WO2019172010A1 - めっき膜、及びめっき被覆部材 - Google Patents

めっき膜、及びめっき被覆部材 Download PDF

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Publication number
WO2019172010A1
WO2019172010A1 PCT/JP2019/007181 JP2019007181W WO2019172010A1 WO 2019172010 A1 WO2019172010 A1 WO 2019172010A1 JP 2019007181 W JP2019007181 W JP 2019007181W WO 2019172010 A1 WO2019172010 A1 WO 2019172010A1
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WIPO (PCT)
Prior art keywords
plating film
plating
film
ratio
conductive bonding
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
Application number
PCT/JP2019/007181
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English (en)
French (fr)
Inventor
健吾 後藤
細江　晃久
正 有川
佐藤　裕也
正敏 永嶋
翔平 村上
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.)
ALMT Corp
Sumitomo Electric Industries Ltd
Original Assignee
ALMT Corp
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 ALMT Corp, Sumitomo Electric Industries Ltd filed Critical ALMT Corp
Priority to JP2020504936A priority Critical patent/JP7101756B2/ja
Priority to KR1020207024953A priority patent/KR102549377B1/ko
Priority to US16/977,841 priority patent/US11380602B2/en
Priority to EP19764913.0A priority patent/EP3763851A4/en
Priority to CN201980017596.7A priority patent/CN111819310B/zh
Publication of WO2019172010A1 publication Critical patent/WO2019172010A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Definitions

  • the present disclosure relates to a plating film and a plating coating member.
  • This application claims priority based on Japanese Patent Application No. 2018-041281, which is a Japanese patent application filed on March 7, 2018. All the descriptions described in the Japanese patent application are incorporated herein by reference.
  • Patent Document 1 discloses that thallium is added as a crystal modifier in a gold plating film covering a silver wire.
  • the plating film according to the present disclosure is: A plating film containing Au and Tl, Tl oxide containing Tl 2 O is provided on the surface of the plating film, In the surface, the ratio of Tl atoms constituting Tl 2 O to the total of Tl atoms constituting Tl oxide and Tl atoms constituting Tl simple substance is 40% or more.
  • the plated coating member according to the present disclosure is A plating coating member comprising a base material and a plating film that covers the base material, and being joined to a mating member via a conductive joining material,
  • the plating film is a plating film according to the present disclosure.
  • Drawing 1 is a schematic structure figure showing a plating covering member concerning an embodiment.
  • 2 shows the sample No. 1 of Test Example 1.
  • FIG. 4 is a photograph showing a wet state of the plated coating member of 1-4 and a conductive bonding material.
  • FIG. 3 shows the sample No. 1 of Test Example 1.
  • 1-11 is a photograph showing a wet state with a conductive bonding material, which is a plated coating member of 1-11.
  • a plating-coated member whose substrate is coated with a plating film may be bonded to a mating member via a conductive bonding material such as an Ag paste.
  • a conductive bonding material such as an Ag paste.
  • the plating film of the plating covering member has a wet area ratio (wet area ratio) of 90% or more with respect to the total area of the bonding region with the conductive bonding material.
  • wet area ratio wet area ratio
  • an object of the present disclosure is to provide a plating film having excellent wettability with a conductive bonding material.
  • Another object of the present disclosure is to provide a plating-coated member having excellent wettability with a conductive bonding material. [Effects of the present disclosure] The plated film and the plated coating member are excellent in wettability with the conductive bonding material.
  • a plating film according to an embodiment of the present disclosure is a plating film containing Au and Tl, and includes a Tl oxide containing Tl 2 O on the surface of the plating film, and the Tl oxide is formed on the surface.
  • the ratio of Tl atoms constituting Tl 2 O to the total of Tl atoms constituting Tl atoms constituting Tl simple substance is 40% or more.
  • Tl 2 O is excellent in wettability with the conductive bonding material. Therefore, on the surface of the plating film, the ratio of Tl atoms constituting Tl 2 O is 40% or more with respect to the total of Tl atoms constituting Tl oxide and Tl atoms constituting Tl alone,
  • the plating film is excellent in wettability with the conductive bonding material. Specifically, in the plating film, the ratio of the wetted area (wet area ratio) to the total area of the bonding region with the conductive bonding material can satisfy 90% or more. By being excellent in wettability between the plating film and the conductive bonding material, it is possible to improve the bondability between the plating film and the mating member via the conductive bonding material.
  • the content of Tl contained in the entire plating film may be 10 ppm or more and 600 ppm or less by mass ratio.
  • Tl in the plating film When the content of Tl contained in the entire plating film is 10 ppm or more, Tl in the plating film is concentrated on the surface, and Tl 2 O is easily present on the surface of the plating film, and the wettability with the conductive bonding material. It is easy to obtain a plating film excellent in. When a large amount of Tl is contained inside the plating film, the plating film tends to be peeled off from the substrate to be coated. When the content of Tl contained in the entire plating film is 600 ppm or less, the content of Tl inside the plating film after the concentration of Tl on the surface of the plating film can be sufficiently reduced, and the substrate is reduced. Therefore, it is easy to suppress peeling of the plating film.
  • an average thickness is 0.1 ⁇ m or more.
  • the average thickness of the plating film is 0.1 ⁇ m or more, it is easy to suppress corrosion due to oxidation of the base material on which the plating film is coated.
  • the plating coating member which concerns on embodiment of this indication is a plating coating member provided with a base material and the plating film which coat
  • the plating film is the plating film according to any one of (1) to (3).
  • the plating coating member is provided with a plating film according to an embodiment of the present disclosure, so that it has excellent wettability with the conductive bonding material and excellent bonding properties with the mating member via the conductive bonding material. Moreover, since the plating film is excellent in wettability with the conductive bonding material, it is difficult to form a gap between the conductive bonding material and the plating film, and the thermal resistance due to the gap can be reduced. Since the thermal resistance of the conductive bonding material can be reduced, heat transfer between the mating member and the plated coating member can be favorably performed via the conductive bonding material.
  • the plating covering member is a heat dissipation member
  • the conductive bonding material is an Ag paste
  • the counterpart member is a semiconductor chip
  • the heat generated by the semiconductor chip can be released to the heat dissipation member via the conductive bonding material, The failure of the semiconductor chip can be prevented.
  • the base material includes a plate material and a film mainly containing Ni that covers the plate material, and the plate material includes Cu, Ag, Al, Mo, W, and A metal containing one or more selected from Mg, or a composite material containing one or more selected from Cu, Ag, Al, Mo, W, and Mg and one or more selected from diamond and silicon carbide. Is mentioned.
  • the plating coated member itself is excellent in heat dissipation, and the plate material, which is the main component member of the base material, is coated with a film containing Ni as a main component, thereby preventing corrosion of the base material due to oxidation or the like. Easy to suppress.
  • the plating film 3 according to the embodiment contains Au and Tl.
  • the plating film 3 according to the embodiment includes a Tl oxide 32 containing Tl 2 O on the surface of the plating film 3, and the ratio of Tl atoms constituting Tl 2 O on the surface of the plating film 3 is Tl oxide.
  • One of the features is that it is 40% or more based on the total of Tl atoms constituting Tl atoms and Tl atoms constituting Tl simple substance.
  • ratio X the ratio of the Tl atoms constituting Tl 2 O to the total of the Tl atoms constituting the Tl oxide 32 and the Tl atoms constituting the Tl simple substance 31 on the surface of the plating film 3 is also referred to as “ratio X”.
  • the plating film 3 is mainly made of gold (Au). “Mainly composed of Au” means containing 99 mass% or more of Au, and may be pure Au or an Au alloy containing one or more kinds of Co, Ni, Fe, Cu, Sn, Ag and the like.
  • the plating film 3 mainly composed of Au is excellent in electrical conductivity, bondability with a mating member through a conductive bonding material, corrosion resistance, and the like.
  • the plating film 3 contains thallium (Tl).
  • Tl is described in detail in the method for producing a plating film described later, but is included as a crystal modifier.
  • Tl exists in the crystal grains 30 a of Au inside the plating film 3, exists in the crystal grain boundaries 30 b, or exists on the surface of the plating film 3.
  • the Tl existing inside the plating film 3 is typically present as a single Tl 31.
  • Tl present on the surface of the plating film 3 typically exists as a single Tl 31 and a Tl oxide 32.
  • the Tl simple substance 31 and the Tl oxide 32 are shown in the same size and are shown with an appropriate interval. What is the actual Tl simple substance and the Tl oxide? Different size and spacing.
  • the Tl simple substance 31 and the Tl oxide 32 existing on the surface of the plating film 3 will be described in detail in a plating film manufacturing method described later.
  • the Tl simple substance existing inside the plating film 3 is used. 31 is formed by moving to the surface of the plating film 3. Therefore, Tl contained in the plating film 3 is concentrated on the surface of the plating film 3, and mainly exists as a Tl simple substance 31 and a Tl oxide 32 on the surface of the plating film 3.
  • Tl oxide 32 present on the surface of the plating film 3 examples include Tl 2 O and Tl 2 O 3 .
  • Tl 2 O contributes to improvement of wettability between the plating film 3 and the conductive bonding material.
  • Tl 2 O 3 reduces the wettability between the plating film 3 and the conductive bonding material.
  • the Tl simple substance 31 also reduces the wettability between the plating film 3 and the conductive bonding material.
  • Tl 2 O present on the surface of the plating film 3 is exposed from the surface of the plating film 3.
  • the Tl 2 O present on the surface of the plating film 3 may adhere to the surface of the plating film 3, or part of the Tl 2 O may be embedded in the plating film 3 and the rest may be exposed from the plating film 3.
  • Tl 2 O only needs to be embedded in the plating film 3 to such an extent that the Tl 2 O can be held in the plating film 3, and the exposed portion from the plating film 3 is preferably wide. When the exposed portion of Tl 2 O comes into contact with the conductive bonding material, wettability can be improved.
  • the ratio X is 40% or more.
  • the ratio X is 40% or more, the wettability with the conductive bonding material can be improved, and the bondability with the counterpart member through the conductive bonding material can be improved.
  • the value of the ratio X is larger, the wettability with the conductive bonding material can be improved.
  • the ratio X exceeds a certain amount, wettability (wetting area ratio) can be saturated.
  • the ratio X can be measured by X-ray photoelectron spectroscopy (XPS).
  • XPS X-ray photoelectron spectroscopy
  • Tl oxide Tl 2 O
  • Tl 2 O 3 Tl oxide
  • the peak of Tl alone and the peak of Tl 2 O 3 are detected at substantially the same position, and the intensity of 117.4 eV is measured as Tl alone.
  • Tl 2 O 3 can be regarded as the height A of the total peak intensity.
  • the Tl 2 O peak is detected separately from the Tl single peak and the Tl 2 O 3 peak, and the intensity of 118.6 eV can be regarded as the intensity B of the Tl 2 O peak intensity.
  • the ratio X is a ratio of the intensity of each peak ( ⁇ B / (A + B) ⁇ ⁇ 100).
  • the content of Tl contained in the entire plating film 3 is 10 to 600 ppm by mass.
  • Tl in the plating film 3 is concentrated on the surface of the plating film 3, and Tl 2 O is easily present on the surface of the plating film 3.
  • the content of Tl contained in the entire plating film 3 is 600 ppm or less, in the manufacturing process of the plating film 3, the Tl inside the plating film 3 after the concentration of Tl on the surface of the plating film 3 is concentrated. Therefore, it is easy to suppress the plating film 3 from being peeled from the substrate on which the plating film 3 is coated.
  • the ratio X has substantially no correlation with the content of Tl contained in the entire plating film 3.
  • the content of Tl contained in the entire plating film 3 can be measured, for example, by performing ICP (Inductively Coupled Plasma) emission spectroscopic analysis. Specifically, the plating film 3 is dissolved with an acid or the like, and ICP emission spectroscopic analysis is performed using the dissolved solution as a sample.
  • the content of Tl contained in the entire plating film 3 is further 30 to 500 ppm, particularly 60 to 400 ppm.
  • the average thickness of the plating film 3 is 0.1 ⁇ m or more.
  • the average thickness of the plating film 3 is 0.1 ⁇ m or more, it is easy to suppress corrosion due to oxidation or the like of the substrate 2 on which the plating film 3 is coated.
  • the average thickness of the plating film 3 is 5.0 ⁇ m or less because the cost increases and the industrial productivity decreases as the thickness increases.
  • the average thickness of the plating film 3 is observed, for example, by observing a cross section in the thickness direction of the plating film 3 with a scanning electron microscope (SEM) at a 3000-fold field of view (for example, five or more locations).
  • SEM scanning electron microscope
  • the thickness of the plating film 3 is measured at a plurality of points (for example, 10 points or more) at regular intervals, and the average of all the micrographs is calculated.
  • the average thickness of the plating film 3 is further 0.3 to 3.0 ⁇ m, particularly 0.5 to 2.0 ⁇ m.
  • the plating film 3 described above constitutes the plating coating member 1 by being coated on the base material 2.
  • the plated coating member 1 according to the embodiment is bonded to the mating member via a conductive bonding material.
  • the plating covering member 1 is a member equipped in a semiconductor device, for example.
  • the plating coating member 1 is a semiconductor chip or a heat dissipation member to which the semiconductor chip is attached.
  • An example of the conductive bonding material is an Ag paste.
  • the base material 2 includes a plate material and a film 23 mainly composed of Ni that covers the plate material.
  • the plate material is a metal containing at least one selected from Cu, Ag, Al, Mo, W, and Mg, or at least one selected from Cu, Ag, Al, Mo, W, and Mg, and diamond and silicon carbide. It is mentioned that it consists of a composite material containing 1 or more types selected from.
  • the plate material is a metal plate containing Cu, and has a laminated structure in which a first metal plate 21 made of a Cu alloy is sandwiched between a pair of second metal plates 22 made of Cu alone. The average thickness of the first metal plate 21 and the second metal plate 22 can be selected as desired.
  • the film 23 containing Ni as a main component covers the entire surface of the plate material.
  • Ni as a main component means containing 90 mass% or more of Ni, which may be pure Ni or Ni alloy containing one or more kinds of Co, Pd and the like.
  • the film 23 mainly composed of Ni may be formed by a plating method such as electric Ni plating, electroless Ni—P plating, or electroless Ni—B plating, or may be formed by a physical vapor deposition method such as a sputtering method or a vapor deposition method. May be.
  • the average thickness of the film 23 containing Ni as a main component is, for example, 1.0 to 10 ⁇ m.
  • the plating film 3 covers the entire surface of the film 23 containing Ni as a main component. In FIG. 1, the thickness of each member is shown to be thicker than the actual thickness for easy understanding. If the base material 2 is a member which can be coat
  • the plating covering member 1 according to the embodiment includes the plating film 3 according to the above-described embodiment on the surface of the base material 2, the plating covering member 1 is excellent in wettability with the conductive bonding material.
  • the plating covering member 1 according to the embodiment has a wet area ratio of 90% or more with the conductive bonding material.
  • the wet area ratio is the ratio of the wet area to the total area of the bonding region between the plating film 3 and the conductive bonding material.
  • the wetted area ratio of the plating film 3 with the conductive bonding material can be measured by, for example, observing a sample in which the conductive bonding material is attached to the plating coating member 1 with an optical microscope and analyzing the micrograph. .
  • the wet area ratio is 90% or more, it is difficult to form a gap at the joint between the plating covering member 1 and the mating member, and the plating covering member 1 and the mating member can be favorably joined.
  • the plating film 3 and the plating covering member 1 described above can be manufactured by a process including a plating process, a heat treatment process, and an oxidation process.
  • plating is performed on a surface of the object to be plated using a plating bath containing Au and Tl until the plating film has a desired thickness.
  • the plating object is, for example, the base material 2 in which the surface of a plate material is coated with a film 23 containing Ni as a main component (see FIG. 1).
  • the plating method is, for example, electrolytic plating in which an object to be plated (base material 2) is immersed in a plating bath and electrodeposited. When plating only a part of the plating object (base material 2), masking is performed on a region where plating is not performed.
  • Tl contained in the plating bath is contained as a crystal modifier.
  • the crystal adjusting agent for example, thallium formate, thallium malonate, thallium sulfate, thallium nitrate, thallium cyanate and the like are used.
  • the content of Tl contained in the plating bath is 0.5 to 30 ppm. When the content of Tl contained in the plating bath is 0.5 ppm or more, the content of Au can be relatively reduced, and the cost of the plating bath can be reduced. In addition, the Au complex contained in the plating bath can be stabilized, the life of the plating bath can be improved, and the components constituting the plating bath can be easily managed.
  • the content of Tl contained in the plating bath is 30 ppm or less, it is easy to form a plating film uniformly on the plating object (base material 2).
  • a known plating bath can be used as the composition of the plating bath.
  • the content of Tl contained in the formed plating film, the thickness of the plating film, and the like can be adjusted.
  • adjusting the current value for energizing the plating bath, adjusting the temperature of the plating bath, and the like can be mentioned.
  • the content of Tl contained in the formed plating film can be increased by increasing the value of the current applied to the plating bath or lowering the temperature of the plating bath.
  • the plating conditions of the plating bath may be adjusted so that the content of Tl contained in the entire plating film to be formed is 10 to 600 ppm.
  • the plating film formed by the plating process described above has Tl almost uniformly in the thickness direction of the plating film.
  • Tl contained in the plating film formed in the plating step exists mainly in the Au crystal grain boundary as a single Tl within the plating film, and may also exist in the Au crystal grain.
  • the plating film formed in the plating step is referred to as a first plating film
  • the plating coating member including the first plating film is referred to as a first plating coating member.
  • the first plating covering member is heat-treated in an atmosphere substantially free of oxygen element.
  • Tl existing inside the first plating film is concentrated on the surface of the first plating film.
  • Tl mainly present at the crystal grain boundary of Au is the surface of the first plating film.
  • the atmosphere substantially free of oxygen element means that the oxygen concentration is 20 ppm or less by mass ratio.
  • Examples of the atmosphere that does not substantially contain an oxygen element include an H 2 gas atmosphere, an inert gas atmosphere such as Ar and N 2 , and a mixed gas atmosphere of H 2 gas and inert gas.
  • the heat treatment temperature is 200 to 500 ° C.
  • the heat treatment temperature is 200 to 500 ° C.
  • Au of the first plating film can be recrystallized, and at the same time, at least a part of Tl existing at the grain boundary of Au is regenerated as the first plating film. Can be moved to the surface.
  • the higher the heat treatment temperature the more Tl present in the Au grain boundaries can be moved to the surface of the first plating film.
  • the heat treatment temperature is further 250 to 480 ° C., particularly 300 to 450 ° C.
  • the holding time for the heat treatment is 1 to 10 minutes.
  • Au of the first plating film can be recrystallized, and at least a part of Tl present at the grain boundary of Au is first generated along with the recrystallization of Au. It can be moved to the surface of the plating film.
  • the longer the heat treatment is held the more Tl present in the Au crystal grain boundary can be moved to the surface of the first plating film.
  • the Au of the first plating film is sufficiently recrystallized if the heat treatment is held for 10 minutes. Therefore, the manufacturing time can be shortened by setting the heat treatment holding time to 10 minutes or less.
  • the holding time for the heat treatment is further 2 to 8 minutes, particularly 3 to 5 minutes.
  • Tl is concentrated on the surface of the plating film.
  • Tl present on the surface of the plating film is present mainly as a single Tl immediately after the heat treatment.
  • a plating film obtained by subjecting the first plating film to a heat treatment step is referred to as a second plating film, and a plating coating member including the second plating film is referred to as a second plating coating member.
  • the second plating covering member is left in an atmosphere containing an oxygen element.
  • Tl present on the surface of the second plating film is oxidized to form Tl oxide.
  • This Tl oxide is Tl 2 O and Tl 2 O 3 .
  • the atmosphere containing an oxygen element means, for example, that the oxygen concentration is 500 ppm or more by mass ratio.
  • the atmosphere containing the oxygen element includes air.
  • the leaving in the atmosphere containing the oxygen element is preferably performed at room temperature. This is because when the oxidation process is performed at normal temperature in the air, no special atmosphere control or temperature control is required.
  • the standing time in an atmosphere containing oxygen element is 1 to 24 hours. By setting the standing time to 1 hour or longer, 40% or more of Tl out of Tl existing on the surface of the second plating film can be oxidized to Tl 2 O. The remainder of Tl present on the surface of the second plating film exists as Tl alone or is oxidized to Tl 2 O 3 .
  • the standing time exceeds a certain length the oxidation to Tl 2 O can be saturated.
  • Tl of the second plating film can be sufficiently oxidized to Tl 2 O if the standing time in the atmosphere containing oxygen element is 24 hours. Therefore, the manufacturing time can be shortened by setting the leaving time in the atmosphere containing the oxygen element to 24 hours or less.
  • the oxidation of Tl depends on external factors such as moisture. Therefore, the standing time in the atmosphere containing oxygen element may be appropriately adjusted according to external factors.
  • Tl existing on the surface of the second plating film is easily oxidized to Tl 2 O, and thus the standing time can be shortened.
  • the standing time in the atmosphere containing oxygen element is further 3 to 20 hours, particularly 6 to 16 hours.
  • the plating film 3 obtained by subjecting the second plating film to an oxidation process includes a Tl oxide 32 containing Tl 2 O on the surface of the plating film 3.
  • the ratio X in the plating film 3 is 40% or more.
  • Tl on the surface of the plating film 3 has only to be present above 40% Tl 2 O, not particularly limited to the remainder of the form.
  • the plating film 3 includes the Tl oxide 32 containing Tl 2 O on the surface thereof, and the ratio X is 40% or more on the surface of the plating film 3, so that wettability with the conductive bonding material is achieved. Can be improved.
  • the plating film 3 can satisfy a wet area ratio of 90% or more with the conductive bonding material. Therefore, the plating covering member 1 which concerns on embodiment provided with the said plating film 3 can improve the joining property with the other party member via an electroconductive joining material.
  • the plating covering member 1 which concerns on embodiment provided with the said plating film 3 can improve the joining property with the other party member via an electroconductive joining material.
  • it is difficult for voids to be formed at the joint between the plated coating member 1 and the mating member, and the thermal resistance that can occur at the joint can be reduced.
  • the plating covering member 1 is a heat radiating member and the counterpart member is a semiconductor chip, the heat generated by the semiconductor chip can be released well to the heat radiating member, and the failure of the semiconductor chip can be
  • the content of Tl contained in the entire plating film 3 is 10 ppm or more, so that Tl in the plating film 3 is concentrated on the surface, and Tl 2 O is added to the surface of the plating film 3. Easy to exist. Since Tl contained in the plating film 3 is mainly present on the surface of the plating film 3 and is small inside the plating film 3, the plating film 3 is peeled off from the mating member covered with the plating film 3. Can be suppressed.
  • Test Example 1 A sample of a plating coated member provided with a plating film containing Au and Tl was prepared, and the ratio of Tl 2 O present on the surface of the plating film of each sample and the wet area ratio were examined.
  • Example preparation The surface of the object to be plated was subjected to electrolytic plating using a plating bath containing Au and Tl (Sample Nos. 1-1 to 1-4, 1-11).
  • a metal plate having a laminated structure in which a first metal plate made of a Cu—Mo-based alloy is sandwiched between second metal plates made of Cu alone is prepared, and the surface of this metal plate is mainly composed of Ni.
  • membrane (electric Ni plating film) to be used was used (refer FIG. 1).
  • a plating bath prepared by adjusting potassium gold cyanide and thallium nitrate was used.
  • the electrolytic plating was performed until the Tl concentration was 10 ppm by mass, the current density was 0.5 A / dm 2 , the temperature of the plating bath was 60 ° C., and the thickness of the plating film was 1.5 ⁇ m.
  • the content of Tl in the entire plated film obtained by this plating condition was 35 ppm by mass ratio.
  • each sample whose surface was electroplated was subjected to heat treatment at 310 ° C. for 1 minute in an H 2 gas atmosphere.
  • sample No. Nos. 1-1 to 1-4 were left for a standing time shown in Table 1 in a room temperature atmosphere.
  • sample No. An Ag paste was applied to 1-1 to 1-4.
  • 50 ⁇ l of the Ag paste was dropped on the sample, and then the droplet was spread using a squeegee. The squeegee height was 30 ⁇ m.
  • sample No. For No. 1-11 the Ag paste was applied immediately after the heat treatment without being left in the room temperature atmosphere. In any sample, the application area of the Ag paste was set to 3.0 mm ⁇ 2.5 mm.
  • the sample no. In 1-2 to 1-4, the ratio of Tl atoms constituting Tl 2 O to the total of Tl atoms constituting Tl oxide and Tl atoms constituting Tl simple substance on the plating film surface is 40% or more. It can be seen that the wet area ratio is 90% or more and the wettability is excellent. This is presumably because Tl concentrated on the surface of the plating film by the heat treatment was sufficiently oxidized because it was left for 1 hour or more after the heat treatment. On the other hand, after the heat treatment, the sample no. For 1-1, the above ratio is 32%, and the wetted area ratio is 85%, indicating that the wettability is poor. In addition, immediately after the heat treatment, the sample No.
  • the above ratio is 28%, and the wetted area ratio is 80%, which indicates that the wettability is very poor. This is because the standing time after the heat treatment is short or not left, so that the Tl concentrated on the surface of the plating film by the heat treatment is not sufficiently oxidized, and the wettability such as Tl alone or Tl 2 O 3 is reduced on the surface of the plating film. This is probably due to the remaining Tl.
  • Test Example 2 A sample of the plating coated member provided with a plating film containing Au and Tl was prepared, and the content of Tl contained in the entire plating film of each sample and the wet area ratio were examined.
  • Example preparation Electroplating was performed on the surface of the plating object using a plating bath containing Au and Tl (Sample Nos. 2-1 to 2-4). The same substrate as in Test Example 1 was used as the plating object.
  • the plating bath used was prepared by adjusting potassium gold cyanide and thallium nitrate as in Test Example 1, and the plating conditions were the Tl concentration (mass ratio), current density, and temperature shown in Table 2.
  • Table 2 also shows the Tl content of the entire plated film obtained under each plating condition. The thickness of the plating film was 1 ⁇ m for all samples.
  • Each sample whose surface was electroplated on the surface of the base material was subjected to a heat treatment at 310 ° C. for 1 minute in an H 2 gas atmosphere and then left at room temperature for 14 hours.
  • the paste was applied.
  • the application area of the Ag paste was set to 3.0 mm ⁇ 2.5 mm.
  • the wet area ratio did not depend on the content of Tl contained in the entire plating film. This is presumably because, when a certain amount of Tl is contained in the plating film, the Tl concentrated on the surface of the plating film by the heat treatment is sufficiently oxidized by leaving it sufficiently after the heat treatment. Since the wet area ratio does not depend on the content of Tl contained in the entire plating film, the content of Au can be relatively reduced by increasing the content of Tl contained in the entire plating film. Expected to reduce costs. Also, by increasing the content of Tl contained in the entire plating film, it is possible to stabilize the Au complex in the plating bath, improve the life of the plating bath, and easily manage the components constituting the plating bath. Expected to be able to.

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Abstract

Ａｕ及びＴｌを含むめっき膜であって、前記めっき膜の表面にＴｌ２Ｏを含むＴｌ酸化物を備え、前記表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合が４０％以上であるめっき膜。

Description

めっき膜、及びめっき被覆部材
　本開示は、めっき膜、及びめっき被覆部材に関する。本出願は、２０１８年３月７日に出願した日本特許出願である特願２０１８－０４１２８１号に基づく優先権を主張する。当該日本特許出願に記載された全ての記載内容は、参照によって本明細書に援用される。
　特許文献１には、銀線を被覆する金めっき膜中に、結晶調整剤としてタリウムが添加されることが開示されている。
特開平１１－２４３１１１号公報
　本開示に係るめっき膜は、
　Ａｕ及びＴｌを含むめっき膜であって、
　前記めっき膜の表面にＴｌ２Ｏを含むＴｌ酸化物を備え、
　前記表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合が４０％以上である。
　本開示に係るめっき被覆部材は、
　基材と、前記基材を被覆するめっき膜とを備え、導電性接合材料を介して相手部材に接合されるめっき被覆部材であって、
　前記めっき膜は、上記本開示に係るめっき膜である。
図１は、実施形態に係るめっき被覆部材を示す概略構成図である。 図２は、試験例１の試料Ｎｏ．１－４のめっき被覆部材であって、導電性接合材料との濡れ状態を示す写真である。 図３は、試験例１の試料Ｎｏ．１－１１のめっき被覆部材であって、導電性接合材料との濡れ状態を示す写真である。
[本開示が解決しようとする課題]
　基材にめっき膜が被覆されためっき被覆部材は、Ａｇペーストなどの導電性接合材料を介して相手部材に接合されることがある。このとき、めっき被覆部材と導電性接合材料との濡れ性が良好であることが望まれる。具体的には、めっき被覆部材のめっき膜は、導電性接合材料との接合領域の全面積に対する濡れている面積の割合（濡れ面積率）が、９０％以上であることが望まれる。しかし、従来では、タリウムを含む金めっき膜において、濡れ面積率を９０％以上とすることについては、十分な検討がなされていない。
　そこで、本開示は、導電性接合材料との濡れ性に優れるめっき膜を提供することを目的の一つとする。また、本開示は、導電性接合材料との濡れ性に優れるめっき被覆部材を提供することを別の目的の一つとする。
[本開示の効果]
　上記めっき膜及び上記めっき被覆部材は、導電性接合材料との濡れ性に優れる。
　［本開示の実施形態の説明］
　最初に、本開示の実施形態の内容を列記して説明する。
　（１）本開示の実施形態に係るめっき膜は、Ａｕ及びＴｌを含むめっき膜であって、前記めっき膜の表面にＴｌ２Ｏを含むＴｌ酸化物を備え、前記表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合が４０％以上である。
　Ｔｌ酸化物のうちＴｌ２Ｏは、導電性接合材料との濡れ性に優れる。よって、めっき膜の表面において、Ｔｌ２Ｏを構成するＴｌ原子の割合が、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対して４０％以上であることで、上記めっき膜は、導電性接合材料との濡れ性に優れる。具体的には、上記めっき膜は、導電性接合材料との接合領域の全面積に対する濡れている面積の割合（濡れ面積率）が９０％以上を満たすことができる。めっき膜と導電性接合材料との濡れ性に優れることで、導電性接合材料を介しためっき膜と相手部材との接合性を向上できる。
　（２）上記めっき膜の一例として、前記めっき膜全体に含まれるＴｌの含有量が、質量割合で１０ｐｐｍ以上６００ｐｐｍ以下であることが挙げられる。
　めっき膜全体に含まれるＴｌの含有量が１０ｐｐｍ以上であることで、めっき膜中のＴｌを表面に濃化し、めっき膜の表面にＴｌ２Ｏを存在させ易く、導電性接合材料との濡れ性に優れるめっき膜を得易い。めっき膜の内部にＴｌが多く含まれると、被覆される基材に対してめっき膜が剥がれ易い傾向にある。めっき膜全体に含まれるＴｌの含有量が６００ｐｐｍ以下であることで、めっき膜の表面にＴｌを濃化させた後のめっき膜の内部のＴｌの含有量を十分に低減でき、基材に対してめっき膜が剥がれることを抑制し易い。
　（３）上記めっき膜の一例として、平均厚さが、０．１μｍ以上であることが挙げられる。
　めっき膜の平均厚さが０．１μｍ以上であることで、めっき膜が被覆される基材の酸化などによる腐食を抑制し易い。
　（４）本開示の実施形態に係るめっき被覆部材は、基材と、前記基材を被覆するめっき膜とを備え、導電性接合材料を介して相手部材に接合されるめっき被覆部材であって、前記めっき膜は、上記（１）から（３）のいずれかに記載のめっき膜である。
　上記めっき被覆部材は、本開示の実施形態に係るめっき膜を備えることで、導電性接合材料との濡れ性に優れ、導電性接合材料を介した相手部材との接合性に優れる。また、めっき膜が導電性接合材料との濡れ性に優れることで、導電性接合材料とめっき膜との間に空隙が形成され難く、空隙に起因する熱抵抗を低減できる。導電性接合材料の熱抵抗を低減できることで、導電性接合材料を介した、相手部材とめっき被覆部材との両者間の熱の移動を良好に行うことができる。例えば、めっき被覆部材が放熱部材、導電性接合材料がＡｇペースト、及び相手部材が半導体チップである場合、半導体チップの発する熱を、導電性接合材料を介して放熱部材に放出することができ、半導体チップの故障を防止できる。
　（５）上記めっき被覆部材の一例として、前記基材は、板材と、前記板材を被覆するＮｉを主成分とする膜とを備え、前記板材は、Ｃｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上を含む金属、又はＣｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上と、ダイヤモンド及び炭化ケイ素から選択される一種以上とを含む複合材料からなることが挙げられる。
　上記構成によれば、めっき被覆部材自体の放熱性に優れ、かつ、基材の主要構成部材である板材がＮｉを主成分とする膜で被覆されることで、酸化などによる基材の腐食を抑制し易い。
　［本開示の実施形態の詳細］
　以下、図１を参照して、本開示の実施形態に係るめっき膜、及びこのめっき膜を備えるめっき被覆部材を具体的に説明する。なお、本開示はこれらの例示に限定されるものではなく、請求の範囲によって示され、請求の範囲と均等の意味及び範囲内でのすべての変更が含まれることが意図される。また本明細書において「Ａ～Ｂ」という形式の表記は、範囲の上限下限（すなわちＡ以上Ｂ以下）を意味し、Ａにおいて単位の記載がなく、Ｂにおいてのみ単位が記載されている場合、Ａの単位とＢの単位とは同じである。
　≪めっき膜≫
　実施形態に係るめっき膜３は、Ａｕ及びＴｌを含む。実施形態に係るめっき膜３は、めっき膜３の表面にＴｌ２Ｏを含むＴｌ酸化物３２を備え、そのめっき膜３の表面において、Ｔｌ２Ｏを構成するＴｌ原子の割合が、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対して４０％以上である点を特徴の一つとする。以下、めっき膜３の表面における、Ｔｌ酸化物３２を構成するＴｌ原子とＴｌ単体３１を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合を「割合Ｘ」とも記す。
　めっき膜３は、金（Ａｕ）を主体とする。Ａｕを主体とするとは、Ａｕを９９質量％以上含むことを言い、純Ａｕでもよく、Ｃｏ、Ｎｉ、Ｆｅ、Ｃｕ、Ｓｎ、Ａｇなどを一種以上含むＡｕ合金でもよい。Ａｕを主体とするめっき膜３は、電気伝導性、導電性接合材料を介した相手部材との接合性、耐食性などに優れる。
　めっき膜３は、タリウム（Ｔｌ）を含む。Ｔｌは、後述するめっき膜の製造方法にて詳述するが、結晶調整剤として含まれる。Ｔｌは、めっき膜３の内部においてＡｕの結晶粒３０ａ内に存在したり、結晶粒界３０ｂに存在したり、めっき膜３の表面に存在したりする。めっき膜３の内部に存在するＴｌは、代表的には、Ｔｌ単体３１で存在する。めっき膜３の表面に存在するＴｌは、代表的には、Ｔｌ単体３１およびＴｌ酸化物３２で存在する。なお、図１では、分かり易いように、Ｔｌ単体３１とＴｌ酸化物３２とを同じサイズで図示すると共に、適当な間隔を有して図示しており、実際のＴｌ単体およびＴｌ酸化物とはサイズおよび間隔が異なる。
　めっき膜３の表面に存在するＴｌ単体３１およびＴｌ酸化物３２は、後述するめっき膜の製造方法にて詳述するが、めっき膜３の製造過程において、めっき膜３の内部に存在するＴｌ単体３１がめっき膜３の表面に移動することで形成される。そのため、めっき膜３に含まれるＴｌは、めっき膜３の表面に濃化しており、そのめっき膜３の表面において、主にＴｌ単体３１およびＴｌ酸化物３２として存在する。
　めっき膜３の表面に存在するＴｌ酸化物３２は、Ｔｌ２ＯおよびＴｌ２Ｏ３が挙げられる。Ｔｌ２Ｏは、めっき膜３と導電性接合材料との濡れ性の向上に寄与する。一方、Ｔｌ２Ｏ３は、めっき膜３と導電性接合材料との濡れ性を低下させる。また、Ｔｌ単体３１も、めっき膜３と導電性接合材料との濡れ性を低下させる。
　めっき膜３の表面に存在するＴｌ２Ｏは、めっき膜３の表面から露出している。めっき膜３の表面に存在するＴｌ２Ｏは、めっき膜３の表面に付着していたり、一部がめっき膜３に埋設され、残部がめっき膜３から露出して存在していたりする。Ｔｌ２Ｏは、めっき膜３に保持可能な程度にめっき膜３に埋設されていればよく、めっき膜３からの露出部分は広い方が好ましい。Ｔｌ２Ｏの露出部分が導電性接合材料と接触することで、濡れ性を向上できる。
　上述のように、本実施形態において割合Ｘは４０％以上である。割合Ｘが４０％以上であることで、導電性接合材料との濡れ性を向上でき、導電性接合材料を介した相手部材との接合性を向上できる。割合Ｘの値は、大きいほど導電性接合材料との濡れ性を向上できるため、５０％以上、更に６０％以上、特に８０％以上であることが挙げられる。なお、割合Ｘがある程度の量を超えると、濡れ性（濡れ面積率）が飽和し得る。
　割合Ｘは、Ｘ線光電子分光法（ＸＰＳ：Ｘ－ｒａｙ　Ｐｈｏｔｏｅｌｅｃｔｒｏｎ　Ｓｐｅｃｔｒｏｓｃｏｐｙ）により測定できる。Ｔｌ酸化物は、Ｔｌ２ＯとＴｌ２Ｏ３の二種が存在し得る。ＸＰＳにより、１１０ｅＶから１３５ｅＶの範囲を０．２ｅＶステップで測定したナロースキャンのスペクトルでは、Ｔｌ単体のピークとＴｌ２Ｏ３のピークとはほぼ同じ位置に検出され、１１７．４ｅＶの強度をＴｌ単体とＴｌ２Ｏ３の合計のピークの強度の高さＡとみなすことができる。一方、Ｔｌ２Ｏのピークは、Ｔｌ単体のピーク及びＴｌ２Ｏ３のピークと分離して検出され、１１８．６ｅＶの強度をＴｌ２Ｏのピークの強度の高さＢと見なすことができる。本願において、割合Ｘは、各ピークの強度の高さの比（｛Ｂ／（Ａ＋Ｂ）｝×１００）とする。
　めっき膜３全体に含まれるＴｌの含有量は、質量割合で１０～６００ｐｐｍが挙げられる。めっき膜３全体に含まれるＴｌの含有量が１０ｐｐｍ以上であることで、めっき膜３中のＴｌをめっき膜３の表面に濃化し、めっき膜３の表面にＴｌ２Ｏを存在させ易い。一方、めっき膜３全体に含まれるＴｌの含有量が６００ｐｐｍ以下であることで、めっき膜３の製造過程において、めっき膜３の表面にＴｌを濃化させた後のめっき膜３の内部のＴｌの含有量を十分に低減でき、めっき膜３が被覆される基材に対してめっき膜３が剥がれることを抑制し易い。なお、割合Ｘは、めっき膜３全体に含まれるＴｌの含有量と実質的に相関関係を有しない。めっき膜３全体に含まれるＴｌの含有量は、例えば、ＩＣＰ（Ｉｎｄｕｃｔｉｖｅｌｙ　Ｃｏｕｐｌｅｄ　Ｐｌａｓｍａ）発光分光分析を行うことで測定できる。具体的には、めっき膜３を酸などで溶解し、溶解した溶液をサンプルとしてＩＣＰ発光分光分析を行う。めっき膜３全体に含まれるＴｌの含有量は、更に３０～５００ｐｐｍ、特に６０～４００ｐｐｍが挙げられる。
　めっき膜３の平均厚さは、０．１μｍ以上が挙げられる。めっき膜３の平均厚さが０．１μｍ以上であることで、めっき膜３が被覆される基材２の酸化などによる腐食を抑制し易い。一方、めっき膜３の平均厚さは、厚くなるほどコストが増大し、工業生産性が低下するため、５．０μｍ以下が挙げられる。めっき膜３の平均厚さは、例えば、めっき膜３の厚さ方向の断面を走査型電子顕微鏡（ＳＥＭ）により３０００倍の視野で複数箇所（例えば、５箇所以上）観察し、各顕微鏡写真中のめっき膜３の厚さを等間隔に複数点（例えば、１０点以上）測定し、全顕微鏡写真における平均を算出することで得られる。めっき膜３の平均厚さは、更に０．３～３．０μｍ、特に０．５～２．０μｍが挙げられる。
　≪めっき被覆部材≫
　上述しためっき膜３は、基材２に被覆されることで、めっき被覆部材１を構成する。実施形態に係るめっき被覆部材１は、導電性接合材料を介して相手部材に接合される。めっき被覆部材１は、例えば、半導体装置に装備される部材である。具体的には、めっき被覆部材１は、半導体チップや、半導体チップが装着される放熱部材である。導電性接合材料は、Ａｇペーストが挙げられる。
　基材２は、板材と、板材を被覆するＮｉを主成分とする膜２３とを備える。板材は、Ｃｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上を含む金属、又はＣｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上と、ダイヤモンド及び炭化ケイ素から選択される一種以上とを含む複合材料からなることが挙げられる。本例では、板材は、Ｃｕを含む金属板であり、Ｃｕ合金からなる第一金属板２１を、Ｃｕ単体からなる一対の第二金属板２２で挟み込んだ積層構造を有する。第一金属板２１及び第二金属板２２の平均厚さは、所望の厚さを適宜選択できる。Ｎｉを主成分とする膜２３は、板材の表面を全面に亘って被覆している。Ｎｉを主成分とするとは、Ｎｉを９０質量％以上含むことを言い、純Ｎｉでもよく、Ｃｏ、Ｐｄなどを一種以上含むＮｉ合金でもよい。Ｎｉを主成分とする膜２３は、電気Ｎｉめっき、無電解Ｎｉ－Ｐめっき、無電解Ｎｉ－Ｂめっきといっためっき法で形成してもよく、またスパッタ法や蒸着法といった物理蒸着法で形成してもよい。Ｎｉを主成分とする膜２３の平均厚さは、例えば、１．０～１０μｍが挙げられる。そして、めっき膜３は、Ｎｉを主成分とする膜２３の表面を全面に亘って被覆している。なお、図１では、分かり易いように、各部材の厚さを実際の厚さよりも厚く図示している。基材２は、実施形態に係るめっき膜３で被覆できる部材であれば、その材質及び構造は特に問わない。
　実施形態に係るめっき被覆部材１は、基材２の表面に上述した実施形態に係るめっき膜３を備えるため、導電性接合材料との濡れ性に優れる。具体的には、実施形態に係るめっき被覆部材１は、導電性接合材料との濡れ面積率が９０％以上である。濡れ面積率とは、めっき膜３と導電性接合材料との接合領域の全面積に対する濡れている面積の割合である。めっき膜３における導電性接合材料との濡れ面積率は、例えば、めっき被覆部材１に導電性接合材料を付着させた試料について、光学顕微鏡により観察し、その顕微鏡写真を画像解析することによって測定できる。上記濡れ面積率が９０％以上であることで、めっき被覆部材１と相手部材との接合部に空隙が形成され難く、めっき被覆部材１と相手部材とを良好に接合できる。
　≪めっき膜の製造方法及びめっき被覆部材の製造方法≫
　上述しためっき膜３及びめっき被覆部材１は、めっき工程と、熱処理工程と、酸化工程とを含む過程により製造できる。
　〔めっき工程〕
　めっき工程では、めっき対象物の表面の少なくとも一部に、Ａｕ及びＴｌを含むめっき浴を用いて、めっき膜が所望の厚さになるまでめっきする。めっき対象物は、例えば、板材の表面にＮｉを主成分とする膜２３が被覆された基材２である（図１を参照）。めっき方法は、例えば、めっき対象物（基材２）をめっき浴に浸漬して電着する電解めっきである。めっき対象物（基材２）の一部にのみめっきを行う場合、めっきを行わない領域にマスキングを施す。
　めっき浴に含まれるＴｌは、結晶調整剤として含まれる。結晶調整剤としては、例えば、ギ酸タリウム、マロン酸タリウム、硫酸タリウム、硝酸タリウム、シアン酸タリウムなどが用いられる。めっき浴に含まれるＴｌの含有量は、０．５～３０ｐｐｍが挙げられる。めっき浴に含まれるＴｌの含有量が０．５ｐｐｍ以上であることで、相対的にＡｕの含有量を少なくでき、めっき浴のコストを低減できる。また、めっき浴に含まれるＡｕの錯体を安定化でき、めっき浴の寿命を向上したり、めっき浴を構成する成分の管理を容易にできたりする。一方、めっき浴に含まれるＴｌの含有量が３０ｐｐｍ以下であることで、めっき対象物（基材２）へ均一にめっき膜を形成し易い。めっき浴の組成は、公知のめっき浴を利用できる。
　めっき浴のめっき条件を調整することによって、形成されるめっき膜に含まれるＴｌの含有量、めっき膜の厚さなどを調整することができる。例えば、めっき浴に通電する電流値を調整すること、めっき浴の温度を調整することなどが挙げられる。具体的には、めっき浴に通電する電流値を大きくしたり、めっき浴の温度を低くしたりすることで、形成されるめっき膜に含まれるＴｌの含有量を多くできる。めっき浴のめっき条件は、形成されるめっき膜全体に含まれるＴｌの含有量が１０～６００ｐｐｍとなるように調整することが挙げられる。
　上述しためっき工程で形成されるめっき膜は、めっき膜の厚さ方向にほぼ均一にＴｌが存在している。具体的には、めっき工程で形成されるめっき膜に含まれるＴｌは、めっき膜の内部において、主にＴｌ単体でＡｕの結晶粒界に存在し、Ａｕの結晶粒内にも存在し得る。以下、めっき工程で形成されるめっき膜を、第一めっき膜と呼び、この第一めっき膜を備えるめっき被覆部材を第一めっき被覆部材と呼ぶ。
　〔熱処理工程〕
　熱処理工程では、上記第一めっき被覆部材を、実質的に酸素元素を含まない雰囲気中で熱処理する。第一めっき被覆部材を熱処理することで、第一めっき膜の内部に存在するＴｌが、第一めっき膜の表面に濃化される。具体的には、第一めっき被覆部材を熱処理することで、第一めっき膜のＡｕが再結晶化されることに伴い、主にＡｕの結晶粒界に存在するＴｌが第一めっき膜の表面に移動する。
　実質的に酸素元素を含まない雰囲気とは、酸素濃度が質量割合で２０ｐｐｍ以下のことを言う。実質的に酸素元素を含まない雰囲気は、Ｈ２ガス雰囲気、Ａｒ、Ｎ２などの不活性ガス雰囲気、Ｈ２ガスと不活性ガスとの混合ガス雰囲気などが挙げられる。
　熱処理温度は、２００～５００℃が挙げられる。熱処理温度を２００℃以上とすることで、第一めっき膜のＡｕを再結晶化できると共に、Ａｕの再結晶化に伴い、Ａｕの結晶粒界に存在するＴｌの少なくとも一部を第一めっき膜の表面に移動させることができる。熱処理温度が高いほど、Ａｕの結晶粒界に存在するＴｌをより多く第一めっき膜の表面に移動させることができる。一方、熱処理温度を５００℃以下とすることで、基材２のＮｉ、すなわちＮｉを主成分とする膜２３中のＮｉが第一めっき膜の表面まで拡散することを抑制できる。熱処理温度は、更に２５０～４８０℃、特に３００～４５０℃が挙げられる。
　熱処理の保持時間は、１～１０分が挙げられる。熱処理の保持時間を１分以上とすることで、第一めっき膜のＡｕを再結晶化できると共に、Ａｕの再結晶化に伴い、Ａｕの結晶粒界に存在するＴｌの少なくとも一部を第一めっき膜の表面に移動させることができる。熱処理の保持時間が長いほど、Ａｕの結晶粒界に存在するＴｌをより多く第一めっき膜の表面に移動させることができる。第一めっき膜のＡｕは、熱処理の保持時間を１０分もすれば十分に再結晶化される。そのため、熱処理の保持時間を１０分以下とすることで、製造時間を短くできる。熱処理の保持時間は、更に２～８分、特に３～５分が挙げられる。
　第一めっき膜に熱処理工程を施して得られるめっき膜は、めっき膜の表面にＴｌが濃化している。このめっき膜の表面に存在するＴｌは、熱処理直後において、主にＴｌ単体で存在している。以下、第一めっき膜に熱処理工程を施して得られるめっき膜を、第二めっき膜と呼び、この第二めっき膜を備えるめっき被覆部材を第二めっき被覆部材と呼ぶ。
　〔酸化工程〕
　酸化工程では、上記第二めっき被覆部材を、酸素元素を含む雰囲気中で放置する。第二めっき被覆部材を酸素元素を含む雰囲気中で放置することで、第二めっき膜の表面に存在するＴｌが酸化されてＴｌ酸化物が形成される。このＴｌ酸化物は、Ｔｌ２ＯおよびＴｌ２Ｏ３である。
　酸素元素を含む雰囲気とは、例えば、酸素濃度が質量割合で５００ｐｐｍ以上のことを言う。酸素元素を含む雰囲気は、大気が挙げられる。この酸素元素を含む雰囲気での放置は、常温で行うことが好ましい。大気中で常温にて酸化工程を行うと、格別の雰囲気制御や温度制御を必要としないからである。酸素元素を含む雰囲気での放置時間は、１～２４時間が挙げられる。放置時間を１時間以上とすることで、第二めっき膜の表面に存在するＴｌのうち割合で４０％以上のＴｌをＴｌ２Ｏに酸化することができる。第二めっき膜の表面に存在するＴｌの残部は、Ｔｌ単体のまま存在したり、Ｔｌ２Ｏ３に酸化されたりする。酸素元素を含む雰囲気での放置時間は、長いほど第二めっき膜の表面に存在するＴｌをＴｌ２Ｏに酸化し易い。なお、放置時間がある程度の長さを超えると、Ｔｌ２Ｏへの酸化が飽和し得る。第二めっき膜のＴｌは、酸素元素を含む雰囲気での放置時間を２４時間もすれば十分にＴｌ２Ｏに酸化できる。そのため、酸素元素を含む雰囲気での放置時間を２４時間以下とすることで、製造時間を短くできる。なお、Ｔｌの酸化は、湿気などの外的要因に依存する。そのため、酸素元素を含む雰囲気での放置時間は、外的要因に合わせて適宜調整すればよい。例えば、湿気が多い場合、第二めっき膜の表面に存在するＴｌをＴｌ２Ｏに酸化し易いため、放置時間を短くできる。酸素元素を含む雰囲気での放置時間は、更に３～２０時間、特に６～１６時間が挙げられる。
　第二めっき膜に酸化工程を施して得られるめっき膜３は、図１に示すように、めっき膜３の表面にＴｌ２Ｏを含むＴｌ酸化物３２を備える。このめっき膜３における割合Ｘは４０％以上である。なお、めっき膜３の表面におけるＴｌは、Ｔｌ２Ｏで４０％以上存在していればよく、残部の形態を特に問わない。
　≪効果≫
　実施形態に係るめっき膜３は、その表面にＴｌ２Ｏを含むＴｌ酸化物３２を備え、そのめっき膜３の表面において割合Ｘが４０％以上であることで、導電性接合材料との濡れ性を向上できる。具体的には、上記めっき膜３は、導電性接合材料との濡れ面積率が９０％以上を満たすことができる。よって、上記めっき膜３を備える実施形態に係るめっき被覆部材１は、導電性接合材料を介した相手部材との接合性を向上できる。上記濡れ面積率が９０％以上を満たすことで、めっき被覆部材１と相手部材との接合部に空隙が形成され難く、接合部に生じ得る熱抵抗を低減できる。そうすることで、例えば、めっき被覆部材１が放熱部材であり、相手部材が半導体チップである場合、半導体チップの発する熱を放熱部材に良好に放出することができ、半導体チップの故障を防止できる。
　実施形態に係るめっき膜３は、めっき膜３全体に含まれるＴｌの含有量が１０ｐｐｍ以上であることで、めっき膜３中のＴｌを表面に濃化し、めっき膜３の表面にＴｌ２Ｏを存在させ易い。めっき膜３に含まれるＴｌは、主としてめっき膜３の表面に存在しており、めっき膜３の内部には少ないため、めっき膜３が被覆される相手部材に対してめっき膜３が剥がれることを抑制できる。
　［試験例１］
　Ａｕ及びＴｌを含むめっき膜を備えるめっき被覆部材の試料を作製し、各試料のめっき膜の表面に存在するＴｌ２Ｏの割合と、濡れ面積率を調べた。
　≪試料の作製≫
　めっき対象物の表面に、Ａｕ及びＴｌを含むめっき浴を用いて電解めっきを施した（試料Ｎｏ．１－１～１－４、１－１１）。めっき対象物には、Ｃｕ－Ｍｏ系合金からなる第一金属板を、Ｃｕ単体からなる第二金属板で挟み込んだ積層構造の金属板を用意し、この金属板の表面を、Ｎｉを主成分とする膜（電気Ｎｉめっき膜）で被覆した基材を用いた（図１を参照）。基材の大きさは、５．０ｍｍ×５．０ｍｍ×１．０ｍｍとした。めっき浴には、シアン化金カリウムと、硝酸タリウムとを調整したものを用いた。めっき条件は、Ｔｌ濃度を質量割合で１０ｐｐｍ、電流密度を０．５Ａ／ｄｍ２、めっき浴の温度を６０℃とし、めっき膜の厚さが１．５μｍになるまで電解めっきを行った。このめっき条件によって得られるめっき膜全体のＴｌの含有量は、質量割合で３５ｐｐｍであった。
　基材の表面に電解めっきを施した各試料に、Ｈ２ガス雰囲気中で３１０℃×１分の熱処理を施した。熱処理を施した試料のうち、試料Ｎｏ．１－１～１－４は、常温大気中で、表１に示す放置時間だけ放置した。その後、試料Ｎｏ．１－１～１－４に、Ａｇペーストを塗布した。Ａｇペーストの塗布方法は、Ａｇペーストを試料の上に５０μｌ滴下後、スキージを用いて液滴を広げた。スキージ高さは３０μｍとした。熱処理を施した試料のうち、試料Ｎｏ．１－１１は、常温大気中で放置せずに、熱処理後すぐにＡｇペーストを塗布した。いずれの試料も、Ａｇペーストの塗布面積を３．０ｍｍ×２．５ｍｍとした。
　≪めっき膜表面のＴｌ２Ｏの割合≫
　作製した各試料のめっき被覆部材について、めっき膜の表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合をＸＰＳにより測定した。その結果を表１に併せて示す。
　≪濡れ面積率≫
　作製した各試料のめっき被覆部材について、めっき膜とＡｇペーストとの濡れ面積率を測定した。濡れ面積率は、光学顕微鏡を用いて、Ａｇペーストの塗布面積内で、Ａｇペーストが濡れている面積の割合を求めた。その結果を表１に併せて示す。また、試料Ｎｏ．１－４及び試料Ｎｏ．１－１１のめっき被覆部材について、めっき膜に対するＡｇペーストの濡れ状態を示す写真を図２及び図３にそれぞれ示す。図２及び図３において、黒い部分はＡｇペーストを弾いている部分であり、その他の部分はＡｇペーストが濡れている部分である。
Figure JPOXMLDOC01-appb-T000001
　表１に示すように、熱処理後に１時間以上放置してからＡｇペーストを塗布した試料Ｎｏ．１－２～１－４は、めっき膜表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合が４０％以上であり、濡れ面積率が９０％以上と濡れ性に優れることがわかる。これは、熱処理後に１時間以上放置したため、熱処理によってめっき膜表面に濃化したＴｌが十分に酸化されたことによると思われる。一方、熱処理後に１時間未満放置してからＡｇペーストを塗布とした試料Ｎｏ．１－１は、上記割合が３２％であり、濡れ面積率が８５％と濡れ性に劣ることがわかる。また、熱処理後すぐにＡｇペーストを塗布した試料Ｎｏ．１－１１は、上記割合が２８％であり、濡れ面積率が８０％と非常に濡れ性に劣ることがわかる。これは、熱処理後の放置時間が短い又は放置していないため、熱処理によってめっき膜表面に濃化したＴｌが十分に酸化されず、めっき膜表面にＴｌ単体やＴｌ２Ｏ３といった濡れ性を低下させるＴｌが残存していることによると思われる。
　［試験例２］
　Ａｕ及びＴｌを含むめっき膜を備えるめっき被覆部材の試料を作製し、各試料のめっき膜全体に含まれるＴｌの含有量と、濡れ面積率を調べた。
　≪試料の作製≫
　めっき対象物の表面に、Ａｕ及びＴｌを含むめっき浴を用いて電解めっきを施した（試料Ｎｏ．２－１～２－４）。めっき対象物は、試験例１と同様の基材を用いた。めっき浴は、試験例１と同様のシアン化金カリウムと、硝酸タリウムとを調整したものを用い、めっき条件は、表２に示すＴｌ濃度（質量割合）、電流密度、温度とした。各めっき条件によって得られるめっき膜全体のＴｌの含有量を表２に併せて示す。めっき膜の厚さは、いずれの試料も１μｍとした。
　基材の表面に電解めっきを施した各試料に、Ｈ２ガス雰囲気中で３１０℃×１分の熱処理を施した後、常温大気中で１４時間放置してから、試験例１と同様にＡｇペーストを塗布した。いずれの試料も、Ａｇペーストの塗布面積を３．０ｍｍ×２．５ｍｍとした。
　≪Ｔｌの含有量≫
　作製した各試料のめっき被覆部材について、めっき膜全体に含まれるＴｌの含有量をＩＣＰ発光分光分析により測定した。その結果を表２に併せて示す。
　≪濡れ面積率≫
　作製した各試料のめっき被覆部材について、めっき膜とＡｇペーストとの濡れ面積率を試験例１と同様に測定した。その結果を表２に併せて示す。
Figure JPOXMLDOC01-appb-T000002
　表２に示すように、濡れ面積率は、めっき膜全体に含まれるＴｌの含有量に依存しないことがわかった。これは、めっき膜内にある程度のＴｌが含まれると、熱処理後に十分に放置を行うことで、熱処理によってめっき膜表面に濃化したＴｌが十分に酸化されることによると思われる。濡れ面積率が、めっき膜全体に含まれるＴｌの含有量に依存しないため、めっき膜全体に含まれるＴｌの含有量を多くすることで、相対的にＡｕの含有量を少なくでき、めっき浴のコストを低減できると期待される。また、めっき膜全体に含まれるＴｌの含有量を多くすることで、めっき浴中のＡｕの錯体を安定化でき、めっき浴の寿命を向上したり、めっき浴を構成する成分の管理を容易にできたりすると期待される。
　１　めっき被覆部材、２　基材、２１　第一金属板、２２　第二金属板、２３　Ｎｉを主成分とする膜、３　めっき膜、３０ａ　結晶粒、３０ｂ　結晶粒界、３１　Ｔｌ単体、３２　Ｔｌ酸化物。

Claims (5)

  1. 　Ａｕ及びＴｌを含むめっき膜であって、
    　前記めっき膜の表面にＴｌ２Ｏを含むＴｌ酸化物を備え、
    　前記表面において、Ｔｌ酸化物を構成するＴｌ原子とＴｌ単体を構成するＴｌ原子との合計に対するＴｌ２Ｏを構成するＴｌ原子の割合が４０％以上であるめっき膜。
  2. 　前記めっき膜全体に含まれるＴｌの含有量が、質量割合で１０ｐｐｍ以上６００ｐｐｍ以下である請求項１に記載のめっき膜。
  3. 　平均厚さが、０．１μｍ以上である請求項１又は請求項２に記載のめっき膜。
  4. 　基材と、前記基材を被覆するめっき膜とを備え、導電性接合材料を介して相手部材に接合されるめっき被覆部材であって、
    　前記めっき膜は、請求項１から請求項３のいずれか１項に記載のめっき膜であるめっき被覆部材。
  5. 　前記基材は、板材と、前記板材を被覆するＮｉを主成分とする膜とを備え、
    　前記板材は、Ｃｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上を含む金属、又はＣｕ、Ａｇ、Ａｌ、Ｍｏ、Ｗ、及びＭｇから選択される一種以上と、ダイヤモンド及び炭化ケイ素から選択される一種以上とを含む複合材料からなる請求項４に記載のめっき被覆部材。
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