JP4091753B2 - Method for producing silicon nitride strip - Google Patents
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- JP4091753B2 JP4091753B2 JP2001175658A JP2001175658A JP4091753B2 JP 4091753 B2 JP4091753 B2 JP 4091753B2 JP 2001175658 A JP2001175658 A JP 2001175658A JP 2001175658 A JP2001175658 A JP 2001175658A JP 4091753 B2 JP4091753 B2 JP 4091753B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、直動軸受用レール等の厳しい真直度が要求される窒化珪素製細長物の製造方法に関する。特に詳しくは、焼成時に反りが発生しやすい直動軸受用レール等の窒化珪素製細長物について、焼成後に所定の加熱処理を施して反りを矯正する窒化珪素製細長物の製造方法に関するものである。
【０００２】
【従来の技術】
従来から、直動軸受用レールや、軸、熱電対保護管などのセラミック製細長物に対し、寸法精度の良好なものが望まれている。
【０００３】
上記のセラミック製細長物は、焼成時に反りが発生しやすく、寸法精度に狂いが生じることが多い。反りの原因としては、焼成炉内の温度差、成形体の形状、成形体の密度差等が考えられる。このような反り解消手段としては、細長物では、従来から、成形体を吊って焼成する、いわゆる吊り焼成が採られているが、反り解消のためには充分ではなかった。
【０００４】
一方、反り量を加味して焼結体寸法を設定すると、原料ロスや研削代が増加し、コストアップにつながる。特に、直動軸受用レール等は、厳しい真直度が要求されるため、焼結体の反り具合によって焼成後の研削代が所定以上に大きくなりコストに大きく影響する。
そこで、特開昭６１−４４７８２号公報では、セラミック磁器をスライシング後、３〜１０ｇ／ｃｍ2の加重をかけ５００〜９００℃の範囲で熱処理を行うことにより、スライシングによる歪み（反り）を取り除くことが提案されている。
【０００５】
しかしながら、この方法によっても、直動軸受用レール等の窒化珪素製細長物に発生した反りを充分に矯正することはできなかった。
また、形状の異なる細長物の場合、錘の設置面積が狭く、錘を安定して設置できない為、錘を細長物に安定して設置する方法を検討する必要があった。
【０００６】
【発明が解決しようとする課題】
従って、本発明は、上記した従来の問題に鑑みてなされたものであり、その目的は、厳しい真直度が要求されるとともに焼成時に反りが発生しやすい直動軸受用レール等の窒化珪素製細長物について、複数個の窒化珪素製細長物を同時に反り矯正することにより、作業効率を大幅に向上することができるため、強度等の特性低下がなく、反りが矯正された真直度の優れた窒化珪素製細長物を低コストで製造することができる窒化珪素製細長物の製造方法を提供することにある。
【０００７】
【課題を解決するための手段】
すなわち、本発明によれば、窒化珪素製細長物の焼結体を、三角形状の三辺を構成するように保持用治具にそれぞれ載置し、押圧用治具で挟み押圧した状態で、１３００〜１５００℃の範囲の温度で加熱することにより、反りを矯正することを特徴とする窒化珪素製細長物の製造方法が、提供される。
【０００８】
また、本発明によれば、窒化珪素製細長物の焼結体を、三角形状の三辺を構成するようにそれぞれ配置した一段目を保持用治具に載置し、該細長物焼結体の反りが互い違いになるように、該細長物焼結体を多段に積み重ねた後、押圧用治具で挟み押圧した状態で、１３００〜１５００℃の範囲の温度で加熱することにより、反りを矯正することを特徴とする窒化珪素製細長物の製造方法が、提供される。
このとき、一段目と最上段目の細長物焼結体の反り方向は、同一であることが好ましく、更に、一段目が、細長物焼結体の反りの凸部が上になるように保持用治具に載置されることが好ましい。
【０００９】
また、本発明では、細長物焼結体に、５ＭＰａ以上の曲げ応力を付与することが好ましく、更に細長物焼結体の長手方向に垂直な方向に曲げ応力を付与することが好ましい。
【００１０】
これらの窒化珪素製細長物の具体例としては、厳しい真直度が要求される直動軸受用レールや軸が挙げられる。
【００１１】
なお、本発明において、「細長物」とは、図３に示すような単純形状を想定した場合、次式で表されるように、断面における外周寸法（外周長）の総和に対して３倍以上の長さを有する部材をいう。
（２０＋２０＋１０＋１０）×３≦Ａ（長さ：１８０以上）
（１０×π）×３≦Ａ（長さ：３０π以上）
【００１２】
【発明の実施の形態】
以下、本発明をその実施の形態に従ってさらに詳しく説明するが、本発明はこれらの実施の形態に限定されるものではない。
本発明（第一発明）では、窒化珪素製細長物の焼結体を、三角形状の三辺を構成するように保持用治具にそれぞれ載置し、押圧用治具で挟み押圧した状態で、１３００〜１５００℃の範囲の温度で加熱することにより、反りを矯正することに特徴を有する。
また、本発明（第二発明）では、窒化珪素製細長物の焼結体を、三角形状の三辺を構成するようにそれぞれ配置した一段目を保持用治具に載置し、細長物焼結体の反りが互い違いになるように、細長物焼結体を多段に積み重ねた後、押圧用治具で挟み押圧した状態で、１３００〜１５００℃の範囲の温度で加熱することにより、反りを矯正することに特徴を有する。
【００１３】
ここで、本発明の主な特徴は、図１（ａ）に示すように、３体の細長物焼結体（１０ａ〜１０ｃ）を三角形になるように保持用治具上に載置することにある。
これにより、細長物焼結体１０を多段に積み重ね、押圧用治具で挟み押圧した場合（図２参照）であっても載置安定性に優れ、且つ３組の細長物焼結体（１０ａ〜１０ｃ）に均一に荷重を掛けることができる。
【００１４】
また、本発明では、図２（ｂ）に示すように、細長物焼結体１０の反りが互い違いになるように、細長物焼結体１０を多段に積み重ね、且つ一段目と最上段目の細長物焼結体の反り方向を同一にすることが好ましい。
本発明では、細長物焼結体１０の反りの凸部を対向させて積むことにより、矯正の曲げ応力が作用する断面係数を１製品分とすることができ、押圧用治具１４で挟み押圧した時に、段数の多少に関わらず、全ての細長物焼結体１０に有効に荷重を負荷させることができるため、一度に強度等の特性低下がなく、反りが矯正された真直度の優れた窒化珪素製細長物を大量に得ることができる。
一方、細長物焼結体１０の反りの凸部を対向させず、同方向に積み上げると、矯正の曲げ応力の作用する断面係数が、製品を積んだ個数分となるため、大量に処理する場合は矯正に多大な荷重を必要とし、油圧荷重など重荷重を負荷できる装置が必要となり、経済的でない。
【００１５】
更に、本発明では、一段目が、細長物焼結体の反りの凸部が上になるように保持用治具に載置することが、細長物焼結体を多段に積み重ねる際の安定性を向上させる上で好ましい。
【００１６】
以下、本発明の反り矯正方法について更に詳細に説明する。
本発明では、窒化珪素製細長物の焼結体に対して、反りを矯正する方向に５ＭＰａ以上の曲げ応力を付与する。曲げ応力としては、好ましくは８ＭＰａ以上、さらに好ましくは１０ＭＰａ以上である。曲げ応力が５ＭＰａ未満の場合には、反り矯正の効果が低い。
細長物焼結体に対する曲げ応力の付与方向は、反りの矯正方向、通常は厚み方向である。
【００１７】
また、細長物焼結体に対しては、曲げ応力を付加するとともに、１３００〜１５００℃の範囲の温度で加熱処理を施す。１３００℃未満の温度では、反り矯正効果を得ることができず、一方、１５００℃を超える温度で加熱処理を施すと、反りの矯正は可能でも、得られる細長物焼結体の強度が著しく低下する。
なお、加熱処理は、窒化珪素製の焼結体が対象であることから、通常、窒素雰囲気等の不活性雰囲気で行われる。また、加熱圧力としては限定されず、常圧、加圧のいずれの圧力条件でも、当該処理を行うことができるが、ＨＩＰなどの高圧焼結を行ったものに対しては加圧下の方が好ましい。
【００１８】
本発明では、窒化珪素製細長物の焼結体を対象とする。このような窒化珪素焼結体の細長物は、たとえば次のようにして製造することができる。
まず、窒化珪素原料に焼結助剤と適当量のバインダーを添加、混合する。この混合物を成形後仮焼してバインダーを除去し、得られた仮焼体を窒素雰囲気中、１７００〜１８００℃程度の高温で焼結することにより窒化珪素焼結体を得る。次いで、得られた窒化珪素焼結体をスライスなどの加工により、窒化珪素製細長物の焼結体を得ることができる。
なお、スライスなどの加工を行わず、直接焼結体として細長物として得ることももちろん可能である。
上記のようにして得られる窒化珪素製細長物の焼結体は、通常真直度が低く、反り等が生じており、寸法精度が劣っている。本発明では、このような窒化珪素製細長物の焼結体を対象とするものである。
【００１９】
【実施例】
（実施例１）
窒化珪素原料に焼結助剤と所定量のバインダーを添加し、混合機にて混合した後、スプレードライヤーにて乾燥造粒した。この造粒原料をゴム型より構成される成形型に充填し、静水圧プレス機により成形し角柱成形体を製作した。
これらの成形体を大気中４００℃にて仮焼しバインダーを除去した後、ＮＣフライス盤により所定形状に加工した。
【００２０】
これらを高圧窒素雰囲気中で１７００℃×１ｈｒ焼成し窒化珪素製の角柱（１２ｍｍ×１０ｍｍ×長さ３００ｍｍ）焼結体を得た。
得られた窒化珪素製角柱焼結体の中から反り量１ｍｍ以上のものを３体選択し、ＳｉＣ基板１２上に三角形を描くように置き、更に窒化珪素角柱焼結体１０の曲げ応力が５ＭＰａになるような荷重用ＳｉＣ基板１４を上から載せた（図１参照）。
この状態で、常圧窒素雰囲気中にて処理温度１３００℃、１５００℃にてそれぞれ１時間キープして反り修正を行った。
【００２１】
得られた反り修正品の反り量を測定した。その後、反り修正品から試験片を切りだしＪＩＳ Ｒ１６０１に基づき４点曲げ強度測定を、ＪＩＳ Ｒ１６０７に基づき破壊靭性測定を行った。合格値は、反り量０．５ｍｍ以下、曲げ強度９００ＭＰａ以上、破壊靭性値５．８ＭＰaｍ1/2以上とし、○と表示した。不合格品は、×と表示した。その結果を表１に示す。
【００２２】
（実施例２）
実施例１と同様に製作した窒化珪素角柱焼結体の中から反り量１ｍｍ以上のものを６３体選択した。
まず、３体選択し、ＳｉＣ基板１２上に三角形を描くように置いた後、反り方向が互い違いになるように、各辺に２１体ずつ積み上げ、更に窒化珪素角柱焼結体１０の曲げ応力が５ＭＰａになるような荷重用ＳｉＣ基板１４を上から載せた（図２参照）。
この状態で、実施例１と同様の反り修正を行い評価した。その結果を表１に示す。
【００２３】
（比較例１）
処理温度を１２５０℃、１５５０℃とした以外は、実施例１と同様に窒化珪素製角柱焼結体を製造し、評価を行った。その結果を表１に示す。
【００２４】
（比較例２）
曲げ応力を４ＭＰａになるように設定した以外は、実施例１と同様に窒化珪素製角柱焼結体を製造し、評価を行った。その結果を表１に示す。
【００２５】
【表１】
まず、表１の結果から明らかなように、角柱焼結体に付与する最大曲げ応力が５ＭＰａ以上、及び加熱処理温度が１３００〜１５００℃の範囲という要件が臨界的であるということがわかる。この範囲を逸脱した温度で加熱した場合には、反り矯正が不十分であるか、あるいは得られる角柱焼結体の曲げ強度が著しく低下している。
【００２７】
【発明の効果】
以上説明したように、本発明方法によれば、厳しい真直度が要求されるとともに焼成時に反りが発生しやすい直動軸受用レール等の窒化珪素製細長物について、複数個の窒化珪素製細長物を同時に反り矯正することにより、作業効率を大幅に向上することができるため、強度等の特性低下がなく、反りが矯正された真直度の優れた窒化珪素製細長物を低コストで製造することができる。
【図面の簡単な説明】
【図１】 細長物焼結体の反り矯正方法の一例を示すものであり、（ａ）は正面図、（ｂ）は（ａ）のＡ−Ａ断面図である。
【図２】 細長物焼結体の反り矯正方法の他の例を示すものであり、（ａ）は正面図、（ｂ）は（ａ）のＡ−Ａ断面図である。
【図３】 単純形状の細長物を示す斜視図である。
【符号の説明】
１０…細長物焼結体（窒化珪素角柱焼結体）、１２…保持用治具（ＳｉＣ基板）、１４…押圧用治具（荷重用ＳｉＣ基板）。[0001]
BACKGROUND OF THE INVENTION
TECHNICAL FIELD The present invention relates to a method for manufacturing an elongated product made of silicon nitride that requires strict straightness such as a rail for a linear motion bearing. More particularly, the present invention relates to a method for manufacturing a silicon nitride elongated product that corrects warpage by performing a predetermined heat treatment after firing for a silicon nitride elongated product such as a rail for a linear motion bearing that is likely to be warped during firing. .
[0002]
[Prior art]
2. Description of the Related Art Conventionally, it has been desired that a ceramic bearing such as a linear motion bearing rail, a shaft, a thermocouple protective tube, and the like has good dimensional accuracy.
[0003]
The above-mentioned ceramic elongated products are likely to be warped during firing, and are often distorted in dimensional accuracy. As a cause of the warp, a temperature difference in the firing furnace, a shape of the molded body, a density difference of the molded body, and the like are considered. As such warp eliminating means, so-called suspension firing, in which a molded product is suspended and fired, has been conventionally used for slender products, but this has not been sufficient for eliminating warp.
[0004]
On the other hand, if the size of the sintered body is set in consideration of the amount of warpage, the raw material loss and the grinding allowance increase, leading to an increase in cost. In particular, since a linear bearing rail or the like requires a strict straightness, the grinding allowance after firing becomes larger than a predetermined value due to the warpage of the sintered body, which greatly affects the cost.
Therefore, in Japanese Patent Laid-Open No. 61-44782, after slicing a ceramic porcelain, a strain of 3 to 10 g / cm 2 is applied and heat treatment is performed in a range of 500 to 900 ° C. to remove distortion (warp) due to slicing. Has been proposed.
[0005]
However, even with this method, it has not been possible to sufficiently correct the warp generated in the elongated silicon nitride material such as the rail for the linear motion bearing.
In the case of elongated objects having different shapes, the installation area of the weight is narrow and the weight cannot be stably installed. Therefore, it has been necessary to examine a method for stably installing the weight on the elongated object.
[0006]
[Problems to be solved by the invention]
Accordingly, the present invention has been made in view of the above-described conventional problems, and an object of the present invention is to make a silicon nitride elongated body such as a rail for a linear motion bearing that requires strict straightness and easily warps during firing. Since the work efficiency can be greatly improved by simultaneously correcting the warpage of a plurality of silicon nitride strips, there is no deterioration in properties such as strength, and the nitridation is excellent in straightness with the warpage corrected. An object of the present invention is to provide a method for producing a silicon nitride elongated product, which can produce a silicon elongated product at a low cost.
[0007]
[Means for Solving the Problems]
That is, according to the present invention, the sintered compact of silicon nitride is placed on the holding jig so as to constitute the triangular three sides, and is sandwiched and pressed by the pressing jig, A method for producing an elongated product made of silicon nitride, characterized by correcting warpage by heating at a temperature in the range of 1300 to 1500 ° C., is provided.
[0008]
In addition, according to the present invention, the sintered body of the elongated product made of silicon nitride is placed on the holding jig arranged in the first stage so as to constitute the three sides of the triangle , Warp is corrected by heating at a temperature in the range of 1300-1500 ° C. in a state where the elongated sintered bodies are stacked in multiple stages and then sandwiched and pressed by a pressing jig so that the warpage of the sheet is staggered. A method for producing a silicon nitride strip is provided.
At this time, it is preferable that the warp directions of the elongated sintered body at the first stage and the uppermost stage are the same, and further, the first stage is held so that the convex portion of the warped elongated body is at the top. It is preferably placed on a jig for use.
[0009]
In the present invention, it is preferable to apply a bending stress of 5 MPa or more to the elongated product sintered body, and it is preferable to apply a bending stress in a direction perpendicular to the longitudinal direction of the elongated product sintered body.
[0010]
Specific examples of these silicon nitride strips include linear bearing rails and shafts that require strict straightness.
[0011]
In the present invention, the “elongated object” is assumed to be three times the sum of the outer peripheral dimensions (outer peripheral length) in the cross section, as represented by the following equation, assuming a simple shape as shown in FIG. The member which has the above length is said.
(20 + 20 + 10 + 10) × 3 ≦ A (length: 180 or more)
(10 × π) × 3 ≦ A (length: 30π or more)
[0012]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in more detail according to the embodiments thereof, but the present invention is not limited to these embodiments.
In the present invention (first invention), the sintered compact of silicon nitride is placed on the holding jig so as to constitute three triangular sides, and is sandwiched and pressed by the pressing jig. It is characterized by correcting the warp by heating at a temperature in the range of 1300 to 1500 ° C.
Further, in the present invention (second invention), the sintered body of the elongated silicon nitride material is placed on the holding jig arranged in the first stage so as to constitute the triangular three sides, and the elongated product is fired. After stacking the elongated sintered bodies in multiple stages so that the warping of the bonded body is staggered, the warping is caused by heating at a temperature in the range of 1300 to 1500 ° C. while being sandwiched and pressed by a pressing jig. Characterized by straightening.
[0013]
Here, the main feature of the present invention is that, as shown in FIG. 1A, three elongated sintered bodies (10a to 10c) are placed on a holding jig so as to form a triangle. It is in.
Thereby, even when the elongated product sintered
[0014]
Further, in the present invention, as shown in FIG. 2 (b), the elongated product sintered
In the present invention, the convex sections of warpage of the elongated sintered
On the other hand, when stacking in the same direction without facing the warped convex parts of the elongated product sintered
[0015]
Furthermore, in the present invention, the first stage is placed on the holding jig so that the warped convex part of the elongated product sintered body is on top, so that the stability when stacking the elongated product sintered body in multiple stages is increased. It is preferable for improving the ratio.
[0016]
Hereinafter, the warp correction method of the present invention will be described in more detail.
In the present invention, a bending stress of 5 MPa or more is applied to the silicon nitride elongated product in the direction of correcting warpage. The bending stress is preferably 8 MPa or more, more preferably 10 MPa or more. When the bending stress is less than 5 MPa, the effect of warp correction is low.
The direction in which the bending stress is applied to the elongated product sintered body is the correction direction of warpage, usually the thickness direction.
[0017]
The elongated product sintered body is subjected to heat treatment at a temperature in the range of 1300 to 1500 ° C. while applying bending stress. When the temperature is lower than 1300 ° C., the warp correction effect cannot be obtained. On the other hand, when heat treatment is performed at a temperature higher than 1500 ° C., the warp can be corrected, but the strength of the obtained elongated sintered body is significantly reduced. To do.
Note that the heat treatment is usually performed in an inert atmosphere such as a nitrogen atmosphere because a sintered body made of silicon nitride is an object. In addition, the heating pressure is not limited, and the treatment can be performed under any pressure condition of normal pressure or pressurization. However, for those subjected to high pressure sintering such as HIP, the pressure is lower. preferable.
[0018]
In the present invention, a sintered body of an elongated product made of silicon nitride is an object. Such an elongated product of a silicon nitride sintered body can be produced, for example, as follows.
First, a sintering aid and an appropriate amount of binder are added to and mixed with the silicon nitride raw material. The mixture is calcined after molding to remove the binder, and the resulting calcined body is sintered at a high temperature of about 1700 to 1800 ° C. in a nitrogen atmosphere to obtain a silicon nitride sintered body. Next, the obtained silicon nitride sintered body can be processed by slicing or the like to obtain an elongated silicon nitride sintered body.
Needless to say, it is possible to obtain an elongated product directly as a sintered body without processing such as slicing.
The sintered body of elongated silicon nitride obtained as described above usually has low straightness, warpage, etc., and dimensional accuracy is inferior. The present invention is directed to a sintered body of such an elongated product made of silicon nitride.
[0019]
【Example】
Example 1
A sintering aid and a predetermined amount of binder were added to the silicon nitride raw material, mixed with a mixer, and then dried and granulated with a spray dryer. This granulated raw material was filled in a mold composed of a rubber mold and molded by a hydrostatic press to produce a prismatic molded body.
These molded bodies were calcined at 400 ° C. in the atmosphere to remove the binder, and then processed into a predetermined shape by an NC milling machine.
[0020]
These were fired at 1700 ° C. for 1 hr in a high-pressure nitrogen atmosphere to obtain a silicon nitride prism (12 mm × 10 mm × length 300 mm) sintered body.
Three of the obtained silicon nitride prismatic sintered bodies having a warpage amount of 1 mm or more are selected, placed on the
In this state, the warpage was corrected by keeping at a treatment temperature of 1300 ° C. and 1500 ° C. for 1 hour in a normal pressure nitrogen atmosphere.
[0021]
The amount of warpage of the obtained warp corrected product was measured. Thereafter, a test piece was cut out from the warp-corrected product, a four-point bending strength measurement was performed based on JIS R1601, and a fracture toughness measurement was performed based on JIS R1607. The acceptable values were warped amount 0.5 mm or less, bending strength 900 MPa or more, fracture toughness value 5.8 MPa 1/2 or more, and indicated as ◯. An unacceptable product was indicated as x. The results are shown in Table 1.
[0022]
(Example 2)
63 silicon nitride prismatic sintered bodies manufactured in the same manner as in Example 1 were selected with a warpage of 1 mm or more.
First, after selecting three bodies and placing them in a triangular shape on the
In this state, the same warp correction as in Example 1 was performed for evaluation. The results are shown in Table 1.
[0023]
(Comparative Example 1)
A silicon nitride prismatic sintered body was produced and evaluated in the same manner as in Example 1 except that the treatment temperatures were 1250 ° C. and 1550 ° C. The results are shown in Table 1.
[0024]
(Comparative Example 2)
A silicon nitride prismatic sintered body was produced and evaluated in the same manner as in Example 1 except that the bending stress was set to 4 MPa. The results are shown in Table 1.
[0025]
[Table 1]
First, as is clear from the results in Table 1, it is understood that the requirements that the maximum bending stress applied to the prismatic sintered body is 5 MPa or more and the heat treatment temperature is in the range of 1300 to 1500 ° C. are critical. When heated at a temperature outside this range, the warp correction is insufficient or the bending strength of the resulting prismatic sintered body is significantly reduced.
[0027]
【The invention's effect】
As described above, according to the method of the present invention, a plurality of silicon nitride strips are required for silicon nitride strips such as rails for linear motion bearings that require strict straightness and are likely to warp during firing. By simultaneously correcting the warpage, the work efficiency can be greatly improved, so that it is possible to produce silicon nitride strips with excellent straightness with reduced warpage and no deterioration in properties such as strength, at low cost. Can do.
[Brief description of the drawings]
1A and 1B show an example of a method for correcting warpage of a long and narrow sintered body, in which FIG. 1A is a front view and FIG. 1B is a cross-sectional view taken along line AA in FIG.
FIGS. 2A and 2B show another example of a method for correcting warpage of an elongated product sintered body, wherein FIG. 2A is a front view, and FIG. 2B is a cross-sectional view taken along line AA in FIG.
FIG. 3 is a perspective view showing an elongated object having a simple shape.
[Explanation of symbols]
DESCRIPTION OF
Claims (10)
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| JP2001175658A JP4091753B2 (en) | 2001-06-11 | 2001-06-11 | Method for producing silicon nitride strip |
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| JP2001175658A JP4091753B2 (en) | 2001-06-11 | 2001-06-11 | Method for producing silicon nitride strip |
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| JP4091753B2 true JP4091753B2 (en) | 2008-05-28 |
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| US7948075B2 (en) | 2008-03-10 | 2011-05-24 | Hitachi Metals, Ltd. | Silicon nitride substrate, method of manufacturing the same, and silicon nitride circuit board and semiconductor module using the same |
| JP6994863B2 (en) * | 2017-08-03 | 2022-01-14 | 日本特殊陶業株式会社 | Manufacturing method of ceramic parts |
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