solder layer include a method of heating the solder layer to a temperature equal to or higher than the melting point of the solder material constituting the solder layer. Due to the influence of the oxide film, the solder layer may not melt even if it is heated at a temperature equal to or higher than the melting point, it may not spread even if it melts, or it may not unify. Therefore, it is preferable to expose the solder layer to a reducing atmosphere to remove the oxide film on the surface of the solder layer, and then heat the solder layer to a temperature equal to or higher than the melting point of the solder material. Further, it is preferable that the solder layer is melted in a reducing atmosphere. By melting the solder layer in a reducing atmosphere, melting, wetting and spreading of the solder layer and coalescence can proceed more efficiently.
  • the method for creating a reducing atmosphere is not particularly limited as long as the above effects can be obtained, and for example, there is a method using hydrogen gas, hydrogen radical, formic acid gas, or the like.
  • a hydrogen reduction furnace, a hydrogen radical reduction furnace, a formic acid reduction furnace, or a conveyor furnace or a continuous furnace thereof the solder layer can be melted in a reduction atmosphere.
  • These devices may be equipped with a heating device, a chamber filled with an inert gas (nitrogen, argon, etc.), a mechanism for evacuating the inside of the chamber, etc., which makes it easier to control the reducing gas. Become. Further, if the inside of the chamber can be evacuated, voids can be removed by reducing the pressure after the solder layer is melted and coalesced, and solder particles having further excellent connection stability can be obtained.
  • Profiles such as reduction of the solder layer, melting conditions, temperature, and adjustment of the atmosphere in the furnace may be appropriately set in consideration of the melting point, particle size, recess size, substrate material, etc. of the solder layer.
  • a substrate having a solder layer formed on a convex portion is inserted into a furnace, evacuated, and then a reducing gas is introduced to fill the inside of the furnace with the reducing gas to form an oxide film on the surface of the solder layer.
  • the reducing gas is removed by evacuation, and then heated above the melting point of the solder layer to melt and coalesce the solder layer to form solder particles on the convex parts, and then nitrogen gas.
  • the temperature inside the furnace can be returned to room temperature to obtain solder particles.
  • a substrate having a solder layer formed on a convex portion is inserted into a furnace, evacuated, and then a reducing gas is introduced to fill the inside of the furnace with the reducing gas, and then a heater in the furnace is used.
  • the reducing gas is removed by vacuuming, and then the solder layer is heated to a temperature equal to or higher than the melting point of the solder layer to melt and coalesce the solder layer.
  • the temperature inside the furnace can be returned to room temperature after filling with nitrogen gas to obtain the solder particles.
  • a substrate having a solder layer formed on a convex portion is inserted into a furnace, and after vacuuming, a reducing gas is introduced to fill the inside of the furnace with the reducing gas, and a heater in the furnace is used.
  • the substrate is heated above the melting point of the solder layer to remove the surface oxide film of the solder layer by reduction, and at the same time, the solder layer is melted and united to form solder particles on the convex portions, which are reduced by vacuuming.
  • the solder particles can be obtained by filling with nitrogen gas and then returning the temperature in the furnace to room temperature. In this case, since it is sufficient to adjust the temperature rise and fall in the furnace once, there is an advantage that the processing can be performed in a short time.
  • the inside of the furnace may be made into a reducing atmosphere again, and a step of removing the surface oxide film that could not be completely removed may be further added. As a result, it is possible to reduce the residue such as the solder layer remaining without being fused and a part of the oxide film remaining without being fused.
  • a substrate having a solder layer formed on a convex portion can be placed on a conveyor and passed through a plurality of zones in succession to obtain solder particles.
  • a substrate having a solder layer formed on a convex portion is placed on a conveyor set at a constant speed, passed through a zone filled with an inert gas such as nitrogen or argon at a temperature lower than the melting point of the solder layer, and then passed.
  • the surface oxide film of the solder layer is removed by passing through a zone where a reducing gas such as formic acid gas having a temperature lower than the melting point of the solder layer is present, and then nitrogen, argon or the like having a temperature higher than the melting point of the solder layer is not used.
  • Solder particles can be obtained by passing through a zone filled with active gas to melt and coalesce the solder layer, and then through a cooling zone filled with an inert gas such as nitrogen or argon.
  • a substrate having a solder layer formed on a convex portion is placed on a conveyor set at a constant speed, passed through a zone filled with an inert gas such as nitrogen or argon at a temperature equal to or higher than the melting point of the solder layer, and then passed.
  • the surface oxide film of the solder layer is removed, melted and coalesced by passing through a zone where a reducing gas such as formic acid gas having a temperature equal to or higher than the melting point of the solder layer exists, and then inert such as nitrogen and argon.
  • Solder particles can be obtained by passing through a gas-filled cooling zone. Since the conveyor furnace can be processed at atmospheric pressure, a film-like material can be continuously processed by roll-to-roll.
  • a continuous roll product of a substrate in which a solder layer is formed on a convex portion is produced, a roll unwinder is installed on the inlet side of the conveyor furnace, and a roll winder is installed on the outlet side of the conveyor furnace to maintain a constant speed.
  • a roll unwinder is installed on the inlet side of the conveyor furnace
  • a roll winder is installed on the outlet side of the conveyor furnace to maintain a constant speed.
  • the formed solder particles may be transported and stored in a state of being formed on the convex portion of the substrate.
  • a substrate in which solder particles are formed on the convex portion can be suitably handled as a substrate with solder particles.
  • a substrate with solder particles includes a substrate having a plurality of convex portions and a plurality of solder particles arranged on the convex portions of the substrate.
  • the average particle size of the solder particles is 100 nm or more and less than 1 ⁇ m, and the C.I. V. The value may be 20% or less.
  • the formed solder particles may be recovered from the convex portion.
  • the resin material may be arranged so as to face the convex portion of the substrate, and the solder particles on the convex portion may be transferred to the resin material. At this time, if the convex portions are regularly arranged, the solder particles can be regularly arranged on the resin material.
  • FIG. 5 is a cross-sectional view schematically showing an example of a state in which solder particles are formed on the convex portion of the substrate.
  • the substrate 100 with solder particles shown in FIG. 5 is obtained by subjecting the substrate 10 on which the solder layer 50 shown in FIG. 4 is formed to a fusion step.
  • the solder particles 1 are formed on the convex portions 11 of the base 10 having a plurality of convex portions 11.
  • FIG. 7 is a cross-sectional view schematically showing another example of a state in which solder particles are formed on the convex portion of the substrate.
  • the base 110 with solder particles shown in FIG. 7 is obtained by subjecting the base 10 on which the solder layer 50 and the solder layer 51 shown in FIG. 6 are formed to a fusion step.
  • the solder particles 1 are formed on the convex portions 11 of the base 10 having a plurality of convex portions 11.
  • solder particles 2 derived from the solder layer 51 are formed on the bottom portion 12 between the convex portions 11.
  • solder particles 2 do not always show a small particle size distribution, in this embodiment, it is preferable to collect or transfer only the solder particles 1.
  • the solder particles 2 are fixed to the bottom portion 12 of the substrate 10 and exist at a position lower than the solder particles 1 on the convex portion 11. Therefore, for example, by arranging the resin material so as to face the convex portion 11 of the substrate 10 and transferring the solder particles 1 on the convex portion 11 to the resin material, only the solder particles 1 can be recovered. ..
  • solder particles having a uniform size regardless of the material and shape of the solder material.
  • indium-based solder can be precipitated by plating, but it is difficult to precipitate it in the form of particles, and it is soft and difficult to handle.
  • indium-based solder particles having a uniform particle size can be easily produced.
  • the formed solder particles can be handled in a state of being formed on the convex portion of the substrate, the solder particles can be transported and stored without being deformed.
  • the formed solder particles are simply formed on the convex portion of the substrate, they can be easily taken out, and the solder particles can be collected, surface-treated, etc. without being deformed.
  • solder material may have a large variation in size and particle size distribution, or may have a distorted shape, and if a solder layer can be formed on the convex portion by a method such as sputtering, plating, or spray coating, the present invention. It can be used as a raw material for the production method of the embodiment.
  • the shape of the convex portion of the substrate can be freely designed by a photolithography method, an imprint method, a machining method, an electron beam processing method, a radiation processing method, or the like. Since the size of the solder particles depends on the amount of the solder layer formed on the convex portion, the size of the solder particles can be freely designed by the design of the convex portion in the manufacturing method of the present embodiment.
  • solder particles have an average particle size of 100 nm or more and 30 ⁇ m or less, and have a C.I. V. The value is 20% or less, preferably the average particle size is 100 nm or more and less than 1 ⁇ m, C.I. V. The value is 20% or less.
  • solder particles have both a small average particle size and a narrow particle size distribution, and can be suitably used as conductive particles applied to an anisotropic conductive material having high conductivity reliability and insulation reliability.
  • the solder particles according to this embodiment are manufactured by the above-mentioned manufacturing method.
  • the average particle size of the solder particles is not particularly limited as long as it is within the above range, and may be, for example, 30 ⁇ m or less, 15 ⁇ m or less, 10 ⁇ m or less, 5 ⁇ m or less, 3 ⁇ m or less, or 2 ⁇ m or less, preferably less than 1 ⁇ m.
  • the average particle size of the solder particles may be, for example, 100 nm or more, 200 nm or more, 300 nm or more, 400 nm or 500 nm or more.
  • the average particle size of the solder particles can be measured using various methods according to the size. For example, a dynamic light scattering method, a laser diffraction method, a centrifugal sedimentation method, an electrical detection band method, a resonance type mass measurement method, or the like can be used. Further, a method of measuring the particle size from an image obtained by an optical microscope, an electron microscope, or the like can be used. Specific devices include a flow-type particle image analyzer, a microtrack, a Coulter counter, and the like.
  • C. of solder particles V The value is preferably 20% or less, more preferably 10% or less, still more preferably 7% or less, and particularly preferably 5% or less, from the viewpoint of achieving more excellent conductivity reliability and insulation reliability.
  • the lower limit of the value is not particularly limited.
  • C.I. V. The value may be 1% or more, and may be 2% or more.
  • a flat surface portion may be formed on a part of the surface of the solder particles, and at this time, the surface other than the flat surface portion is preferably spherical crown-shaped. That is, the solder particles may have a flat surface portion and a spherical crown-shaped curved surface portion.
  • the ratio (A / B) of the diameter A of the flat surface portion to the diameter B of the solder particles may be, for example, more than 0.01 and less than 1.0 (0.01 ⁇ A / B ⁇ 1.0), and may be 0.1. It may be ⁇ 0.9. Since the solder particles have a flat surface portion, the seating of the solder particles is improved and the handleability is improved.
  • solder particles when arranging solder particles on an object to be connected by solder particles such as electrodes, it is easy to arrange them in a predetermined position because there is a flat part, and it is soldered by vibration, wind, external force, static electricity, etc. It has the effect of suppressing the movement of particles from a predetermined position. Further, when the member on which the solder particles are arranged is tilted, there is an effect that the solder particles are hard to move due to gravity as compared with, for example, spherical solder particles having no flat portion.
  • solder particles are formed on the convex portion of the substrate.
  • the flat surface portion may be formed at the contact surface between the solder particles and the top portion of the convex portion.
  • solder particles When a quadrangle circumscribing the projected image of solder particles is created by two pairs of parallel lines, and the distance between the opposing sides is X and Y (where Y ⁇ X), the ratio of Y to X (Y / X) may be more than 0.8 and less than 1.0 (0.8 ⁇ Y / X ⁇ 1.0), and may be 0.9 or more and less than 1.0.
  • solder particles can be said to be particles closer to a true sphere. According to the manufacturing method of the present embodiment described above, such solder particles can be easily obtained.
  • solder particles are close to a true sphere, for example, when a plurality of opposing electrodes are electrically connected via the solder particles, the contact between the solder particles and the electrodes is less likely to be uneven, and a stable connection can be obtained. Tend. Further, when a conductive film or resin in which solder particles are dispersed in a resin material is produced, high dispersibility is obtained, and dispersion stability during production tends to be obtained.
  • solder particles are dispersed in a resin material
  • FIG. 8 is a diagram showing distances X and Y (where Y ⁇ X) between opposite sides when a quadrangle circumscribing a projected image of solder particles is created by two pairs of parallel lines.
  • a quadrangle circumscribing a projected image of solder particles is created by two pairs of parallel lines.
  • an arbitrary particle is observed with a scanning electron microscope to obtain a projected image.
  • Two pairs of parallel lines are drawn with respect to the obtained projected image, and the pair of parallel lines are arranged at the position where the distance between the parallel lines is the minimum, and the other pair of parallel lines are arranged at the position where the distance between the parallel lines is the maximum.
  • Find the Y / X of the particle This operation is performed on 300 solder particles, the average value is calculated, and the Y / X of the solder particles is obtained.
  • the solder particles may contain tin or a tin alloy.
  • tin alloy for example, In—Sn alloy, In—Sn—Ag alloy, Sn—Au alloy, Sn—Bi alloy, Sn—Bi—Ag alloy, Sn—Ag—Cu alloy, Sn—Cu alloy and the like are used. be able to. Specific examples of these tin alloys include the following examples.
  • the solder particles may contain indium or an indium alloy.
  • the indium alloy for example, an In—Bi alloy, an In—Ag alloy, or the like can be used. Specific examples of these indium alloys include the following examples. -In-Bi (In66.3% by mass, Bi33.7% by mass, melting point 72 ° C.) -In-Bi (In33.0% by mass, Bi67.0% by mass, melting point 109 ° C) -In-Ag (In97.0% by mass, Ag3.0% by mass, melting point 145 ° C)
  • the above tin alloy or indium alloy can be selected according to the application (temperature at the time of use) of the solder particles.
  • an In—Sn alloy or a Sn—Bi alloy may be used, and in this case, the solder particles can be fused at 150 ° C. or lower.
  • a material having a high melting point such as Sn—Ag—Cu alloy or Sn—Cu alloy is used, high reliability can be maintained even after being left at a high temperature.
  • the solder particles may contain one or more selected from Ag, Cu, Ni, Bi, Zn, Pd, Pb, Au, P and B.
  • Ag or Cu may be contained from the following viewpoints. That is, when the solder particles contain Ag or Cu, the melting point of the solder particles can be lowered to about 220 ° C., and the bonding strength with the electrode is further improved, so that better conduction reliability can be obtained. It will be easier.
  • the Cu content of the solder particles is, for example, 0.05 to 10% by mass, and may be 0.1 to 5% by mass or 0.2 to 3% by mass.
  • the Cu content is 0.05% by mass or more, it becomes easy to achieve better solder connection reliability.
  • the Cu content is 10% by mass or less, the melting point is low and the solder particles tend to have excellent wettability, and as a result, the connection reliability of the joint portion by the solder particles tends to be good.
  • the Ag content of the solder particles is, for example, 0.05 to 10% by mass, and may be 0.1 to 5% by mass or 0.2 to 3% by mass.
  • the Ag content is 0.05% by mass or more, it becomes easy to achieve better solder connection reliability.
  • the Ag content is 10% by mass or less, the melting point is low and the solder particles tend to have excellent wettability, and as a result, the connection reliability of the joint portion by the solder particles tends to be good.
  • solder particles is not particularly limited, and for example, it can be suitably used as conductive particles for an anisotropic conductive material.
  • applications such as ball grid array connection method (BGA connection), which is widely used for mounting semiconductor integrated circuits, are used to electrically connect electrodes, and parts such as MEMS are sealed, sealed, brazed, and high. It can also be suitably used for applications such as a spacer for controlling a sheath gap. That is, the solder particles can be used for general applications in which conventional solder is used.
  • BGA connection ball grid array connection method
  • Step a1 Preparation of a substrate A substrate (polyimide film, thickness 50 ⁇ m) having a plurality of convex portions having a top diameter of 0.15 ⁇ m ⁇ , a bottom diameter of 0.15 ⁇ m ⁇ , and a height of 0.13 ⁇ m was prepared. The plurality of protrusions were regularly arranged at intervals of 0.15 ⁇ m.
  • Step b1 Formation of Solder Layer
  • the substrate having a plurality of convex portions obtained in the step a1 was put into a sputtering apparatus (manufactured by Arios Co., Ltd.), and after evacuation, argon gas was added to make the inside of the apparatus an argon atmosphere of 1 Pa. .. Then, sputtering was carried out under the following conditions for the time shown in Table 1 to form a solder layer.
  • Target Sn-Bi solder plate (melting point 139 ° C) Input power ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ 60W
  • Step c1 Formation of solder particles
  • the substrate having the solder layer obtained in step b1 is put into a formic acid radical reduction furnace (reflow equipment manufactured by Shinko Seiki Co., Ltd.), vacuumed, and then formic acid mixed nitrogen gas (formic acid content 4). %) was introduced into the furnace to fill the inside of the furnace. Then, the inside of the furnace was adjusted to 120 ° C., and the reduction treatment was carried out for 5 minutes. Then, after heating to 180 ° C., the gas in the furnace is removed by vacuuming, nitrogen is introduced into the furnace to return it to atmospheric pressure, and then the temperature inside the furnace is lowered to room temperature to form solder particles. bottom.
  • the substrate having the solder particles obtained in step c1 was fixed on the conductive tape fixed to the surface of the SEM observation pedestal. Then, platinum sputtering was carried out under the conditions of 20 mA and 60 seconds. The diameter of 200 core-shell type solder particles was measured by SEM, and the average particle diameter and C.I. V. The value was calculated. The results are shown in Table 1.
  • Example 2 to 12 Solder particles were prepared and evaluated in the same manner as in Example 1 with the top diameter, bottom diameter, height, interval, sputtering time and material shown in Table 1. The results are shown in Table 1. Further, FIG. 12 shows an SEM image of the solder particles obtained in Example 2.
  • Examples 13 to 17 Solder particles were produced in the same manner as in Example 1 with the top diameter, bottom diameter, height, spacing, sputtering time and material shown in Table 1, except that the following step c2 was performed instead of step c1. And evaluated. The results are shown in Table 1.
  • the SEM image of the substrate prepared in Example 13 is shown in FIG. 9, the SEM image of the solder layer formed on the substrate is shown in FIG. 10, and the SEM image of the solder particles formed is shown in FIG.
  • Step c2 Formation of solder particles
  • the substrate having the solder layer obtained in step b1 is put into a hydrogen radical reduction furnace (plasma reflow device manufactured by Shinko Seiki Co., Ltd.), vacuumed, and then hydrogen gas is introduced into the furnace.
  • the inside of the furnace was filled with hydrogen gas.
  • the inside of the furnace was adjusted to 130 ° C. and irradiated with hydrogen radicals for 5 minutes.
  • the hydrogen gas in the furnace is removed by vacuuming, and after heating to 165 ° C., nitrogen is introduced into the furnace to return it to atmospheric pressure, and then the temperature inside the furnace is lowered to room temperature to remove the solder particles. Formed.
  • solder particles were prepared and evaluated in the same manner as in Example 2 except that a smooth substrate (polyimide film, thickness 50 ⁇ m) having no convex portion was prepared. The results are shown in Table 1. An SEM image of the obtained solder particles is shown in FIG.
  • Solder particles 10 ... Base, 11,21 ... Convex, 12, 22 ... Bottom, 50 ... Solder layer, 100, 110 ... Base with solder particles.

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