JPH08119744A - Production of silicon nitride sintered compact - Google Patents
Production of silicon nitride sintered compactInfo
- Publication number
- JPH08119744A JPH08119744A JP6274232A JP27423294A JPH08119744A JP H08119744 A JPH08119744 A JP H08119744A JP 6274232 A JP6274232 A JP 6274232A JP 27423294 A JP27423294 A JP 27423294A JP H08119744 A JPH08119744 A JP H08119744A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- silicon nitride
- sintered compact
- sintered body
- gas
- 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
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 25
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052786 argon Inorganic materials 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000003825 pressing Methods 0.000 abstract 3
- 230000002706 hydrostatic effect Effects 0.000 abstract 2
- 229910018404 Al2 O3 Inorganic materials 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- -1 argon gas Chemical compound 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001513 hot isostatic pressing Methods 0.000 description 7
- 239000002609 medium Substances 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002245 particle 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6587—Influencing the atmosphere by vaporising a solid material, e.g. by using a burying of sacrificial powder
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、窒化けい素焼結体の製
造方法に関し、特に、鏡面研磨により極めて平滑な表面
が得られる窒化けい素焼結体の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silicon nitride sintered body, and more particularly, to a method for producing a silicon nitride sintered body which can obtain an extremely smooth surface by mirror polishing.
【０００２】[0002]
【従来の技術】窒化けい素焼結体は、機械的強度、硬
度、耐熱性に優れているとともに剛性が高く熱膨張係数
も小さいことから、金属圧延ロール、工業用ミラー、成
形用型等の材料に使用することが検討されている。窒化
けい素焼結体をこれらの用途に用いる場合、研磨した焼
結体の表面が欠陥のない、言い換えれば研磨表面が極め
て平滑な焼結体とすることが要求されている。2. Description of the Related Art A silicon nitride sintered body is excellent in mechanical strength, hardness and heat resistance and has high rigidity and a small coefficient of thermal expansion, so that it is used as a material for metal rolling rolls, industrial mirrors, molding dies, etc. Is being considered for use. When the silicon nitride sintered body is used for these purposes, it is required that the surface of the polished sintered body is free of defects, that is, the polished surface is extremely smooth.
【０００３】これら工業用ミラー、成形用型等の材料に
検討されている窒化けい素焼結体の製造は、一般に、窒
化けい素粉末にＹ2Ｏ3、Ａｌ2Ｏ3、ＭｇＯ等の焼結助剤
を添加し常圧焼結した後、さらに、圧媒ガスとして高圧
の窒素ガスを用いて熱間静水圧加圧（ＨＩＰ）処理する
ことにより、焼結体に残存したポアを低減して研磨表面
を平滑とする製造方法が採られている。The production of a silicon nitride sintered body, which has been studied as a material for these industrial mirrors, molding dies, etc., is generally carried out by sintering Y 2 O 3 , Al 2 O 3 , MgO or the like into silicon nitride powder. After adding an auxiliary agent and performing normal pressure sintering, hot isostatic pressing (HIP) treatment is further performed using high pressure nitrogen gas as a pressure medium gas to reduce pores remaining in the sintered body. A manufacturing method is adopted in which the polished surface is smooth.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、従来の
方法で製造された焼結体では、焼結体中のポアは低減さ
れたものの、研磨表面の平滑性が、金属圧延ロール、工
業用ミラー、成形用型等に使用するにはまだ不充分であ
った。However, in the sintered body manufactured by the conventional method, although the pores in the sintered body were reduced, the smoothness of the polished surface was improved by metal rolling rolls, industrial mirrors, It was still insufficient for use as a molding die.
【０００５】本発明は、上述した従来の窒化けい素焼結
体の製造方法が有する課題に鑑みなされたものであっ
て、その目的は、工業用ミラー、成形用型等に使用でき
る極めて平滑な研磨表面が得られる窒化けい素焼結体の
製造方法を提供することにある。The present invention has been made in view of the problems of the above-described conventional method for producing a silicon nitride sintered body, and its purpose is to provide an extremely smooth polishing that can be used for industrial mirrors, molding dies and the like. It is an object of the present invention to provide a method for producing a silicon nitride sintered body having a surface.
【０００６】[0006]
【課題を解決するための手段】本発明者等は、上記目的
を達成するため鋭意研究した結果、常圧焼結した後、そ
の焼結体を、窒化けい素などの粉末中に埋設し、窒素以
外の圧媒ガスを用いてさらにＨＩＰ処理すれば、得られ
た焼結体の研磨表面の平滑性は、大幅に改善されるとの
知見を得て本発明を完成した。Means for Solving the Problems The inventors of the present invention have conducted extensive studies to achieve the above object, and as a result, after pressureless sintering, the sintered body was embedded in powder such as silicon nitride, The present invention has been completed based on the finding that the smoothness of the polished surface of the obtained sintered body is significantly improved by further HIP treatment using a pressure medium gas other than nitrogen.
【０００７】上記圧媒ガスとして、窒素ガス以外のガス
を用いるのは、窒素ガスによりＨＩＰ処理すると、焼結
体に色むらを伴う変質相を生じ、この変質相が研磨した
ときの平滑性を低下させることによる。この変質相は、
高圧の窒素が焼結体中に侵入し、焼結体中の成分と反応
して生じるものと考えられ、焼結体中の成分と反応しな
い窒素ガス以外の不活性ガスを用いれば変質相が生成し
ないので、その結果、均質な焼結体となり、表面平滑性
が向上するものと思われる。As the pressure medium gas, a gas other than nitrogen gas is used. When the HIP process is performed with nitrogen gas, an altered phase with uneven color is generated in the sintered body, and the altered phase shows smoothness when polished. By lowering. This alteration phase is
It is considered that high-pressure nitrogen penetrates into the sintered body and reacts with the components in the sintered body, and if an inert gas other than nitrogen gas that does not react with the components in the sintered body is used, the altered phase Since it does not form, it is considered that as a result, a homogeneous sintered body is obtained and the surface smoothness is improved.
【０００８】また、常圧焼結した焼結体を窒化けい素な
どの粉末中に埋設するのは、圧媒ガスに窒素ガスを使わ
ないため、焼結体表面近傍の成分が一部分解、揮散して
焼結体表面がポーラスとなるので、これらの粉末で覆っ
て分解、揮散を抑えるのである。これに使用する粉末と
しては、焼結体と同じ成分を持つ窒化けい素（Ｓｉ
3Ｎ4）粉末は勿論、その他酸化けい素（ＳｉＯ2）粉
末、あるいはこれらの混合粉末が挙げられる。さらにこ
れらの粉末に炭素質（Ｃ）粉末を加えたものも有効であ
る。Further, the reason why the pressure-sintered sintered body is embedded in powder such as silicon nitride is that nitrogen gas is not used as a pressure medium gas, so that some components near the surface of the sintered body are decomposed and volatilized. Then, since the surface of the sintered body becomes porous, it is covered with these powders to suppress decomposition and volatilization. The powder used for this is silicon nitride (Si
Not only 3 N 4 ) powder but also other silicon oxide (SiO 2 ) powder, or a mixed powder thereof. Further, those obtained by adding carbonaceous (C) powder to these powders are also effective.
【０００９】以下、本発明をさらに詳細に述べると、先
ず窒化けい素粉末に焼結助剤としてＹ2Ｏ3、Ａｌ2Ｏ3、
ＭｇＯ等を添加して慣用の方法で混合、成形し、その成
形体を窒素ガス中で慣用の方法で常圧焼結する。常圧焼
結した焼結体を、窒化けい素粉末、または酸化けい素粉
末、あるいは窒化けい素と酸化けい素の混合粉末、若し
くはこれらの粉末に炭素質粉末を加えた粉末中に埋設す
る。The present invention will be described in more detail below. First, Y 2 O 3 , Al 2 O 3 , and
MgO and the like are added and mixed and molded by a conventional method, and the molded body is sintered under normal pressure in nitrogen gas under a normal pressure. The pressure-sintered sintered body is embedded in a silicon nitride powder, a silicon oxide powder, a mixed powder of silicon nitride and silicon oxide, or a powder obtained by adding a carbonaceous powder to these powders.
【００１０】粉末中に埋設した焼結体を、圧媒ガスとし
て従来の窒素ガスでなく、例えば不活性ガスであるアル
ゴン（Ａｒ）ガスなどを用いてさらにＨＩＰ処理するこ
とによって、研磨表面が極めて平滑な焼結体を製造する
ことができる。The sintered surface embedded in the powder is further subjected to HIP treatment by using, for example, an inert gas such as argon (Ar) gas as a pressure medium gas instead of the conventional nitrogen gas, and thereby the polished surface is extremely polished. A smooth sintered body can be manufactured.
【００１１】[0011]
【実施例】以下、本発明の実施例を比較例と共に挙げ、
本発明をより詳細に説明する。EXAMPLES Examples of the present invention will be given below together with comparative examples.
The present invention will be described in more detail.
【００１２】（実施例１〜８） （１）常圧焼結 原料として平均粒径が０．７μｍのα型窒化けい素粉末
に、５重量％のＹ2Ｏ3粉末、および５重量％のＡｌ2Ｏ3
粉末を加え、メタノールを分散媒としてポットミルで混
合後乾燥した。この粉末をプレス成形して縦５０ｍｍ、
横３５ｍｍ、厚さ１０ｍｍの成形体を作製した。この成
形体を窒素ガス中で１７００℃の温度で３時間焼成し
た。Examples 1 to 8 (1) Pressureless Sintering As raw materials, α-type silicon nitride powder having an average particle size of 0.7 μm was added to 5 wt% Y 2 O 3 powder, and 5 wt%. Al 2 O 3
The powder was added, mixed with a pot mill using methanol as a dispersion medium, and then dried. This powder is press-formed into a length of 50 mm,
A molded body having a width of 35 mm and a thickness of 10 mm was produced. The compact was fired in nitrogen gas at a temperature of 1700 ° C. for 3 hours.
【００１３】（２）加圧焼結 得られた焼結体を、表１に示す割合に調製した粉末中に
埋設し、アルゴンガス中で１５００ｋｇ／ｃｍ2の圧力
で、表１に示す温度でＨＩＰ処理した。(2) Pressure Sintering The obtained sintered body was embedded in the powder prepared in the proportions shown in Table 1, at a pressure of 1500 kg / cm 2 in argon gas, and at the temperature shown in Table 1. HIP treated.
【００１４】（３）表面仕上げ 得られた焼結体の表面を、平面研削し、ラッピングした
後、粒径が１μｍのダイアモンド砥粒でポリッシングし
て表面仕上げした。(3) Surface Finishing The surface of the obtained sintered body was surface-ground and lapped, and then surface-finished by polishing with diamond abrasive grains having a grain size of 1 μm.
【００１５】（４）評価 表面仕上げした表面の表面粗さを、表面粗さ計により測
定した。その結果を表１に示す。(4) Evaluation The surface roughness of the surface-finished surface was measured by a surface roughness meter. Table 1 shows the results.
【００１６】（比較例１〜４）比較のために、実施例と
同じ原料を用いて実施例と同じ方法で常圧焼結した。そ
の焼結体を、表１に示す粉末中に埋設し、実施例と同じ
圧力の窒素ガス中で、表１に示す温度でＨＩＰ処理した
（比較例１）。また、粉末中に埋設せずに実施例と同じ
圧力のアルゴン、または窒素ガス中で、表１に示す温度
でＨＩＰ処理した（比較例２〜４）。(Comparative Examples 1 to 4) For comparison, the same raw materials as in Example were used and pressureless sintering was performed in the same manner as in Example. The sintered body was embedded in the powder shown in Table 1 and subjected to HIP treatment at a temperature shown in Table 1 in a nitrogen gas having the same pressure as that of the example (Comparative Example 1). Further, HIP treatment was performed at a temperature shown in Table 1 in argon or nitrogen gas having the same pressure as that of the example without embedding in the powder (Comparative Examples 2 to 4).
【００１７】得られた焼結体を実施例と同じ方法で表面
仕上げし、評価した。その結果を表１に示す。The obtained sintered body was surface-finished and evaluated in the same manner as in the examples. Table 1 shows the results.
【００１８】[0018]
【表１】 [Table 1]
【００１９】表１から明らかなように、実施例１〜８に
おいては、研磨した表面の表面粗さは、Ｒｍａｘで１
９．１ｎｍ以下と非常に平滑な表面となっている。As is clear from Table 1, in Examples 1 to 8, the surface roughness of the polished surface was 1 at Rmax.
It has a very smooth surface of 9.1 nm or less.
【００２０】これに対して加圧焼結を本発明の範囲外、
即ち、窒素ガス中では、焼結体を粉末中に埋設してもＲ
ｍａｘがかなり大きくなっており（比較例１）、また、
アルゴンガス中でも、焼結体を粉末中に埋設しないとや
はり平滑性が悪くなっている（比較例２）。一方、従来
の方法で製造した焼結体の平滑性も本発明の実施例より
明らかに良くなく（比較例３）、また、その処理温度を
高くしても実施例にみられるほどには平滑にはならない
結果となっている（比較例４）。On the other hand, pressure sintering is outside the scope of the present invention,
That is, in nitrogen gas, even if the sintered body is embedded in the powder, R
max is considerably large (Comparative Example 1),
Even in the argon gas, the smoothness is poor unless the sintered body is embedded in the powder (Comparative Example 2). On the other hand, the smoothness of the sintered body produced by the conventional method is obviously not better than that of the example of the present invention (Comparative Example 3), and even if the treatment temperature is increased, it is as smooth as that of the example. The result does not satisfy (Comparative Example 4).
【００２１】[0021]
【発明の効果】本発明の方法で窒化けい素焼結体を製造
することにより、研磨した表面が極めて平滑な焼結体を
得ることができた。これにより、金属圧延ロール、工業
用ミラー、成形用型等に使用可能な材料として提供する
ことができるようになった。EFFECTS OF THE INVENTION By producing a silicon nitride sintered body by the method of the present invention, it was possible to obtain a sintered body having an extremely smooth polished surface. As a result, it can be provided as a material that can be used for metal rolling rolls, industrial mirrors, molding dies, and the like.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０４Ｂ 35/64 ３０２ Ｚ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI technical display location C04B 35/64 302 Z
Claims (1)
圧焼結した後、さらに加圧焼結する窒化けい素焼結体の
製造方法において、該加圧焼結する方法が、常圧焼結し
た焼結体を、窒化けい素および／または酸化けい素の粉
末中に、またはそれらに炭素質粉末を加えた粉末中に埋
設し、圧媒ガスに窒素以外の不活性ガスを用いて熱間靜
水圧加圧処理するものであることを特徴とする窒化けい
素焼結体の製造方法。1. A method for producing a silicon nitride sintered body, which comprises mixing raw materials, molding the mixture, sintering the compact under normal pressure, and further sintering under pressure. The pressure-sintered sintered body is embedded in a powder of silicon nitride and / or silicon oxide or a powder obtained by adding a carbonaceous powder to the powder, and an inert gas other than nitrogen is used as the pressure medium gas. A method for manufacturing a silicon nitride sintered body, characterized in that the hot-hydraulic pressure treatment is performed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6274232A JPH08119744A (en) | 1994-10-14 | 1994-10-14 | Production of silicon nitride sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6274232A JPH08119744A (en) | 1994-10-14 | 1994-10-14 | Production of silicon nitride sintered compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08119744A true JPH08119744A (en) | 1996-05-14 |
Family
ID=17538855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6274232A Pending JPH08119744A (en) | 1994-10-14 | 1994-10-14 | Production of silicon nitride sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08119744A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209725A (en) * | 2020-10-15 | 2021-01-12 | 郑州航空工业管理学院 | Pretreatment method for sintering silicon nitride ceramic, silicon nitride ceramic and preparation method thereof |
-
1994
- 1994-10-14 JP JP6274232A patent/JPH08119744A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209725A (en) * | 2020-10-15 | 2021-01-12 | 郑州航空工业管理学院 | Pretreatment method for sintering silicon nitride ceramic, silicon nitride ceramic and preparation method thereof |
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