JPH01138175A - Calcination of aln - Google Patents
Calcination of alnInfo
- Publication number
- JPH01138175A JPH01138175A JP62297222A JP29722287A JPH01138175A JP H01138175 A JPH01138175 A JP H01138175A JP 62297222 A JP62297222 A JP 62297222A JP 29722287 A JP29722287 A JP 29722287A JP H01138175 A JPH01138175 A JP H01138175A
- Authority
- JP
- Japan
- Prior art keywords
- sintering
- raw material
- aln
- firing temperature
- impurity
- 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.)
- Pending
Links
- 238000001354 calcination Methods 0.000 title abstract 4
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 238000010304 firing Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 12
- 239000012535 impurity Substances 0.000 abstract description 20
- 238000010438 heat treatment Methods 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 239000008187 granular material Substances 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/58—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
- C04B35/581—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 aluminium nitride
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
皮業上皇丑■分匪
本発明は焼結助剤を添加したＡＩＮ焼結原料を焼成する
方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for firing an AIN sintering raw material to which a sintering aid has been added.
従米勿孜素
ＩＣ用基板としてＡβＮ焼結体が使用されている。これ
は集積度が高くなると放熱が重要課題となり、このため
には熱伝導率の高いＡ６Ｎが有効であるからである。An AβN sintered body is used as a substrate for an IC. This is because heat dissipation becomes an important issue as the degree of integration increases, and A6N, which has high thermal conductivity, is effective for this purpose.
ところでＡｆｆＮは焼結により製造されるが、ＡＩＮ焼
結原料中、特に表面に存在する酸素等の不純物がＡ１、
Ｎと反応すると熱電導性の良くないＡ７！−０−Ｎ化合
物が生成する。従って、この生成を抑制して良好な熱電
導性を確保すべく、酸化カルシウム（ＣａＯ）、酸化イ
ツトリウム（Ｙｚ０３）等の焼結助剤を添加したＡＮＮ
焼結原料を用いて非酸化雰囲気下で焼成していた。By the way, AffN is manufactured by sintering, but impurities such as oxygen present in the AIN sintering raw material, especially on the surface, cause A1,
A7 has poor thermal conductivity when it reacts with N! -0-N compound is produced. Therefore, in order to suppress this generation and ensure good thermal conductivity, ANN added with sintering aids such as calcium oxide (CaO) and yttrium oxide (Yz03)
Sintering raw materials were used and fired in a non-oxidizing atmosphere.
この焼結助剤を添加する理由は、焼結助剤が焼結過程で
ＡＡＮ焼結原料中の不純物酸素や金属と反応して（以下
不純物トラップという）液相を形成し、焼結を促進する
からである。またこの液相は焼結中に外部へ排出するた
め、結晶粒界に存在する液相が少なくなり、かつ粒内へ
の不純物酸素の固溶を妨げることにより粒内の不純物酸
素濃度を下げる作用があることに依る。The reason for adding this sintering aid is that during the sintering process, the sintering aid reacts with the impurity oxygen and metal in the AAN sintering raw material to form a liquid phase (hereinafter referred to as an impurity trap), promoting sintering. Because it does. In addition, since this liquid phase is discharged to the outside during sintering, the amount of liquid phase existing at the grain boundaries decreases, and by preventing impurity oxygen from dissolving inside the grains, it has the effect of lowering the impurity oxygen concentration within the grains. It depends on there being.
■ ＜ｌしよ゛と る口 占
さて、従来の焼成方法では所定の焼成温度に一定に保持
した状態で焼結を行なうため、不純物トラップと液相の
排出とが同時的に進行する。このとき、不純物トラップ
が余り行われていない液相が排出されることがあり、こ
の結果、粒内に不純物酸素が未反応のまま残留して熱伝
導率が低下するという問題点があった。■<l<<<1><<1> In the conventional sintering method, sintering is carried out while keeping a predetermined sintering temperature constant, so impurity trapping and liquid phase discharge proceed simultaneously. At this time, a liquid phase in which impurity trapping is not performed may be discharged, and as a result, impurity oxygen remains unreacted within the grains, resulting in a decrease in thermal conductivity.
本発明は斯かる問題点を解決すべくなされたものであり
、不純物の少ない高熱伝導率のＡＩＮ焼結体を製造し得
るＡＡＮ焼成方法を提供することを目的とする。The present invention was made to solve these problems, and an object of the present invention is to provide an AAN sintering method that can produce an AIN sintered body with few impurities and high thermal conductivity.
。 占を”ン るための
本発明に係るＡＮＮ焼成方法は、焼結助剤を添加したＡ
ｌＮ焼結原料を焼成する方法において、前記焼結助剤に
より液相成分が生成する第１の焼成温度にＡｌＮ焼結原
料を加熱保持し、然る後、第１の焼成温度よりも高い第
２の焼成温度に前記Ａ７２Ｎ焼結原料を加熱保持して焼
成することを特徴としている。. The ANN firing method according to the present invention for obtaining a
In a method of firing an IN sintering raw material, the AlN sintering raw material is heated and maintained at a first firing temperature at which a liquid phase component is generated by the sintering aid, and then a second firing temperature higher than the first firing temperature is heated. The method is characterized in that the A72N sintering raw material is heated and held at the firing temperature of 2.
詐−一一一井一
本発明にあっては、第１の焼成温度での加熱保持の際に
主として不純物トラップが起こり、その後の第２の焼成
温度での加熱保持の際に主とじて液相の排出が生じる。In the present invention, impurity traps mainly occur during heating and holding at the first firing temperature, and liquid traps mainly occur during heating and holding at the subsequent second firing temperature. Phase discharge occurs.
実−施一玉 以下、本発明方法を具体的に説明する。implementation - implementation The method of the present invention will be specifically explained below.
まず、ＡＡＮ焼結体用の主原料（粉末）に焼結助剤、例
えばＹ２Ｏ，、ＣａＯ等の粉末を添加し、これを有機溶
媒、例えばキシレン中でボールミルを用いて混合してス
ラリーを得る。然る後、スラリーを脱水、乾燥する。こ
れにより、有機溶媒が除去され、粉末が得られる。First, a sintering aid such as Y2O, CaO, etc. powder is added to the main raw material (powder) for the AAN sintered body, and this is mixed in an organic solvent such as xylene using a ball mill to obtain a slurry. . After that, the slurry is dehydrated and dried. This removes the organic solvent and yields a powder.
得られた粉末に有機バインダー、例えばパラフィンを添
加して整粒し、これを直径：１２龍φ、厚み：４ｍｍｔ
の円板状に、金型を用いて１乃至ｌ。An organic binder, such as paraffin, is added to the obtained powder, which is then sized to form a powder with a diameter of 12 mm and a thickness of 4 mm.
1 to 1 liter using a mold into a disc shape.
５ｔ／ｃＩＩｔの圧力でプレス成形したのち、大気中で
脱バインダー処理を行ない、その後、非酸化雰囲気、例
えばＮ２雰囲気下で焼成する。After press-molding at a pressure of 5t/cIIt, the binder is removed in the air, and then fired in a non-oxidizing atmosphere, for example, an N2 atmosphere.
この焼成は、図に示す如く、焼結助剤により液相成分が
生成する１５００℃乃至１７００℃の第１の焼成温度Ａ
に、ＡｌＮ焼結原料を加熱保持し、次いで、第１の焼成
温度Ａよりも高い通常の焼成温度である１７５０℃乃至
１９５０℃の第２の焼成温度ＢにＡｌＮ焼結原料を加熱
保持して行なう。As shown in the figure, this firing is carried out at a first firing temperature A of 1500°C to 1700°C at which a liquid phase component is generated by the sintering aid.
The AlN sintering raw material is heated and held, and then the AlN sintering raw material is heated and held at a second firing temperature B of 1750°C to 1950°C, which is a normal firing temperature higher than the first firing temperature A. Let's do it.
なお、第１．第２の焼成温度Ａ及びＢの最適値は添加す
る焼結助剤により異なるが、夫々１５００乃至１７００
℃、１７５０乃至１９５０℃の範囲で選択使用するのが
好ましい。In addition, 1. The optimal values of the second firing temperatures A and B vary depending on the sintering aid added, but are 1500 to 1700, respectively.
It is preferable to select and use the temperature within the range of 1750 to 1950°C.
第１の焼成温度Ａを１５００℃乃至１７００℃とするこ
とについては次の理由による。即ち、１５００℃未満で
は液相状態を作りにくく、また１７００℃を越えると不
純物トラップと液相の排出とが同時に進行し、従来と変
わらない焼結が行われるようになるからである。The reason for setting the first firing temperature A to 1500°C to 1700°C is as follows. That is, if the temperature is lower than 1500°C, it is difficult to create a liquid phase state, and if the temperature exceeds 1700°C, trapping of impurities and discharge of the liquid phase proceed at the same time, resulting in sintering that is no different from conventional sintering.
表は、焼結助剤としてＹ２Ｏ３を使用し、これを１ｗｔ
％と３ｗｔ％との２レベルで添加した２種類のＡβＮ焼
結原料夫々を、第１の焼成温度Ａを１５００．１６００
．１７ＱＯ°Ｃの３レベルで変えて５時間加熱保持した
のち、１８５０℃に一定に保った第２の焼成温度で５時
間加熱保持して計６個のＡ６Ｎ焼結体を得、それぞれに
ついてレーザーフラッシュ法により熱伝導率を測定した
結果をまとめた表である。なお、比較のために第１の焼
成を行わない場合と、第１の焼成温度Ａを１４５０℃、
１７５０℃とした場合に得たＡＩＮ焼結体の熱伝導率の
測定結果を併せて示している。The table shows that Y2O3 is used as a sintering aid, and 1wt of this is used as a sintering aid.
Two types of AβN sintering raw materials added at two levels of % and 3wt% were added at a first firing temperature A of 1500.1600
．． After heating and holding for 5 hours at 3 levels of 17QO°C, heating and holding for 5 hours at the second firing temperature kept constant at 1850°C to obtain a total of 6 A6N sintered bodies, each of which was heated with a laser flash. This is a table summarizing the results of measuring thermal conductivity using the method. For comparison, the case where the first firing was not performed and the case where the first firing temperature A was 1450°C,
The measurement results of the thermal conductivity of the AIN sintered body obtained at 1750°C are also shown.
表
この表より理解される如く、従来同様に第２の焼成温度
Ｂのみで焼成、即ち焼成温度を変えずルベルで焼成した
場合（比較例１）には熱伝導率が１２０と低いが、２レ
ベルで焼成温度を変える場合（実施例１，３．５）には
それを１９０以上と高くすることができる。Ｙ２Ｏ３の
添加量を増加した場合でも前同様の効果があり（実施例
２゜４．６、比較例２）、またその結果得られる熱伝導
率はＹｚＯ：＋の添加目的からして当然であるが、Ｙ２
Ｏ３の添加量の増量により向上する。第１の焼成温度Ａ
が低い場合（比較例３，４）には不純物トラップが起こ
りに＜＜、従来方法（比較例１゜２）の熱伝導率より少
し良くなるが余り変わらない。逆に第１の焼成温度Ａが
高い場合（比較例５゜６）には不純物トラップと液相の
排出とが同時に進行するため、従来と、殆ど変わらない
結果となる。Table As can be understood from this table, the thermal conductivity is as low as 120 when firing only at the second firing temperature B, that is, when firing at Lebel without changing the firing temperature (Comparative Example 1), as in the conventional case. When the firing temperature is changed by level (Example 1, 3.5), it can be increased to 190 or higher. Even when the amount of Y2O3 added was increased, the same effect as before was obtained (Example 2゜4.6, Comparative Example 2), and the resulting thermal conductivity was natural considering the purpose of adding YzO:+. However, Y2
This can be improved by increasing the amount of O3 added. First firing temperature A
When the thermal conductivity is low (Comparative Examples 3 and 4), impurity traps occur, and the thermal conductivity is slightly better than that of the conventional method (Comparative Example 1°2), but not significantly different. On the other hand, when the first firing temperature A is high (Comparative Example 5°6), impurity trapping and liquid phase discharge proceed simultaneously, resulting in almost the same results as before.
光里■四且
以上詳述した如く本発明による場合には第１の焼成温度
での加熱保持の際に主として不純物トラップが起こり、
その後の第２の焼成温度での加熱保持の際に主として液
相の排出が生じるため、粒内の不純物酸素濃度および不
純物の少ない高熱伝導率のＡｌｘが製造できるという優
れた効果を奏する。As detailed above, in the case of the present invention, impurity traps mainly occur during heating and holding at the first firing temperature,
Since the liquid phase is mainly discharged during subsequent heating and holding at the second firing temperature, an excellent effect is produced in that Alx with high thermal conductivity and low impurity oxygen concentration in the grains can be produced.
図面は本発明方法による場合の焼成温度の説明図である
。The drawing is an explanatory diagram of the firing temperature in the case of the method of the present invention.
Claims (1)
法において、 前記焼結助剤により液相成分が生成する第１の焼成温度
にＡｌＮ焼結原料を加熱保持し、然る後、第１の焼成温
度よりも高い第２の焼成温度に前記ＡｌＮ焼結原料を加
熱保持して焼成することを特徴とするＡｌＮ焼成方法。(1) In a method of firing an AlN sintering raw material to which a sintering aid has been added, the AlN sintering raw material is heated and maintained at a first firing temperature at which a liquid phase component is generated by the sintering aid, and then An AlN firing method, characterized in that the AlN sintering raw material is heated and held at a second firing temperature higher than the first firing temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62297222A JPH01138175A (en) | 1987-11-25 | 1987-11-25 | Calcination of aln |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62297222A JPH01138175A (en) | 1987-11-25 | 1987-11-25 | Calcination of aln |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01138175A true JPH01138175A (en) | 1989-05-31 |
Family
ID=17843755
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62297222A Pending JPH01138175A (en) | 1987-11-25 | 1987-11-25 | Calcination of aln |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01138175A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2022210517A1 (en) * | 2021-03-31 | 2022-10-06 |
-
1987
- 1987-11-25 JP JP62297222A patent/JPH01138175A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2022210517A1 (en) * | 2021-03-31 | 2022-10-06 | ||
| WO2022210517A1 (en) * | 2021-03-31 | 2022-10-06 | デンカ株式会社 | Aluminium nitride sintered body, production method for same, circuit board, and laminated substrate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH06135771A (en) | High heat conductivity silicon nitride sintered compact and its production | |
| JPH01138175A (en) | Calcination of aln | |
| US4798764A (en) | Arsenate dopant sources and method of making the sources | |
| JP2578113B2 (en) | Method for producing high thermal conductive aluminum nitride sintered body | |
| JP2578114B2 (en) | Method for producing high thermal conductive aluminum nitride sintered body | |
| JPH05147910A (en) | Aluminum nitride-based powder and its production | |
| JPH0567593B2 (en) | ||
| CN109320258A (en) | A kind of polycrystalline silicon ingot casting silicon nitride kiln furniture material and preparation method thereof | |
| JPS62252374A (en) | Manufacture of aluminum nitride sintered body | |
| JPH02233560A (en) | High-strength calcined sialon-based compact | |
| JPH06116039A (en) | Aluminum nitride sintered compact | |
| JPS62167208A (en) | Production of aluminum nitride powder | |
| JPH04124064A (en) | Production of highly heat-conductive silicon carbide | |
| JP3834930B2 (en) | Magnesium siliconitride sintered body and method for producing the same | |
| JP2671539B2 (en) | Method for producing silicon nitride sintered body | |
| JPH0459609A (en) | Production of aluminum nitride powder | |
| JPH0321500B2 (en) | ||
| JPH02116678A (en) | Production of sintered silicon carbide body | |
| JP2704194B2 (en) | Black aluminum nitride sintered body | |
| JP2577155B2 (en) | Silicon nitride sintered body | |
| JPH04951B2 (en) | ||
| JPH01138174A (en) | Production of sintered aluminum nitride | |
| JPH0686332B2 (en) | Manufacturing method of sialon-based ceramic tool for cutting cast iron | |
| JPH06247772A (en) | Production of aluminum nitride sintered compact | |
| JPS63277571A (en) | Production of sintered aluminum nitride having high thermal conductivity |