JP6360157B2 - 熱硬化性樹脂組成物、半導体装置及び電気・電子部品 - Google Patents
熱硬化性樹脂組成物、半導体装置及び電気・電子部品 Download PDFInfo
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- JP6360157B2 JP6360157B2 JP2016511170A JP2016511170A JP6360157B2 JP 6360157 B2 JP6360157 B2 JP 6360157B2 JP 2016511170 A JP2016511170 A JP 2016511170A JP 2016511170 A JP2016511170 A JP 2016511170A JP 6360157 B2 JP6360157 B2 JP 6360157B2
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
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- UVZICZIVKIMRNE-UHFFFAOYSA-N thiodiacetic acid Chemical compound OC(=O)CSCC(O)=O UVZICZIVKIMRNE-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/10—Esters
- C08F20/12—Esters of monohydric alcohols or phenols
- C08F20/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F20/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Description
ここで使用されるカルボキシル基を含む有機化合物としては、分子量が110〜20000の有機カルボン酸から選ばれる1種以上の有機化合物が挙げられ、例えば、ヘキサン酸、ヘプタン酸、オクタン酸、ノナン酸、デカン酸、ウンデカン酸、ドデカン酸、テトラデカン酸、エイコサン酸、ドコサン酸、2−エチルヘキサン酸、オレイン酸、リノール酸、リノレン酸、末端ジプロピオン酸ポリエチレンオキシドのようなカルボン酸が挙げられる。さらに、上記有機化合物としては、上記したカルボン酸のカルボン酸誘導体も使用できる。
市販されている具体的なシリコーンパウダーとしては、例えば、信越化学工業(株)製のシリコーン複合パウダー(KMP−600、KMP−601、KMP−602、KMP−605、X−52−7030など)、シリコーンゴムパウダー(KMP−597、KMP−598、KMP−594、X−52−875など)、シリコーンレジンパウダー(KMP−590、KMP−701、X−52−854、X−52−1621など)が挙げられ、これらを単独もしくは、2種類以上組み合わせて使用してもよい。
ここで、シリコーンパウダーを使用する場合は、平均粒子径0.5から10μmが好ましく、さらに好ましくは0.8〜5μmである。シリコーンパウダーの平均粒子径がこの範囲にあると有効な「物理的障害効果」を発現し、焼成ボイドの発生しない樹脂組成物が得られる。この平均粒子径は、レーザー回折式粒度分布測定装置で測定して得られた個数基準の平均粒子径をいう。
圧縮弾性率および圧縮回復率が上記の範囲にあると、樹脂組成物の加熱硬化や焼結時において、ボイドの発生を抑制できるのに加え、樹脂と銀粒子やチップ等との密着性が改善され、実装時や高温保持時において、チップの歪みや変形を抑制できる樹脂組成物が得られる。
微小圧縮試験器(例えば、島津ダイナミック超微小硬度計DUH−W201[島津製作所製])を用いて、ダイヤモンド製の直径50μmの円柱の平滑端面で、樹脂粒子を圧縮速度2.6mN/秒、及び最大試験荷重10gの条件下で圧縮し、30%圧縮変形における荷重値(N)と30%圧縮変形における変位(mm)を測定し、上記数式(1)により算出する。
圧縮回復率(%)=[(L1−L2)/L1]×100 …(2)
圧縮回復率は、20℃の雰囲気下、圧縮変形状態からの形状回復率のことであり、その算出は特公平7−95165号公報に記載の方法に準拠して、微小圧縮試験器(例えば、島津ダイナミック超微小硬度計DUH−W201[島津製作所製])を用いて、ダイヤモンド製の直径50μmの円柱の平滑端面で、球状樹脂粒子を圧縮速度2.6mN/秒、及び最大試験荷重10gの条件下で圧縮し、荷重と変形量のヒステリシス曲線から求めた、総変形量(L1)及び塑性変形量(L2)の比を%で表した値である。
上記した共重合体は、それぞれカルボキシル基が水酸基を有する(メタ)アクリレートあるいはグリシジル基を有する(メタ)アクリレートと反応することで得ることが、水酸基が極性基を有さない(メタ)アクリル酸およびその誘導体と反応することで得ることが、グリシジル基が極性基を有さない(メタ)アクリル酸およびその誘導体と反応することで得ることが、可能である。
そして、ポリ(メタ)アクリレートで(メタ)アクリル基を有する化合物は、ポリ(メタ)アクリレートポリオールと(メタ)アクリル酸又はその誘導体との反応により得ることが可能である。
ヒドロキシル基を有する(メタ)アクリレートは、ポリオール化合物と(メタ)アクリル酸及びその誘導体とを反応することで得ることが可能である。この反応は、公知反応を使用することができ、ポリオール化合物に対し、通常0.5〜5倍モルのアクリル酸エステル又はアクリル酸を使用する。
また、ヒドロキシル基を有する(メタ)アクリルアミドは、ヒドロキシル基を有するアミン化合物と(メタ)アクリル酸及びその誘導体とを反応させることで得ることが可能である。(メタ)アクリル酸エステルとアミン化合物とを反応させて(メタ)アクリルアミド類を製造する方法は、(メタ)アクリル酸エステルの二重結合が極めて反応性に富む為に、アミン、シクロペンタジエン、アルコール等を予め二重結合に保護基として付加させ、アミド化終了後加熱して保護基を脱離させ目的物を製造するのが一般的である。
このようにヒドロキシル基を含有することにより、還元効果による焼結性が促進されると共に、接着性が向上する。
ここで、脂肪族炭化水素基は、直鎖状、分枝鎖状及び環状のいずれの形態でもよく、炭素数が6以上であることが好ましく、炭素数が12以上であることがより好ましく、炭素数が24以上であることが特に好ましい。また、この脂肪族炭化水素基はマレイミド基に直接結合していることが好ましい。
このようなマレイミド樹脂の具体例としては、BMI−1500(デジグナーモレキュールズ社製、商品名;分子量 1500)、BMI−1700(デジグナーモレキュールズ社製、商品名;分子量 1700)、等が挙げられる。
本発明の半導体装置は、上記した熱硬化性樹脂組成物を用いて、半導体素子を素子支持部材となる基板上に接着してなるものである。すなわち、ここで熱硬化性樹脂組成物はダイアタッチペーストとして使用される。
表1及び表2の配合に従って各成分を混合し、ロールで混練し、樹脂ペーストを得た。得られた樹脂ペーストを以下の方法で評価した。その結果を表1及び表2に併せて示す。なお、実施例及び比較例で用いた材料は、下記の通りの市販品を使用した。
(A2):球状銀微粒子(三ツ星ベルト(株)製、商品名:MDot;平均粒径:50nm)
(B):銀粉(福田金属箔粉工業(株)製、商品名:AgC−212D;平均粒子径:5μm)
(C1):球状樹脂粒子1(信越化学工業(株)製、商品名:KMP−600;平均粒子径:1μm、圧縮弾性率(30%K値):5300N/mm2、圧縮回復率:100%)
(C2):球状樹脂粒子2(綜研化学(株)製、商品名:MX−1500;平均粒子径:15μm、圧縮弾性率(30%K値):1500N/mm2、圧縮回復率:25%、CV値2%)
(C3):球状樹脂粒子3(積水化学(株)製、商品名:ミクロパールAUEZ−035A;平均粒子径:35μm、Au層:20nm、中間Ni層:30nm、圧縮弾性率(30%K値):750N/mm2、圧縮回復率:10%、CV値5%)
(C4):球状樹脂粒子4(積水化学(株)製、商品名:ミクロパールAUE−035A;平均粒子径:35μm、Au層:20nm、中間Ni層:30nm、圧縮弾性率(30%K値):4600N/mm2、圧縮回復率:55%、CV値5%)
(D2):イミド拡張型ビスマレイミド(デジグナーモレキュールズ社製、商品名:BMI−1500;数平均分子量 1500)
(D3):ジアリルビスフェノールAジグリシジルエーテル型エポキシ樹脂(日本化薬株式会社製、商品名:RE−810NM;エポキシ当量 223、加水分解性塩素 150ppm(1N KOH−エタノール、ジオキサン溶媒、還流30分)
(D4):4−ヒドロキシブチルアクリレート(日本化成株式会社製、商品名:4HBA)
重合開始剤:ジクミルパーオキサイド(日本油脂(株)製、商品名:パークミルD;急速加熱試験における分解温度:126℃)
(E):リンゴ酸(東京化成工業(株)製)
(F):ジエチレングリコール(東京化成工業(株)製)
[粘度]
E型粘度計(3°コーン)を用いて、25℃、5rpmでの値を測定した。
[ポットライフ]
25℃の恒温槽内に樹脂ペーストを放置した時の粘度が初期粘度の1.5倍以上増粘するまでの日数を測定した。
4mm×4mmの接合面に金蒸着層を設けた裏面金チップを、半導体用樹脂ペーストを用いて、無垢の銅フレーム及びPPF(Ni−Pd/Auめっきした銅フレーム)にマウントし、200℃、60分で硬化した。硬化及び吸湿処理(85℃、相対湿度85%、72時間)後、マウント強度測定装置を用い、260℃での熱時ダイシェア強度を測定した。
4mm×4mmの接合面に金蒸着層を設けた裏面金チップを、半導体用樹脂ペーストを用いて、表面にNi−Pd/AuめっきしたMo基板にマウントし、200℃、60分で硬化した。高温熱処理として加熱処理(250℃の加熱処理を、100時間及び1000時間)並びに冷熱サイクル処理(−40℃から250℃まで昇温し、また−40℃に冷却する操作を1サイクルとし、これを100サイクル及び1000サイクル)後のそれぞれについて、マウント強度測定装置を用い、260℃での熱時ダイシェア強度を測定した。
JIS R 1611−1997に従い、レーザーフラッシュ法により硬化物の熱伝導率を測定した。
[電気抵抗]
導電ペーストを、ガラス基板(厚み1mm)にスクリーン印刷法により厚み200μmとなるように塗布し、200℃、60分で硬化した。得られた配線を製品名「MCP−T600」(三菱化学(株)製)を用い4端子法にて電気抵抗を測定した。
6mm×6mmの接合面に金蒸着層を設けた裏面金シリコンチップを得られた樹脂ペーストを用いて銅フレーム及びPPFにマウントし、ホットプレート上で、200℃、60秒間の加熱硬化(HP硬化)又はオーブンを使用し、200℃、60分の加熱硬化(OV硬化)を行った。これを京セラケミカル(株)製エポキシ封止材(商品名:KE−G3000D)を用い、下記の条件で成形したパッケージを85℃、相対湿度85%、168時間吸湿処理した後、IRリフロー処理(260℃、10秒)及び冷熱サイクル処理(−55℃から150℃まで昇温し、また−55℃に冷却する操作を1サイクルとし、これを1000サイクル)を行い、各処理後それぞれのパッケージの内部クラックの発生数を超音波顕微鏡で観察した。5個のサンプルについてクラックの発生したサンプル数を示す。
チップ:シリコンチップ及び裏面金メッキチップ
リードフレーム:PPF及び銅
封止材の成形:175℃、2分間
ポストモールドキュアー:175℃、8時間
導電性ペーストを、スタンピング法により凹型のリフレクター構造を側面に有する発光装置用酸化アルミニウム基板へ塗布し、600μm角の銀蒸着層を設けた発光素子をマウントし、200℃、60分の加熱硬化を行った。次いで、発光素子の電極と基板の電極とを金ワイヤーで配線し、シリコーン樹脂(信越化学工業(株)製)で封止した。この状態で通電試験(試験条件25℃、50mA)を、500時間経過後、1000時間経過後、及び2000時間経過後の反射率の初期値に対する低下を下記式にて算出した。
初期値に対する反射率の低下率(%)=(t時間後の反射率)÷(初期反射率)×100
マイクロフォーカスX線検査装置(SMX−1000、島津製作所社製)を用いて観察し、ボイド率が5%未満を「○」、5%以上8%未満を「△」、8%以上を「×」と評価した。尚、上記ボイド率は、X線透過装置によりはんだ接合部を接合面に対し垂直方向から観察し、ボイド面積と接合部面積を求め、下式により算出した。
ボイド率(%)=ボイド面積÷(ボイド面積+接合部面積)×100
8mm×8mmの接合面に金蒸着層を設けた裏面金チップを、半導体用樹脂ペーストを用いて、表面にNi−Pd/AuめっきしたMo基板にマウントし、200℃、60分で硬化して作製した半導体パッケージのパッケージ反りを室温にて測定した。測定装置はシャドウモアレ測定装置(ThermoireAXP:Akrometrix製)を用いて、電子情報技術産業協会規格のJEITA ED−7306に準じて測定した。具体的には、測定領域の基板面の全データの最小二乗法によって算出した仮想平面を基準面とし、その基準面から垂直方向の最大値をAとし、最小値をBとした時の、|A|+|B|の値(Coplanarity)をパッケージ反り値とし、次のように評価した。
○:5μm未満、△:5μm以上10μm未満、×:10μm以上
Claims (16)
- (A)厚さ又は短径が1〜200nmの銀微粒子と、(B)前記(A)成分以外の平均粒子径が0.2μm超30μm以下である銀粉と、(C)樹脂粒子と、(D)熱硬化性樹脂と、を含み、
前記(A)成分の銀微粒子と前記(B)成分の銀粉の合計量を100質量部としたとき、前記(C)成分が0.01〜1質量部、前記(D)成分が1〜20質量部、配合されていることを特徴とする熱硬化性樹脂組成物。 - 前記(A)銀微粒子として、(A1)中心粒子径が0.3〜15μm、厚さが10〜200nmのプレート型銀微粒子を含んでなる請求項1記載の熱硬化性樹脂組成物。
- 前記(A)銀微粒子として、(A2)平均粒子径10〜200nmの球状銀微粒子を含んでなる請求項1又は2記載の熱硬化性樹脂組成物。
- 前記(A)成分の銀微粒子が、100℃〜250℃で自己焼結するものである請求項1乃至3のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(A)成分と前記(B)成分の質量比が、10:90〜90:10である請求項1乃至4のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(C)樹脂粒子の平均粒子径が0.5〜50μmであることを特徴とする請求項1乃至5のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(C)樹脂粒子が、ジビニルベンゼン、メタクリル酸メチル樹脂(PMMA)、メタクリル酸エチル樹脂(PEMA)、メタクリル酸ブチル樹脂(PBMA)、メタクリル酸メチル−メタクリル酸エチル共重合体およびこれらの混合物、またはシリコーンパウダーの何れかである請求項1乃至6のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(C)樹脂粒子の圧縮弾性率が200〜3000N/mm2、圧縮回復率30%以下であることを特徴とする請求項1乃至7のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(C)樹脂粒子が、平均粒子径が0.5〜10μmのシリコーンパウダー、および/または、圧縮弾性率が200〜3000N/mm 2 、圧縮回復率30%以下である架橋重合体である樹脂粒子であることを特徴とする請求項1乃至7のいずれか1項記載の熱硬化性樹脂組成物。
- 前記(D)熱硬化性樹脂が、シアネート樹脂、エポキシ樹脂、アクリル樹脂又はマレイミド樹脂ある請求項1乃至9のいずれか1項記載の熱硬化性樹脂組成物。
- さらに、(E)フラックスを含有し、前記(A)成分の銀微粒子と前記(B)成分の銀粉の合計量を100質量部としたとき、前記(E)成分が0.01〜5質量部配合される請求項1乃至11のいずれか1項記載の熱硬化性樹脂組成物。
- さらに、(F)溶剤を含有し、前記(A)成分の銀微粒子と前記(B)成分の銀粉の合計量を100質量部としたとき、前記(F)溶剤が7〜20質量部配合される請求項1乃至12のいずれか1項記載の熱硬化性樹脂組成物。
- 請求項1乃至13のいずれか1項記載の樹脂組成物をダイアタッチ材料とし、半導体素子を基板上に接着したことを特徴とする半導体装置。
- 前記半導体素子が、発光素子であることを特徴とする請求項14記載の半導体装置。
- 請求項1乃至15のいずれか1項記載の樹脂組成物を放熱部材接着用材料とし、放熱部材を発熱部品に接着したことを特徴とする電気・電子機器。
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US20230411335A1 (en) | 2023-12-21 |
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