JPH01301563A - Production of sintered sic - Google Patents
Production of sintered sicInfo
- Publication number
- JPH01301563A JPH01301563A JP63127542A JP12754288A JPH01301563A JP H01301563 A JPH01301563 A JP H01301563A JP 63127542 A JP63127542 A JP 63127542A JP 12754288 A JP12754288 A JP 12754288A JP H01301563 A JPH01301563 A JP H01301563A
- Authority
- JP
- Japan
- Prior art keywords
- parts
- weight
- molding
- sic
- granules
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 238000000465 moulding Methods 0.000 claims abstract description 44
- 239000008187 granular material Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000011230 binding agent Substances 0.000 claims abstract description 18
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 8
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008117 stearic acid Substances 0.000 claims abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 10
- 239000007921 spray Substances 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000002518 antifoaming agent Substances 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 13
- 238000005452 bending Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 229920001971 elastomer Polymers 0.000 description 6
- 229910052580 B4C Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 238000005238 degreasing Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000555825 Clupeidae Species 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 235000019512 sardine Nutrition 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- -1 sintering aid 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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
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】
〔産業上の利用分野〕
本発明はＳｉＣ焼結体の製造方法に関し、更に詳しくは
、生成形体の強度が強く保形性が良く、更に焼結して緻
密でボアがなく、曲げ強度の高いＳｉＣ焼結体を安定し
、容易に得る方法である。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a method for producing a SiC sintered body, and more specifically, the produced body has strong strength and good shape retention, and is further sintered to be dense and have a bore. This is a method for stably and easily obtaining a SiC sintered body with high bending strength.
従来は、 ＳｉＣセラミックスの成形用バインダーとし
て有機質バインダー、例えばポリビニルアルコール、コ
ンスターチ、糖密、コールタールピッチ、フェノール樹
脂等が使われている。これらのバインダーを使用し、成
形用金型への粉の流れ性、充填性を良くするために顆粒
化し、これを成形し生成形体としている。その場合に、
低い成形圧力で漬れ易い顆粒の時は、生成形体の強度は
弱く、保形性も劣るため複雑な形状のものの加工は難し
い、また低い成形圧力で漬れない顆粒のものは、ラバー
プレス、金型プレス成形の際、成形圧力を極度に高くす
るなどの手段で成形していた。Conventionally, organic binders such as polyvinyl alcohol, corn starch, molasses, coal tar pitch, and phenolic resin have been used as binders for forming SiC ceramics. These binders are granulated to improve the flowability and filling properties of the powder into a molding die, and the granules are molded into a molded product. In that case,
When the granules are easily soaked at low molding pressures, the strength of the formed bodies is weak and the shape retention is poor, making it difficult to process complex shapes.Also, for granules that do not soak under low molding pressures, rubber presses, During press molding, the molding pressure was extremely high.
それによっである程度の生強度の成形体が得られ緻密で
、曲げ強度の高いＳｉＣ焼結体となる場合もあれば成形
圧力を極度に高くしても潰れない場合もあった。As a result, a molded body with a certain degree of green strength can be obtained, and in some cases it becomes a dense SiC sintered body with high bending strength, and in other cases, it does not collapse even when the molding pressure is extremely high.
この様に極度に成形圧力を高くして成形する場合には金
型製作費用が高く、金型の摩耗も早く寿命も短かく、成
形費用の低減を図ることが難しかった。When molding is performed under such extremely high molding pressure, mold manufacturing costs are high, the mold wears quickly, and its lifespan is short, making it difficult to reduce molding costs.
近年、セラミックスの優れた特性に着目され、ル、釣具
、混合用ポール等の実用化が盛んに行なわれており、こ
れ等については緻密でボアがなく、曲げ強度の高いＳｉ
Ｃ焼結体が要求されている。In recent years, attention has been focused on the excellent properties of ceramics, and they are being put to practical use in products such as fishing rods, fishing gear, and mixing poles.
C sintered bodies are required.
例えば、釣ガイドリング等は、全表面が曲面になってい
る為、プレス成形特全面に均一な成形圧力が掛かりにく
く、特に圧力の掛かりにくい箇所はその強度も低く、金
型に付着したり、ボアが発生したり、また、生加工も困
難であった。For example, since the entire surface of fishing guide rings is curved, it is difficult to apply uniform molding pressure to the press molded surface, and the strength is low in areas where pressure is particularly difficult to apply, so it may stick to the mold or Bores occurred, and raw processing was also difficult.
本発明者らは、ＳｉＣ微粉末の顆粒を用いて、ラバープ
レス、金型プレス成形する際に低圧力で成形した成形体
を焼結して何故緻密でボアがなく。The present inventors used granules of SiC fine powder to form compacts under low pressure during rubber press and die press molding, and then sintered them to find out why they were dense and had no bores.
曲げ強度の高いＳ ｒ Ｃ焼結体が造れないのか、その
原因について検討した結果、ラバープレス、金型プレス
成形の際にＳｉＣ微粉末の顆粒の漬れが不充分で、その
成形体の生密度が低いことにあるものと判断し、漬れ易
い顆粒が造れる成形用バインダーを種々検討した。As a result of investigating the cause of the inability to produce SrC sintered bodies with high bending strength, we found that the granules of SiC fine powder were not soaked sufficiently during rubber press and mold press forming, and the formation of the formed body was poor. We determined that this was due to the low density, and investigated various molding binders that can produce granules that are easy to soak.
その結果、緻密でボアのなく、曲げ強度の高いＳｉＣ焼
結体を得ることができたが生成形体の加工時の強度が低
下し、複雑形状の加工が困難となった。そこで更に成形
体の強度が高く、小物でも容易に加工でき、且つ特性の
優れた焼結体を得る成形用バインダーを種々検討し、本
発明に到った。As a result, it was possible to obtain a dense SiC sintered body with no bores and high bending strength, but the strength of the formed body during processing decreased, making it difficult to process complex shapes. Therefore, we investigated various molding binders that can produce sintered bodies that have higher strength, can be easily processed into small objects, and have excellent properties, and have arrived at the present invention.
本発明は、 ＳｉＧのセラミックスの成形において、
ＳｉＣ微粉末１０１１ｆｉｔ部に対し、成形用バインダ
ーとしてポリビニルアルコール（以下ＰＶＡと略す）を
０．５〜２．０重量部、ポリエチレングリコール（以下
ＰＥＧと略す）を１．０〜３．０重量部を添加し、焼結
助剤を更に加え顆粒化し、その顆粒を用いて成形、脱脂
、焼結するＳｉＣ焼結体の製造方法に関するものである
。The present invention provides the following steps in the molding of SiG ceramics:
For 1011 parts of SiC fine powder, 0.5 to 2.0 parts by weight of polyvinyl alcohol (hereinafter abbreviated as PVA) and 1.0 to 3.0 parts by weight of polyethylene glycol (hereinafter abbreviated as PEG) are used as a molding binder. The present invention relates to a method for producing a SiC sintered body, in which SiC sintered bodies are added, further added with a sintering aid, granulated, and the granules are used for molding, degreasing, and sintering.
まずＳｉＣの微粉末に成形用バング−１分散剤、消泡剤
および焼結助剤を所定量加え、更に水を所定量加えた後
、ボールミル等で充分に混合してスラリーを造る０次に
スラリーをスプレードライヤー等により処理して顆粒化
した後、その顆粒をまた金型プレス成形に使用する顆粒
は、前述のＳｉＣの微粉末に成形用バインダーとしてＰ
ＶＡを０．５〜２．０重量部、ＰＥＧを１．０〜３．０
重量部加える他に更に好ましくはステアリン、酸を０．
５〜３．５重量部添加し、分散剤、消泡剤、焼結助剤お
よび水を加えた後、充分に混合したスラリーをスプレー
ドライヤー等により処理して造る。この様にして造られ
た顆粒は、低圧加圧でも良く漬れ、成形後の生成形体の
強度も高く、保形性も良く、特に複雑形状や大型形状用
のラバープレス、金型プレス成形用として適しており、
脱脂、焼結後の組織も緻密で曲げ強度の高いＳｉＣ焼結
体を得ることボアがあると釣糸が切れるとか鰯りが問題
となるため良く顆粒が潰れ、且つ生成形体の強度も強く
する目的のものには、 ＳｉＣ微粉末１００＠ｊ１部に
対し、成形用バインダーとして分子％２０．０００〜３
０．０００（７） ＰＶＡを０．５〜２．０重醍部１分
子ｉ １，０００〜１，５００と分子量１５０〜２５
０の２種炉のＰＥＡを１０：１〜２０：ｌの範囲で混合
したＰＥＧを１．０〜３．０巾μ部、ステアリン酸を０
．５〜３．５毛量部添加し、分散剤、消泡剤、焼結助剤
および水をそれぞれ所定量加えた後、ボールミル等で充
分に混合してスラリー化し、それをスプレードライヤー
等にポール等の成形体を製造した。この様にして造られ
た顆粒は、流動性が良く、低圧加圧でも良く潰れ、成形
後の生強度も強く旋盤等による生加工もできる。プレス
成形用として適しており、脱脂。First, a predetermined amount of BANG-1 dispersant for molding, an antifoaming agent, and a sintering aid are added to SiC fine powder, and then a predetermined amount of water is added, and then thoroughly mixed in a ball mill etc. to create a slurry. After processing the slurry with a spray dryer or the like to make it into granules, the granules used for press molding are made by adding P as a molding binder to the above-mentioned fine SiC powder.
0.5 to 2.0 parts by weight of VA, 1.0 to 3.0 parts of PEG
In addition to adding 0.0 parts by weight, more preferably 0.0 parts of stearin and acid are added.
After adding 5 to 3.5 parts by weight, a dispersant, an antifoaming agent, a sintering aid and water, the thoroughly mixed slurry is processed using a spray dryer or the like. The granules made in this way are well soaked even under low pressure, have high strength and good shape retention after molding, and are especially suitable for rubber press and mold press molding for complex shapes and large shapes. suitable as
To obtain a SiC sintered body with a dense structure and high bending strength after degreasing and sintering.The purpose is to crush the granules well and strengthen the strength of the formed body, since bores can cause problems such as breaking fishing lines and sardines. For 1 part of SiC fine powder 100@j, 20.000 to 3 molecule % is used as a molding binder.
0.000 (7) 0.5-2.0 PVA per molecule i 1,000-1,500 and molecular weight 150-25
1.0 to 3.0 μm width of PEG mixed with 10:1 to 20:1 of PEA from a two-class furnace of 0, and 0 parts of stearic acid.
．． After adding 5 to 3.5 parts of hair, and adding predetermined amounts of dispersant, antifoaming agent, sintering aid, and water, mix thoroughly with a ball mill, etc. to form a slurry, and pour it into a spray dryer, etc. A molded article such as the following was manufactured. The granules produced in this manner have good fluidity, are easily crushed even under low pressure, and have high green strength after molding, and can be processed green using a lathe or the like. Suitable for press molding and degreasing.
焼結後の組織も緻密でボアのないＳｉＣ焼結体を得るこ
とができる。It is possible to obtain a SiC sintered body with a dense structure and no bores after sintering.
成形用バインダーとしてＰＶＡが０．５重量部未満にな
ると成形体の保形性が悪くなり、欠は易く、生加工が困
難となる。またＰＶＡが２．０重量部を越えると、成形
時の顆粒の潰れが悪くなる。同様にＰＥＧが １．０重
量部未満になると保形性が悪く、３、Ｏｉｉ部を越える
と金型等に付着し易くなったり、脱脂時に爆裂が生じた
りする。If the amount of PVA used as a molding binder is less than 0.5 parts by weight, the shape retention of the molded product will be poor, chipping will occur easily, and green processing will become difficult. Moreover, if PVA exceeds 2.0 parts by weight, the granules will not be easily crushed during molding. Similarly, if the PEG content is less than 1.0 parts by weight, the shape retention is poor, and if it exceeds 3.0 parts by weight, it tends to adhere to molds, etc., and may explode during degreasing.
成形用バインダーとしてのステアリン酸は金型プレス成
形時の離型剤として用いるものであるが、これがないと
離型性が悪くなったり、きしみ音が発生したり、更には
金型の摩耗を早め寿命が短かくなる。またステアリン酸
が３゜５重量部を越えると、金型プレス成形された成形
体の保形性が悪くなったり、逆に金型への付着が増大し
て離型性が悪くなったり、脱脂時に爆裂が生じたりする
。好ましいステアリン酸の添加量は０．５〜３．５屯賃
部である。焼結体表面のボアをなくすためのプレス成形
用バインダーとして使用するＰＶＡの分子量が３０ 、
０００を越えると顆粒の潰れに影響し、ボアをなくすこ
とはできないし、分子量が２０，０００未満だと生成形
体の保形性に悪影響をきたすことになる。また２種類の
ＰＥＧの分子量の範囲すなわち１ 、０００〜ｌ 、５
００と１５０〜２５０は顆粒の破砕性を適したものにす
るものであり、その混合比率を１０：ｌ〜２０：ｌにす
ることにより、顆粒の破砕性と保形性とをバランスされ
ることができ、ｌＯ：１未満になると保形性が悪くなり
２０：ｌを越えると破砕性が悪くなる。Stearic acid, which is used as a molding binder, is used as a mold release agent during mold press molding, but without it, mold release properties will be poor, squeaks will occur, and the mold will wear more quickly. Life expectancy will be shortened. Moreover, if stearic acid exceeds 3.5 parts by weight, the shape retention of the molded product press-molded with a mold will deteriorate, or conversely, the adhesion to the mold will increase, resulting in poor mold releasability. Sometimes explosions occur. The preferred amount of stearic acid added is 0.5 to 3.5 parts by weight. The molecular weight of PVA used as a binder for press molding to eliminate bores on the surface of the sintered body is 30.
If the molecular weight exceeds 20,000, it will affect the crushing of the granules, making it impossible to eliminate the bores, and if the molecular weight is less than 20,000, it will have an adverse effect on the shape retention of the formed body. Furthermore, the molecular weight range of the two types of PEG is 1,000 to 1,5
00 and 150 to 250 are suitable for the crushability of the granules, and by setting the mixing ratio to 10:l to 20:l, the crushability and shape retention of the granules can be balanced. If the ratio is less than 10:1, the shape retention will be poor, and if it exceeds 20:1, the crushability will be poor.
本発明で使用できるＳ ｉｃ′ＩＩ１．粉末にはα型、
β型等を含み、微粉末の粒度は平均粒径３ＩＬｍ以下。Sic'II1. which can be used in the present invention. The powder contains α type,
Including β-type, etc., and the average particle size of the fine powder is 3ILm or less.
純度は９５％以上のものである。また、−船釣に使用さ
れる成形用顆粒の大きさは、平均粒径で５０〜１２０Ｊ
ＬＩＩである。その顆粒を使用して成形、脱脂し、 １
７５０〜２１００℃で３時間程度Ａｒ雰囲気中で焼結し
、 ＳｉＣ焼結体を得る。Purity is 95% or higher. - The size of molding granules used for boat fishing is 50 to 120 J in average particle size.
It is LII. Using the granules, mold and degrease, 1
Sintering is performed at 750 to 2100°C for about 3 hours in an Ar atmosphere to obtain a SiC sintered body.
使用される焼結助剤は、Ｃ，Ｂ、Ａ文、Ｂｅ等の公知の
もので、その添加量も従来、知られた範囲がそのまま使
用できる。The sintering aids used are known ones such as C, B, A, Be, etc., and the amount added can be within the conventionally known range.
以下、本発明を実施例をもって説明する。 Hereinafter, the present invention will be explained with reference to examples.
実施例 ｌ
平均粒径０．４５ｇｍのＳｉＣ微粉末１００重量部に対
し、分子ｉ２４，０００（７） ＰＶＡを １．０重り
部、分子量５０．０００のＰＥＧを ２．０重量部、炭
化ホウ素粉末を０．８重量部、カーボンブラック粉末を
２．５重量部に水を添加し、ボールミル中で２０時間混
合して３５％濃度のスラリーをつくり、スプレードライ
ヤーにて平均粒径８５ＪＬｓの顆粒を製造した。Example l For 100 parts by weight of SiC fine powder with an average particle size of 0.45 gm, 1.0 parts by weight of PVA with a molecular i24,000(7), 2.0 parts by weight of PEG with a molecular weight of 50.000, and boron carbide powder. Add water to 0.8 parts by weight of carbon black powder and 2.5 parts by weight of carbon black powder, mix in a ball mill for 20 hours to make a slurry with a concentration of 35%, and use a spray dryer to produce granules with an average particle size of 85 JLs. did.
この顆粒をラバー型に充填し、１．５ｔｏｎ／ ｃ ｒ
ｎ’の圧力で加圧成形し、約外径８０ｍ５φ、長さ １
００ｍ＋ｓの密度２．０５／ ｃ ｍ″の生成形体を得
た。This granule is filled into a rubber mold and 1.5 ton/cr
Pressure molded at a pressure of n', approximately outer diameter 80m5φ, length 1
00 m+s with a density of 2.05/cm'' was obtained.
この生成形体を旋盤にて加工し、５０腸鵬φＸ５ｍ層ｔ
の半加工品とした。この旋盤での生加工中においてチッ
ピング等の欠けも発生せず、寸法通りのものを造ること
ができた０次いで、この半加工品をＮ２雰囲気中で８０
０℃で脱脂し、更にＡｒ雰囲気中で２１００℃で５時間
焼結した。その結果、焼結密度が３．１４ｇ／ｃｍ’、
曲げ強度５０ｋｇ／ｍｒｎ’の緻密な焼結体を得ること
ができた。This formed body was processed on a lathe,
It was made into a semi-processed product. During raw machining on this lathe, no chipping or other chips occurred, and we were able to manufacture products with the correct dimensions.Next, this semi-finished product was processed for 80 minutes in an N2 atmosphere.
It was degreased at 0°C and further sintered at 2100°C for 5 hours in an Ar atmosphere. As a result, the sintered density was 3.14 g/cm',
A dense sintered body with a bending strength of 50 kg/mrn' could be obtained.
比較例 ｌ
平均粒径０．４５７１ｍのＳｉＣ微粉末１００重量部に
対し、分子ｉ２４，０００（７） ＰＶＡヲ２．５重量
部、炭化ホウ素粉末を０．６重量部、カーボンプラー２
り粉末を２．５重量部に水を添加し、ボールミル中で２
０時間混合して３５％濃度のスラリーをつくり、スプレ
ードライヤーにて平均粒径６５鉢濡の顆粒を製造した。Comparative Example l For 100 parts by weight of SiC fine powder with an average particle size of 0.4571 m, 2.5 parts by weight of PVA with molecular i24,000(7), 0.6 parts by weight of boron carbide powder, and carbon puller 2
Water was added to 2.5 parts by weight of the powder, and the mixture was mixed in a ball mill for 2.5 parts by weight.
A slurry with a concentration of 35% was prepared by mixing for 0 hours, and granules with an average particle size of 65 were produced using a spray dryer.
この顆粒をラバー型に充填し、 １．５ｔｏｎ／ ｃｍ
’の圧力で加圧成形し、約外径６０ｍｍφ、長さ １０
０履履の密度１．９８７ｃｍ”の生成形体を得た。The granules were filled into a rubber mold, and the volume was 1.5 ton/cm.
Pressure molded at a pressure of ', approximately outer diameter 60mmφ, length 10
A formed body with a density of 1.987 cm'' was obtained.
この生成形体を旋盤にて加工し５０ｍｍφＸ ５ｍｍｔ
の半加工品とした。This formed body is machined on a lathe to a diameter of 50mmφX 5mmt.
It was made into a semi-processed product.
次いで、この半加工品をＮ２雰囲気中で８００℃で脱脂
し、更にＡｒ雰囲気中で２１００℃で５時間焼結した。This blank was then degreased at 800° C. in a N2 atmosphere and further sintered at 2100° C. for 5 hours in an Ar atmosphere.
その結果、焼結密度が３．１２ｇ／ｃｍ”１曲げ強度４
５に８／ｍｒｎ’の焼結体を得た。As a result, the sintered density was 3.12g/cm"1 and the bending strength was 4.
A sintered body of 5 to 8/mrn' was obtained.
実施例 ２
平均粒径０．４５ＢｍのＳｉＣ微粉末１００重量部に対
し、分子量２４．０００（７） ＰＶＡを０．８重量部
１分子ｉ１．５４０と ２００のＰＥＧを；１１＝＝；
＝＝−５１＝□二１に混合した ＰＥＧを１．５重量部
、ステアリン酸を２．５重着部、カーボンブラック粉末
を２．５重社部、炭化ホウ素粉末を０．６重量部に水を
添加し、ボールミル中で２０時間混合して３５％濃度の
スラリーをつくり、スプレードライヤーにて顆粒化した
。Example 2 To 100 parts by weight of SiC fine powder with an average particle size of 0.45 Bm, 0.8 parts by weight of PVA with a molecular weight of 24.000 (7), 1 molecule of i 1.540 and 200 PEG; 11==;
==-51=□21 was mixed with 1.5 parts by weight of PEG, 2.5 parts by weight of stearic acid, 2.5 parts by weight of carbon black powder, and 0.6 parts by weight of boron carbide powder. Water was added and mixed for 20 hours in a ball mill to make a 35% slurry, which was granulated using a spray dryer.
この顆粒をプレス成形機に自動充填し、１．２ｔｏｎ／
ｃ ｒｎ’の圧力で加圧成形し、外径３０■−φ、内
径２０鳳■φ、厚さ ４■■のリング状の生成形体を得
た。The granules were automatically filled into a press molding machine to produce 1.2 tons/
Pressure molding was performed at a pressure of crn' to obtain a ring-shaped product having an outer diameter of 30 mm, an inner diameter of 20 mm, and a thickness of 4 mm.
この生成形体を旋盤にて内面をＲ状に加工し。The inner surface of this formed body is machined into an R shape using a lathe.
次いでＮ２雰囲気中、８００℃で脱脂し、更にＡｒ雰囲
気中２１００℃で５時間焼結した。Next, it was degreased at 800°C in an N2 atmosphere, and further sintered at 2100°C in an Ar atmosphere for 5 hours.
その結果、生加工時によるクラックの発生はなく、バレ
ル研磨後の製品にはほとんどボアは見られなかった。As a result, no cracks occurred during raw processing, and almost no bores were observed in the product after barrel polishing.
比較例 ２
モ均粒径０．４５終ｍのＳｉＣ微粉末１００重量部に対
し、分子ｒｉ２４，０００（７） ＰＶＡを２．０１７
℃部、ステアリン％ヲ２．５重量部、カーボンブラック
粉末を２．５重量部、炭化ホウ素粉末を０．８重量部に
水を添加し、ボールミル中で２０時間混合して３５％濃
度のスラリーをつくり、スプレードライヤーにて顆粒化
した。Comparative Example 2 2.017 parts of PVA with a molecular ri of 24,000 (7) was added to 100 parts by weight of SiC fine powder with an average particle size of 0.45 m.
℃ parts, 2.5 parts by weight of stearin, 2.5 parts by weight of carbon black powder, and 0.8 parts by weight of boron carbide powder, and mixed in a ball mill for 20 hours to make a slurry with a concentration of 35%. was prepared and granulated using a spray dryer.
この顆粒をプレス成形機に自動充填し、２．０ｔｏｎ／
ｃｎｆの圧力で加圧成形し、外径３０５ｍφ、内径２０
Ｉφ、厚さ ４１のリング状の生成形体を得た。This granule was automatically filled into a press molding machine, and 2.0 tons/
Pressure molded with cnf pressure, outer diameter 305mφ, inner diameter 20
A ring-shaped product having an Iφ and a thickness of 41 mm was obtained.
その後、実施例２と同様に脱脂、焼結した。Thereafter, it was degreased and sintered in the same manner as in Example 2.
その結果、生加工時によるクラックの発生はなかったが
、バレル研磨後の製品にボアが見られるものが５００個
中９Ｓ個あった。As a result, no cracks were found during raw processing, but 9 out of 500 products had bores after barrel polishing.
以上説明した様に本成形用バインダーを用いた顆粒は流
動性が良く、低圧加圧でも良く漬れ、成形後の保形性も
良く、複雑形状の製品でも容易に生加工ができ、複雑形
状や大型形状の製品用とし用部材や釣具部材、混合用ポ
ール等として適した焼結体となる。As explained above, granules made using this molding binder have good fluidity, are well soaked even under low pressure, have good shape retention after molding, and can be easily processed into products with complex shapes. The sintered body is suitable for use in large-sized products, fishing gear parts, mixing poles, etc.
Claims (3)
ダーとしてポリビニルアルコールを０．５〜２．０重量
部、ポリエチレングリコールを０．１〜３．０重量部添
加し、焼結助剤を更に加え、顆粒化し、それを用いて成
形、焼結するＳｉＣ焼結体の製造方法。(1) To 100 parts by weight of SiC fine powder, add 0.5 to 2.0 parts by weight of polyvinyl alcohol and 0.1 to 3.0 parts by weight of polyethylene glycol as a molding binder, and further add a sintering aid. In addition, a method for producing a SiC sintered body, which comprises granulating, molding, and sintering the granulated material.
アリン酸を３．５重量部以下添加したＳｉＣ焼結体の製
造方法。(2) A method for producing a SiC sintered body, further comprising 3.5 parts by weight or less of stearic acid as the molding binder according to claim 1.
ダーとして分子量２０，０００〜３０，０００のポリビ
ニルアルコールを０．５〜２．０重量部、分子量１，０
００〜１，５００と分子量１５０〜２５０の２種類のポ
リエチレングリコールを１０：１〜２０：１の範囲で混
合したポリエチレングリコールを１．０〜３．０重量部
、ステアリン酸を０．５〜３．５重量部添加し、更に焼
結助剤を加え、顆粒化し、それを用いて成形、焼結する
ＳｉＣ焼結体の製造方法。(3) 0.5 to 2.0 parts by weight of polyvinyl alcohol with a molecular weight of 20,000 to 30,000 as a molding binder to 100 parts by weight of SiC fine powder, and 1.0 parts by weight of polyvinyl alcohol with a molecular weight of 1.0
1.0 to 3.0 parts by weight of polyethylene glycol, which is a mixture of two types of polyethylene glycol with a molecular weight of 00 to 1,500 and a molecular weight of 150 to 250, in the range of 10:1 to 20:1, and 0.5 to 3 parts of stearic acid. A method for producing a SiC sintered body by adding .5 parts by weight, further adding a sintering aid, granulating it, molding it and sintering it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63127542A JPH01301563A (en) | 1988-02-05 | 1988-05-25 | Production of sintered sic |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-26293 | 1988-02-05 | ||
| JP2629388 | 1988-02-05 | ||
| JP63127542A JPH01301563A (en) | 1988-02-05 | 1988-05-25 | Production of sintered sic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01301563A true JPH01301563A (en) | 1989-12-05 |
| JPH0469110B2 JPH0469110B2 (en) | 1992-11-05 |
Family
ID=26364057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63127542A Granted JPH01301563A (en) | 1988-02-05 | 1988-05-25 | Production of sintered sic |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01301563A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0688746A1 (en) * | 1994-05-27 | 1995-12-27 | Technische Universiteit Delft | Method of manufacturing molded articles from metallic or ceramic powdered particles and binder system suitable for use therein |
| CN108203300A (en) * | 2018-02-07 | 2018-06-26 | 陕西科谷新材料科技有限公司 | A kind of preparation method of high tenacity, high resistivity silicon carbide ceramics |
-
1988
- 1988-05-25 JP JP63127542A patent/JPH01301563A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0688746A1 (en) * | 1994-05-27 | 1995-12-27 | Technische Universiteit Delft | Method of manufacturing molded articles from metallic or ceramic powdered particles and binder system suitable for use therein |
| NL9400879A (en) * | 1994-05-27 | 1996-01-02 | Univ Delft Tech | A method of manufacturing molded articles from metallic or ceramic powder particles as well as a binder system suitable for use therewith. |
| CN108203300A (en) * | 2018-02-07 | 2018-06-26 | 陕西科谷新材料科技有限公司 | A kind of preparation method of high tenacity, high resistivity silicon carbide ceramics |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0469110B2 (en) | 1992-11-05 |
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