KR100836150B1 - 질화규소 소결체, 질화규소 소결체의 제조 방법 및 질화규소 소결체 기판, 이러한 질화 규소 소결체 기판을 포함하는 회로 기판 - Google Patents
질화규소 소결체, 질화규소 소결체의 제조 방법 및 질화규소 소결체 기판, 이러한 질화 규소 소결체 기판을 포함하는 회로 기판 Download PDFInfo
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- KR100836150B1 KR100836150B1 KR1020070095109A KR20070095109A KR100836150B1 KR 100836150 B1 KR100836150 B1 KR 100836150B1 KR 1020070095109 A KR1020070095109 A KR 1020070095109A KR 20070095109 A KR20070095109 A KR 20070095109A KR 100836150 B1 KR100836150 B1 KR 100836150B1
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- silicon nitride
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- substrate
- rare earth
- nitride sintered
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- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/593—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering
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Abstract
Description
또한 본 발명의 고강도·고열전도성 질화 규소 소결체는, Mg와, La, Y, Gd 및 Yb로 구성된 군으로부터 선택된 적어도 1종의 희토류 원소가 소결 조제의 성분으로서 첨가된 질화 규소 소결체로서, 상기 소결 조제의 성분, 산소, 질소, 실리콘이 포함되는, 평균 입경 20~100nm의 미세 입자가 상기 질화 규소 소결체를 구성하는 질화 규소 입자 내에 석출하고 있고, 상기 미세 입자는 각각 조성이 다른 핵과 주변부로 구성되어 있는 것을 특징으로 한다.
상기 기재의 질화 규소 소결체에 있어서, 상기 미세 입자는 핵의 Mg와 희토류 원소의 함유량이, 주변부의 Mg와 희토류 원소의 함유량보다도 높고, 또한 상기 미세 입자가 비정질인 것이 바람직하다.
본 발명의 질화 규소 소결체는, 상온에서의 열전도율이 100~155W/(m·K) 이고, 상온에 있어서의 3점 굽힘 강도가 600~850MPa인 것이 바람직하다.
β분율(%) = [(Iβ(101)+Iβ(210))/(Iβ(101)+Iβ(210)+Iα(102)+Iα(210))]×100 …(1)
Iβ(101) : β형 Si3N4의 (101)면 회절 피크 강도,
Iβ(210) : β형 Si3N4의 (210)면 회절 피크 강도,
Iα(102) : α형 Si3N4의 (102)면 회절 피크 강도, 및
Iα(210) : α형 Si3N4의 (210)면 회절 피크 강도.
산소함유량이 0.2~0.5중량%이며, 평균입경이 0.2∼10㎛ 이고, 어스팩트비가 4~10인 제1 질화규소 분말 1∼50중량부와, 평균 입경이 0.2∼4㎛의 α형의 제 2 질화규소 분말 99∼50중량부와, Mg를 MgO로 환산하고, La, Y, Gd 및 Yb로 구성된 군으로부터 선택된 적어도 1종의 희토류 원소를 희토류 산화물(RExOy)로 환산하고, 상기 MgO와 상기 희토류 원소의 산화물 환산 함유량의 합계가 0.6~7중량%이고, 또한 MgO/RExOy로 표시되는 중량비가 1~70인 소결 조제를 혼합하고, 1,800~1,950℃의 온도 및 5~9기압의 압력의 질소 분위기 중에서 소결하는 것을 특징으로 한다.
본 발명의 질화규소 소결체의 제조 방법에 있어서, 1650~1850℃의 온도 및 5~9기압의 압력의 질소 분위기 중에서 예비 소성하는 것이 바람직하다.
Ra가 20㎛를 초과하면, 질화규소기판에 금속회로판을 접합했을 때 접합계면에 국소적으로 보이드(Void)가 생성되어, 접합강도의 현저한 저하를 초래한다. 한편, Ra가 0.2㎛ 미만에서는, 보이드의 생성을 억제할 수 있지만, 앵커링 효과가 얻어지지 않기 때문에, 역시 충분한 접합강도를 얻을 수 없다.
샘플 No. | 질화규소 원료분말 | 열처리 조건 | ||||
산소 (wt%) | 비표면적 (m2/g) | 평균입경 (㎛) | 압력 (MPa) | 온도 (℃) | 시간 (hr) | |
51 | 0.5 | 10.0 | 0.7 | 0.9 | 1,950 | 10 |
52 | 0.5 | 10.0 | 0.7 | 0.9 | 1,950 | 10 |
53 | 0.5 | 10.0 | 0.7 | 0.9 | 1,950 | 10 |
54 | 0.5 | 10.0 | 0.7 | 0.9 | 1,950 | 10 |
55 | 0.5 | 10.0 | 0.7 | 0.9 | 1,900 | 10 |
60 | 1.2 | 12.0 | 0.55 | 0.9 | 1,800 | 10 |
61 | 1.2 | 12.0 | 0.55 | 0.9 | 1,800 | 10 |
62 | 1.2 | 12.0 | 0.55 | 0.9 | 1,800 | 10 |
샘플 No. | 제 1 질화규소 분말 | |||||
β분율 (%) | 불순물 | 평균 입경 (㎛) | 어스팩트 비 | |||
O (wt%) | Fe (ppm) | Al (ppm) | ||||
51 | 100 | 0.3 | 30 | 50 | 2 | 5 |
52 | 100 | 0.3 | 30 | 50 | 2 | 5 |
53 | 100 | 0.3 | 30 | 50 | 2 | 5 |
54 | 100 | 0.3 | 30 | 50 | 2 | 5 |
55 | 90 | 0.3 | 30 | 50 | 2 | 5 |
60 | 90 | 1.0 | 30 | 50 | 2 | 5 |
61 | 90 | 1.0 | 30 | 50 | 2 | 5 |
62 | 90 | 1.0 | 30 | 50 | 2 | 5 |
샘플 No. | 소결 조건 | 미세 입자의 유무 | 열전도율 (W/m·K) | ||
온도 (℃) | 시간 (hr) | 질소압 (MPa) | |||
51 | 1,900 | 10 | 0.7 | 유 | 110 |
52 | 1,950 | 20 | 0.7 | 유 | 125 |
53 | 1,950 | 30 | 0.7 | 유 | 138 |
54 | 1,950 | 40 | 0.7 | 유 | 145 |
55 | 1,900 | 20 | 0.9 | 유 | 115 |
60 | 1,850 | 5 | 0.7 | 무 | 68 |
61 | 1,900 | 5 | 0.9 | 무 | 70 |
62 | 1,950 | 5 | 0.7 | 무 | 80 |
샘플 No. | 질화규소기판 | |||
Ra (㎛) | 질화규소 입자의 면적율 (%) | 입계상 면적율(%) | L (㎛) | |
71 | 5.0 | 85 | 15 | 15.0 |
72 | 2.0 | 90 | 10 | 5.0 |
73 | 0.8 | 90 | 10 | 1.5 |
74 | 5.0 | 85 | 15 | 15.0 |
75 | 2.0 | 90 | 10 | 5.0 |
76 | 0.8 | 90 | 10 | 1.5 |
77 | 5.0 | 85 | 15 | 15.0 |
78 | 2.0 | 90 | 10 | 5.0 |
79 | 5.0 | 85 | 15 | 15.0 |
80 | 2.0 | 90 | 10 | 5.0 |
91 | 0.1 | 90 | 10 | 1.2 |
92 | 22.0 | 90 | 10 | 38.0 |
93 | 2.0 | 60 | 40 | 5.0 |
94 | 0.6 | 90 | 10 | 0.8 |
95 | 10.0 | 90 | 10 | 45.0 |
96 | 22.0 | 90 | 10 | 2.5 |
97 | 22.0 | 90 | 10 | 2.5 |
98 | 22.0 | 90 | 10 | 2.5 |
샘플 No. | 접합 금속 | 접합 방법 | 필 강도 시험 | |
강도 (kN/m) | 파괴 부위 | |||
71 | Cu | 브레이징 | 31.0 | Cu |
72 | Cu | 브레이징 | 30.5 | Cu |
73 | Cu | 브레이징 | 28.0 | Cu |
74 | Cu | 직접 접합 | 27.5 | Cu |
75 | Cu | 직접 접합 | 26.0 | Cu |
76 | Cu | 직접 접합 | 25.5 | Cu |
77 | Al | 브레이징 | 25.0 | Al |
78 | Al | 브레이징 | 24.0 | Al |
79 | Al | 직접 접합 | 22.0 | Al |
80 | Al | 직접 접합 | 22.2 | Al |
91 | Cu | 브레이징 | 8.5 | 접합 계면 |
92 | Cu | 브레이징 | 9.5 | 접합 계면 |
93 | Cu | 브레이징 | 5.5 | 접합 계면 |
94 | Cu | 브레이징 | 7.0 | 접합 계면 |
95 | Cu | 브레이징 | 6.5 | 접합 계면 |
96 | Al | 직접 접합 | 7.0 | 접합 계면 |
97 | Al | 브레이징 | 6.5 | 접합 계면 |
98 | Al | 직접 접합 | 6.2 | 접합 계면 |
Claims (10)
- Mg와, La, Y, Gd 및 Yb로 구성된 군으로부터 선택된 적어도 1종의 희토류 원소가 소결 조제의 성분으로서 첨가된 질화규소 소결체이고, Mg를 MgO로 환산하고, 희토류 원소를 희토류 산화물(RExOy)로 환산하였을 때 상기 MgO와 상기 희토류 원소의 산화물 환산 함유량의 합계가 0.6∼7중량%이고, 또한 MgO/RExOy로 표시되는 중량비가 1~70인 것을 특징으로 하는 질화규소 소결체.
- Mg와, La, Y, Gd 및 Yb로 구성된 군으로부터 선택된 적어도 1종의 희토류 원소가 소결 조제의 성분으로서 첨가된 질화 규소 소결체로서, 상기 소결 조제의 성분, 산소, 질소, 실리콘이 포함되는, 평균 입경 20~100nm의 미세 입자가 상기 질화 규소 소결체를 구성하는 질화 규소 입자 내에 석출하고 있고, 상기 미세 입자는 각각 조성이 다른 핵과 주변부로 구성되어 있는 것을 특징으로 하는 질화규소 소결체.
- 제2항에 있어서,상기 미세 입자는 핵의 Mg와 희토류 원소의 함유량이 주변부의 Mg와 희토류 원소의 함유량보다도 높은 것을 특징으로 하는 질화규소 소결체.
- 제2항에 있어서,상기 미세 입자가 비정질인 것을 특징으로 하는 질화규소 소결체.
- 제1항 내지 제4항 중 어느 한 항에 있어서,상온에 있어서의 열전도율이 100~155W/(m·K)이고, 상온에 있어서의 3점 굽힘 강도가 600~850MPa인 것을 특징으로 하는 질화규소 소결체.
- 질화규소 분말 중에 존재하는 β형 결정상의 Cu-Kα선을 이용한 X선 회절 강도비로부터 하기 식(1)에 의해 구해지는 β분율이 30 내지 100%이고,β분율(%) = [(Iβ(101)+Iβ(210))/(Iβ(101)+Iβ(210)+Iα(102)+Iα(210))] ×100 …(1)Iβ(101) : β형 Si3N4의 (101)면 회절 피크 강도,Iβ(210) : β형 Si3N4의 (210)면 회절 피크 강도,Iα(102) : α형 Si3N4의 (102)면 회절 피크 강도, 및Iα(210) : α형 Si3N4의 (210)면 회절 피크 강도.산소 함유량이 0.2~0.5중량%이고, 평균 입경이 0.2∼10㎛이며, 어스펙트비가 4 ~ 10인 제 1 질화규소 분말 1∼50중량부와, 평균 입경이 0.2∼4㎛의 α형의 제 2 질화규소 분말 99∼50중량부와, Mg를 MgO로 환산하고, La, Y, Gd 및 Yb로 구성된 군으로부터 선택된 적어도 1종의 희토류 원소를 희토류 산화물(RExOy)로 환산하고, 상기 MgO와 상기 희토류 원소의 산화물 환산 함유량의 합계가 0.6~7중량%이고, 또한 MgO/RexOy로 표시되는 중량비가 1~70인 소결 조제를 혼합하고, 1,800~1,950℃의 온도 및 5~9기압의 압력의 질소 분위기 중에서 소결하는 것을 특징으로 하는 질화규소 소결체의 제조 방법.
- 제6항에 있어서,1,650∼1,850℃의 온도 및 5~9기압의 압력의 질소 분위기 중에서 예비 소성하는 것을 특징으로 하는 질화규소 소결체의 제조 방법.
- 질화 규소 입자와 입계상으로 이루어지는 질화 규소 소결체로 이루어지는 질화 규소 기판으로서, 기판 표면에서의 상기 질화 규소 입자와 상기 입계상의 합계 면적율을 100%로 했을 때, 상기 질화 규소 입자의 면적율이 70~100%이고, 표면에 노출한 질화 규소 입자의 최고의 산정부와, 질화 규소 입자 또는 입계상의 최저의 곡저부와의 거리 L이 1~40㎛이고, 중심선 평균 표면 조도 Ra가 0.2~20㎛의 표면 성상을 가지는 것을 특징으로 하는 질화 규소 기판.
- 제8항에 따른 질화 규소 기판의 적어도 일면에 Al 혹은 Cu의 회로판을 접합하여 이루어지는 것을 특징으로 하는 질화 규소 회로 기판.
- 삭제
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- 2001-09-19 DE DE10165107.4A patent/DE10165107B3/de not_active Expired - Lifetime
- 2001-09-20 CN CNB011379634A patent/CN1192989C/zh not_active Expired - Lifetime
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KR20180061861A (ko) | 2016-11-30 | 2018-06-08 | 주식회사 유라테크 | 초고온에 적합한 적층식 온도 센서 |
KR20180078747A (ko) | 2016-12-30 | 2018-07-10 | 주식회사 유라테크 | 글로우 플러그용 세라믹 발열체 및 이를 포함하는 글로우 플러그 |
US11046617B2 (en) | 2017-09-20 | 2021-06-29 | Lg Chem, Ltd. | Tape casting slurry composition for preparing silicon nitride sintered body |
Also Published As
Publication number | Publication date |
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KR100833962B1 (ko) | 2008-05-30 |
DE10146227B4 (de) | 2015-01-29 |
DE10165107B3 (de) | 2015-06-18 |
DE10146227A1 (de) | 2002-08-14 |
US6846765B2 (en) | 2005-01-25 |
CN1192989C (zh) | 2005-03-16 |
KR20020024534A (ko) | 2002-03-30 |
US7031166B2 (en) | 2006-04-18 |
CN1356292A (zh) | 2002-07-03 |
KR20070103330A (ko) | 2007-10-23 |
US20020164475A1 (en) | 2002-11-07 |
DE10165080B4 (de) | 2015-05-13 |
US20050094381A1 (en) | 2005-05-05 |
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