TWI746807B - Copper/ceramic bonded body, insulating circuit substrate, method of manufacturing copper/ceramic bonded body and method of manufacturing insulating circuit substrate - Google Patents

Copper/ceramic bonded body, insulating circuit substrate, method of manufacturing copper/ceramic bonded body and method of manufacturing insulating circuit substrate Download PDF

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TWI746807B
TWI746807B TW107106520A TW107106520A TWI746807B TW I746807 B TWI746807 B TW I746807B TW 107106520 A TW107106520 A TW 107106520A TW 107106520 A TW107106520 A TW 107106520A TW I746807 B TWI746807 B TW I746807B
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copper
active metal
ceramic
ceramic substrate
layer
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TW107106520A
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TW201841871A (en
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寺伸幸
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日商三菱綜合材料股份有限公司
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Abstract

In a copper/ceramic bonded body of the present invention, a copper member including copper or copper alloy and a ceramic member including aluminum nitride or silicon nitride are bonded. In between the copper member and the ceramic member, an active metal nitride layer including a nitride of one or more kinds of active metals selected from Ti, Zr, Nb and Hf is formed at a ceramic member side. A Mg solid solution layer in which Mg is solid-solved into a matrix phase of Cu are formed between the active metal nitride layer and the copper member. Active metals are in the Mg solid solution layer.

Description

銅／陶瓷接合體，絕緣電路基板，及銅／陶瓷接合體的製造方法，絕緣電路基板的製造方法Copper/ceramic junction body, insulated circuit board, and copper/ceramic junction body manufacturing method, insulated circuit board manufacturing method

本發明有關由銅或銅合金所成之銅構件與由氮化鋁或氮化矽所成之陶瓷構件被接合而構成之銅/陶瓷接合體，絕緣電路基板，及銅/陶瓷接合體的製造方法，絕緣電路基板的製造方法。 　　本申請案基於2017年2月28日於日本申請之特願2017-036841號、及2018年1月25日於日本申請之特願2018-010964號而主張優先權，將其內容援用於此。The present invention relates to the manufacture of copper/ceramic joints, insulated circuit substrates, and copper/ceramic joints formed by joining a copper component made of copper or copper alloy and a ceramic component made of aluminum nitride or silicon nitride. Method, manufacturing method of insulated circuit board.　　 This application claims priority based on Japanese Patent Application No. 2017-036841 filed on February 28, 2017 in Japan, and Japanese Patent Application No. 2018-010964 filed on January 25, 2018, and the content is used here.

功率模組、LED模組及熱電模組中，具備下述構造，即，於在絕緣層的一方的面形成有由導電材料所成之電路層的絕緣電路基板，接合著功率半導體元件、LED元件及熱電元件。 　　例如，為了控制風力發電、電動車、混合動力汽車等而使用之大電力控制用的功率半導體元件，動作時的發熱量多。因此，作為搭載功率半導體元件之基板，以往便廣泛使用一種絕緣電路基板，其具備了例如由氮化鋁或氮化矽等所成之陶瓷基板、及在此陶瓷基板的一方的面接合導電性優良的金屬板而形成之電路層。作為絕緣電路基板，也有人提供一種在陶瓷基板的另一方的面接合金屬板來形成金屬層之物。Power modules, LED modules, and thermoelectric modules have a structure in which a circuit layer made of a conductive material is formed on an insulating circuit board on one surface of an insulating layer, and power semiconductor elements and LEDs are bonded to each other. Components and thermoelectric components.　　For example, power semiconductor elements for large power control used to control wind power generation, electric vehicles, hybrid vehicles, etc., generate a lot of heat during operation. Therefore, as a substrate on which power semiconductor elements are mounted, an insulated circuit substrate has been widely used in the past. It has, for example, a ceramic substrate made of aluminum nitride or silicon nitride, and a conductive surface is bonded to one side of the ceramic substrate. A circuit layer formed from a good metal plate. As an insulated circuit board, some people also provide a metal layer formed by bonding a metal plate to the other side of the ceramic substrate.

例如，專利文獻1中，提出一種將構成電路層及金屬層之第一金屬板及第二金屬板訂為銅板，而將此銅板藉由DBC法(Direct Bonded Copper；直接覆銅法)直接接合至陶瓷基板而成之絕緣電路基板。此DBC法中，利用銅與銅氧化物之共晶反應，令液相發生於銅板與陶瓷基板之界面，藉此將銅板與陶瓷基板接合。For example, in Patent Document 1, it is proposed that the first metal plate and the second metal plate constituting the circuit layer and the metal layer are ordered as copper plates, and the copper plates are directly bonded by the DBC method (Direct Bonded Copper; direct copper clad method) To the insulated circuit substrate made of ceramic substrate. In this DBC method, the eutectic reaction of copper and copper oxide is used to cause the liquid phase to occur at the interface between the copper plate and the ceramic substrate, thereby joining the copper plate and the ceramic substrate.

專利文獻2中，提出一種在陶瓷基板的一方的面及另一方的面將銅板接合，藉此形成電路層及金屬層之絕緣電路基板。此絕緣電路基板中，令Ag-Cu-Ti系硬銲材介於陶瓷基板的一方的面及另一方的面而配置銅板，進行加熱處理，藉此讓銅板被接合(即所謂活性金屬硬銲法)。此活性金屬硬銲法中，使用含有活性金屬亦即Ti之硬銲材，因此熔融的硬銲材與陶瓷基板之潤濕性會提升，陶瓷基板與銅板會被良好地接合。Patent Document 2 proposes an insulated circuit board in which a circuit layer and a metal layer are formed by bonding copper plates on one surface and the other surface of a ceramic substrate. In this insulated circuit substrate, the Ag-Cu-Ti brazing material is interposed on one side and the other side of the ceramic substrate to arrange the copper plates, and heat treatment is performed to bond the copper plates (the so-called active metal brazing) Law). In this active metal brazing method, a brazing material containing Ti, which is an active metal, is used. Therefore, the wettability of the molten brazing material and the ceramic substrate is improved, and the ceramic substrate and the copper plate are well joined.

專利文獻3中，提出一種含有由Cu-Mg-Ti合金所成之粉末的膏，作為於高溫的氮氣環境下將銅板與陶瓷基板接合時所使用之接合用硬銲材。此專利文獻3中，具備藉由於氮氣環境下以560～800℃加熱而接合之構成，Cu-Mg-Ti合金中的Mg會昇華而不會殘存於接合界面，且實質上不會形成氮化鈦(TiN)。 [先前技術文獻] [專利文獻]Patent Document 3 proposes a paste containing a powder made of Cu-Mg-Ti alloy as a bonding brazing material used when bonding a copper plate and a ceramic substrate in a high-temperature nitrogen atmosphere. This patent document 3 has a structure for bonding by heating at 560 to 800°C in a nitrogen atmosphere. The Mg in the Cu-Mg-Ti alloy will sublime without remaining at the bonding interface, and substantially no nitride will be formed. Titanium (TiN). [Prior Art Document] [Patent Document]

[專利文獻1] 日本特開平04-162756號公報 　　[專利文獻2] 日本特許第3211856號公報 　　[專利文獻3] 日本特許第4375730號公報[Patent Document 1] Japanese Patent Laid-Open No. 04-162756 　　 [Patent Document 2] Japanese Patent No. 3211856 　　 [Patent Document 3] Japanese Patent No. 4375730

[發明所欲解決之問題][The problem to be solved by the invention]

然而，如專利文獻1所揭示般，當藉由DBC法將陶瓷基板與銅板接合的情形下，必須將接合溫度訂為1065℃以上(銅與銅氧化物之共晶點溫度以上)，因此接合時陶瓷基板有劣化之虞。However, as disclosed in Patent Document 1, in the case of joining a ceramic substrate and a copper plate by the DBC method, the joining temperature must be set to 1065°C or higher (the eutectic point temperature of copper and copper oxide or higher). There is a risk of deterioration of the ceramic substrate.

如專利文獻2所揭示般，當藉由活性金屬硬銲法將陶瓷基板與銅板接合的情形下，由於硬銲材含有Ag，Ag會存在於接合界面，因此容易發生遷移(migration)，而無法使用於高耐壓用途。此外，接合溫度被訂為900℃這一相對高溫，因此仍舊有陶瓷基板劣化的問題。As disclosed in Patent Document 2, when a ceramic substrate and a copper plate are joined by an active metal brazing method, since the brazing material contains Ag, Ag will be present at the joint interface, so migration is likely to occur and cannot Used in high pressure applications. In addition, the bonding temperature is set at a relatively high temperature of 900°C, so there is still a problem of deterioration of the ceramic substrate.

如專利文獻3所揭示般，當使用由含有Cu-Mg-Ti合金所成之粉末的膏所成之接合用硬銲材而於氮氣環境下接合的情形下，氣體會殘存於接合界面，而有容易發生部分放電的問題。此外，由於使用合金粉，因應合金粉的組成不均，熔融狀況會變得不均一，而有局部性地形成界面反應不充分的區域之虞。此外，膏中含有的有機物會殘存於接合界面，而有接合變得不充分之虞。As disclosed in Patent Document 3, when a brazing material for bonding made of a paste containing a powder of Cu-Mg-Ti alloy is used for bonding in a nitrogen atmosphere, gas will remain at the bonding interface, and There is a problem of partial discharge. In addition, due to the use of alloy powders, due to the uneven composition of the alloy powders, the melting conditions may become uneven, and there is a possibility that regions with insufficient interfacial reactions may be formed locally. In addition, organic substances contained in the paste may remain at the bonding interface, and bonding may become insufficient.

本發明係有鑑於前述事態而研發，目的在於提供一種銅構件與陶瓷構件確實地被接合，而耐遷移性優良之銅/陶瓷接合體，絕緣電路基板，及上述的銅/陶瓷接合體的製造方法，絕緣電路基板的製造方法。 [解決問題之技術手段]The present invention was developed in view of the foregoing situation, and aims to provide a copper/ceramic joint body, an insulated circuit board, and the above-mentioned copper/ceramic joint body, which are reliably joined to a copper member and a ceramic member and have excellent migration resistance Method, manufacturing method of insulated circuit board. [Technical means to solve the problem]

為解決這樣的問題，達成前述目的，本發明的一個態樣之銅/陶瓷接合體，係由銅或銅合金所成之銅構件、與由氮化鋁或氮化矽所成之陶瓷構件被接合而構成之銅/陶瓷接合體，其特徵為，在前述銅構件與前述陶瓷構件之間，於前述陶瓷構件側，形成有含有從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的氮化物之活性金屬氮化物層，在此活性金屬氮化物層與前述銅構件之間形成有Mg固溶於Cu的母相中而成之Mg固溶層，前述Mg固溶層中，存在前述活性金屬。In order to solve this problem and achieve the aforementioned object, one aspect of the copper/ceramic joint of the present invention is a copper member made of copper or copper alloy, and a ceramic member made of aluminum nitride or silicon nitride is combined The copper/ceramic joined body formed by bonding is characterized in that between the copper member and the ceramic member, on the ceramic member side, one or more selected from Ti, Zr, Nb, and Hf is formed An active metal nitride layer of active metal nitride, between the active metal nitride layer and the aforementioned copper member, a Mg solid solution layer formed by solid dissolving Mg in the mother phase of Cu is formed, the aforementioned Mg solid solution layer Among them, the aforementioned active metals are present.

此構成之銅/陶瓷接合體中，在由銅或銅合金所成之銅構件、與由氮化鋁或氮化矽所成之陶瓷構件之間，於前述陶瓷構件側，形成有含有從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的氮化物之活性金屬氮化物層。此活性金屬氮化物層，是藉由配設於陶瓷構件與銅構件之間的活性金屬和陶瓷構件中的氮反應而形成之物，陶瓷構件會充分地反應。 　　在活性金屬氮化物層與前述銅構件之間，形成有Mg固溶於Cu的母相中而成之Mg固溶層，此Mg固溶層中存在前述活性金屬，故配設於陶瓷構件與銅構件之間的Mg會朝銅構件側充分地擴散，又，Cu和活性金屬會充分地反應。 　　是故，在銅構件與陶瓷構件之接合界面，界面反應會充分地進行，能夠獲得銅構件與陶瓷構件確實地被接合而成之銅/陶瓷接合體。此外，接合界面中不存在Ag，故耐遷移性亦優良。In the copper/ceramic joint body of this structure, between the copper member made of copper or copper alloy and the ceramic member made of aluminum nitride or silicon nitride, on the side of the ceramic member, there is formed a layer containing Ti , Zr, Nb, Hf selected one or two or more active metal nitride active metal nitride layer. The active metal nitride layer is formed by reacting the active metal disposed between the ceramic member and the copper member and the nitrogen in the ceramic member, and the ceramic member will fully react. Between the active metal nitride layer and the copper member, a Mg solid solution layer in which Mg is solid-dissolved in the mother phase of Cu is formed. The active metal is present in the Mg solid solution layer, so it is arranged on the ceramic member and The Mg between the copper members diffuses sufficiently toward the copper member side, and Cu and the active metal fully react.　　 Therefore, at the bonding interface between the copper member and the ceramic member, the interfacial reaction proceeds sufficiently, and a copper/ceramic joint body in which the copper member and the ceramic member are reliably joined can be obtained. In addition, there is no Ag in the bonding interface, so migration resistance is also excellent.

本發明的一個態樣之銅/陶瓷接合體中，亦可構成為，前述Mg固溶層中，分散有含有Cu與前述活性金屬之金屬間化合物相。 　　Mg固溶層中的活性金屬，當含有Ti，Zr，Hf作為活性金屬的情形下，會以Cu與前述活性金屬之金屬間化合物相的方式存在。因此，Mg固溶層中存在Cu與前述活性金屬之金屬間化合物相，藉此，配設於陶瓷構件與銅構件之間的Mg會朝銅構件側充分地擴散，Cu和活性金屬會充分地反應，能夠獲得銅構件與陶瓷構件確實地被接合而成之銅/陶瓷接合體。In the copper/ceramic joint of one aspect of the present invention, it may be configured that an intermetallic compound phase containing Cu and the active metal is dispersed in the Mg solid solution layer. When the active metal in the Mg solid solution layer contains Ti, Zr, and Hf as the active metal, it will exist as an intermetallic compound phase between Cu and the aforementioned active metal. Therefore, there is an intermetallic compound phase between Cu and the aforementioned active metal in the Mg solid solution layer, whereby the Mg arranged between the ceramic member and the copper member will diffuse to the copper member side sufficiently, and Cu and the active metal will fully diffuse By reaction, a copper/ceramic joined body in which a copper member and a ceramic member are joined reliably can be obtained.

本發明的一個態樣之銅/陶瓷接合體中，較佳是，在前述活性金屬氮化物層的內部，分散有Cu粒子。 　　在此情形下，銅構件的Cu會和陶瓷構件充分地反應，可獲得銅構件與陶瓷構件強固地被接合而成之銅/陶瓷接合體。Cu粒子，為Cu單體或含有Cu之金屬間化合物，於形成活性金屬氮化物層時，藉由存在於液相中的Cu析出而生成。In the copper/ceramic joined body of one aspect of the present invention, it is preferable that Cu particles are dispersed in the active metal nitride layer.　　In this case, the Cu of the copper member will react with the ceramic member sufficiently, and a copper/ceramic joint body in which the copper member and the ceramic member are strongly joined can be obtained. Cu particles are Cu alone or intermetallic compounds containing Cu, and are generated by precipitation of Cu existing in the liquid phase when forming the active metal nitride layer.

本發明的一個態樣之銅/陶瓷接合體中，前述活性金屬亦可為Ti。 　　在此情形下，會形成氮化鈦層作為前述活性金屬氮化物層，前述Mg固溶層中，會分散有含有Cu與Ti之金屬間化合物相，能夠提供一種銅構件與陶瓷構件確實地被接合，而耐遷移性優良之銅/陶瓷接合體。In the copper/ceramic joint body of one aspect of the present invention, the aforementioned active metal may also be Ti. In this case, a titanium nitride layer will be formed as the active metal nitride layer, and the Mg solid solution layer will be dispersed with an intermetallic compound phase containing Cu and Ti, which can provide a copper component and a ceramic component that are reliably combined Bonded copper/ceramic bonded body with excellent migration resistance.

本發明的一個態樣之銅/陶瓷接合體中，較佳是，在前述陶瓷構件與前述銅構件之間，前述陶瓷構件的接合面起算往前述銅構件側50μm為止之區域中的Cu2 Mg相的面積率為15%以下。 　　在此情形下，脆弱的Cu2 Mg相的面積率會被限制在15%以下，故例如即使實施了超音波接合等的情形下，仍可抑制接合界面中的破裂等的發生。In the copper/ceramic joint body of one aspect of the present invention, it is preferable that between the ceramic member and the copper member, the joint surface of the ceramic member is Cu 2 Mg in a region up to 50 μm from the copper member side The area ratio of the phase is 15% or less. In this case, the area ratio of the fragile Cu 2 Mg phase is limited to 15% or less. Therefore, even when ultrasonic bonding is performed, for example, the occurrence of cracks in the bonding interface can be suppressed.

本發明的一個態樣之絕緣電路基板，係由銅或銅合金所成之銅板被接合至由氮化鋁或氮化矽所成之陶瓷基板的表面而構成之絕緣電路基板，其特徵為，在前述銅板與前述陶瓷基板之間，於前述陶瓷基板側，形成有含有從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的氮化物之活性金屬氮化物層，在此活性金屬氮化物層與前述銅板之間形成有Mg固溶於Cu的母相中而成之Mg固溶層，前述Mg固溶層中，存在前述活性金屬。 　　此構成之絕緣電路基板中，銅板與陶瓷基板會確實地被接合，並且耐遷移性優良，於高耐壓條件下仍能高可靠性性使用。One aspect of the insulated circuit substrate of the present invention is an insulated circuit substrate formed by bonding a copper plate made of copper or copper alloy to the surface of a ceramic substrate made of aluminum nitride or silicon nitride, and is characterized in that: Between the copper plate and the ceramic substrate, on the ceramic substrate side, an active metal nitride layer containing nitrides of one or more active metals selected from Ti, Zr, Nb, and Hf is formed, where A Mg solid solution layer in which Mg is solid-dissolved in a Cu matrix is formed between the active metal nitride layer and the copper plate, and the active metal is present in the Mg solid solution layer.　　In the insulated circuit substrate of this structure, the copper plate and the ceramic substrate are surely joined, and the resistance to migration is excellent, and it can be used with high reliability under high withstand voltage conditions.

本發明的一個態樣之絕緣電路基板中，亦可構成為，前述Mg固溶層中，分散有含有Cu與前述活性金屬之金屬間化合物相。 　　Mg固溶層中的活性金屬，當含有Ti，Zr，Hf作為活性金屬的情形下，會以Cu與前述活性金屬之金屬間化合物相的方式存在。因此，Mg固溶層中以Cu與前述活性金屬之金屬間化合物相的方式存在，藉此，能夠獲得銅板與陶瓷基板確實地被接合而成之絕緣電路基板。In the insulated circuit board of one aspect of the present invention, it may be configured that an intermetallic compound phase containing Cu and the active metal is dispersed in the Mg solid solution layer. When the active metal in the Mg solid solution layer contains Ti, Zr, and Hf as the active metal, it will exist as an intermetallic compound phase between Cu and the aforementioned active metal. Therefore, the Mg solid solution layer exists as an intermetallic compound phase of Cu and the aforementioned active metal, and thereby, an insulated circuit board in which a copper plate and a ceramic substrate are reliably joined can be obtained.

本發明的一個態樣之絕緣電路基板中，較佳是，在前述活性金屬氮化物層的內部，分散有Cu粒子。 　　在此情形下，銅板的Cu會和陶瓷基板充分地反應，可獲得銅板與陶瓷基板強固地被接合而成之絕緣電路基板。Cu粒子，為Cu單體或含有Cu之金屬間化合物，於形成活性金屬氮化物層時，藉由存在於液相中的Cu析出而生成。In the insulated circuit board of one aspect of the present invention, it is preferable that Cu particles are dispersed in the active metal nitride layer.　　In this case, the Cu of the copper plate reacts sufficiently with the ceramic substrate, and an insulated circuit substrate in which the copper plate and the ceramic substrate are strongly joined can be obtained. Cu particles are Cu alone or intermetallic compounds containing Cu, and are generated by precipitation of Cu existing in the liquid phase when forming the active metal nitride layer.

本發明的一個態樣之絕緣電路基板中，前述活性金屬亦可為Ti。 　　在此情形下，會形成氮化鈦層作為前述活性金屬氮化物層，前述Mg固溶層中，會分散有含有Cu與Ti之金屬間化合物相，能夠提供一種銅板與陶瓷基板確實地被接合，而耐遷移性優良之絕緣電路基板。In the insulated circuit substrate of one aspect of the present invention, the aforementioned active metal may also be Ti. In this case, a titanium nitride layer will be formed as the active metal nitride layer, and the Mg solid solution layer will be dispersed with an intermetallic compound phase containing Cu and Ti, which can provide a copper plate and a ceramic substrate that can be reliably joined , And an insulated circuit board with excellent migration resistance.

本發明的一個態樣之絕緣電路基板中，較佳是，在前述陶瓷基板與前述銅板之間，前述陶瓷基板的接合面起算往前述銅板側50μm為止之區域中的Cu2 Mg相的面積率為15%以下。 　　在此情形下，脆弱的Cu2 Mg相的面積率會被限制在15%以下，故例如即使實施了超音波接合等的情形下，仍可抑制接合界面中的破裂等的發生。In the insulated circuit board of one aspect of the present invention, it is preferable that the area ratio of the Cu 2 Mg phase in a region 50 μm from the side of the copper plate between the ceramic substrate and the copper plate and the bonding surface of the ceramic substrate is calculated Less than 15%. In this case, the area ratio of the fragile Cu 2 Mg phase is limited to 15% or less. Therefore, even when ultrasonic bonding is performed, for example, the occurrence of cracks in the bonding interface can be suppressed.

本發明的一個態樣之銅/陶瓷接合體的製造方法，係製造上述之銅/陶瓷接合體的方法，其特徵為，具備：活性金屬及Mg配置工程，在前述銅構件與前述陶瓷構件之間，配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體及Mg單體；及層積工程，將前述銅構件與前述陶瓷構件，介著活性金屬及Mg予以層積；及接合工程，將介著活性金屬及Mg而被層積之前述銅構件與前述陶瓷構件，在朝層積方向予以加壓之狀態下，於真空環境下做加熱處理而接合；前述活性金屬及Mg配置工程中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內。A method of manufacturing a copper/ceramic joint body according to one aspect of the present invention is a method of manufacturing the above-mentioned copper/ceramic joint body, and is characterized in that it comprises an active metal and Mg arrangement process, and the copper member and the ceramic member are arranged between the copper member and the ceramic member In between, one or more active metal monomers and Mg monomers selected from Ti, Zr, Nb, and Hf are arranged; and the lamination process is to interpose the aforementioned copper member and the aforementioned ceramic member with the active metal and Mg Laminating; and the joining process, the above-mentioned copper member and the above-mentioned ceramic member, which are laminated via active metal and Mg, are heated in a vacuum environment under pressure in the lamination direction to join; Mg and configure the active metal works, the active metal content is set at 2 or less in the range of 0.4μmol / cm 2 or more 47.0μmol / cm, the Mg content is set at 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm Inside.

按照此構成之銅/陶瓷接合體的製造方法，是在前述銅構件與前述陶瓷構件之間配置活性金屬的單體及Mg單體，在將它們朝層積方向予以加壓的狀態下，於真空環境下做加熱處理，故在接合界面不會殘存氣體或有機物的殘渣等。此外，由於配置活性金屬的單體及Mg單體，故沒有組成的不均，會均一地發生液相。 　　活性金屬及Mg配置工程中，是將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內，故能夠充分地獲得界面反應所必要之液相，並且能夠抑制陶瓷構件的必要以上的反應。 　　故，能夠獲得銅構件與陶瓷構件確實地被接合而成之銅/陶瓷接合體。此外，接合不使用Ag，故能夠獲得耐遷移性優良的銅/陶瓷接合體。According to the method of manufacturing the copper/ceramic joint body with this structure, the active metal monomer and Mg monomer are arranged between the copper member and the ceramic member, and they are pressed in the stacking direction. Heat treatment is performed in a vacuum environment, so no gas or organic residues will remain at the joint interface. In addition, since the active metal monomer and Mg monomer are arranged, there is no unevenness in composition, and a liquid phase is uniformly generated. Active metals and engineering Mg configuration, the amount of active metal is set within a range of 2 or less 0.4μmol / cm 2 or more 47.0μmol / cm, the Mg content is set at 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm Therefore, it is possible to sufficiently obtain the liquid phase necessary for the interface reaction, and it is possible to suppress more than necessary reactions of the ceramic member. Therefore, a copper/ceramic joined body in which a copper member and a ceramic member are reliably joined can be obtained. In addition, since Ag is not used for bonding, a copper/ceramic bonded body with excellent migration resistance can be obtained.

本發明的一個態樣之銅/陶瓷接合體的製造方法中，較佳是，前述接合工程中的加壓荷重被訂為0.049MPa以上3.4MPa以下的範圍內，前述接合工程中的加熱溫度，當Cu與Mg是在接觸狀態下被層積的情形下訂為500℃以上850℃以下的範圍內，當Cu與Mg是在非接觸狀態下被層積的情形下訂為670℃以上850℃以下的範圍內。In the method of manufacturing a copper/ceramic joined body according to one aspect of the present invention, it is preferable that the pressing load in the joining process is set within a range of 0.049 MPa or more and 3.4 MPa or less, and the heating temperature in the joining process is When Cu and Mg are laminated in the contact state, it is set to be in the range of 500°C to 850°C, and when Cu and Mg are laminated in the non-contact state, it is set to be 670°C to 850°C Within the following range.

在此情形下，前述接合工程中的加壓荷重是被訂為0.049MPa以上3.4MPa以下的範圍內，故能夠使陶瓷構件與銅構件與活性金屬及Mg密合，於加熱時能夠促進它們的界面反應。 　　前述接合工程中的加熱溫度，當Cu與Mg是在接觸狀態下被層積的情形下訂為比Cu與Mg的共晶溫度還高之500℃以上，當Cu與Mg是在非接觸狀態下被層積的情形下訂為比Mg的熔點還高之670℃以上，故於接合界面能夠充分地使液相發生。 　　前述接合工程中的加熱溫度是被訂為850℃以下，故能夠抑制Cu與活性金屬之共晶反應的發生，能夠抑制液相過度地生成。此外，對陶瓷構件之熱負荷會變小，能夠抑制陶瓷構件的劣化。In this case, the pressurizing load in the aforementioned joining process is set within the range of 0.049 MPa to 3.4 MPa, so that the ceramic member and the copper member can be closely adhered to the active metal and Mg, and they can be promoted during heating. Interface reaction. The heating temperature in the aforementioned bonding process, when Cu and Mg are laminated in the contact state, is set to be 500°C higher than the eutectic temperature of Cu and Mg, and when Cu and Mg are in the non-contact state In the case of being laminated, it is set to be 670°C or more higher than the melting point of Mg, so that the liquid phase can be sufficiently generated at the joint interface. "The heating temperature in the aforementioned joining process is set at 850°C or lower, so the occurrence of the eutectic reaction between Cu and the active metal can be suppressed, and the excessive generation of the liquid phase can be suppressed. In addition, the thermal load on the ceramic member is reduced, and the deterioration of the ceramic member can be suppressed.

本發明的一個態樣之絕緣電路基板的製造方法，係製造由銅或銅合金所成之銅板被接合至由氮化鋁或氮化矽所成之陶瓷基板的表面而構成之絕緣電路基板的絕緣電路基板的製造方法，其特徵為，具備：活性金屬及Mg配置工程，在前述銅板與前述陶瓷基板之間，配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體及Mg單體；及層積工程，將前述銅板與前述陶瓷基板，介著活性金屬及Mg予以層積；及接合工程，將介著活性金屬及Mg而被層積之前述銅板與前述陶瓷基板，在朝層積方向予以加壓之狀態下，於真空環境下做加熱處理而接合；前述活性金屬及Mg配置工程中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內。 　　按照此構成之絕緣電路基板的製造方法，能夠獲得銅板與陶瓷基板被確實地接合而成之絕緣電路基板。此外，接合不使用Ag，故能夠獲得耐遷移性優良的絕緣電路基板。An aspect of the method for manufacturing an insulated circuit board of the present invention is to manufacture an insulated circuit board in which a copper plate made of copper or copper alloy is joined to the surface of a ceramic substrate made of aluminum nitride or silicon nitride. The method of manufacturing an insulated circuit board is characterized by: an active metal and Mg arrangement process, and one or more active metals selected from Ti, Zr, Nb, and Hf are arranged between the aforementioned copper plate and the aforementioned ceramic substrate The monomer and Mg monomer; and the lamination process, in which the copper plate and the ceramic substrate are layered via the active metal and Mg; and the bonding process, the copper plate and the copper plate that are layered via the active metal and Mg The aforementioned ceramic substrates are joined by heat treatment in a vacuum environment while they are pressurized in the stacking direction; in the aforementioned active metal and Mg arrangement process, the amount of active metal is set to be 0.4 μmol/cm 2 or more and 47.0 μmol/ In the range of cm 2 or less, the amount of Mg is set to be in the range of 7.0 μmol/cm 2 or more and 143.2 μmol/cm 2 or less. According to the manufacturing method of the insulated circuit board of this structure, the insulated circuit board which the copper plate and the ceramic board were joined reliably can be obtained. In addition, since Ag is not used for bonding, an insulated circuit board excellent in migration resistance can be obtained.

本發明的一個態樣之絕緣電路基板的製造方法中，較佳是，前述接合工程中的加壓荷重被訂為0.049MPa以上3.4MPa以下的範圍內，前述接合工程中的加熱溫度，當Cu與Mg是在接觸狀態下被層積的情形下訂為500℃以上850℃以下的範圍內，當Cu與Mg是在非接觸狀態下被層積的情形下訂為670℃以上850℃以下的範圍內。In the method of manufacturing an insulated circuit board of one aspect of the present invention, it is preferable that the pressurizing load in the bonding process is set within a range of 0.049 MPa to 3.4 MPa, and the heating temperature in the bonding process is set as Cu When it is laminated with Mg in the contact state, it is set to be within the range of 500°C to 850°C. When Cu and Mg are laminated in the non-contact state, it is set to be 670°C to 850°C. Within range.

在此情形下，前述接合工程中的加壓荷重是被訂為0.049MPa以上3.4MPa以下的範圍內，故能夠使陶瓷基板與銅板與活性金屬及Mg密合，於加熱時能夠促進它們的界面反應。 　　前述接合工程中的加熱溫度，當Cu與Mg是在接觸狀態下被層積的情形下訂為比Cu與Mg的共晶溫度還高之500℃以上，當Cu與Mg是在非接觸狀態下被層積的情形下訂為比Mg的熔點還高之670℃以上，故於接合界面能夠充分地使液相發生。 　　前述接合工程中的加熱溫度是被訂為850℃以下，故能夠抑制Cu與活性金屬之共晶反應的發生，能夠抑制液相過度地生成。此外，對陶瓷基板之熱負荷會變小，能夠抑制陶瓷基板的劣化。 [發明之功效]In this case, the pressing load in the aforementioned joining process is set within the range of 0.049 MPa or more and 3.4 MPa or less. Therefore, the ceramic substrate and the copper plate can be closely adhered to the active metal and Mg, and the interface between them can be promoted during heating. reaction. The heating temperature in the aforementioned bonding process, when Cu and Mg are laminated in the contact state, is set to be 500°C higher than the eutectic temperature of Cu and Mg, and when Cu and Mg are in the non-contact state In the case of being laminated, it is set to be 670°C or more higher than the melting point of Mg, so that the liquid phase can be sufficiently generated at the joint interface. "The heating temperature in the aforementioned joining process is set at 850°C or lower, so the occurrence of the eutectic reaction between Cu and the active metal can be suppressed, and the excessive generation of the liquid phase can be suppressed. In addition, the thermal load on the ceramic substrate is reduced, and the deterioration of the ceramic substrate can be suppressed. [Effects of Invention]

按照本發明，可提供一種銅構件與陶瓷構件確實地被接合，而耐遷移性優良之銅/陶瓷接合體，絕緣電路基板，及上述的銅/陶瓷接合體的製造方法，絕緣電路基板的製造方法。According to the present invention, it is possible to provide a copper/ceramic joint body, an insulated circuit board, and a method for manufacturing the above-mentioned copper/ceramic joint body, and a manufacturing method of the above-mentioned copper/ceramic joint body, and the production of the insulated circuit board method.

以下參照所附圖面說明本發明之實施形態。Hereinafter, embodiments of the present invention will be described with reference to the drawings.

(第1實施形態) 　　針對本發明之第1實施形態，參照圖1至圖4說明之。 　　本實施形態之銅/陶瓷接合體，係被做成藉由陶瓷構件即陶瓷基板11與銅構件即銅板22(電路層12)及銅板23(金屬層13)被接合而構成之絕緣電路基板10。 　　圖1揭示本發明第1實施形態之絕緣電路基板10及使用了此絕緣電路基板10之功率模組1。(First Embodiment) "The first embodiment of the present invention will be described with reference to Figs. 1 to 4). The copper/ceramic joint body of this embodiment is an insulated circuit substrate 10 formed by joining a ceramic substrate 11 which is a ceramic member and a copper plate 22 (circuit layer 12) and a copper plate 23 (metal layer 13) which are copper members. .　　 FIG. 1 shows an insulated circuit board 10 according to the first embodiment of the present invention and a power module 1 using the insulated circuit board 10.

此功率模組1，具備絕緣電路基板10、及在此絕緣電路基板10的一方側(圖1中上側)介著第1銲料層2而被接合之半導體元件3、及在絕緣電路基板10的另一方側(圖1中下側)介著第2銲料層8而被接合之散熱座(heatsink)51。This power module 1 includes an insulated circuit board 10, a semiconductor element 3 that is joined to one side of the insulated circuit board 10 (upper side in FIG. 1) via a first solder layer 2, and an insulated circuit board 10 On the other side (the lower side in FIG. 1 ), a heat sink 51 is joined via the second solder layer 8.

絕緣電路基板10，具備陶瓷基板11、及配設於此陶瓷基板11的一方的面(圖1中上面)之電路層12、及配設於陶瓷基板11的另一方的面(圖1中下面)之金屬層13。 　　陶瓷基板11，為防止電路層12與金屬層13之間的電性連接之物，本實施形態中由絕緣性高的氮化鋁來構成。陶瓷基板11的厚度，被設定成0.2～1.5mm的範圍內，本實施形態中被設定成0.635mm。The insulated circuit substrate 10 includes a ceramic substrate 11, a circuit layer 12 disposed on one surface of the ceramic substrate 11 (upper surface in FIG. 1), and a circuit layer 12 disposed on the other surface of the ceramic substrate 11 (lower surface in FIG. 1 ) The metal layer 13. The "ceramic substrate 11" is to prevent electrical connection between the circuit layer 12 and the metal layer 13. In this embodiment, it is made of aluminum nitride with high insulation. The thickness of the ceramic substrate 11 is set in the range of 0.2 to 1.5 mm, and is set to 0.635 mm in this embodiment.

電路層12，如圖4所示，是藉由在陶瓷基板11的一方的面接合由銅或銅合金所成之銅板22而形成。本實施形態中，作為構成電路層12的銅板22，使用無氧銅的壓延板。在此電路層12，形成有電路圖樣，其一方的面(圖1中上面)，為供半導體元件3搭載之搭載面。電路層12的厚度被設定成0.1mm以上2.0mm以下的範圍內，本實施形態中被設定成0.6mm。The circuit layer 12 is formed by bonding a copper plate 22 made of copper or copper alloy to one surface of the ceramic substrate 11 as shown in FIG. 4. In this embodiment, as the copper plate 22 constituting the circuit layer 12, a rolled plate of oxygen-free copper is used. In this circuit layer 12, a circuit pattern is formed, and one surface (the upper surface in FIG. 1) of the circuit layer 12 is a mounting surface on which the semiconductor element 3 is mounted. The thickness of the circuit layer 12 is set to be in the range of 0.1 mm or more and 2.0 mm or less, and is set to 0.6 mm in this embodiment.

金屬層13，如圖4所示，是藉由在陶瓷基板11的另一方的面接合由銅或銅合金所成之銅板23而形成。本實施形態中，作為構成金屬層13的銅板23，使用無氧銅的壓延板。金屬層13的厚度被設定成0.1mm以上2.0mm以下的範圍內，本實施形態中被設定成0.6mm。The metal layer 13 is formed by bonding a copper plate 23 made of copper or copper alloy to the other surface of the ceramic substrate 11 as shown in FIG. 4. In this embodiment, as the copper plate 23 constituting the metal layer 13, a rolled plate of oxygen-free copper is used. The thickness of the metal layer 13 is set in the range of 0.1 mm or more and 2.0 mm or less, and is set to 0.6 mm in this embodiment.

散熱座51，為用來將前述的絕緣電路基板10冷卻之物，本實施形態中以由熱傳導性良好的材質所構成之散熱板來構成。本實施形態中，散熱座51以熱傳導性優良的銅或銅合金來構成。散熱座51和絕緣電路基板10的金屬層13，介著第2銲料層8而被接合。The heat sink 51 is used to cool the aforementioned insulated circuit board 10, and in this embodiment, it is composed of a heat sink made of a material with good thermal conductivity. In this embodiment, the heat sink 51 is made of copper or copper alloy excellent in thermal conductivity. The heat sink 51 and the metal layer 13 of the insulating circuit board 10 are joined via the second solder layer 8.

陶瓷基板11與電路層12(銅板22)、及陶瓷基板11與金屬層13(銅板23)，如圖4所示，是介著由從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬所成之活性金屬膜24(本實施形態中為Ti膜)及Mg膜25而被接合。 　　於陶瓷基板11與電路層12(銅板22)之接合界面及陶瓷基板11與金屬層13(銅板23)之接合界面，如圖2所示，具備形成於陶瓷基板11側之活性金屬氮化物層31(本實施形態中為氮化鈦層)與Mg固溶於Cu的母相中而成之Mg固溶層32所層積之構造。The ceramic substrate 11 and the circuit layer 12 (copper plate 22), and the ceramic substrate 11 and the metal layer 13 (copper plate 23), as shown in FIG. 4, are interposed by one or two types selected from Ti, Zr, Nb, and Hf The active metal film 24 (Ti film in this embodiment) made of the above active metal and the Mg film 25 are joined. The bonding interface between the ceramic substrate 11 and the circuit layer 12 (copper plate 22) and the bonding interface between the ceramic substrate 11 and the metal layer 13 (copper plate 23) are provided with an active metal nitride layer formed on the ceramic substrate 11 side, as shown in FIG. 31 (titanium nitride layer in this embodiment) and Mg solid solution layer 32 formed by solid dissolving Mg in the Cu matrix.

Mg固溶層32中，含有上述的活性金屬。本實施形態中，Mg固溶層32中，分散有含有Cu與活性金屬(Ti)之金屬間化合物相33。本實施形態中，作為活性金屬使用Ti，作為構成含有Cu與Ti之金屬間化合物相33的金屬間化合物，例如可舉出Cu4 Ti，Cu3 Ti2 ，Cu4 Ti3 ，CuTi，CuTi2 ，CuTi3 等。 　　此Mg固溶層32中的Mg的含有量，被訂為0.01原子%以上0.5原子%以下的範圍內。Mg固溶層32的厚度，被訂為0.1μm以上80μm以下的範圍內。Mg固溶層32中的Mg的含有量，較佳是被訂為0.01原子%以上0.3原子%以下的範圍內，但不限定於此。The Mg solid solution layer 32 contains the above-mentioned active metal. In this embodiment, in the Mg solid solution layer 32, an intermetallic compound phase 33 containing Cu and active metal (Ti) is dispersed. In this embodiment, Ti is used as the active metal. Examples of the intermetallic compound constituting the intermetallic compound phase 33 containing Cu and Ti include Cu 4 Ti, Cu 3 Ti 2 , Cu 4 Ti 3 , CuTi, and CuTi 2 , CuTi 3 and so on. The content of Mg in the Mg solid solution layer 32 is set to be in the range of 0.01 atomic% or more and 0.5 atomic% or less. The thickness of the Mg solid solution layer 32 is set within the range of 0.1 μm or more and 80 μm or less. The content of Mg in the Mg solid solution layer 32 is preferably set within the range of 0.01 atomic% to 0.3 atomic %, but it is not limited to this.

本實施形態中，在活性金屬氮化物層31(氮化鈦層)的內部，分散有Cu粒子35。 　　分散在活性金屬氮化物層31(氮化鈦層)內之Cu粒子35的粒徑，被訂為10nm以上100nm以下的範圍內。此外，活性金屬氮化物層31(氮化鈦層)當中與陶瓷基板11之界面起算至活性金屬氮化物層31(氮化鈦層)的厚度的20%為止之界面鄰近區域中的Cu濃度，被訂為0.3原子%以上15原子%以下的範圍內。 　　活性金屬氮化物層31(氮化鈦層)的厚度，被訂為0.03μm以上1.2μm以下的範圍內。活性金屬氮化物層31(氮化鈦層)當中與陶瓷基板11之界面起算至活性金屬氮化物層31(氮化鈦層)的厚度的20%為止之界面鄰近區域中的Cu濃度，較佳是被訂為0.3原子%以上12原子%以下的範圍內，但不限定於此。In this embodiment, Cu particles 35 are dispersed in the active metal nitride layer 31 (titanium nitride layer). "The particle size of the Cu particles 35 dispersed in the active metal nitride layer 31 (titanium nitride layer) is set to be in the range of 10 nm or more and 100 nm or less. In addition, the Cu concentration in the area adjacent to the interface of the active metal nitride layer 31 (titanium nitride layer) from the interface with the ceramic substrate 11 to 20% of the thickness of the active metal nitride layer 31 (titanium nitride layer), It is set within the range of 0.3 atomic% to 15 atomic %. "The thickness of the active metal nitride layer 31 (titanium nitride layer) is set to be in the range of 0.03 μm or more and 1.2 μm or less. The Cu concentration in the adjacent area of the active metal nitride layer 31 (titanium nitride layer) from the interface with the ceramic substrate 11 to 20% of the thickness of the active metal nitride layer 31 (titanium nitride layer) is preferably It is set within the range of 0.3 atomic% or more and 12 atomic% or less, but it is not limited to this.

本實施形態中，在陶瓷基板11與電路層12之間，陶瓷基板11的接合面起算至往電路層12側50μm為止之區域中的Cu2 Mg相的面積率，被訂為15%以下。陶瓷基板11的接合面起算至往電路層12側50μm為止之區域中的Cu2 Mg相的面積率，較佳是被訂為0.01%以上10%以下，但不限定於此。 　　本實施形態中，上述的Cu2 Mg相，是訂為以電子探針顯微分析儀取得Mg的元素MAP，於確認有Mg的存在之區域中Mg濃度為30原子%以上40原子%以下之區域。 In the present embodiment, the area ratio of the Cu 2 Mg phase in the area 50 μm from the bonding surface of the ceramic substrate 11 to the circuit layer 12 side between the ceramic substrate 11 and the circuit layer 12 is set to 15% or less. The area ratio of the Cu 2 Mg phase in the area 50 μm from the bonding surface of the ceramic substrate 11 to the circuit layer 12 side is preferably set to 0.01% or more and 10% or less, but it is not limited to this. In this embodiment, the above-mentioned Cu 2 Mg phase is set as the element MAP of Mg obtained by an electron probe microanalyzer. The Mg concentration in the region where the presence of Mg is confirmed is 30 atomic% or more and 40 atomic% or less. area.

針對上述本實施形態之絕緣電路基板10的製造方法，參照圖3及圖4說明之。The manufacturing method of the insulated circuit board 10 of this embodiment mentioned above is demonstrated with reference to FIG. 3 and FIG. 4. FIG.

如圖4所示，在作為電路層12之銅板22與陶瓷基板11之間、及作為金屬層13之銅板23與陶瓷基板11之間，各自配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體(本實施形態中為Ti單體)及Mg單體(活性金屬及Mg配置工程S01)。本實施形態中，藉由蒸鍍活性金屬(Ti)及Mg，會形成活性金屬膜24(Ti膜)及Mg膜25，Mg膜25和銅板22會在非接觸狀態下被層積。 　　此活性金屬及Mg配置工程S01中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內(本實施形態中，將Ti訂為0.02mg/cm2 以上2.25mg/cm2 以下的範圍內)，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內(0.17mg/cm2 以上3.48mg/cm2 以下的範圍內)。 　　活性金屬量的下限較佳是訂為2.8μmol/cm2 以上，活性金屬量的上限較佳是訂為18.8μmol/cm2 以下。此外，Mg量的下限較佳是訂為8.8μmol/cm2 以上，Mg量的上限較佳是訂為37.0μmol/cm2 以下。As shown in FIG. 4, between the copper plate 22 as the circuit layer 12 and the ceramic substrate 11, and between the copper plate 23 as the metal layer 13 and the ceramic substrate 11, one type selected from Ti, Zr, Nb, and Hf is respectively arranged Or two or more active metal monomers (Ti monomer in this embodiment) and Mg monomer (active metal and Mg arrangement process S01). In this embodiment, by vapor deposition of active metal (Ti) and Mg, an active metal film 24 (Ti film) and a Mg film 25 are formed, and the Mg film 25 and the copper plate 22 are laminated in a non-contact state. In this active metal and Mg configuration project S01, the amount of active metal is set to be within the range of 0.4 μmol/cm 2 or more and 47.0 μmol/cm 2 or less (in this embodiment, Ti is set to be 0.02 mg/cm 2 or more and 2.25 mg/cm2). or less in the range of 2 cm), the amount of Mg is set within a range of (0.17mg / cm 2 or more 3.48mg / cm 2 or less in the range of 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm). The lower limit of the amount of active metal is preferably set to 2.8 μmol/cm 2 or more, and the upper limit of the amount of active metal is preferably set to 18.8 μmol/cm 2 or less. In addition, the lower limit of the amount of Mg is preferably set to 8.8 μmol/cm 2 or more, and the upper limit of the amount of Mg is preferably set to 37.0 μmol/cm 2 or less.

接著，將銅板22與陶瓷基板11與銅板23，介著活性金屬膜24(Ti膜)及Mg膜25予以層積(層積工程S02)。Next, the copper plate 22, the ceramic substrate 11, and the copper plate 23 are laminated via the active metal film 24 (Ti film) and the Mg film 25 (layering process S02).

將被層積的銅板22、陶瓷基板11、銅板23朝層積方向加壓，並且裝入真空爐內加熱，將銅板22與陶瓷基板11與銅板23接合(接合工程S03)。 　　接合工程S03中的加壓荷重，被訂為0.049MPa以上3.4MPa以下的範圍內。接合工程S03中的加壓荷重，較佳是被訂為0.294MPa以上1.47MPa以下的範圍內，但不限定於此。 　　接合工程S03中的加熱溫度，由於Cu與Mg是在非接觸狀態下被層積，因此被訂為Mg的熔點以上之670℃以上850℃以下的範圍內。加熱溫度的下限較佳是訂為700℃以上。 　　接合工程S03中的真空度，較佳是訂為1×10-6 Pa以上1×10-2 Pa以下的範圍內。 　　加熱溫度下的保持時間，較佳是訂為5min以上360min以下的範圍內。為了減低上述的Cu2 Mg相的面積率，較佳是將加熱溫度下的保持時間的下限訂為60min以上。此外，加熱溫度下的保持時間的上限較佳是訂為240min以下。The laminated copper plate 22, the ceramic substrate 11, and the copper plate 23 are pressurized in the lamination direction and heated in a vacuum furnace to join the copper plate 22, the ceramic substrate 11 and the copper plate 23 (joining process S03). The pressurized load in the joining process S03 is set within the range of 0.049 MPa or more and 3.4 MPa or less. The pressing load in the joining process S03 is preferably set to be within the range of 0.294 MPa or more and 1.47 MPa or less, but it is not limited to this. The heating temperature in the bonding process S03 is that Cu and Mg are laminated in a non-contact state, and therefore are set to be in the range of 670°C to 850°C above the melting point of Mg. The lower limit of the heating temperature is preferably set to 700°C or higher. The degree of vacuum in the bonding process S03 is preferably set to be in the range of 1×10 -6 Pa or more and 1×10 -2 Pa or less. The holding time at the heating temperature is preferably set to be in the range of 5 minutes or more and 360 minutes or less. In order to reduce the area ratio of the aforementioned Cu 2 Mg phase, it is preferable to set the lower limit of the holding time at the heating temperature to 60 min or more. In addition, the upper limit of the holding time at the heating temperature is preferably set to 240 min or less.

像以上這樣，藉由活性金屬及Mg配置工程S01、與層積工程S02、與接合工程S03，製造本實施形態之絕緣電路基板10。As described above, the insulating circuit board 10 of this embodiment is manufactured by the active metal and Mg arrangement process S01, the lamination process S02, and the bonding process S03.

在絕緣電路基板10的金屬層13的另一方的面側將散熱座51接合(散熱座接合工程S04)。 　　將絕緣電路基板10與散熱座51，介著銲料材予以層積而裝入加熱爐，介著第2銲料層8將絕緣電路基板10與散熱座51予以銲接。The heat sink 51 is bonded to the other surface side of the metal layer 13 of the insulating circuit board 10 (heat sink bonding process S04).　　 The insulated circuit board 10 and the heat sink 51 are laminated via a solder material, and are placed in a heating furnace, and the insulated circuit board 10 and the heat sink 51 are soldered via the second solder layer 8.

接著，在絕緣電路基板10的電路層12的一方的面，將半導體元件3藉由銲接而接合(半導體元件接合工程S05)。 　　藉由以上的工程，製造出圖1所示之功率模組1。Next, on one surface of the circuit layer 12 of the insulating circuit board 10, the semiconductor element 3 is joined by soldering (semiconductor element joining process S05).　　 Through the above process, the power module 1 shown in Figure 1 is manufactured.

按照做成以上這樣的構成之本實施形態之絕緣電路基板10(銅/陶瓷接合體)，由無氧銅所成之銅板22(電路層12)及銅板23(金屬層13)與由氮化鋁所成之陶瓷基板11，是介著活性金屬膜24(Ti膜)及Mg膜25而被接合，在陶瓷基板11與電路層12(銅板22)及陶瓷基板11與金屬層13(銅板23)之接合界面，層積有形成於陶瓷基板11側之活性金屬氮化物層31(氮化鈦層)與Mg固溶於Cu的母相中而成之Mg固溶層32。According to the insulated circuit board 10 (copper/ceramic junction) of the present embodiment with the above-mentioned structure, the copper plate 22 (circuit layer 12) and the copper plate 23 (metal layer 13) made of oxygen-free copper are combined with nitride The ceramic substrate 11 made of aluminum is joined via the active metal film 24 (Ti film) and the Mg film 25. The ceramic substrate 11 and the circuit layer 12 (copper plate 22) and the ceramic substrate 11 and the metal layer 13 (copper plate 23) At the bonding interface of ), the active metal nitride layer 31 (titanium nitride layer) formed on the ceramic substrate 11 side and the Mg solid solution layer 32 formed by solid dissolving in the mother phase of Cu are laminated.

活性金屬氮化物層31(氮化鈦層)，是藉由配設於陶瓷基板11與銅板22、23之間的活性金屬(Ti)和陶瓷基板11的氮反應而形成。因此，本實施形態中，於接合界面，陶瓷基板11會充分地反應。此外，以層積於活性金屬氮化物層31(氮化鈦層)之方式，形成有Mg固溶於Cu的母相中而成之Mg固溶層32，此Mg固溶層32中含有上述的活性金屬。本實施形態中，Mg固溶層32中分散有含有Cu與活性金屬(Ti)之金屬間化合物相33，故配設於陶瓷基板11與銅板22，23之間的Mg會朝銅板22，23側充分地擴散。因此，本實施形態中，於接合界面，Cu與活性金屬(Ti)會充分地反應。The active metal nitride layer 31 (titanium nitride layer) is formed by reacting the active metal (Ti) disposed between the ceramic substrate 11 and the copper plates 22 and 23 and the nitrogen of the ceramic substrate 11. Therefore, in this embodiment, the ceramic substrate 11 fully reacts at the bonding interface. In addition, a Mg solid solution layer 32 in which Mg is solid-dissolved in the mother phase of Cu is formed by being laminated on the active metal nitride layer 31 (titanium nitride layer). The Mg solid solution layer 32 contains the above Of active metals. In this embodiment, the Mg solid solution layer 32 is dispersed with an intermetallic compound phase 33 containing Cu and active metal (Ti), so the Mg disposed between the ceramic substrate 11 and the copper plates 22, 23 will face the copper plates 22, 23 Fully spread on the side. Therefore, in this embodiment, Cu and active metal (Ti) fully react at the bonding interface.

故，在陶瓷基板11與銅板22，23之接合界面會充分地進行界面反應，能夠獲得電路層12(銅板22)與陶瓷基板11、金屬層13(銅板23)與陶瓷基板11確實地被接合而成之絕緣電路基板10(銅/陶瓷接合體)。此外，接合界面中沒有Ag存在，故能夠獲得耐遷移性優良的絕緣電路基板10(銅/陶瓷接合體)。Therefore, sufficient interfacial reactions occur at the bonding interface between the ceramic substrate 11 and the copper plates 22 and 23, and the circuit layer 12 (copper plate 22) and the ceramic substrate 11, and the metal layer 13 (copper plate 23) and the ceramic substrate 11 can be reliably joined. Manufactured insulated circuit board 10 (copper/ceramic junction body). In addition, since Ag does not exist in the bonding interface, an insulated circuit board 10 (copper/ceramic bonded body) having excellent migration resistance can be obtained.

特別是，本實施形態中，在活性金屬氮化物層31(氮化鈦層)的內部分散有Cu粒子35，故銅板22，23的Cu會在陶瓷基板11的接合面充分地反應。因此，可獲得銅板22，23與陶瓷基板11強固地被接合而成之絕緣電路基板10(銅/陶瓷接合體)。In particular, in the present embodiment, the Cu particles 35 are dispersed in the active metal nitride layer 31 (titanium nitride layer), so the Cu of the copper plates 22 and 23 fully react on the joint surface of the ceramic substrate 11. Therefore, the insulated circuit board 10 (copper/ceramic joint body) in which the copper plates 22, 23 and the ceramic substrate 11 are strongly joined can be obtained.

本實施形態中，在陶瓷基板11與電路層12(銅板22)之間，陶瓷基板11的接合面起算至往電路層12(銅板22)側50μm為止之區域中的Cu2 Mg相的面積率係被限制在15%以下，故即使實施了例如超音波接合等的情形下，仍可抑制接合界面中的破裂等的發生。 In this embodiment, between the ceramic substrate 11 and the circuit layer 12 (copper plate 22), the area ratio of the Cu 2 Mg phase in the area from the bonding surface of the ceramic substrate 11 to 50 μm from the circuit layer 12 (copper plate 22) side The system is limited to 15% or less, so even when ultrasonic bonding is performed, for example, the occurrence of cracks in the bonding interface can be suppressed.

按照本實施形態之絕緣電路基板10(銅/陶瓷接合體)的製造方法，係具備：在銅板22、23與陶瓷基板11之間配置活性金屬(Ti)的單體(活性金屬膜24)及Mg單體(Mg膜25)之活性金屬及Mg配置工程S01；及介著該些活性金屬膜24及Mg膜25將銅板22、23與陶瓷基板11予以層積之層積工程S02；及將被層積的銅板22、陶瓷基板11、銅板23於朝層積方向加壓的狀態下，於真空環境下予以加熱處理而接合之接合工程S03；故在接合界面不會殘存氣體或有機物的殘渣等。此外，由於配置活性金屬(Ti)的單體及Mg單體，故沒有組成的不均，會均一地發生液相。The manufacturing method of the insulated circuit board 10 (copper/ceramic joint) according to the present embodiment includes: disposing a single active metal (Ti) (active metal film 24) between the copper plates 22, 23 and the ceramic substrate 11, and Mg monomer (Mg film 25) active metal and Mg arrangement process S01; and a layering process S02 of laminating copper plates 22, 23 and ceramic substrate 11 via these active metal films 24 and Mg film 25; and Bonding process S03 where the laminated copper plate 22, ceramic substrate 11, and copper plate 23 are heated in a vacuum environment under pressure in the lamination direction to bond; therefore, no gas or organic residues remain at the bonding interface Wait. In addition, since the monomer of active metal (Ti) and the monomer of Mg are arranged, there is no unevenness in the composition, and the liquid phase is uniformly generated.

活性金屬及Mg配置工程S01中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內(本實施形態中，將Ti訂為0.02mg/cm2 以上2.25mg/cm2 以下的範圍內)，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內(0.17mg/cm2 以上3.48mg/cm2 以下的範圍內)，故能夠充分獲得界面反應所必要的液相，並且能夠抑制陶瓷基板11的必要以上的反應。 　　故，能夠獲得銅板22，23與陶瓷基板11確實地被接合而成之絕緣電路基板10(銅/陶瓷接合體)。此外，接合不使用Ag，故能夠獲得耐遷移性優良的絕緣電路基板10。In the active metal and Mg configuration process S01, the amount of active metal is set to be within the range of 0.4 μmol/cm 2 or more and 47.0 μmol/cm 2 or less (in this embodiment, Ti is set to be 0.02 mg/cm 2 or more and 2.25 mg/cm in the range of 2 or less), the Mg content is set in the range of (0.17mg / cm 2 or more 3.48mg / cm 2 or less in the range of 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm), it is possible to obtain sufficiently interface The liquid phase is necessary for the reaction, and more than necessary reaction of the ceramic substrate 11 can be suppressed. Therefore, it is possible to obtain the insulated circuit board 10 (copper/ceramic bonded body) in which the copper plates 22, 23 and the ceramic substrate 11 are reliably bonded. In addition, since Ag is not used for bonding, an insulated circuit board 10 excellent in migration resistance can be obtained.

當活性金屬量未滿0.4μmol/cm2 (Ti量未滿0.02mg/cm2 )、及Mg量未滿7.0μmol/cm2 (未滿0.17mg/cm2 )的情形下，界面反應會變得不充分，接合率恐會低落。此外，當活性金屬量超出47.0μmol/cm2 (Ti量超出2.25mg/cm2 )的情形下，會過度地生成活性金屬多而相對硬的金屬間化合物相33，Mg固溶層32會變得過硬，陶瓷基板11恐會發生破裂。此外，當Mg量超出143.2μmol/cm2 (超出3.48mg/ cm2 )的情形下，陶瓷基板11的分解反應會變得過度，Al會過度地生成，而會大量產生它們和Cu或和活性金屬(Ti)或和Mg之金屬間化合物，陶瓷基板11恐會發生破裂。 　　基於以上事實，本實施形態中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內(將Ti量訂為0.02mg/cm2 以上2.25mg/cm2 以下的範圍內)，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內(0.17mg/cm2 以上3.48mg/cm2 以下的範圍內)。When the amount of active metal is less than 0.4 μmol/cm 2 (the amount of Ti is less than 0.02 mg/cm 2 ), and the amount of Mg is less than 7.0 μmol/cm 2 (less than 0.17 mg/cm 2 ), the interface reaction will change Insufficient gains may reduce the engagement rate. In addition, when the amount of active metal exceeds 47.0 μmol/cm 2 (the amount of Ti exceeds 2.25 mg/cm 2 ), the relatively hard intermetallic compound phase 33 with a large amount of active metal will be excessively generated, and the Mg solid solution layer 32 will become If it is too hard, the ceramic substrate 11 may crack. In addition, when the amount of Mg exceeds 143.2 μmol/cm 2 (exceeds 3.48 mg/cm 2 ), the decomposition reaction of the ceramic substrate 11 will become excessive, and Al will be excessively generated, and a large amount of them and Cu or reactive activity will be generated. Metal (Ti) or an intermetallic compound with Mg, the ceramic substrate 11 may be cracked. Based on the above facts, the present embodiment, the amount of active metal is set within a range of 2 or less 0.4μmol / cm 2 or more 47.0μmol / cm (Ti content is set at 2 or less in the range of 0.02mg / cm 2 or more 2.25mg / cm endo), the Mg content is set in the range of (0.17mg / cm 2 or more 3.48mg / cm 2 or less in the range of 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm).

本實施形態中，接合工程S03中的加壓荷重是被訂為0.049MPa以上，故能夠使陶瓷基板11與銅板22、23與活性金屬膜24(Ti膜)及Mg膜25密合，於加熱時能夠促進它們的界面反應。此外，接合工程S03中的加壓荷重是被訂為3.4MPa以下，故能夠抑制陶瓷基板11的破裂等。In this embodiment, the pressing load in the bonding process S03 is set to 0.049 MPa or more. Therefore, the ceramic substrate 11 and the copper plates 22, 23 can be brought into close contact with the active metal film 24 (Ti film) and the Mg film 25 and heated Time can promote their interface reaction. In addition, since the pressing load in the joining process S03 is set to 3.4 MPa or less, it is possible to suppress cracks and the like of the ceramic substrate 11.

本實施形態中，Cu與Mg是在非接觸狀態下被層積，接合工程S03中的加熱溫度是被訂為Mg的熔點以上之670℃以上，故於接合界面能夠充分地令液相發生。另一方面，接合工程S03中的加熱溫度是被訂為850℃以下，故能夠抑制Cu與活性金屬(Ti)之共晶反應的發生，能夠抑制液相過度地生成。此外，對陶瓷基板11之熱負荷會變小，能夠抑制陶瓷基板11的劣化。In this embodiment, Cu and Mg are laminated in a non-contact state, and the heating temperature in the bonding process S03 is set at 670°C or more, which is the melting point of Mg, so that the liquid phase can be sufficiently generated at the bonding interface. On the other hand, the heating temperature in the joining process S03 is set to 850°C or lower, so the occurrence of the eutectic reaction between Cu and the active metal (Ti) can be suppressed, and the excessive generation of the liquid phase can be suppressed. In addition, the thermal load on the ceramic substrate 11 is reduced, and the deterioration of the ceramic substrate 11 can be suppressed.

(第2實施形態) 　　針對本發明之第2實施形態，參照圖5至圖8說明之。 　　本實施形態之銅/陶瓷接合體，係被做成藉由陶瓷構件即陶瓷基板111與銅構件即銅板122(電路層112)被接合而構成之絕緣電路基板110。 　　圖5揭示本發明第2實施形態之絕緣電路基板110及使用了此絕緣電路基板110之功率模組101。(Second Embodiment) "The second embodiment of the present invention will be described with reference to FIGS. 5 to 8. "The copper/ceramic bonded body of this embodiment is an insulated circuit board 110 formed by bonding a ceramic substrate 111 as a ceramic member and a copper plate 122 (circuit layer 112) as a copper member.　　 FIG. 5 shows the insulated circuit board 110 of the second embodiment of the present invention and the power module 101 using the insulated circuit board 110.

此功率模組101，具備絕緣電路基板110、及在此絕緣電路基板110的一方側(圖5中上側)的面介著銲料層2而被接合之半導體元件3、及配置於絕緣電路基板110的另一方側(圖5中下側)之散熱座151。 　　銲料層2，例如訂為Sn-Ag系、Sn-In系、或是Sn-Ag-Cu系的銲料材。This power module 101 includes an insulated circuit board 110, and a semiconductor element 3 that is bonded to one side (upper side in FIG. 5) of the insulated circuit board 110 via a solder layer 2, and is arranged on the insulated circuit board 110 The heat sink 151 on the other side (the lower side in FIG. 5). The "solder layer 2" is ordered as a solder material of Sn-Ag system, Sn-In system, or Sn-Ag-Cu system, for example.

絕緣電路基板110，具備陶瓷基板111、及配設於此陶瓷基板111的一方的面(圖5中上面)之電路層112、及配設於陶瓷基板111的另一方的面(圖5中下面)之金屬層113。 　　陶瓷基板111，為防止電路層112與金屬層113之間的電性連接之物，本實施形態中由絕緣性高的氮化矽來構成。陶瓷基板111的厚度，被設定成0.2～1.5mm的範圍內，本實施形態中被設定成0.32mm。The insulated circuit substrate 110 includes a ceramic substrate 111, a circuit layer 112 arranged on one side of the ceramic substrate 111 (upper side in FIG. 5), and a circuit layer 112 arranged on the other side of the ceramic substrate 111 (lower side in FIG. 5). ) The metal layer 113.　　The ceramic substrate 111 is to prevent electrical connection between the circuit layer 112 and the metal layer 113. In this embodiment, it is made of silicon nitride with high insulation. The thickness of the ceramic substrate 111 is set in the range of 0.2 to 1.5 mm, and is set to 0.32 mm in this embodiment.

電路層112，如圖8所示，是藉由在陶瓷基板111的一方的面接合由銅或銅合金所成之銅板122而形成。本實施形態中，作為構成電路層112的銅板122，使用無氧銅的壓延板。在此電路層112，形成有電路圖樣，其一方的面(圖5中上面)，為供半導體元件3搭載之搭載面。電路層112的厚度被設定成0.1mm以上2.0mm以下的範圍內，本實施形態中被設定成0.6mm。The circuit layer 112, as shown in FIG. 8, is formed by bonding a copper plate 122 made of copper or a copper alloy to one surface of the ceramic substrate 111. In this embodiment, as the copper plate 122 constituting the circuit layer 112, a rolled plate of oxygen-free copper is used. In this circuit layer 112, a circuit pattern is formed, and one surface (the upper surface in FIG. 5) of the circuit layer 112 is a mounting surface on which the semiconductor element 3 is mounted. The thickness of the circuit layer 112 is set in the range of 0.1 mm or more and 2.0 mm or less, and is set to 0.6 mm in this embodiment.

金屬層113，如圖8所示，是藉由在陶瓷基板111的另一方的面接合鋁板123而形成。本實施形態中，金屬層113，是以由純度99.99mass%以上的鋁(即所謂4N鋁)的壓延板所成之鋁板123被接合至陶瓷基板111而形成。此鋁板123，0.2%安全限應力被訂為30N/mm2 以下。金屬層113(鋁板123)的厚度被設定成0.5mm以上6mm以下的範圍內，本實施形態中被設定成2.0mm。金屬層113，如圖8所示，是藉由鋁板123使用Al-Si系硬銲材128被接合至陶瓷基板111而形成。The metal layer 113 is formed by bonding an aluminum plate 123 to the other surface of the ceramic substrate 111 as shown in FIG. 8. In this embodiment, the metal layer 113 is formed by bonding an aluminum plate 123 made of a rolled plate of aluminum with a purity of 99.99 mass% or more (that is, so-called 4N aluminum) to the ceramic substrate 111. For this aluminum plate 123, the 0.2% safety limit stress is set as 30N/mm 2 or less. The thickness of the metal layer 113 (aluminum plate 123) is set in the range of 0.5 mm or more and 6 mm or less, and is set to 2.0 mm in this embodiment. As shown in FIG. 8, the metal layer 113 is formed by bonding an aluminum plate 123 to the ceramic substrate 111 using an Al-Si-based brazing material 128.

散熱座151，為用來將前述的絕緣電路基板110冷卻之物，本實施形態中以由熱傳導性良好的材質所構成之散熱板來構成。本實施形態中，散熱座151以A6063(鋁合金)來構成。本實施形態中，此散熱座151，是在絕緣電路基板110的金屬層113，例如使用Al-Si系硬銲材而接合。The heat sink 151 is used to cool the aforementioned insulated circuit board 110. In this embodiment, a heat sink made of a material with good thermal conductivity is used. In this embodiment, the heat sink 151 is made of A6063 (aluminum alloy). In this embodiment, the heat sink 151 is joined to the metal layer 113 of the insulated circuit board 110 using, for example, Al-Si-based brazing material.

陶瓷基板111與電路層112(銅板122)，如圖8所示，是介著由從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬所成之活性金屬膜124(本實施形態中為Ti膜)及Mg膜125而被接合。 　　於陶瓷基板111與電路層112(銅板122)之接合界面，如圖6所示，層積有形成於陶瓷基板111側之活性金屬氮化物層131(本實施形態中為氮化鈦層)與Mg固溶於Cu的母相中而成之Mg固溶層132。The ceramic substrate 111 and the circuit layer 112 (copper plate 122), as shown in FIG. 8, are interposed by an active metal film 124 (this In the embodiment, the Ti film) and the Mg film 125 are joined. At the bonding interface between the ceramic substrate 111 and the circuit layer 112 (copper plate 122), as shown in FIG. 6, an active metal nitride layer 131 (a titanium nitride layer in this embodiment) and an active metal nitride layer 131 (a titanium nitride layer in this embodiment) formed on the ceramic substrate 111 side are laminated The Mg solid solution layer 132 is formed by solid dissolving Mg in the mother phase of Cu.

Mg固溶層132中，含有上述的活性金屬。本實施形態中，Mg固溶層132中，分散有含有Cu與活性金屬(Ti)之金屬間化合物相133。本實施形態中，作為活性金屬使用Ti，作為構成含有Cu與Ti之金屬間化合物相133的金屬間化合物，例如可舉出Cu4 Ti，Cu3 Ti2 ，Cu4 Ti3 ，CuTi，CuTi2 ，CuTi3 等。 　　此Mg固溶層132中的Mg的含有量，被訂為0.01原子%以上0.5原子%以下的範圍內。Mg固溶層132的厚度，被訂為0.1μm以上80μm以下的範圍內。The Mg solid solution layer 132 contains the above-mentioned active metal. In this embodiment, in the Mg solid solution layer 132, an intermetallic compound phase 133 containing Cu and active metal (Ti) is dispersed. In this embodiment, Ti is used as the active metal. Examples of the intermetallic compound constituting the intermetallic compound phase 133 containing Cu and Ti include Cu 4 Ti, Cu 3 Ti 2 , Cu 4 Ti 3 , CuTi, and CuTi 2 , CuTi 3 and so on. The content of Mg in the Mg solid solution layer 132 is set to be in the range of 0.01 atomic% to 0.5 atomic %. The thickness of the Mg solid solution layer 132 is set to be in the range of 0.1 μm or more and 80 μm or less.

本實施形態中，在活性金屬氮化物層131(氮化鈦層)的內部，分散有Cu粒子135。 　　分散在活性金屬氮化物層131(氮化鈦層)內之Cu粒子135的粒徑，被訂為10nm以上100nm以下的範圍內。活性金屬氮化物層131(氮化鈦層)當中與陶瓷基板111之界面起算至活性金屬氮化物層131(氮化鈦層)的厚度的20%為止之界面鄰近區域中的Cu濃度，被訂為0.3原子%以上15原子%以下的範圍內。 　　活性金屬氮化物層131(氮化鈦層)的厚度，被訂為0.03μm以上1.2μm以下的範圍內。In this embodiment, Cu particles 135 are dispersed in the active metal nitride layer 131 (titanium nitride layer). "The particle size of the Cu particles 135 dispersed in the active metal nitride layer 131 (titanium nitride layer) is set to be in the range of 10 nm or more and 100 nm or less. The Cu concentration in the area adjacent to the active metal nitride layer 131 (titanium nitride layer) from the interface with the ceramic substrate 111 to 20% of the thickness of the active metal nitride layer 131 (titanium nitride layer) is determined It is in the range of 0.3 atomic% or more and 15 atomic% or less. The thickness of the active metal nitride layer 131 (titanium nitride layer) is set to be in the range of 0.03 μm or more and 1.2 μm or less.

本實施形態中，在陶瓷基板111與電路層112之間，陶瓷基板111的接合面起算至往電路層112側50μm為止之區域中的Cu2 Mg相的面積率，被訂為15%以下。 In this embodiment, the area ratio of the Cu 2 Mg phase in the area 50 μm from the bonding surface of the ceramic substrate 111 to the circuit layer 112 side between the ceramic substrate 111 and the circuit layer 112 is set to 15% or less.

針對上述本實施形態之絕緣電路基板110的製造方法，參照圖7及圖8說明之。The method of manufacturing the insulated circuit board 110 of the present embodiment described above will be described with reference to FIGS. 7 and 8.

如圖8所示，在作為電路層112之銅板122與陶瓷基板111之間，配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體(本實施形態中為Ti單體)及Mg單體(活性金屬及Mg配置工程S101)。本實施形態中，藉由蒸鍍活性金屬(Ti)及Mg，會形成活性金屬膜124(Ti膜)及Mg膜125，Mg膜125會以接觸銅板122之方式形成。 　　此活性金屬及Mg配置工程S101中，將活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內(本實施形態中，將Ti訂為0.02mg/cm2 以上2.25mg/cm2 以下的範圍內)，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內(0.17mg/cm2 以上3.48mg/cm2 以下的範圍內)。As shown in FIG. 8, between the copper plate 122 as the circuit layer 112 and the ceramic substrate 111, a single type or two or more types of active metals selected from Ti, Zr, Nb, and Hf are arranged (in this embodiment, it is Ti monomer) and Mg monomer (active metal and Mg configuration process S101). In this embodiment, an active metal film 124 (Ti film) and a Mg film 125 are formed by vapor deposition of active metal (Ti) and Mg, and the Mg film 125 is formed in contact with the copper plate 122. In this active metal and Mg configuration process S101, the amount of active metal is set to be within the range of 0.4 μmol/cm 2 or more and 47.0 μmol/cm 2 or less (in this embodiment, Ti is set to be 0.02 mg/cm 2 or more and 2.25 mg/cm2). or less in the range of 2 cm), the amount of Mg is set within a range of (0.17mg / cm 2 or more 3.48mg / cm 2 or less in the range of 2 or less 143.2μmol / cm 2 or more 7.0μmol / cm).

當活性金屬量未滿0.4μmol/cm2 (Ti量未滿0.02mg/cm2 )、及Mg量未滿7.0μmol/cm2 (未滿0.17mg/cm2 )的情形下，界面反應會變得不充分，接合率恐會低落。此外，當活性金屬量超出47.0μmol/cm2 (Ti量超出2.25mg/cm2 )的情形下，會過度地生成活性金屬多而相對硬的金屬間化合物相133，Mg固溶層132會變得過硬，陶瓷基板111恐會發生破裂。此外，當Mg量超出143.2μmol /cm2 (超出3.48mg/ cm2 )的情形下，陶瓷基板111的分解反應會變得過度，Al會過度地生成，而會大量產生它們和Cu或和活性金屬(Ti)或和Mg之金屬間化合物，陶瓷基板111恐會發生破裂。 　　活性金屬量的下限較佳是訂為2.8μmol/cm2 以上，活性金屬量的上限較佳是訂為18.8μmol/cm2 以下。此外，Mg量的下限較佳是訂為8.8μmol/cm2 以上，Mg量的上限較佳是訂為37.0μmol/cm2 以下。When the amount of active metal is less than 0.4 μmol/cm 2 (the amount of Ti is less than 0.02 mg/cm 2 ), and the amount of Mg is less than 7.0 μmol/cm 2 (less than 0.17 mg/cm 2 ), the interface reaction will change Insufficient gains may reduce the engagement rate. In addition, when the amount of active metal exceeds 47.0 μmol/cm 2 (the amount of Ti exceeds 2.25 mg/cm 2 ), a relatively hard intermetallic compound phase 133 with a large amount of active metal will be excessively generated, and the Mg solid solution layer 132 will become If it is too hard, the ceramic substrate 111 may crack. In addition, when the amount of Mg exceeds 143.2 μmol/cm 2 (exceeds 3.48 mg/cm 2 ), the decomposition reaction of the ceramic substrate 111 will become excessive, and Al will be excessively generated, and a large amount of them and Cu or reactive activity will be generated. With metal (Ti) or an intermetallic compound with Mg, the ceramic substrate 111 may crack. The lower limit of the amount of active metal is preferably set to 2.8 μmol/cm 2 or more, and the upper limit of the amount of active metal is preferably set to 18.8 μmol/cm 2 or less. In addition, the lower limit of the amount of Mg is preferably set to 8.8 μmol/cm 2 or more, and the upper limit of the amount of Mg is preferably set to 37.0 μmol/cm 2 or less.

接著，將銅板122與陶瓷基板111，介著活性金屬膜124(Ti膜)及Mg膜125予以層積(層積工程S102)。 　　本實施形態中，如圖8所示，在陶瓷基板111的另一方的面側，介著Al-Si系硬銲材128，層積作為金屬層113之鋁板123。Next, the copper plate 122 and the ceramic substrate 111 are laminated via the active metal film 124 (Ti film) and the Mg film 125 (layering process S102). "In this embodiment, as shown in FIG. 8, on the other surface side of the ceramic substrate 111, the Al-Si-based brazing material 128 is interposed, and the aluminum plate 123 as the metal layer 113 is laminated.

將被層積的銅板122、陶瓷基板111、銅板123朝層積方向加壓，並且裝入真空爐內加熱，將銅板122與陶瓷基板111與鋁板123接合(接合工程S103)。 　　接合工程S103中的加壓荷重，被訂為0.049MPa以上3.4MPa以下的範圍內。接合工程S103中的加壓荷重，較佳是被訂為0.294MPa以上1.47MPa以下的範圍內，但不限定於此。The laminated copper plate 122, the ceramic substrate 111, and the copper plate 123 are pressurized in the stacking direction and heated in a vacuum furnace to join the copper plate 122, the ceramic substrate 111 and the aluminum plate 123 (joining process S103).　　 The pressurizing load in the joining process S103 is set within the range of 0.049 MPa or more and 3.4 MPa or less. The pressing load in the joining process S103 is preferably set to be in the range of 0.294 MPa or more and 1.47 MPa or less, but it is not limited to this.

接合工程S103中的加熱溫度，由於Cu與Mg是在接觸狀態下被層積，因此訂為Mg與Cu的共晶溫度以上之500℃以上，且Cu與活性金屬(Ti)的共晶溫度以下之850℃以下。加熱溫度的下限較佳是訂為700℃以上。 　　本實施形態中，是將鋁板123使用Al-Si系硬銲材128來接合，因此加熱溫度訂為600℃以上650℃以下的範圍內。 　　接合工程S103中的真空度，較佳是訂為1×10-6 Pa以上1×10-2 Pa以下的範圍內。 　　加熱溫度下的保持時間，較佳是訂為5min以上360min以下的範圍內。為了減低上述的Cu2 Mg相的面積率，較佳是將加熱溫度下的保持時間的下限訂為60min以上。加熱溫度下的保持時間的上限較佳是訂為240min以下。The heating temperature in the bonding process S103, because Cu and Mg are laminated in the contact state, it is set at 500°C or more above the eutectic temperature of Mg and Cu, and below the eutectic temperature of Cu and active metal (Ti) Below 850℃. The lower limit of the heating temperature is preferably set to 700°C or higher. In this embodiment, the aluminum plates 123 are joined using the Al-Si-based brazing material 128, so the heating temperature is set within the range of 600°C or more and 650°C or less. The degree of vacuum in the bonding process S103 is preferably set to be in the range of 1×10 -6 Pa or more and 1×10 -2 Pa or less. The holding time at the heating temperature is preferably set to be in the range of 5 minutes or more and 360 minutes or less. In order to reduce the area ratio of the aforementioned Cu 2 Mg phase, it is preferable to set the lower limit of the holding time at the heating temperature to 60 min or more. The upper limit of the holding time at the heating temperature is preferably set to 240 min or less.

像以上這樣，藉由活性金屬及Mg配置工程S101、與層積工程S102、與接合工程S103，製造本實施形態之絕緣電路基板110。As described above, the insulating circuit board 110 of this embodiment is manufactured by the active metal and Mg arrangement process S101, the lamination process S102, and the bonding process S103.

在絕緣電路基板110的金屬層113的另一方的面側將散熱座151接合(散熱座接合工程S104)。 　　將絕緣電路基板110與散熱座151，介著硬銲材予以層積，朝層積方向加壓並且裝入真空爐內進行硬銲。如此一來，便將絕緣電路基板110的金屬層113與散熱座151接合。此時，作為硬銲材，例如能夠使用厚度20～110μm的Al-Si系硬銲材箔，硬銲溫度較佳是設定成比接合工程S103中的加熱溫度還低溫。The heat sink 151 is bonded to the other surface side of the metal layer 113 of the insulated circuit board 110 (heat sink bonding process S104).　　The insulated circuit board 110 and the heat sink 151 are laminated via a brazing material, pressurized in the lamination direction, and loaded into a vacuum furnace for brazing. In this way, the metal layer 113 of the insulated circuit substrate 110 and the heat sink 151 are joined. At this time, as the brazing material, for example, an Al-Si-based brazing material foil having a thickness of 20 to 110 μm can be used, and the brazing temperature is preferably set to be lower than the heating temperature in the joining process S103.

接著，在絕緣電路基板110的電路層112的一方的面，將半導體元件3藉由銲接而接合(半導體元件接合工程S105)。 　　藉由以上的工程，製造出圖5所示之功率模組101。Next, on one surface of the circuit layer 112 of the insulating circuit board 110, the semiconductor element 3 is joined by soldering (semiconductor element joining step S105).　　 Through the above process, the power module 101 shown in FIG. 5 is manufactured.

按照做成以上這樣的構成之本實施形態之絕緣電路基板110(銅/陶瓷接合體)，銅板122(電路層112)與由氮化矽所成之陶瓷基板111，是介著活性金屬膜124(Ti膜)及Mg膜125而被接合，在陶瓷基板111與電路層112(銅板122)之接合界面，層積有形成於陶瓷基板111側之活性金屬氮化物層131(氮化鈦層)與Mg固溶於Cu的母相中而成之Mg固溶層132，在此Mg固溶層132內，存在有活性金屬。本實施形態中，係分散有含有Cu與活性金屬(Ti)之金屬間化合物相133，故如同第1實施形態般，能夠獲得電路層112(銅板122)與陶瓷基板111確實地被接合而成之絕緣電路基板110(銅/陶瓷接合體)。此外，接合界面中沒有Ag存在，故能夠獲得耐遷移性優良的絕緣電路基板110(銅/陶瓷接合體)。According to the insulated circuit board 110 (copper/ceramic junction) of the present embodiment having the above-mentioned structure, the copper plate 122 (circuit layer 112) and the ceramic substrate 111 made of silicon nitride are interposed with an active metal film 124 (Ti film) and Mg film 125 are joined. At the joint interface between the ceramic substrate 111 and the circuit layer 112 (copper plate 122), an active metal nitride layer 131 (titanium nitride layer) formed on the ceramic substrate 111 side is laminated The Mg solid solution layer 132 formed by dissolving Mg with Mg in the matrix phase of Cu, and the active metal is present in the Mg solid solution layer 132. In this embodiment, the intermetallic compound phase 133 containing Cu and active metal (Ti) is dispersed. Therefore, as in the first embodiment, the circuit layer 112 (copper plate 122) and the ceramic substrate 111 can be reliably joined. The insulated circuit substrate 110 (copper/ceramic junction). In addition, since Ag is not present in the bonding interface, an insulated circuit board 110 (copper/ceramic bonded body) having excellent migration resistance can be obtained.

本實施形態中，在活性金屬氮化物層131(氮化鈦層)的內部分散有Cu粒子135，故銅板122的Cu會變得在陶瓷基板111的接合面充分地反應，可獲得電路層112(銅板122)與陶瓷基板111強固地被接合而成之絕緣電路基板110(銅/陶瓷接合體)。In this embodiment, the Cu particles 135 are dispersed in the active metal nitride layer 131 (titanium nitride layer), so the Cu of the copper plate 122 will fully react on the joint surface of the ceramic substrate 111, and the circuit layer 112 can be obtained. (Copper plate 122) Insulated circuit board 110 (copper/ceramic bonded body) formed by strongly bonding ceramic substrate 111.

本實施形態中，在陶瓷基板111與電路層112(銅板122)之間，陶瓷基板111的接合面起算至往電路層112(銅板122)側50μm為止之區域中的Cu2 Mg相的面積率係被限制在15%以下，故即使實施了例如超音波接合等的情形下，仍可抑制接合界面中的破裂等的發生。 In this embodiment, between the ceramic substrate 111 and the circuit layer 112 (copper plate 122), the area ratio of the Cu 2 Mg phase in the area from the bonding surface of the ceramic substrate 111 to 50 μm toward the circuit layer 112 (copper plate 122) side The system is limited to 15% or less, so even when ultrasonic bonding is performed, for example, the occurrence of cracks in the bonding interface can be suppressed.

按照本實施形態之絕緣電路基板110(銅/陶瓷接合體)的製造方法，如同第1實施形態般，在電路層112(銅板122)與陶瓷基板111之接合界面，能夠使液相適度地出現而充分地使其界面反應，能夠獲得銅板122與陶瓷基板111確實地被接合而成之絕緣電路基板110(銅/陶瓷接合體)。此外，接合不使用Ag，故能夠獲得耐遷移性優良的絕緣電路基板110。According to the manufacturing method of the insulated circuit board 110 (copper/ceramic joint) of this embodiment, as in the first embodiment, a liquid phase can be appropriately formed at the bonding interface between the circuit layer 112 (copper plate 122) and the ceramic substrate 111 The interface reaction is sufficiently made to obtain an insulated circuit substrate 110 (copper/ceramic joint body) in which the copper plate 122 and the ceramic substrate 111 are reliably joined. In addition, since Ag is not used for bonding, it is possible to obtain an insulated circuit board 110 having excellent migration resistance.

本實施形態中，Cu與Mg是在接觸狀態下被層積，接合工程S103中的加熱溫度是被訂為Cu與Mg的共晶溫度以上之500℃以上，故於接合界面能夠充分地令液相發生。 　　本實施形態中，於層積工程S102，是在陶瓷基板111的另一面側將鋁板123介著Al-Si系硬銲材128而層積，而將銅板122與陶瓷基板111、陶瓷基板111與鋁板123予以同時接合，故能夠效率良好地製造具備由銅所成之電路層112與由鋁所成之金屬層113的絕緣電路基板110。此外，能夠抑制絕緣電路基板110中的翹曲的發生。In this embodiment, Cu and Mg are laminated in a contact state, and the heating temperature in the bonding process S103 is set at 500°C or more, which is the eutectic temperature of Cu and Mg. Therefore, the bonding interface can sufficiently make the liquid Phase occurs. In this embodiment, in the layering process S102, the aluminum plate 123 is layered on the other side of the ceramic substrate 111 through the Al-Si brazing material 128, and the copper plate 122 and the ceramic substrate 111, and the ceramic substrate 111 The aluminum plates 123 are joined at the same time, so the insulated circuit board 110 provided with the circuit layer 112 made of copper and the metal layer 113 made of aluminum can be efficiently manufactured. In addition, the occurrence of warpage in the insulated circuit board 110 can be suppressed.

以上已說明了本發明之實施形態，但本發明並不限定於此，在不脫離其發明技術思想之範圍內可適當變更。 　　例如，雖說明了將構成電路層或金屬層之銅板訂為無氧銅的壓延板，但不限定於此，亦可為由其他的銅或銅合金所構成之物。The embodiments of the present invention have been described above, but the present invention is not limited to this, and can be appropriately changed without departing from the scope of the technical idea of the invention. "For example, although it has been described that the copper plate constituting the circuit layer or the metal layer is ordered as a rolled plate of oxygen-free copper, it is not limited to this, and may be made of other copper or copper alloy.

第2實施形態中，雖說明了將構成金屬層之鋁板訂為純度99.99mass%的純鋁的壓延板，但不限定於此，亦可為由純度99mass%的鋁(2N鋁)等其他的鋁或鋁合金所構成之物。In the second embodiment, although the aluminum sheet constituting the metal layer is described as a rolled sheet made of pure aluminum with a purity of 99.99mass%, it is not limited to this, and may be made of aluminum (2N aluminum) with a purity of 99mass%. Something made of aluminum or aluminum alloy.

作為散熱座雖舉散熱板為例說明，但不限定於此，散熱座的構造並無特別限定。例如，亦可為具有供冷媒流通的流路之物或具備了冷卻鰭片之物。作為散熱座亦能使用含有鋁或鋁合金之複合材(例如AlSiC等)。 　　在散熱座的頂板部或在散熱板與金屬層之間，亦可設置由鋁或鋁合金或是含有鋁之複合材(例如AlSiC等)所成之緩衝層。Although the heat sink is taken as an example for the description of the heat sink, it is not limited to this, and the structure of the heat sink is not particularly limited. For example, it may be a thing having a flow path through which a refrigerant circulates or a thing equipped with cooling fins. A composite material containing aluminum or aluminum alloy (such as AlSiC, etc.) can also be used as a heat sink. "On the top plate of the heat sink or between the heat sink and the metal layer, a buffer layer made of aluminum or aluminum alloy or a composite material containing aluminum (such as AlSiC, etc.) can also be provided.

本實施形態中，雖說明了活性金屬及Mg配置工程中，是將活性金屬膜(Ti膜)及Mg膜予以成膜，但不限定於此，亦可將活性金屬與Mg予以共蒸鍍。在此情形下同樣地，被成膜之活性金屬膜及Mg膜，並未被合金化，而是配置活性金屬的單體及Mg單體。當藉由共蒸鍍將活性金屬及Mg膜成膜的情形下，Mg與Cu會成為接觸狀態，因此能夠將接合工程中的加熱溫度的下限訂為500℃以上。In this embodiment, although the active metal and Mg arrangement process is described as forming an active metal film (Ti film) and a Mg film, it is not limited to this, and the active metal and Mg may be co-evaporated. In this case, similarly, the active metal film and the Mg film to be formed are not alloyed, but the active metal monomer and Mg monomer are arranged. When the active metal and the Mg film are formed by co-evaporation, Mg and Cu will be in contact. Therefore, the lower limit of the heating temperature in the joining process can be set to 500° C. or more.

本實施形態中，雖說明了使用Ti作為活性金屬，但不限定於此，作為活性金屬亦可使用從Ti，Zr，Nb，Hf選擇之1種或2種以上。 　　當使用了Zr作為活性金屬的情形下，Mg固溶層中，Zr會以與Cu之金屬間化合物相的方式存在。作為構成此金屬間化合物相之金屬間化合物，例如可舉出Cu5 Zr，Cu51 Zr14 ，Cu8 Zr3 ，Cu10 Zr7 ，CuZr，Cu5 Zr8 ，CuZr2 等。 　　當使用了Hf作為活性金屬的情形下，Mg固溶層中，Hf會以與Cu之金屬間化合物相的方式存在。作為構成此金屬間化合物相之金屬間化合物，例如可舉出Cu51 Hf14 ，Cu8 Hf3 ，Cu10 Hf7 ，CuHf2 等。 　　當使用了Ti及Zr作為活性金屬的情形下，Mg固溶層中，Ti及Zr會以含有Cu與活性金屬之金屬間化合物相的方式存在。作為構成此金屬間化合物相之金屬間化合物，可舉出Cu1.5 Zr0.75 Ti0.75 等。 　　當使用了Nb作為活性金屬的情形下，Mg固溶層中，Nb會固溶於Mg固溶層而存在。In this embodiment, although Ti is described as the active metal, it is not limited to this. As the active metal, one or two or more selected from Ti, Zr, Nb, and Hf may also be used. When Zr is used as the active metal, in the Mg solid solution layer, Zr will exist as an intermetallic compound phase with Cu. Examples of the intermetallic compound constituting the intermetallic compound phase include Cu 5 Zr, Cu 51 Zr 14 , Cu 8 Zr 3 , Cu 10 Zr 7 , CuZr, Cu 5 Zr 8 , CuZr 2 and the like. When Hf is used as the active metal, in the Mg solid solution layer, Hf will exist as an intermetallic compound phase with Cu. Examples of the intermetallic compound constituting the intermetallic compound phase include Cu 51 Hf 14 , Cu 8 Hf 3 , Cu 10 Hf 7 , CuHf 2 and the like. When Ti and Zr are used as the active metal, Ti and Zr will exist in the Mg solid solution layer as an intermetallic compound phase containing Cu and the active metal. Examples of the intermetallic compound constituting the intermetallic compound phase include Cu 1.5 Zr 0.75 Ti 0.75 and the like. When Nb is used as the active metal, in the Mg solid solution layer, Nb will be dissolved in the Mg solid solution layer and exist.

活性金屬及Mg配置工程中，只要將接合界面中的活性金屬量訂為0.4μmol/cm2 以上47.0μmol/cm2 以下的範圍內，將Mg量訂為7.0μmol/cm2 以上143.2μmol/cm2 以下的範圍內即可，例如亦可像Mg膜/活性金屬膜/Mg膜這樣將活性金屬膜與Mg膜予以多層地層積。或者是，亦可在活性金屬膜與Mg膜之間將Cu膜成膜。 　　活性金屬的單體及Mg單體，可配置箔材，亦可藉由濺鍍來成膜。In the active metal and Mg configuration process, as long as the amount of active metal in the joint interface is set within the range of 0.4μmol/cm 2 or more and 47.0 μmol/cm 2 or less, the amount of Mg is set to be 7.0 μmol/cm 2 or more and 143.2 μmol/cm The range of 2 or less may be sufficient. For example, the active metal film and the Mg film may be laminated in multiple layers like Mg film/active metal film/Mg film. Alternatively, the Cu film may be formed between the active metal film and the Mg film. Active metal monomers and Mg monomers can be equipped with foils, and can also be sputtered to form films.

本實施形態中，雖說明了在絕緣電路基板的電路層搭載功率半導體元件來構成功率模組之物，但不限定於此。例如，亦可在絕緣電路基板搭載LED元件來構成LED模組，亦可在絕緣電路基板的電路層搭載熱電元件來構成熱電模組。 [實施例]In this embodiment, although a power semiconductor element is mounted on the circuit layer of an insulated circuit board to form a power module, it is not limited to this. For example, an LED element may be mounted on an insulated circuit board to form an LED module, or a thermoelectric element may be mounted on the circuit layer of the insulated circuit board to form a thermoelectric module. [Example]

說明為確認本發明的有效性而進行之確認實驗。A confirmation experiment performed to confirm the effectiveness of the present invention will be described.

＜實施例1＞ 　　形成了表1所示構造之銅/陶瓷接合體。詳言之，是在40mm見方的陶瓷基板的兩面，如表1所示，層積將Ti單體及Mg單體作為活性金屬予以成膜而成之銅板，以表1所示之接合條件接合，形成了銅/陶瓷接合體。 　　陶瓷基板的厚度當氮化鋁的情形下使用了厚度0.635mm，當氮化矽的情形下使用了厚度0.32mm。此外，接合時的真空爐的真空度訂為5×10-3 Pa。<Example 1> A copper/ceramic joint body having the structure shown in Table 1 was formed. Specifically, it is a copper plate formed by laminating Ti and Mg as active metals on both sides of a 40mm square ceramic substrate, as shown in Table 1, and bonding under the bonding conditions shown in Table 1. , Forming a copper/ceramic joint body. The thickness of the ceramic substrate is 0.635mm in the case of aluminum nitride, and 0.32mm in the case of silicon nitride. In addition, the vacuum degree of the vacuum furnace at the time of bonding is set to 5×10 -3 Pa.

針對依此方式獲得的銅/陶瓷接合體，觀察接合界面來確認活性金屬氮化物層(氮化鈦層)、Mg固溶層、金屬間化合物相、活性金屬氮化物層(氮化鈦層)中的Cu粒子的有無及Cu濃度。此外，依以下方式評估了銅/陶瓷接合體的初始接合率、冷熱循環後的陶瓷基板的破裂、遷移性。For the copper/ceramic joint obtained in this way, observe the joint interface to confirm the active metal nitride layer (titanium nitride layer), Mg solid solution layer, intermetallic compound phase, and active metal nitride layer (titanium nitride layer) The presence or absence of Cu particles and the concentration of Cu. In addition, the initial bonding rate of the copper/ceramic bonded body, the fracture and migration of the ceramic substrate after the cooling and heating cycle were evaluated in the following manner.

(Mg固溶層) 　　對於銅板與陶瓷基板之接合界面，使用EPMA裝置(日本電子公司製JXA-8539F)，以倍率2000倍、加速電壓15kV的條件觀察包含接合界面之區域(400μm×600μm)，從陶瓷基板表面(活性金屬氮化物層表面)朝向銅板側以10μm間隔的10點進行定量分析，將Mg濃度為0.01原子%以上之區域訂為Mg固溶層。(Mg solid solution layer) 　　For the bonding interface between the copper plate and the ceramic substrate, use an EPMA device (JXA-8539F manufactured by JEOL Ltd.) to observe the area including the bonding interface (400μm×600μm) at a magnification of 2000 times and an acceleration voltage of 15kV. Quantitative analysis was performed at 10 points at 10 μm intervals from the surface of the ceramic substrate (the surface of the active metal nitride layer) toward the copper plate, and the area where the Mg concentration was 0.01 at% or more was designated as the Mg solid solution layer.

(Mg固溶層中的活性金屬的有無(金屬間化合物相的有無) 　　對於銅板與陶瓷基板之接合界面，使用電子探針顯微分析儀(日本電子公司製JXA-8539F)，以倍率2000倍、加速電壓15kV的條件取得包含接合界面之區域(400μm ×600μm)的活性金屬(Ti)的元素MAP，確認了活性金屬(Ti)的有無。此外，以確認到活性金屬(Ti)的存在之區域內的定量分析的5點平均，將滿足Cu濃度為5原子%以上，且活性金屬濃度(Ti濃度)為16原子以上90原子%以下之區域訂為金屬間化合物相。(Presence of active metal in the Mg solid solution layer (presence of intermetallic compound phase) 　　 For the bonding interface between the copper plate and the ceramic substrate, use an electron probe microanalyzer (JXA-8539F manufactured by JEOL Ltd.) at a magnification of 2000 times The element MAP of the active metal (Ti) in the area (400 μm × 600 μm) of the joint interface was obtained under the conditions of acceleration voltage of 15kV, and the presence of active metal (Ti) was confirmed. In addition, the presence of active metal (Ti) was confirmed The 5-point average of the quantitative analysis in the area defines the area satisfying that the Cu concentration is 5 atomic% or more and the active metal concentration (Ti concentration) is 16 atomic% or more and 90 atomic% or less as the intermetallic compound phase.

(活性金屬氮化物層) 　　對於銅板與陶瓷基板之接合界面，使用掃描型穿透電子顯微鏡(FEI公司製Titan ChemiSTEM(附EDS檢測器))，以倍率115000倍、加速電壓200kV的條件進行觀察，能量分散型X射線分析法(賽默飛世爾科技公司製NSS7)進行測繪(mapping)，於活性金屬(Ti)和N重疊之區域，藉由照射縮細至1nm程度之電子束(NBD(奈米射束繞射)法)來獲得電子繞射圖形，確認了活性金屬氮化物層(氮化鈦層)的有無。 　　對確認到活性金屬氮化物層(氮化鈦層)之區域中確認Cu粒子的有無，將由此區域中的定量分析的5點平均所獲得之Cu濃度，訂為分散於活性金屬氮化物層(氮化鈦層)內之Cu的平均濃度。(Active metal nitride layer) 　　 The bonding interface between the copper plate and the ceramic substrate was observed using a scanning transmission electron microscope (Titan ChemiSTEM manufactured by FEI (with EDS detector)) at a magnification of 115,000 times and an acceleration voltage of 200kV. Energy dispersive X-ray analysis (NSS7 manufactured by Thermo Fisher Scientific) is used for mapping. In the area where the active metal (Ti) and N overlap, the electron beam (NBD (Nei The meter beam diffraction method) was used to obtain an electron diffraction pattern, and the presence or absence of an active metal nitride layer (titanium nitride layer) was confirmed. Regarding the area where the active metal nitride layer (titanium nitride layer) is confirmed for the presence or absence of Cu particles, the Cu concentration obtained by the 5-point average of the quantitative analysis in this area is ordered to be dispersed in the active metal nitride layer ( The average concentration of Cu in the titanium nitride layer).

(初始接合率) 　　銅板與陶瓷基板之接合率，是使用超音波探傷裝置(日立電力解決方案公司製FineSAT200)使用以下式子求出。所謂初始接合面積，是訂為接合前的應接合面積，亦即銅板的接合面的面積。超音波探傷像中，剝離是以接合部內的白色部分表示，因此將此白色部分的面積訂為剝離面積。 (接合率)={(初始接合面積)-(剝離面積)}/(初始接合面積)×100(Initial bonding rate) The bonding rate between the copper plate and the ceramic substrate is calculated using the following formula using an ultrasonic flaw detection device (FineSAT200 manufactured by Hitachi Electric Power Solutions). The so-called initial bonding area is set as the area to be bonded before bonding, that is, the area of the bonding surface of the copper plate. In the ultrasonic flaw detection image, peeling is indicated by the white part in the joint, so the area of this white part is defined as the peeling area. (Joining rate)=((Initial joining area)-(Peeling area))/(Initial joining area)×100

(陶瓷基板的破裂) 　　使用冷熱衝撃試驗機(ESPEC公司製TSA-72ES)，於氣相下，將循環實施了300循環，該循環係1循環為-50℃下10分鐘與150℃下10分鐘。 　　評估負荷了上述的冷熱循環後之陶瓷基板的破裂的有無。(Crack of ceramic substrate) 　　 Using a hot and cold impact tester (TSA-72ES manufactured by ESPEC), in the gas phase, the cycle was carried out for 300 cycles. The cycle system is 1 cycle at -50°C for 10 minutes and 150°C for 10 minutes .　　Evaluate the presence or absence of cracks in the ceramic substrate after being subjected to the above-mentioned thermal cycle.

(遷移) 　　以電路層的電路圖樣間距離0.8mm、溫度60℃、濕度95%RH、電壓DC50V之條件，放置500小時後，測定了電路圖樣間的電阻。將電阻值成為1×106 Ω以下的情形判斷為短路，訂為「B」。將電阻值未成為1×106 Ω以下的情形訂為「A」。(Migration) The resistance between the circuit patterns of the circuit layer was measured after the distance between the circuit patterns of the circuit layer was 0.8mm, the temperature was 60°C, the humidity was 95%RH, and the voltage was DC50V. When the resistance value becomes 1×10 6 Ω or less, it is judged as a short circuit, and it is designated as "B". The case where the resistance value is not 1×10 6 Ω or less is referred to as "A".

評估結果如表2所示。此外，本發明例5的觀察結果如圖9A、圖9B及圖9C所示。The evaluation results are shown in Table 2. In addition, the observation results of Example 5 of the present invention are shown in FIG. 9A, FIG. 9B, and FIG. 9C.

Figure 02_image001
Figure 02_image001

Figure 02_image003
Figure 02_image003

活性金屬及Mg配置工程中，於活性金屬量(Ti量)為0.1μmol/cm2 (0.005mg/cm2 )這樣比本發明之範圍還少的比較例1中，初始接合率變低。推測是因為Mg固溶層中不存在活性金屬(Ti)作為金屬間化合物相，界面反應不充分的緣故。 　　活性金屬及Mg配置工程中，於活性金屬量(Ti量)為66.9μmol/cm2 (3.20mg/cm2 )這樣比本發明之範圍還多的比較例2中，確認到陶瓷基板的破裂。推測是因為大量形成了相對硬的金屬間化合物相的緣故。In the active metal and Mg arrangement process, in Comparative Example 1, where the amount of active metal (the amount of Ti) is 0.1 μmol/cm 2 (0.005 mg/cm 2 ), which is less than the scope of the present invention, the initial bonding rate becomes low. Presumably, it is because there is no active metal (Ti) as an intermetallic compound phase in the Mg solid solution layer, and the interfacial reaction is insufficient. In the active metal and Mg arrangement process, the amount of active metal (Ti amount) was 66.9 μmol/cm 2 (3.20 mg/cm 2 ) in Comparative Example 2, which was larger than the scope of the present invention, and cracking of the ceramic substrate was confirmed. Presumably, it is because a relatively hard intermetallic compound phase is formed in a large amount.

活性金屬及Mg配置工程中，於Mg量為2.1μmol/cm2 (0.05mg/cm2 )這樣比本發明之範圍還少的比較例3中，初始接合率變低。推測是因為未觀察到Mg固溶層，界面反應不充分的緣故。 　　活性金屬及Mg配置工程中，於Mg量為220.1μmol /cm2 (5.35mg/cm2 )這樣比本發明之範圍還多的比較例4中，確認到陶瓷基板的破裂。推測是因為陶瓷基板的分解反應過度，Al過度地生成，而大量生成了它們和Cu或和活性金屬(Ti)或和Mg的金屬間化合物的緣故。In the active metal and Mg arrangement process, in Comparative Example 3, which has a Mg amount of 2.1 μmol/cm 2 (0.05 mg/cm 2 ), which is less than the scope of the present invention, the initial bonding rate becomes low. It is presumed that the Mg solid solution layer was not observed and the interface reaction was insufficient. In the active metal and Mg placement process, in Comparative Example 4, where the amount of Mg was 220.1 μmol/cm 2 (5.35 mg/cm 2 ), which was larger than the scope of the present invention, cracking of the ceramic substrate was confirmed. It is presumed that the decomposition reaction of the ceramic substrate was excessive, Al was excessively generated, and a large amount of intermetallic compounds between them and Cu, active metal (Ti), or Mg were generated.

於使用Ag-Cu-Ti硬銲材將陶瓷基板與銅板接合而成之習知例中，遷移被判斷為「B」。推測是因為接合界面中有Ag存在的緣故。In the conventional example where the ceramic substrate and the copper plate are joined using Ag-Cu-Ti brazing material, the migration is judged as "B". Presumably, it is due to the presence of Ag in the bonding interface.

相對於此，本發明例1～12中，初始接合率亦高，亦未確認到陶瓷基板的破裂。此外，遷移亦良好。 　　如圖9A、圖9B及圖9C所示，觀察接合界面之結果，觀察到活性金屬氮化物層31(氮化鈦層)、Mg固溶層32，並觀察到在此Mg固溶層32的內部分散有金屬間化合物相33。In contrast, in Examples 1 to 12 of the present invention, the initial bonding rate was also high, and cracking of the ceramic substrate was not confirmed. In addition, the migration is also good. As shown in FIGS. 9A, 9B, and 9C, the result of observing the bonding interface shows that the active metal nitride layer 31 (titanium nitride layer) and the Mg solid solution layer 32 are observed, and the Mg solid solution layer 32 is observed here. An intermetallic compound phase 33 is dispersed inside.

＜實施例2＞ 　　形成了表3所示構造之銅/陶瓷接合體。詳言之，是在40mm見方的陶瓷基板的兩面，如表3所示，層積將活性金屬的單體及Mg單體予以成膜而成之銅板，以表3所示之接合條件接合，形成了銅/陶瓷接合體。陶瓷基板的厚度當氮化鋁的情形下使用了厚度0.635mm，當氮化矽的情形下使用了厚度0.32mm。此外，接合時的真空爐的真空度訂為5×10-3 Pa。<Example 2> A copper/ceramic joint body having the structure shown in Table 3 was formed. Specifically, it is a copper plate formed by laminating active metal monomers and Mg monomers on both sides of a 40mm square ceramic substrate, as shown in Table 3, and bonding under the bonding conditions shown in Table 3. A copper/ceramic junction is formed. The thickness of the ceramic substrate is 0.635mm in the case of aluminum nitride, and 0.32mm in the case of silicon nitride. In addition, the vacuum degree of the vacuum furnace at the time of bonding is set to 5×10 -3 Pa.

針對依此方式獲得的銅/陶瓷接合體，如同實施例1般，觀察接合界面，確認了活性金屬氮化物層、Mg固溶層、Mg固溶層中的活性金屬的有無(金屬間化合物相的有無)、活性金屬氮化物層中的Cu粒子的有無及Cu濃度。此外，銅/陶瓷接合體的初始接合率、冷熱循環後的陶瓷基板的破裂、遷移性，係如同實施例1般評估。評估結果如表4所示。For the copper/ceramic joint obtained in this way, the joint interface was observed as in Example 1, and the presence or absence of active metal (intermetallic compound phase) in the active metal nitride layer, Mg solid solution layer, and Mg solid solution layer was confirmed. The presence or absence of), the presence or absence of Cu particles in the active metal nitride layer and the Cu concentration. In addition, the initial bonding rate of the copper/ceramic bonded body, the fracture and migration of the ceramic substrate after the cooling and heating cycle, were evaluated in the same manner as in Example 1. The evaluation results are shown in Table 4.

Figure 02_image005
Figure 02_image005

Figure 02_image007
Figure 02_image007

活性金屬及Mg配置工程中，於活性金屬量(Zr量)為50.4μmol/cm2 這樣比本發明之範圍還多的比較例21、及活性金屬量(Nb量)為61.2μmol/cm2 這樣比本發明之範圍還多的比較例22中，確認到陶瓷基板的破裂。推測是因為Mg固溶層中存在的活性金屬量多，Mg固溶層變硬了的緣故。 　　活性金屬及Mg配置工程中，於活性金屬量(Hf量)為0.2μmol/cm2 這樣比本發明之範圍還少的比較例23、及活性金屬量(Hf量＋Nb量)為0.2μmol/cm2 這樣比本發明之範圍還少的比較例24中，初始接合率變低。In the active metal and Mg configuration process, the amount of active metal (Zr amount) is 50.4 μmol/cm 2 in Comparative Example 21, which is larger than the scope of the present invention, and the amount of active metal (Nb amount) is 61.2 μmol/cm 2 In Comparative Example 22, which is more than the scope of the present invention, cracking of the ceramic substrate was confirmed. It is presumed that the amount of active metal present in the Mg solid solution layer is large, and the Mg solid solution layer is hardened. In the active metal and Mg configuration process, the amount of active metal (Hf amount) is 0.2 μmol/cm 2 in Comparative Example 23, which is less than the scope of the present invention, and the amount of active metal (Hf amount + Nb amount) is 0.2 μmol/cm 2 In Comparative Example 24, which is smaller than the scope of the present invention, the initial bonding rate becomes low.

相對於此，本發明例21～27中，初始接合率亦高，亦未確認到陶瓷基板的破裂。此外，遷移亦良好。In contrast, in Examples 21 to 27 of the present invention, the initial bonding rate was also high, and cracking of the ceramic substrate was not confirmed. In addition, the migration is also good.

由以上事實，確認了按照本發明例，可提供一種銅構件與陶瓷構件會確實地被接合，耐遷移性優良之銅/陶瓷接合體(絕緣電路基板)。From the above facts, it was confirmed that according to the example of the present invention, a copper member and a ceramic member can be reliably joined, and a copper/ceramic joined body (insulated circuit board) having excellent migration resistance can be provided.

＜實施例3＞ 　　形成了表5所示構造之絕緣電路基板。詳言之，是在40mm見方的陶瓷基板的兩面，如表5所示，層積將活性金屬的單體及Mg單體予以成膜而成之銅板，以表5所示之接合條件接合，形成了具有電路層之絕緣電路基板。陶瓷基板的厚度當氮化鋁的情形下使用了厚度0.635mm，當氮化矽的情形下使用了厚度0.32mm。此外，接合時的真空爐的真空度訂為5×10-3 Pa。<Example 3> An insulated circuit board having the structure shown in Table 5 was formed. Specifically, it is a copper plate formed by laminating active metal monomers and Mg monomers on both sides of a 40mm square ceramic substrate, as shown in Table 5, and bonding under the bonding conditions shown in Table 5. An insulated circuit substrate with a circuit layer is formed. The thickness of the ceramic substrate is 0.635mm in the case of aluminum nitride, and 0.32mm in the case of silicon nitride. In addition, the vacuum degree of the vacuum furnace at the time of bonding is set to 5×10 -3 Pa.

針對依此方式獲得的絕緣電路基板，依以下方式評估了陶瓷基板與電路層之接合界面中的Cu2 Mg相的面積率、及超音波接合至電路層之端子的拉伸強度。With respect to the insulated circuit substrate obtained in this way, the area ratio of the Cu 2 Mg phase in the bonding interface between the ceramic substrate and the circuit layer and the tensile strength of the terminal ultrasonically bonded to the circuit layer were evaluated in the following manner.

(Cu2 Mg相的面積率) 　　對於銅板與陶瓷基板之接合界面，使用電子探針顯微分析儀(日本電子公司製JXA-8539F)，以倍率750倍、加速電壓15kV的條件取得包含接合界面之區域(120μm×160μm)的Mg的元素MAP，以確認到Mg的存在之區域內的定量分析的5點平均，將Mg濃度滿足30原子%以上40原子%以下之區域訂為Cu2 Mg相。 　　於觀察視野內，求出陶瓷基板的接合面與從陶瓷基板的接合面起算往銅板側50μm為止之區域的面積A。於此區域內求出Cu2 Mg相的面積B，求出Cu2 Mg相的面積率B/A×100(%)。如上述般以5視野測定Cu2 Mg相的面積率，將其平均值記載於表5。(Cu 2 Mg phase area ratio) For the bonding interface between the copper plate and the ceramic substrate, an electron probe microanalyzer (JXA-8539F manufactured by JEOL Ltd.) was used to obtain the bonding interface at a magnification of 750 times and an acceleration voltage of 15kV. The elemental MAP of Mg in the region (120μm×160μm) is determined by the 5-point average of quantitative analysis in the region where the presence of Mg is confirmed, and the region where the Mg concentration meets 30 atomic% or more and 40 atomic% or less is defined as the Cu 2 Mg phase . In the observation field of view, the area A of the bonding surface of the ceramic substrate and the area from the bonding surface of the ceramic substrate to the copper plate side 50 μm was determined. Cu 2 Mg phase is obtained within this area of B, Cu 2 Mg phase is determined the area ratio B / A × 100 (%) . The area ratio of the Cu 2 Mg phase was measured with 5 fields of view as described above, and the average value is shown in Table 5.

(拉伸強度) 　　如圖10A及圖10B所示，在絕緣電路基板的電路層的上方，使用包含平台40之超音波金屬接合機(超音波工業公司製60C-904)，將銅端子(寬幅：5mm、厚度T：1.0 mm、長度L1 ：20mm、長度L2 ：10mm)以壓潰(collapse)量0.3mm的條件予以超音波接合。 　　將以工具速度Y為5mm/s，平台速度X為5mm/s的條件將銅端子拉伸時之斷裂荷重除以接合面積而成之值訂為拉伸強度，記載於表5。(Tensile strength) As shown in Fig. 10A and Fig. 10B, above the circuit layer of the insulated circuit board, using an ultrasonic metal bonding machine (60C-904 manufactured by Ultrasonic Industry Co., Ltd.) including a platform 40, the copper terminals (wide Width: 5 mm, thickness T: 1.0 mm, length L 1 : 20 mm, length L 2 : 10 mm), ultrasonic bonding was performed under the condition of a collapse amount of 0.3 mm. The tensile strength was defined as the value obtained by dividing the breaking load of the copper terminal by the joint area under the condition that the tool speed Y was 5 mm/s and the platform speed X was 5 mm/s.

Figure 02_image009
Figure 02_image009

比較本發明例31～43，確認到Cu2 Mg相的面積率愈低，拉伸強度愈變高。故，確認了當欲使超音波接合性提升的情形下，將Cu2 Mg相的面積率抑制得較低是有效的。 [產業利用性]Comparing Examples 31 to 43 of the present invention, it was confirmed that the lower the area ratio of the Cu 2 Mg phase, the higher the tensile strength. Therefore, it was confirmed that when it is desired to improve the ultrasonic bonding properties, it is effective to suppress the area ratio of the Cu 2 Mg phase to a low level. [Industrial Utilization]

按照本發明，能夠提供一種銅構件與陶瓷構件確實地被接合，而耐遷移性優良之銅/陶瓷接合體，絕緣電路基板，及上述的銅/陶瓷接合體的製造方法，絕緣電路基板的製造方法。According to the present invention, it is possible to provide a copper/ceramic joint body, an insulated circuit board, and a method for manufacturing the above-mentioned copper/ceramic joint body, and a manufacturing method of the above-mentioned copper/ceramic joint body, and an insulated circuit board method.

10、110‧‧‧絕緣電路基板11、111‧‧‧陶瓷基板12、112‧‧‧電路層13、113‧‧‧金屬層22、23、122‧‧‧銅板31、131‧‧‧活性金屬氮化物層32、132‧‧‧Mg固溶層33、133‧‧‧金屬間化合物相35、135‧‧‧Cu粒子10、110‧‧‧Insulated circuit substrate 11,111‧‧‧Ceramic substrate 12,112‧‧‧Circuit layer 13,113‧‧‧Metal layer 22,23,122‧‧‧Copper plate 31,131‧‧‧Reactive metal Nitride layer 32, 132‧‧‧Mg solid solution layer 33, 133‧‧‧Intermetallic compound phase 35, 135‧‧‧Cu particles

[圖1] 使用了本發明第1實施形態之絕緣電路基板的功率模組的概略說明圖。 　　[圖2] 本發明第1實施形態之絕緣電路基板的電路層(銅構件)及金屬層(銅構件)與陶瓷基板(陶瓷構件)之接合界面的模型圖。 　　[圖3] 本發明第1實施形態之絕緣電路基板的製造方法示意流程圖。 　　[圖4] 本發明第1實施形態之絕緣電路基板的製造方法示意說明圖。 　　[圖5] 使用了本發明第2實施形態之絕緣電路基板的功率模組的概略說明圖。 　　[圖6] 本發明第2實施形態之絕緣電路基板的電路層(銅構件)與陶瓷基板(陶瓷構件)之接合界面的模型圖。 　　[圖7] 本發明第2實施形態之絕緣電路基板的製造方法示意流程圖。 　　[圖8] 本發明第2實施形態之絕緣電路基板的製造方法示意說明圖。 　　[圖9A] 本發明例5之銅/陶瓷接合體中的銅板與陶瓷基板之接合界面的觀察結果。 　　[圖9B] 本發明例5之銅/陶瓷接合體中的銅板與陶瓷基板之接合界面的觀察結果。 　　[圖9C] 本發明例5之銅/陶瓷接合體中的銅板與陶瓷基板之接合界面的觀察結果。 　　[圖10A] 實施例3中的拉伸強度的測定方法示意說明圖。 　　[圖10B] 實施例3中的拉伸強度的測定方法示意說明圖。[Fig. 1] A schematic explanatory diagram of a power module using the insulated circuit board according to the first embodiment of the present invention.　　[FIG. 2] A model diagram of the bonding interface between the circuit layer (copper member) and the metal layer (copper member) of the insulated circuit substrate of the first embodiment of the present invention and the ceramic substrate (ceramic member).　　[FIG. 3] A schematic flow chart of the manufacturing method of the insulated circuit board according to the first embodiment of the present invention.　　[FIG. 4] A schematic explanatory view of the manufacturing method of the insulated circuit board according to the first embodiment of the present invention.　　 [FIG. 5] A schematic explanatory diagram of a power module using the insulated circuit board according to the second embodiment of the present invention.　　[FIG. 6] A model diagram of the bonding interface between the circuit layer (copper member) of the insulated circuit board and the ceramic substrate (ceramic member) in the second embodiment of the present invention.　　[FIG. 7] A schematic flow chart of a manufacturing method of an insulated circuit board according to the second embodiment of the present invention.　　[FIG. 8] A schematic explanatory diagram of a method of manufacturing an insulated circuit board according to a second embodiment of the present invention.　　 [FIG. 9A] Observation results of the bonding interface between the copper plate and the ceramic substrate in the copper/ceramic joint of Example 5 of the present invention.　　 [Figure 9B] Observation results of the joint interface between the copper plate and the ceramic substrate in the copper/ceramic joint of Example 5 of the present invention.　　 [Figure 9C] Observation results of the joint interface between the copper plate and the ceramic substrate in the copper/ceramic joint of Example 5 of the present invention.　　 [Fig. 10A] A schematic explanatory diagram of the method of measuring the tensile strength in Example 3.　　 [Fig. 10B] A schematic explanatory diagram of the method of measuring the tensile strength in Example 3.

11‧‧‧陶瓷基板 11‧‧‧Ceramic substrate

12‧‧‧電路層 12‧‧‧Circuit layer

13‧‧‧金屬層 13‧‧‧Metal layer

22、23‧‧‧銅板 22, 23‧‧‧copper plate

31‧‧‧活性金屬氮化物層 31‧‧‧Active metal nitride layer

32‧‧‧Mg固溶層 32‧‧‧Mg solid solution layer

33‧‧‧金屬間化合物相 33‧‧‧Intermetallic compound phase

35‧‧‧Cu粒子 35‧‧‧Cu particles

Claims (14)

一種銅/陶瓷接合體，係由銅或銅合金所成之銅構件、與由氮化鋁或氮化矽所成之陶瓷構件被接合而構成之銅/陶瓷接合體，其特徵為，在前述銅構件與前述陶瓷構件之間，於前述陶瓷構件側，形成有含有從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的氮化物之活性金屬氮化物層，在前述活性金屬氮化物層與前述銅構件之間形成有Mg固溶於Cu的母相中而成之Mg固溶層，前述Mg固溶層中，存在前述活性金屬。 A copper/ceramic joint body is a copper/ceramic joint body formed by joining a copper member made of copper or copper alloy and a ceramic member made of aluminum nitride or silicon nitride, and is characterized in that: Between the copper member and the ceramic member, on the ceramic member side, an active metal nitride layer containing nitrides of one or more active metals selected from Ti, Zr, Nb, and Hf is formed. A Mg solid solution layer in which Mg is solid-dissolved in a Cu matrix is formed between the metal nitride layer and the copper member, and the active metal is present in the Mg solid solution layer. 如申請專利範圍第1項所述之銅/陶瓷接合體，其中，前述Mg固溶層中，分散有含有Cu與前述活性金屬之金屬間化合物相。 The copper/ceramic joint body described in the first item of the patent application, wherein the Mg solid solution layer is dispersed with an intermetallic compound phase containing Cu and the active metal. 如申請專利範圍第1項或第2項所述之銅/陶瓷接合體，其中，在前述活性金屬氮化物層的內部，分散有Cu粒子。 The copper/ceramic joint body described in item 1 or item 2 of the scope of the patent application, wherein Cu particles are dispersed in the active metal nitride layer. 如申請專利範圍第1項或第2項所述之銅/陶瓷接合體，其中，前述活性金屬為Ti。 The copper/ceramic joint body described in item 1 or item 2 of the scope of patent application, wherein the aforementioned active metal is Ti. 如申請專利範圍第1項或第2項所述之銅/陶瓷接合 體，其中，在前述陶瓷構件與前述銅構件之間，前述陶瓷構件的接合面起算往前述銅構件側50μm為止之區域中的Cu2Mg相的面積率為15%以下。 The copper/ceramic joint as described in item 1 or item 2 of the scope of the patent application, wherein between the ceramic member and the copper member, the joint surface of the ceramic member is in the area 50μm from the side of the copper member The area ratio of the Cu 2 Mg phase is 15% or less. 一種絕緣電路基板，係由銅或銅合金所成之銅板被接合至由氮化鋁或氮化矽所成之陶瓷基板的表面而構成之絕緣電路基板，其特徵為，在前述銅板與前述陶瓷基板之間，於前述陶瓷基板側，形成有含有從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的氮化物之活性金屬氮化物層，在此活性金屬氮化物層與前述銅板之間形成有Mg固溶於Cu的母相中而成之Mg固溶層，前述Mg固溶層中，存在前述活性金屬。 An insulated circuit substrate is an insulated circuit substrate formed by bonding a copper plate made of copper or copper alloy to the surface of a ceramic substrate made of aluminum nitride or silicon nitride, and is characterized in that the copper plate and the ceramic Between the substrates, on the ceramic substrate side, an active metal nitride layer containing nitrides of one or two or more active metals selected from Ti, Zr, Nb, and Hf is formed, where the active metal nitride layer and A Mg solid solution layer in which Mg is dissolved in a Cu matrix is formed between the copper plates, and the active metal is present in the Mg solid solution layer. 如申請專利範圍第6項所述之絕緣電路基板，其中，前述Mg固溶層中，分散有含有Cu與前述活性金屬之金屬間化合物相。 In the insulated circuit board described in the scope of patent application item 6, wherein, in the Mg solid solution layer, an intermetallic compound phase containing Cu and the active metal is dispersed. 如申請專利範圍第6項或第7項所述之絕緣電路基板，其中，在前述活性金屬氮化物層的內部，分散有Cu粒子。 The insulated circuit board described in item 6 or item 7 of the scope of patent application, wherein Cu particles are dispersed in the active metal nitride layer. 如申請專利範圍第6項或第7項所述之絕緣電路基板，其中，前述活性金屬為Ti。 The insulated circuit board described in item 6 or item 7 of the scope of patent application, wherein the aforementioned active metal is Ti. 如申請專利範圍第6項或第7項所述之絕緣電路基板，其中，在前述陶瓷基板與前述銅板之間，前述陶瓷基板的接合面起算往前述銅板側50μm為止之區域中的Cu2Mg相的面積率為15%以下。 The insulated circuit board described in item 6 or item 7 of the scope of patent application, wherein, between the ceramic substrate and the copper plate, the bonding surface of the ceramic substrate is Cu 2 Mg in the area 50 μm from the copper plate side The area ratio of the phase is 15% or less. 一種銅/陶瓷接合體的製造方法，係製造如申請專利範圍第1項至第5項中任一項所述之銅/陶瓷接合體的銅/陶瓷接合體的製造方法，其特徵為，具備：活性金屬及Mg配置工程，在前述銅構件與前述陶瓷構件之間，配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體及Mg單體；及層積工程，將前述銅構件與前述陶瓷構件，介著前述活性金屬的單體及前述Mg單體予以層積；及接合工程，將介著前述活性金屬的單體及前述Mg單體而被層積之前述銅構件與前述陶瓷構件，在朝層積方向予以加壓之狀態下，於真空環境下做加熱處理而接合；前述活性金屬及Mg配置工程中，前述活性金屬的單體的活性金屬量為0.4μmol/cm2以上47.0μmol/cm2以下，前述Mg單體的Mg量為7.0μmol/cm2以上143.2μmol/cm2以下。 A method for manufacturing a copper/ceramic joint body, which is a method for manufacturing a copper/ceramic joint body as described in any one of items 1 to 5 of the scope of the patent application, characterized in that: : Active metal and Mg arrangement process, between the aforementioned copper member and the aforementioned ceramic member, one or more active metal monomers and Mg monomers selected from Ti, Zr, Nb, and Hf are arranged; and lamination The process of laminating the copper member and the ceramic member through the monomer of the active metal and the monomer of Mg; and the joining process of laminating the monomer of the active metal and the Mg monomer. The aforementioned copper member and the aforementioned ceramic member are joined by heat treatment in a vacuum environment while being pressurized in the lamination direction; in the aforementioned active metal and Mg arrangement process, the amount of active metal of the single active metal It is 0.4 μmol/cm 2 or more and 47.0 μmol/cm 2 or less, and the Mg amount of the aforementioned Mg monomer is 7.0 μmol/cm 2 or more and 143.2 μmol/cm 2 or less. 如申請專利範圍第11項所述之銅/陶瓷接合體的製造方法，其中，前述接合工程中的加壓荷重為0.049MPa以上3.4MPa以下，前述接合工程中的加熱溫度，當前述銅板的Cu與前述 Mg單體的Mg是在接觸狀態下被層積的情形下為500℃以上850℃以下，當前述Cu與前述Mg是在非接觸狀態下被層積的情形下為670℃以上850℃以下。 The method for manufacturing a copper/ceramic joint body as described in claim 11, wherein the pressing load in the joining process is 0.049 MPa or more and 3.4 MPa or less, and the heating temperature in the joining process is equal to the Cu of the copper plate With the aforementioned The Mg of Mg alone is 500°C or more and 850°C or less when it is laminated in a contact state, and 670°C or more and 850°C or less when the Cu and Mg are laminated in a non-contact state. 一種絕緣電路基板的製造方法，係製造由銅或銅合金所成之銅板被接合至由氮化鋁或氮化矽所成之陶瓷基板的表面而構成之絕緣電路基板的絕緣電路基板的製造方法，其特徵為，具備：活性金屬及Mg配置工程，在前述銅板與前述陶瓷基板之間，配置從Ti，Zr，Nb，Hf選擇之1種或2種以上的活性金屬的單體及Mg單體；及層積工程，將前述銅板與前述陶瓷基板，介著前述活性金屬的單體及前述Mg單體予以層積；及接合工程，將介著前述活性金屬的單體及前述Mg單體而被層積之前述銅板與前述陶瓷基板，在朝層積方向予以加壓之狀態下，於真空環境下做加熱處理而接合；前述活性金屬及Mg配置工程中，前述活性金屬的單體的活性金屬量為0.4μmol/cm2以上47.0μmol/cm2以下，前述Mg單體的Mg量為7.0μmol/cm2以上143.2μmol/cm2以下。 A method for manufacturing an insulated circuit substrate, which is a method for manufacturing an insulated circuit substrate in which a copper plate made of copper or copper alloy is joined to the surface of a ceramic substrate made of aluminum nitride or silicon nitride. , It is characterized by having: active metal and Mg arrangement process, between the copper plate and the ceramic substrate, one or more active metal monomers and Mg monomers selected from Ti, Zr, Nb, and Hf are arranged And the lamination process, the above-mentioned copper plate and the above-mentioned ceramic substrate, the above-mentioned active metal monomer and the aforementioned Mg monomer are laminated; and the bonding process, the above-mentioned active metal monomer and the aforementioned Mg monomer are laminated The laminated copper plate and the ceramic substrate are heated in a vacuum environment under pressure in the lamination direction to be joined; in the active metal and Mg arrangement process, the single active metal The amount of active metal is 0.4 μmol/cm 2 or more and 47.0 μmol/cm 2 or less, and the Mg amount of the aforementioned Mg monomer is 7.0 μmol/cm 2 or more and 143.2 μmol/cm 2 or less. 如申請專利範圍第13項所述之絕緣電路基板的製造方法，其中，前述接合工程中的加壓荷重為0.049MPa以上3.4MPa以下，前述接合工程中的加熱溫度，當前述銅板的Cu與前述 Mg單體的Mg是在接觸狀態下被層積的情形下為500℃以上850℃以下，當前述Cu與前述Mg是在非接觸狀態下被層積的情形下為670℃以上850℃以下。 The manufacturing method of the insulated circuit board described in the scope of patent application, wherein the pressure load in the bonding process is 0.049 MPa or more and 3.4 MPa or less, and the heating temperature in the bonding process is when the Cu of the copper plate and the foregoing The Mg of Mg alone is 500°C or more and 850°C or less when it is laminated in a contact state, and 670°C or more and 850°C or less when the Cu and Mg are laminated in a non-contact state.
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