JP2581787B2 - Si 3 lower N 4 lower 4 Tools for powder synthesis - Google Patents
Si 3 lower N 4 lower 4 Tools for powder synthesisInfo
- Publication number
- JP2581787B2 JP2581787B2 JP63328354A JP32835488A JP2581787B2 JP 2581787 B2 JP2581787 B2 JP 2581787B2 JP 63328354 A JP63328354 A JP 63328354A JP 32835488 A JP32835488 A JP 32835488A JP 2581787 B2 JP2581787 B2 JP 2581787B2
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- JP
- Japan
- Prior art keywords
- less
- powder
- synthesis
- tool
- purity
- 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 - Lifetime
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- Compositions Of Oxide Ceramics (AREA)
- Furnace Charging Or Discharging (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明はNH3あるいはNH3を含む雰囲気中にて、Si3N4
粉末の合成を行なう合成炉において使用する匣鉢、蓋、
台板、レール等のSi3N4粉末合成用道具材の化学成分
が、Al2O395.0％以上、SiO25.0％未満、Fe2O3,Na2O0.30
％未満、CaO0.20％未満、MgO0.10％、TiO2、K2O0.05％
未満であるSi3N4粉末合成用道具材に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing Si 3 N 4 in an atmosphere containing NH 3 or NH 3.
A sagger, a lid, used in a synthesis furnace for synthesizing powder,
The chemical composition of Si 3 N 4 powder synthesis tool materials such as base plates and rails is at least 95.0% Al 2 O 3, less than 5.0% SiO 2 , Fe 2 O 3 , Na 2 O 0.30
%, Less than CaO0.20%, MgO0.10%, TiO 2 , K 2 O0.05%
The present invention relates to a tool material for synthesizing Si 3 N 4 powder which is less than.
［従来の技術］ 従来、NH3雰囲気下で高純度のSi3N4粉末を合成してい
るが、合成炉の道具材例えば匣鉢、蓋、台板、レール等
には不純物の混入あるいはNH3ガスによる浸食の問題か
ら高価なSi3N4製のものを使用している。しかしなが
ら、Si3N4製のものを使用した場合は（匣鉢、蓋、台
板、レール等の道具材にSi3N4製のものを使用した場
合）（１）高価になる。（２）炉のスケールアップ（大
型形状品の製造が困難）が難しい。（３）粉体の吸収す
る熱量より合成炉の道具材例えば匣鉢、蓋、台板、レー
ル等の持ち去る熱量が大きい。即ち熱効率が悪いと言う
問題点があった。[Prior art] Conventionally, high-purity Si 3 N 4 powder has been synthesized in an NH 3 atmosphere. Because of the problem of erosion due to three gases, an expensive one made of Si 3 N 4 is used. However, if was made of Si 3 N 4 (sagger, a lid, a base plate, if was made of Si 3 N 4 on the tool material such as rails) (1) becomes expensive. (2) It is difficult to scale up the furnace (it is difficult to manufacture large-sized products). (3) The amount of heat carried away by the tools of the synthesis furnace, such as the sagger, the lid, the base plate, and the rail, is greater than the amount of heat absorbed by the powder. That is, there is a problem that thermal efficiency is poor.
［発明が解決しようとする課題］ 本発明は上記実情に鑑み、種々検討したところ高純度
のAl2O3質を用いればよいことを見出したものである。
即ちSi3N4合成における道具材として、Al2O395.0％以
上、SiO25.0％未満、Fe2O3,Na2O0.30％未満、CaO0.20％
未満、MgO0.1％、TiO2、K2O0.05％未満である高純度のA
l2O3質を用いればよいことを見出したものである。[Problems to be Solved by the Invention] In view of the above-described circumstances, the present invention has made various studies and found that it is sufficient to use high-purity Al 2 O 3 .
That is, as a tool material in the synthesis of Si 3 N 4 , Al 2 O 3 95.0% or more, SiO 2 less than 5.0%, Fe 2 O 3 , Na 2 O less than 0.30%, CaO 0.20%
Less, MgO0.1%, TiO 2, K 2 is less than O0.05% is pure A
They found that l 2 O 3 quality should be used.
［課題を解決するための手段］ 本発明のAl2O395.0％以上、SiO25.0％未満、Fe2O3,Na
2O0.30％未満、CaO0.20％未満、MgO0.10％、TiO2、K2O
0.05％未満である高純度のAl2O3質の道具材は、炉の構
造を台板構造とした場合には、匣鉢に本発明の高純度の
Al2O3質超軽量材（かさ比重1.0以下）を使用することに
より、蓄熱損失を大幅に低減させることができる。[Means for Solving the Problems] 95.0% or more of Al 2 O 3 and less than 5.0% of SiO 2 of the present invention, Fe 2 O 3 , Na
2 O Less than 0.30%, CaO less than 0.20%, MgO 0.10%, TiO 2 , K 2 O
The high-purity Al 2 O 3 tool material of less than 0.05% is provided with the high-purity Al 2 O 3
By using an Al 2 O 3 ultra-light material (bulk specific gravity 1.0 or less), heat storage loss can be significantly reduced.
また、道具材のAl2O3の純度が95.0％未満の場合は、A
l2O3の道具材とSi3N4の合成粉との接触部において、反
応が起きるため、Si3N4の合成粉の純度が低下する。When the purity of the Al 2 O 3 of the tool is less than 95.0%,
In the contact portion of the synthetic powder of l 2 O 3 of tool material and Si 3 N 4, for the reaction to occur, purity of the synthetic powder the Si 3 N 4 is lowered.
SiO25.0％以上含む場合には、炉内で窒化が進行し、
道具材として十分な強度が保持できなくなる。When SiO 2 contains 5.0% or more, nitriding proceeds in the furnace,
It cannot maintain sufficient strength as a tool material.
また、Fe2O3,Na2O0.30％以上、CaO0.20％以上、MgO0.
10％以上、TiO2、K2O0.05％以上含まれると、Si3N4の合
成粉かFe2O3,CaO,Na2O,TiO2,MgO,K2Oの成分により汚染
されることになる。 Further, Fe 2 O 3, Na 2 O0.30% or more, CaO0.20% or more, MgO0.
10% or more, it is contained TiO 2, K 2 O0.05% or more, Si 3 N synthetic powder or Fe 2 O 3 of 4, CaO, Na 2 O, TiO 2, MgO, contaminated by components of K 2 O Will be.
なお、本発明の道具材は使用前に空焼きをした方が良
いものである。何故なら高純度のAl2O3質といっても、A
l2O3の中にはSi質を含んでいるものがあり、Si質を除か
なければならない。したがって、道具材を使用するとき
は空焼きによって含有するSi質を還元をすることによっ
て不純物の少ないSi3N4粉末を得ることができる。It is preferable that the tool of the present invention be baked before use. Because even if it is high purity Al 2 O 3 quality, A
Some l 2 O 3 contains Si, and the Si must be removed. Therefore, when using a tool material, Si 3 N 4 powder with few impurities can be obtained by reducing the Si content contained by baking.
［実施例］ 次に本発明の実施例について説明する。Example Next, an example of the present invention will be described.
外形の形状が150mm×35mm、内形の形状が134mm×25mm
の材質の匣鉢内にSiO2の原料40gを充填し、三段に重ね
合わせたものを台板に載せ、プッシャー炉にて最高高温
1430℃,NH3の流量10l/min,LPG（プロパンガス）の流量
0.3l/min,で合成を行なった。150mm x 35mm outer shape, 134mm x 25mm inner shape
Of filling the raw material 40g of SiO 2 to Napishtim bowl material, loaded with a superposition on the three stages in the base plate, the maximum high temperature at a pusher furnace
1430 ° C, NH 3 flow rate 10l / min, LPG (propane gas) flow rate
The synthesis was performed at 0.3 l / min.
以下、道具材の化学成分値を示す。本発明の実施例A,
B、比較例C,D,E,F,G,Hおよび従来のSi3N4質道具材の化
学成分値およびかさ比重値を示す。Hereinafter, the chemical component values of the tool materials are shown. Example A of the present invention,
B, Comparative Examples C, D, E, F, G, H, and the chemical component values and bulk specific gravity values of the conventional Si 3 N 4 material are shown.
なお、匣鉢と蓋体とは同一材質で製造し、台板とレー
ルは本発明の実施例Ａと同一な材質のものを使用した。The sagger and the lid were made of the same material, and the base plate and the rail were made of the same material as in Example A of the present invention.
また、成分値は全て％で表わす。 All component values are expressed in%.
上記、成分比の表において T.Oは全酸素の含有量を表わす。 In the above component ratio table, TO represents the total oxygen content.
T.Cは全炭素の含有量を表わす。T.C represents the total carbon content.
以上の表より、本発明の実施例A,BのものはT.O≦2.5
％、T.C≦0.1％、Al≦3500PPm、Fe≦100PPm、Ca≦100PP
m、Mg≦100PPmの純度が満足され、道具材としての十分
な強度を保持することができるものである。From the above table, those of Examples A and B of the present invention have TO ≦ 2.5.
%, TC ≦ 0.1%, Al ≦ 3500PPm, Fe ≦ 100PPm, Ca ≦ 100PP
The purity of m, Mg ≦ 100 PPm is satisfied, and sufficient strength as a tool material can be maintained.
これに対して、比較例C,D,E,F,G,Hのものは、Fe2O3,S
iO2,Na2O,CaO,MgOが多く含量され、道具材（匣鉢）に亀
裂発生を起こすものである。また、ＣのものはFe（不純
物）含入量が多く、満足できる道具材にならない。In contrast, those of Comparative Examples C, D, E, F, G, and H were Fe 2 O 3 , S
It contains iO 2 , Na 2 O, CaO, and MgO in large amounts, and causes cracks in tool materials (saggers). C has a high Fe (impurity) content and is not a satisfactory tool.
［発明の効果］ 本発明は高純度のAl2O3道具材を使用するもので、Si3
N4質に比較して安価であり、大型形状品の製造も容易で
あり、加工もも容易である。そして、NH3ガスによる浸
食が少なく、道具材の強度劣化が小さい。また、台板方
式で匣鉢を高純度のAl2O3質超軽量材とすることで、蓄
熱損失（道具材に熱を奪われる）を低減することができ
る。The present invention [Effect of the Invention] is intended to use high-purity Al 2 O 3 tool material of, Si 3
Less expensive compared to N 4 quality, production of large shaped articles it is easy, machining is also easy. And the erosion by NH 3 gas is small, and the strength deterioration of the tool material is small. In addition, heat storage loss (heat is taken away by the tool material) can be reduced by using a high-purity Al 2 O 3 quality ultralight material for the sagger in the base plate method.
Claims (1)
4粉末の合成を行なう合成炉における匣鉢、蓋、台板、
レール等のSi3N4粉末合成用道具材の化学成分が、Al2O3
95.0％以上、SiO25.0％未満、Fe2O3,Na2O0.30％未満、C
aO0.20％未満、MgO0.10％、TiO2、K2O0.05％未満である
ことを特徴とするSi3N4粉末合成用道具材(1) Si 3 N in an NH 3 or an atmosphere containing NH 3 ;
Sagger in the synthesis reactor for performing 4 powder synthesis, the lid, the base plate,
The chemical composition of the tool material for synthesis of Si 3 N 4 powder such as rails is Al 2 O 3
95.0% or more, SiO 2 less than 5.0%, Fe 2 O 3 , Na 2 O less than 0.30%, C
Tool material for Si 3 N 4 powder synthesis characterized by having aO of less than 0.20%, MgO of 0.10%, TiO 2 and K 2 O of less than 0.05%
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63328354A JP2581787B2 (en) | 1988-12-26 | 1988-12-26 | Si 3 lower N 4 lower 4 Tools for powder synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63328354A JP2581787B2 (en) | 1988-12-26 | 1988-12-26 | Si 3 lower N 4 lower 4 Tools for powder synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02172858A JPH02172858A (en) | 1990-07-04 |
| JP2581787B2 true JP2581787B2 (en) | 1997-02-12 |
Family
ID=18209308
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63328354A Expired - Lifetime JP2581787B2 (en) | 1988-12-26 | 1988-12-26 | Si 3 lower N 4 lower 4 Tools for powder synthesis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2581787B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100361113B1 (en) * | 1994-08-18 | 2003-02-05 | 닛뽕도구슈우도오교오가부시끼가이샤 | Alumina-based sintered material for ceramic heater |
| CN113461354B (en) * | 2021-07-01 | 2022-05-17 | 中南大学 | Si with function of improving microwave absorption performance of asphalt concrete pavement3N4Preparation method and application of/Fe composite powder |
-
1988
- 1988-12-26 JP JP63328354A patent/JP2581787B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02172858A (en) | 1990-07-04 |
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