JPS63151681A - Manufacture of silicon nitride sintered body - Google Patents
Manufacture of silicon nitride sintered bodyInfo
- Publication number
- JPS63151681A JPS63151681A JP61297535A JP29753586A JPS63151681A JP S63151681 A JPS63151681 A JP S63151681A JP 61297535 A JP61297535 A JP 61297535A JP 29753586 A JP29753586 A JP 29753586A JP S63151681 A JPS63151681 A JP S63151681A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- silicon nitride
- sintering
- nitride sintered
- manufacture
- 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.)
- Granted
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 8
- 238000005245 sintering Methods 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 4
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052839 forsterite Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 239000013065 commercial product Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 229910052634 enstatite Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910005091 Si3N Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- -1 automobile parts Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007582 slurry-cast process Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は窒化けい素（Ｂ１３Ｎ４ ）焼結体の製造方法
に関し、さらに評しくに、特に肉厚品の焼結性に優れ、
しかもその焼結体内部に色ムラがなく均一でかつ表面に
商品価値を損なう亀の子状模様が見られない焼結体の製
造方法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 a silicon nitride (B13N4) sintered body, and more particularly, it has excellent sinterability especially for thick-walled products,
Moreover, the present invention relates to a method for producing a sintered body which has uniform color without unevenness inside the sintered body and has no tortoise-like pattern on the surface which impairs commercial value.
最近に至り、窒化けい素焼結体は耐熱性、耐熱衝撃性、
耐食性及び…摩耗性に優れているために、自動車部品、
ガスタービン用部材、ノズルやベアリング等の用途に利
用されつつある。Recently, silicon nitride sintered bodies have improved heat resistance, thermal shock resistance,
Due to its excellent corrosion resistance and wear resistance, it is used in automobile parts,
It is being used for gas turbine parts, nozzles, bearings, and other applications.
従来、自動車部品、ガスタービン部材あるいはノズル等
の大型でしかも複雑形状の製品に用いる窒化けい素焼結
体を生産性よく製造する方法としてはＭｇＯ％ Ａｌ２
Ｏ３、Ｙ２Ｏ３等の適当な酸化’ｓｒ焼結助剤に用い、
所定形状に底形した後、非酸化性雰囲気下で焼結する、
いわゆる液相焼結を利用し次常圧焼結法（％公昭５２−
３６４７号公報）や雰囲気加圧焼結法°（％開昭５２−
４７０１５号公報）等が知られている。しかし、これら
の技術では肉厚品の焼結においては、８１３Ｎ４焼結体
の内部は表面に比べ焼結の遅れがあり特に肉厚が太きく
なる程、その傾向か見られ、歪の発生原因となりクラッ
クが発生したり、又不拘−な焼結による内部の色ムラ會
発生する等の欠点がある。Conventionally, MgO% Al2 has been used as a method for manufacturing silicon nitride sintered bodies with high productivity for use in large and complex-shaped products such as automobile parts, gas turbine parts, and nozzles.
Appropriate oxidation 'sr sintering aids such as O3, Y2O3, etc.
After shaping the bottom into a predetermined shape, it is sintered in a non-oxidizing atmosphere.
Using the so-called liquid phase sintering, the next pressureless sintering method (% Kosho 52-
3647 Publication) and atmospheric pressure sintering method
47015) etc. are known. However, with these techniques, when sintering thick-walled products, the interior of the 813N4 sintered body sinters slower than the surface, and this tendency is seen especially as the wall thickness increases, and this is the cause of distortion. This leads to drawbacks such as cracks occurring and internal color unevenness due to unrestricted sintering.
本発明は上記従来技術の問題点を解決するために鋭意研
究しｔ結果、児５ｙ、され友ものであって、８１３Ｎ、
焼結体の製造方法において、署しく焼結性が向上し、肉
厚品の焼結性に優れしかもｆｉ結体内部に色ムラのない
かつ表面に商品価値ケ損なう様な亀の子状模様の見られ
ないＳｉ３Ｎ、焼結体の製造方法を提供するものである
。The present invention has been made as a result of extensive research to solve the problems of the prior art, and is based on
In the manufacturing method of the sintered body, the sinterability is significantly improved, the sinterability of thick-walled products is excellent, and there is no uneven color inside the fi body, and the surface has a tortoise-like pattern that does not damage the commercial value. The present invention provides a method for manufacturing a sintered body of Si3N in which no sintered body is observed.
即ち、本発明は、フォルステライト（Ｍｇ２５１０４）
及び／又にステアタイト（Ｍｇ５ｉＯｓ ） １〜１２
重−１ｉｒ受、ＺｒＯ２ｉ〜５１量％及び残部が実質的
にＳｉ３Ｎ４からなる混合粉末ｈｉ形後非酸化性雰囲気
下で焼結することに％徴とする窒化けい素焼粘体の製造
方法である。That is, the present invention provides forsterite (Mg25104)
and/or steatite (Mg5iOs) 1-12
This is a method for producing a silicon nitride sintered viscous body, in which a mixed powder hi-form consisting of ~51% by weight of ZrO2i and the remainder substantially Si3N4 is sintered in a non-oxidizing atmosphere.
以下、本発明の内容ｋＰ細に説明する。Hereinafter, the contents of the present invention will be explained in detail.
本発明において用いる混合粉末はＭｇ２５１０４、Ｍｇ
５１ｏ３、ＺｒＱ２及び残ｉ：６”実’ＪｌｅＦＩＫＳ
ｉ３Ｎ４からなるものである。The mixed powder used in the present invention is Mg25104, Mg
51o3, ZrQ2 and remaining i: 6" real 'JleFIKS
It consists of i3N4.
こごで混合粉末中の廟２８１０４ 、ＭｇＳｉＯ３の含
有量は、それぞれ単独又は合計で１〜１２重量％である
。１１量噛未勇では焼結体の緻密化が央餉的に困難であ
るし、また、１２重量％ｒ超えると焼結体の高温強度が
低下する傾向があるので好ましくない。１友、ＭｇＯ／
８１０２モル比は、同様な理由により２〜１．１とす
るのが好ｌしい。Ｍｇ、；Ｊ１０４とＭｇＳｉＯ３はい
ずれも市販品が使用できる。The content of 28104 and MgSiO3 in the mixed powder is 1 to 12% by weight, either individually or in total. If the content is 11% by weight, it is difficult to make the sintered body dense, and if it exceeds 12% by weight, the high temperature strength of the sintered body tends to decrease, which is not preferable. 1 friend, MgO/
The molar ratio of 8102 is preferably 2 to 1.1 for the same reason. Commercially available products can be used for both Mg; J104 and MgSiO3.
次に、ＺｒＱ２の含１ｉｒｔｆ１１〜５！ｆｃ４ｒ６る
。Next, ZrQ2 contains 1irtf11~5! fc4r6ru.
１１飯％未満では焼結体表面に亀の子状模様が現われる
ので好筐しくない。ｆた、ｓＴＬ魚％を超えると、焼結
体の高温強度が低下する順回がある。If the content is less than 11%, a tortoise-like pattern will appear on the surface of the sintered body, making the case unfavorable. However, if the sTL weight ratio is exceeded, the high temperature strength of the sintered body will tend to decrease.
尚 ＺｒＱ２ ｈ単斜晶系、ＰＳＺ （部分安定化Ｚｒ
Ｏ２）等が使用できる。Furthermore, ZrQ2 h monoclinic system, PSZ (partially stabilized Zr
O2) etc. can be used.
以上説明し７ｊＭｇ２８１０．、Ｍｇ５ｉ○３、ＺｒＱ
２ ｂ外の残部は実質的に８１３Ｎ、であることが好ま
しい。ここで原料不純物や混合粉砕時に混入する８１０
２等の不可避的成分も包含する。具体的に用いるＳｉ３
Ｎ、はα相分を主体とする８１３Ｎ４が好１しく、その
含有ｍに５０′Ｍ童係以上、より好１しくは７０ｉ！ｉ
ｔ％以上がよい。α相含Ｍ量が５０ｉ＆負弧未満では焼
結過程におけるα相からβ相への転移の際に生成する長
柱状結晶の焼結体中に占める割合が少なくなり、強度が
低下する傾向がある。As explained above, 7jMg2810. , Mg5i○3, ZrQ
Preferably, the remainder other than 2b is substantially 813N. Here, raw material impurities and 810 mixed during mixing and pulverization
It also includes unavoidable components such as No. 2. Specifically used Si3
N is preferably 813N4 which is mainly composed of α phase, and its content m is 50'M or more, more preferably 70i! i
t% or more is preferable. When the α phase M content is less than 50i & negative arc, the proportion of long columnar crystals generated during the transition from α phase to β phase in the sintering process in the sintered body decreases, and the strength tends to decrease. .
本発明による８１３Ｎ４焼結体展品は、表面全体に褐色
を呈しているが、それケ脱色しようとする徊合には８０
０〜１０００°Ｃで２０〜６０分加熱すれはよい。尚、
褐色になる身回は焼結体表面のＺｒＱに帰因するものと
考えられる。The 813N4 sintered body exhibited according to the present invention has a brown color on the entire surface, but it is difficult to remove the color by 813N4.
It is best to heat it at 0-1000°C for 20-60 minutes. still,
The brown color is thought to be due to ZrQ on the surface of the sintered body.
焼結助剤であるＭｇ２８１０４及び／又はＭｇＳ ｉＯ
３とｚｒｃ）２及び上配し７’ＣＳ ｉ ３Ｎ ４粉末
％を混合【する場合には特に限定する必要もなく、公知
の例えはボールミル混合等で実施できる。Sintering aid Mg28104 and/or MgS iO
In the case of mixing 3 and zrc) 2 and the superposition 7'CS i 3N 4 powder%, there is no particular limitation and it can be carried out by known methods such as ball mill mixing.
成形方法については、金型プレス成形、Ｃ工Ｐ成形、押
出し成形、泥漿鋳込成形、射出成形等の成形手段の中か
ら適宜製造しようとする製品の形状に合せて選択するこ
とができる。The molding method can be selected from mold press molding, C/P molding, extrusion molding, slurry casting molding, injection molding, etc. according to the shape of the product to be manufactured.
成形体の焼結については、非酸化性雰囲気下、より好ま
しくは０．６ Ｉｃｇ／ ａｎ”以上の窒素ガス雰囲気
下で行うが、その際の詰粉としては、例えは成形体と同
一組成に近い焼結助剤とＳｉ３Ｎ、とＢＮの混会粉禾等
ｒ便用する。The compact is sintered in a non-oxidizing atmosphere, more preferably in a nitrogen gas atmosphere of 0.6 Icg/an'' or higher. A mixed powder of similar sintering aids, Si3N, and BN is used.
焼結時の焼結温度は１６５０〜１７５０°Ｃの温度が好
ましく、該龜反において、適宜の焼結時間が選択さ几る
。焼結温度か１６５０°Ｃ未満では焼結に要する時間が
長くなゐし、１７５０°Ｃｋ超えると８１．Ｎ、焼結体
の一部が分解し均一な焼結体を得難い傾向がある。The sintering temperature during sintering is preferably 1650 to 1750°C, and an appropriate sintering time is selected depending on the temperature. If the sintering temperature is less than 1650°C, the time required for sintering will be longer, and if it exceeds 1750°C, the time will be 81. When using N, a part of the sintered body tends to decompose, making it difficult to obtain a uniform sintered body.
なお、焼結方法についてに、常圧焼結（ＰＬＳ ）に限
定するものではなく、焼結体の形状、目的物性に応じて
、ホットプレス（ＨＰ）、ｒ！Ｐ！間静水圧プレス（Ｈ
工Ｐ ）等が適宜選択できるが常圧焼結方法を採用すれ
ば生産性において有利である。The sintering method is not limited to pressureless sintering (PLS), but may be hot press (HP), r! P! Hydrostatic press (H
Process P) etc. can be selected as appropriate, but it is advantageous in terms of productivity if the pressureless sintering method is adopted.
次に、本発明を実施例、比較例孕あげ、ざらに具体的に
説明する。Next, the present invention will be explained in detail with examples and comparative examples.
８１３Ｎ、粉末（平均粒径０．７３ μｍ％ α相９０
重！ｔ％）及びＭｇ２５１０４（市販品を粉砕し友もの
、平均粒径１．２μｒＩＬ）、ＭｇＳｉＯ３（市販品ｋ
粉砕し＊ ％の、平均粒径１．３／ＪｒＩＬ）、Ｚｒ
Ｑ２（市販品、平均粒径２μｍ）、Ｍｇｏ （市販品、
平均粒径０．３ μ７７１ ）及びＳ’０２ （日本ア
エロジル社製、商品名「アエロジル」）の焼結助剤を表
に示す組成で混合してなる混合粉末に１．１．１トリク
ロルエタン（商品名「クロロセン」）を加えてボールミ
ルでＩ Ｈｒ湿式混合し、乾燥後、ゴム型に充填し２０
００幻／ｃ１ｒＬ２の成形圧でＣ工Ｐ成形し円柱状成形
体を得几。813N, powder (average particle size 0.73 μm% α phase 90
Heavy! t%), Mg25104 (commercial product crushed, average particle size 1.2μrIL), MgSiO3 (commercial product k
Grinded*%, average particle size 1.3/JrIL), Zr
Q2 (commercial product, average particle size 2 μm), Mgo (commercial product,
1.1.1 trichloroethane ( (trade name "Chlorocene") was added and wet mixed in a ball mill for 1 hour. After drying, it was filled into a rubber mold and mixed for 20 hours.
A cylindrical molded product was obtained by C/P molding at a molding pressure of 00 phantom/c1rL2.
尚、原料の粒度はマイクロトラック粒度分布計（Ｎ＆Ｉ
、社製）上用いて測定した。The particle size of the raw material was measured using a Microtrac particle size distribution meter (N&I
(manufactured by, Inc.).
朋φ 轟富り
次に、この成形体ｖ１００ Ｘ６０ 形状に切
断しグリーン成形体とし、これ七カーボンルツざにセッ
トし各側にて用いる焼結助剤を含ＣＢ Ｎ −Ｅ１１３
Ｎ４系詰粉で取形体會慎って０．６１０９７σ２の窒素
ガス雰囲気下で１７００°Ｃにて１０時間焼成して焼結
体を製造した。次にこの焼結体の気孔高音測定した後、
焼結体ｔダイヤモンドカッターで切断し曲げ強度試片を
切出しｔ０焼結体断面の色ムラ及び焼結体表面の亀の子
状模様の有無について肉眼で観察を行つ友後曲げ強度ケ
測定した。Next, this molded body was cut into a shape of v100 x 60 to form a green molded body, and this was set on a seven-carbon crucible, and the sintering aid used on each side was added to CB N -E113.
The shaped body was packed with N4-based packing powder and fired at 1700°C for 10 hours in a nitrogen gas atmosphere of 0.61097σ2 to produce a sintered body. Next, after measuring the pore treble of this sintered body,
The sintered body was cut with a diamond cutter and a bending strength specimen was cut out, and the bending strength was measured by observing with the naked eye the uneven color of the cross section of the sintered body and the presence or absence of a tortoise-like pattern on the surface of the sintered body. .
気孔率は：Ｊより ２２０５に準拠した方法で測定した
かさ比重′に原料配合基準の理論密度で除し１から減じ
１００に掛けることによって求め友。The porosity is determined by dividing the bulk specific gravity measured in accordance with J. 2205 by the theoretical density based on the raw material composition, subtracting it from 1, and multiplying it by 100.
切り出した曲げ強度試片はＪ工８Ｒ１６０１に準拠して
研削加工し室温にて６点曲げ法により強度測定會行なつ
几。The cut-out bending strength specimens were ground according to J-8R1601, and the strength was measured using the 6-point bending method at room temperature.
以上、物性の測定及び肉眼観察の結果’（ＩＩ”表に示
す。The results of measurements of physical properties and visual observation are shown in Table '(II)'.
表から本発明の実施例は比較に比べて緻密で高強度であ
り表面に亀、の子状模様がなくかつ内部に色ムラのない
均一な肉厚形状の窒化けい素焼結体が得られることがわ
かる。From the table, it can be seen that the examples of the present invention are denser and have higher strength than the comparison, and a silicon nitride sintered body with a uniform thickness and a uniform thickness without any tortoise-like or granite-like patterns on the surface and no uneven color inside can be obtained. I understand.
以下余白
〔発明の効果〕
本発明によれば、商品価値を損なうような、亀の子状模
様が表面になく、しかも焼結体内部にに色ムラもなく、
均一で筒強度な肉厚の窒化けい素焼結体ケ製造すること
ができる。The following margins [Effects of the Invention] According to the present invention, there is no tortoise-like pattern on the surface that impairs commercial value, and there is no uneven color inside the sintered body.
It is possible to manufacture silicon nitride sintered bodies with uniform wall thickness and cylindrical strength.
Claims (1)
又はステアタイト（ＭｇＳｉＯ＿３）１〜１２重量％、
ＺｒＯ＿２１〜５重量％及び残部が実質的にＳｉ＿３Ｎ
＿４からなる混合粉末を成形後非酸化雰囲気下で焼結す
ることを特徴とする窒化けい素焼結体の製造方法。(1) Forsterite (Mg_2SiO_4) and/
or steatite (MgSiO_3) 1 to 12% by weight,
ZrO_21-5% by weight and the balance substantially Si_3N
A method for producing a silicon nitride sintered body, which comprises sintering a mixed powder of _4 in a non-oxidizing atmosphere after molding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61297535A JPH075387B2 (en) | 1986-12-16 | 1986-12-16 | Method for manufacturing silicon nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61297535A JPH075387B2 (en) | 1986-12-16 | 1986-12-16 | Method for manufacturing silicon nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63151681A true JPS63151681A (en) | 1988-06-24 |
| JPH075387B2 JPH075387B2 (en) | 1995-01-25 |
Family
ID=17847793
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61297535A Expired - Fee Related JPH075387B2 (en) | 1986-12-16 | 1986-12-16 | Method for manufacturing silicon nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH075387B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02172866A (en) * | 1988-12-26 | 1990-07-04 | Ngk Spark Plug Co Ltd | Silicon nitride sintered body |
| US5110772A (en) * | 1990-08-30 | 1992-05-05 | W. R. Grace & Co.-Conn. | Fabrication of dense SI3 N4 ceramics using CaO-TiO2 SiO.sub.2 |
| JP2006290709A (en) * | 2005-04-14 | 2006-10-26 | Nippon Steel Corp | Silicon nitride material and its manufacturing method |
-
1986
- 1986-12-16 JP JP61297535A patent/JPH075387B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02172866A (en) * | 1988-12-26 | 1990-07-04 | Ngk Spark Plug Co Ltd | Silicon nitride sintered body |
| US5110772A (en) * | 1990-08-30 | 1992-05-05 | W. R. Grace & Co.-Conn. | Fabrication of dense SI3 N4 ceramics using CaO-TiO2 SiO.sub.2 |
| JP2006290709A (en) * | 2005-04-14 | 2006-10-26 | Nippon Steel Corp | Silicon nitride material and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH075387B2 (en) | 1995-01-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |