JP2580439B2 - High dielectric constant alumina sintered body and method for producing the same - Google Patents
High dielectric constant alumina sintered body and method for producing the sameInfo
- Publication number
- JP2580439B2 JP2580439B2 JP4168076A JP16807692A JP2580439B2 JP 2580439 B2 JP2580439 B2 JP 2580439B2 JP 4168076 A JP4168076 A JP 4168076A JP 16807692 A JP16807692 A JP 16807692A JP 2580439 B2 JP2580439 B2 JP 2580439B2
- Authority
- JP
- Japan
- Prior art keywords
- dielectric constant
- sintered body
- alumina
- high dielectric
- tungsten
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims description 13
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 13
- 239000010937 tungsten Substances 0.000 claims description 13
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- 239000011733 molybdenum Substances 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 239000004065 semiconductor Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000007606 doctor blade method Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、半導体集積回路素子を
収納する半導体素子収納用パッケージや半導体集積回路
素子が搭載される多層配線基板等の絶縁基体に用いられ
る高誘電率アルミナ質焼結体およびその製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high dielectric constant alumina sintered body used for an insulating substrate such as a semiconductor device housing package for housing a semiconductor integrated circuit device or a multilayer wiring board on which the semiconductor integrated circuit device is mounted. And its manufacturing method.
【０００２】[0002]
【従来技術】従来、アルミナを主成分とするアルミナ質
焼結体は、耐熱性を含めて化学的に極めて安定であり、
機械的強度，電気的絶縁性が優れているため、半導体集
積回路素子を収納する半導体素子収納用パッケージや半
導体集積回路素子が搭載される多層配線基板等の絶縁基
体に用いられている（特開昭５４−１０２３１２号公報
参照）。2. Description of the Related Art Conventionally, an alumina-based sintered body containing alumina as a main component is extremely chemically stable including heat resistance.
Because of its excellent mechanical strength and electrical insulation, it is used for insulating bases such as semiconductor element housing packages for housing semiconductor integrated circuit elements and multilayer wiring boards on which semiconductor integrated circuit elements are mounted. See JP-A-54-102312).
【０００３】[0003]
【発明が解決しようとする問題点】しかしながら、この
ようなアルミナ質焼結体では誘電率が小さいという問題
があった。即ち、従来のアルミナ質焼結体は、その電気
的絶縁性等のみ注目して使用されていたため、誘電体と
しては用いられず、その誘電率は９．５以下と小さかっ
た。However, such an alumina-based sintered body has a problem that its dielectric constant is small. That is, since the conventional alumina-based sintered body was used with attention paid only to its electrical insulating property and the like, it was not used as a dielectric, and its dielectric constant was as small as 9.5 or less.
【０００４】本発明は、高誘電率を有する優れた特性の
高誘電率アルミナ質焼結体およびその製造方法を提供す
ることを目的とする。An object of the present invention is to provide a high dielectric constant alumina-based sintered body having a high dielectric constant and excellent characteristics, and a method for producing the same.
【０００５】[0005]
【問題点を解決するための手段】本発明者等は、上記の
問題点に対して検討を行った結果、アルミナに添加する
モリブデンやタングステンの量を増加すると、誘電率が
次第に高くなる傾向にあることを知見し、本発明をする
に至った。[Means for Solving the Problems] The present inventors have studied the above problems, and as a result, as the amount of molybdenum or tungsten added to alumina increases, the dielectric constant tends to gradually increase. Having found that there is, the present invention has been accomplished.
【０００６】即ち、本発明の高誘電率アルミナ質焼結体
は、アルミナを主成分とし、焼結助剤を含むとともに、
モリブデン及びタングステンのうちの少なくとも一種を
３．４５重量％以上含有するとともに、誘電率が１０．
８以上であることを特徴とする。また、本発明の高誘電
率アルミナ質焼結体の製造方法は、アルミナ粉末と、焼
結後に金属モリブデンおよび金属タングステンの少なく
とも一種となる粉末を金属換算で合計３．４５重量％以
上となるように混合し、所定形状に成形し、加湿した水
素−窒素混合ガス雰囲気中で焼成する方法である。That is, the high dielectric constant alumina sintered body of the present invention contains alumina as a main component, contains a sintering aid, and
It contains at least one of molybdenum and tungsten at 3.45% by weight or more and has a dielectric constant of 10.
8 or more. Further, in the method for producing a high dielectric constant alumina-based sintered body according to the present invention, the alumina powder and the powder that becomes at least one of metal molybdenum and metal tungsten after sintering may have a total of 3.45% by weight or more in terms of metal. , Formed into a predetermined shape, and fired in a humidified hydrogen-nitrogen mixed gas atmosphere.
【０００７】ここで、モリブデン及びタングステンの合
計量を３．４５重量％以上含有させたのは、３．４５重
量％よりも少ないと、誘電率１０．８以上を達成するこ
とができないからである。Here, the reason why the total amount of molybdenum and tungsten is contained at least 3.45% by weight is that if the total amount is less than 3.45% by weight, a dielectric constant of at least 10.8 cannot be achieved. .
【０００８】本発明の高誘電率アルミナ質焼結体は、先
ず、アルミナ（Ａｌ2 Ｏ3 ）粉末に対して、ＳｉＯ2 ，
ＣａＯ，ＭｇＯからなる焼結助剤と、焼結後金属モリブ
デン（Ｍｏ）またはタングステン（Ｗ）となるモリブデ
ンまたはタングステンの酸化物あるいは塩類と、必要に
応じて着色剤である酸化クロム（Ｃｒ2 Ｏ3 ）を焼結後
の含有量が前述した範囲となるように秤量し、これに有
機溶媒を添加し、例えば、回転ミルにて混合粉砕し、次
いで混合粉砕物にブチラール樹脂等のバインダーを加え
て混合し、原料スラリーを調整する。The high-dielectric-constant alumina-based sintered body of the present invention is obtained by first converting alumina (Al 2 O 3 ) powder to SiO 2 ,
A sintering aid composed of CaO, MgO, an oxide or salt of molybdenum or tungsten which becomes metallic molybdenum (Mo) or tungsten (W) after sintering, and, if necessary, a chromium oxide (Cr 2 O) 3 ) is weighed so that the content after sintering is in the above-mentioned range, an organic solvent is added thereto, mixed and pulverized by, for example, a rotary mill, and then a binder such as butyral resin is added to the mixed and pulverized product. To mix and adjust the raw slurry.
【０００９】そして、得られたスラリーをドクターブレ
ード法によりシート状に成形し、該成形体を複数枚積層
した後、例えば、加湿した水素−窒素混合ガス雰囲気中
で１５００〜１６００℃の範囲内の焼成温度で２時間焼
成し、アルミナ質焼結体を得る。Then, the obtained slurry is formed into a sheet by a doctor blade method, and a plurality of the formed bodies are laminated, for example, in a humidified hydrogen-nitrogen mixed gas atmosphere at a temperature in the range of 1500 to 1600 ° C. Firing at a firing temperature for 2 hours to obtain an alumina sintered body.
【００１０】ここで、加湿した水素−窒素混合ガス雰囲
気中で焼成したのは、加湿しないとＳｉＯ2 がＳｉＯと
なって蒸発するからであり、上記のように加湿した水素
−窒素混合ガス雰囲気中で焼成することにより、助剤の
主成分であるＳｉＯ2 の蒸発を抑制し、焼結体の緻密化
を促進することができ、これにより、誘電率が上昇する
からである。The reason why the sintering is performed in a humidified hydrogen-nitrogen mixed gas atmosphere is that if not humidified, SiO 2 becomes SiO and evaporates. By sintering, the evaporation of SiO 2 , which is a main component of the auxiliary agent, can be suppressed, and the densification of the sintered body can be promoted, thereby increasing the dielectric constant.
【００１１】また、助剤を添加することにより、アルミ
ナ質焼結体の緻密化を促進することができ、これによ
り、誘電率を向上することができる。さらに、酸化クロ
ム（Ｃｒ2 Ｏ3 ）を添加して、Ｃｒ，Ｍｏ，Ｗにより焼
結体を透過しようとする全波長の光を遮断することがで
き、これにより、パッケージ内に収容されたＩＣの誤作
動を阻止することができる。Further, by adding an auxiliary agent, it is possible to promote the densification of the alumina-based sintered body, thereby improving the dielectric constant. Further, by adding chromium oxide (Cr 2 O 3 ), it is possible to block light of all wavelengths that are going to pass through the sintered body by Cr, Mo, W, and thereby, the IC housed in the package can be blocked. Malfunction can be prevented.
【００１２】[0012]
【作用】本発明の高誘電率アルミナ質焼結体では、アル
ミナに、モリブデン及びタングステンのうちの少なくと
も一種を次第に多く添加すると、誘電率が次第に高くな
り、３．４５重量％以上添加すると誘電率が１０．８以
上となり、従来のアルミナ質焼結体と比較して大幅に誘
電率を向上することができる。In the alumina sintered body having a high dielectric constant of the present invention, the dielectric constant gradually increases when at least one of molybdenum and tungsten is gradually added to alumina, and the dielectric constant increases when 3.45% by weight or more is added. Is 10.8 or more, and the dielectric constant can be greatly improved as compared with the conventional alumina-based sintered body.
【００１３】以下、本発明を次の例で説明する。Hereinafter, the present invention will be described with reference to the following examples.
【００１４】[0014]
【実施例】先ず、純度９９．８％、平均粒径１．８μｍ
のアルミナ（Ａｌ2 Ｏ3 ）粉末と、ＳｉＯ2 ，ＣａＯ，
ＭｇＯからなる焼結助剤と、酸化クロム（Ｃｒ2 Ｏ3 ）
及び、焼結後金属モリブデン（Ｍｏ）またはタングステ
ン（Ｗ）の少なくとも１種となるモリブデンまたはタン
グステンの酸化物あるいは塩類を焼結後の含有量が表１
に示した重量となるように秤量し、有機溶媒およびアル
ミナボールとともに回転ミルにて混合粉砕し、次いで該
混合粉砕物にブチラール樹脂等のバインダーを加えて混
合し、原料スラリーを調整した。EXAMPLE First, the purity was 99.8% and the average particle size was 1.8 μm.
Alumina (Al 2 O 3 ) powder, SiO 2 , CaO,
Sintering aid consisting of MgO and chromium oxide (Cr 2 O 3 )
Table 1 shows that after sintering, the content after sintering of an oxide or a salt of molybdenum or tungsten, which becomes at least one kind of metal molybdenum (Mo) or tungsten (W), is shown in Table 1.
Was weighed so as to have the weight shown in Table 1 above, mixed and pulverized together with an organic solvent and alumina balls in a rotary mill, and then a binder such as butyral resin was added to the mixed and pulverized product to prepare a raw material slurry.
【００１５】かくして得られたスラリーをドクターブレ
ード法によりシート状に成形し、該成形体を複数枚加熱
圧着した後、加湿した水素−窒素混合ガス雰囲気中で１
５００〜１６００℃の範囲内の焼成温度で２時間焼成
し、本発明のアルミナ質焼結体を得た。The slurry thus obtained is formed into a sheet by a doctor blade method, and a plurality of the formed bodies are heated and pressed, and then pressed in a humidified hydrogen-nitrogen mixed gas atmosphere.
Firing was performed at a firing temperature in the range of 500 to 1600 ° C. for 2 hours to obtain an alumina sintered body of the present invention.
【００１６】その後、上記アルミナ質焼結体を直径１０
ｍｍ、厚さ２ｍｍの円板状に研磨加工し、レーザーフラ
ッシュ法により熱電導率を、同様にして研磨加工した長
さ４０ｍｍ、３ｍｍ×４ｍｍ角の角柱を使用して、ＪＩ
Ｓ Ｒ １６０１の規定に基づき３点曲げ強度をそれぞ
れ測定した。Thereafter, the above alumina sintered body is put into a
polished into a disk having a thickness of 2 mm and a thickness of 2 mm, and the thermal conductivity was similarly polished by a laser flash method.
The three-point bending strength was measured based on the specification of SR1601.
【００１７】また、同様にして、縦・横各５０ｍｍ、厚
さ２ｍｍの板状に研磨加工し、ＪＩＳ Ｃ ２１４１の
規定に基づき体積固有抵抗（１００℃、相対湿度５０
％）及び誘電率（室温、１ＭＨｚ）を測定し、誘電損失
を導出した。In the same manner, the plate is polished into a plate having a length and width of 50 mm and a thickness of 2 mm, and has a volume resistivity (100 ° C., relative humidity of 50 mm) in accordance with JIS C 2141.
%) And dielectric constant (room temperature, 1 MHz) were measured to derive a dielectric loss.
【００１８】さらに、上記アルミナ質焼結体の表面にタ
ングステンのメタライズ金属層を被着形成するととも
に、該メタライズ金属層表面にニッケルメッキを行い、
これに低熱膨張の金属片を低融点ロウ材でロウ付けし、
３ｋｇ／ｍｍ2 の引っ張り応力でもって該金属片を引っ
張り、剥離の有無を確認し、メタライズの強度評価を行
った。この結果、本発明のアルミナ質焼結体では、剥離
は無かった。Further, a metallized metal layer of tungsten is deposited on the surface of the alumina sintered body, and nickel plating is performed on the surface of the metallized metal layer.
To this, a low thermal expansion metal piece is brazed with a low melting point brazing material,
The metal piece was pulled with a tensile stress of 3 kg / mm 2 , the presence or absence of peeling was confirmed, and the metallizing strength was evaluated. As a result, there was no peeling in the alumina-based sintered body of the present invention.
【００１９】尚、焼結体中のアルミナ及び各着色剤の量
はＩＣＰ発光分光分析法によりそれぞれ測定した。The amounts of alumina and each colorant in the sintered body were measured by ICP emission spectroscopy.
【００２０】その結果を表１に示す。The results are shown in Table 1.
【００２１】[0021]
【表１】 [Table 1]
【００２２】表１により、本発明の高誘電率アルミナ質
焼結体は、熱伝導率１９W/mK以上、曲げ強度６２kg/mm2
以上、体積固有抵抗３×１０14Ω・ｃｍ以上、誘電率１
０．８以上、誘電損失は７×１０-4以下の優れた特性を
有することが判った。また、本発明の高誘電率アルミナ
質焼結体の色調は黒色であり、メタライズの強度評価に
よる試験の結果、剥離も無かった。According to Table 1, the high dielectric constant alumina sintered body of the present invention has a thermal conductivity of 19 W / mK or more and a bending strength of 62 kg / mm 2.
Above, volume resistivity 3 × 10 14 Ω · cm or more, dielectric constant 1
It was found to have excellent characteristics of 0.8 or more and a dielectric loss of 7 × 10 −4 or less. The color tone of the high-dielectric-constant alumina-based sintered body of the present invention was black, and no peeling was observed as a result of the test by metallization strength evaluation.
【００２３】[0023]
【発明の効果】以上詳述した通り、本発明の高誘電率ア
ルミナ質焼結体では、モリブデン及びタングステンのう
ちの少なくとも一種を３．４５重量％以上添加したの
で、誘電率が１０．８以上となり、従来よりも誘電率を
大幅に向上することができる。As described in detail above, in the high dielectric constant alumina-based sintered body of the present invention, at least one of molybdenum and tungsten is added in an amount of 3.45% by weight or more, so that the dielectric constant is 10.8 or more. Thus, the dielectric constant can be greatly improved as compared with the related art.
Claims (2)
ともに、モリブデンおよびタングステンのうちの少なく
とも一種を３．４５重量％以上含有し、誘電率が１０．
８以上であることを特徴とする高誘電率アルミナ質焼結
体。1. A composition comprising alumina as a main component, a sintering aid, at least one of molybdenum and tungsten at 3.45% by weight or more, and a dielectric constant of 10.
A high dielectric constant alumina-based sintered body having a particle size of 8 or more.
および金属タングステンの少なくとも一種となる粉末を
金属換算で合計３．４５重量％以上となるように混合
し、所定形状に成形し、加湿した水素−窒素混合ガス雰
囲気中で焼成することを特徴とする高誘電率アルミナ質
焼結体の製造方法。2. A mixture of alumina powder and powder that becomes at least one of metal molybdenum and metal tungsten after sintering so as to have a total of 3.45% by weight or more in terms of metal. -A method for producing a high dielectric constant alumina-based sintered body, characterized by firing in a nitrogen mixed gas atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4168076A JP2580439B2 (en) | 1992-06-26 | 1992-06-26 | High dielectric constant alumina sintered body and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4168076A JP2580439B2 (en) | 1992-06-26 | 1992-06-26 | High dielectric constant alumina sintered body and method for producing the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62276728A Division JPH0745335B2 (en) | 1987-10-30 | 1987-10-30 | Colored alumina sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05178656A JPH05178656A (en) | 1993-07-20 |
| JP2580439B2 true JP2580439B2 (en) | 1997-02-12 |
Family
ID=15861401
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4168076A Expired - Fee Related JP2580439B2 (en) | 1992-06-26 | 1992-06-26 | High dielectric constant alumina sintered body and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2580439B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253150B (en) * | 2020-03-03 | 2021-04-16 | 武汉理工大学 | Preparation method of mullite-corundum composite ceramic substrate for electronic packaging |
| CN111825432A (en) * | 2020-07-31 | 2020-10-27 | 中南大学湘雅医院 | A kind of fine grain pink ZTA ceramic and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4985117A (en) * | 1972-12-16 | 1974-08-15 | ||
| JPS53137216A (en) * | 1977-05-06 | 1978-11-30 | Ngk Spark Plug Co | Colored ceramics |
| JPH01119557A (en) * | 1987-10-30 | 1989-05-11 | Kyocera Corp | Colored alumina sintered body |
| JPH0387091A (en) * | 1989-06-15 | 1991-04-11 | Ngk Spark Plug Co Ltd | Alumina multilayer wiring board having high dielectric layer |
-
1992
- 1992-06-26 JP JP4168076A patent/JP2580439B2/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4985117A (en) * | 1972-12-16 | 1974-08-15 | ||
| JPS53137216A (en) * | 1977-05-06 | 1978-11-30 | Ngk Spark Plug Co | Colored ceramics |
| JPH01119557A (en) * | 1987-10-30 | 1989-05-11 | Kyocera Corp | Colored alumina sintered body |
| JPH0387091A (en) * | 1989-06-15 | 1991-04-11 | Ngk Spark Plug Co Ltd | Alumina multilayer wiring board having high dielectric layer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05178656A (en) | 1993-07-20 |
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| LAPS | Cancellation because of no payment of annual fees |