JPH03187976A - Ceramic solid solution powder, its production and ceramic solid solution powder sintered compact - Google Patents
Ceramic solid solution powder, its production and ceramic solid solution powder sintered compactInfo
- Publication number
- JPH03187976A JPH03187976A JP1325342A JP32534289A JPH03187976A JP H03187976 A JPH03187976 A JP H03187976A JP 1325342 A JP1325342 A JP 1325342A JP 32534289 A JP32534289 A JP 32534289A JP H03187976 A JPH03187976 A JP H03187976A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- solid solution
- ceramic solid
- solution powder
- ceramic
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 80
- 239000006104 solid solution Substances 0.000 title claims abstract description 52
- 239000000919 ceramic Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000013078 crystal Substances 0.000 claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000005121 nitriding Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000011780 sodium chloride Substances 0.000 claims abstract description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052593 corundum Inorganic materials 0.000 abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 10
- 229910000505 Al2TiO5 Inorganic materials 0.000 abstract description 5
- 230000002829 reductive effect Effects 0.000 abstract description 4
- 238000005255 carburizing Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- 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、新規なセラミック固溶体粉末およびその製法
並びに該固溶体粉末の焼結体に関するものであり、この
固溶体粉末は、靭性と耐摩耗性を必要とする切削工具や
ダイス、抽伸プラグ等の治具、工具類の原料、熱伝導性
と耐熱衝撃性を必要とするセラミックヒータ−等の電子
分量類の原料、或は耐食性、耐酸化性、耐摩耗性、破壊
靭性等を必要とするメカニカルシールやポンプ等の機械
部品類の原料として有用である。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a novel ceramic solid solution powder, a method for producing the same, and a sintered body of the solid solution powder. The necessary cutting tools, dies, drawing plugs and other jigs, raw materials for tools, electronic materials such as ceramic heaters that require thermal conductivity and thermal shock resistance, or corrosion resistance, oxidation resistance, It is useful as a raw material for mechanical parts such as mechanical seals and pumps that require wear resistance and fracture toughness.
［従来の技術］
ＴｉＣやＴｉＮよりなるセラミックは耐食性および耐摩
耗性に優れたものであるところから、各種セラミック部
品やサーメット、超硬材料、Ｃ−ＢＮ焼結体等の主原料
あるいは副原料として多用さ、れている。[Prior Art] Ceramics made of TiC and TiN have excellent corrosion resistance and wear resistance, so they are used as main or auxiliary raw materials for various ceramic parts, cermets, cemented carbide materials, C-BN sintered bodies, etc. Frequently used.
しかしながら上記のセラミックは耐酸化性が乏しく且つ
熱伝導性が小さいという欠点がある。そこでこうした欠
点を改善するものとして、ＴｉＮにＡＩＮを固溶させた
（Ｔｉ、ＡＩ）Ｎ系のコーテイング膜が開発された（た
とえば特開昭６２−５６５６５号等）。このＴｉＮ−Ａ
ＩＮ系固溶固溶体なるコーテイング膜は、ＴｉＮに比べ
て耐酸化性や熱伝導性に優れ且つ高い硬度を有している
ところから、切削工具等の表面コーテイング材として優
れた性能を発揮する。However, the above ceramics have the drawbacks of poor oxidation resistance and low thermal conductivity. In order to improve these drawbacks, a (Ti, AI)N-based coating film in which AIN is dissolved in TiN has been developed (for example, JP-A-62-56565). This TiN-A
A coating film made of an IN-based solid solution exhibits excellent performance as a surface coating material for cutting tools and the like because it has superior oxidation resistance and thermal conductivity and high hardness compared to TiN.
［発明が解決しようとする課題］
ところが従来の（Ｔｉ、ＡＩ）Ｎ系固溶体は、基材表面
にスパッタリング等によりコーテイング膜として形成さ
れているだけであって、粉末状態のものとして提供され
た例はない。その理由は次の様に考えられる。即ちＴｉ
ＮはＮａＣｌ型の結晶構造を有しているのに対し、ＡＩ
Ｎの結晶構造は６方最密構造であるため、通常のセラミ
ック原料溶解法や粉末焼結法では両者を固溶体化するこ
とができなかったからである。[Problems to be Solved by the Invention] However, conventional (Ti, AI)N-based solid solutions are only formed as a coating film on the surface of a base material by sputtering, etc., and are provided in powder form. There isn't. The reason may be as follows. That is, Ti
While N has a NaCl-type crystal structure, AI
This is because the crystal structure of N is a hexagonal close-packed structure, and therefore it was not possible to form both into a solid solution using ordinary ceramic raw material melting methods or powder sintering methods.
そのため（Ｔｉ、ＡＩ）Ｎ系固溶体は、スパッタリング
法やイオンブレーティング法により薄膜状としてその優
れた特性を享受し得るに留まり、その優れた耐酸化性、
熱伝導性、硬度等の特性を他の分野で有効に生かすこと
がで艶なかった。Therefore, the (Ti, AI)N-based solid solution can only enjoy its excellent properties in the form of a thin film by sputtering or ion blating, and its excellent oxidation resistance,
It was difficult to make effective use of its properties such as thermal conductivity and hardness in other fields.
本発明はこの様な事情に着目してなされたものであって
、その目的は、高硬度で耐酸化性および熱伝導性等の優
れた（Ｔｉ、ＡＩ）（Ｃ，Ｎ）系の固溶体を粉末状のも
のとして提供しようとするものであり、他の目的はその
様な粉末状固溶体を容易に得る。ことのできる方法を確
立しようとするものであり、更に他の目的は（Ｔｉ、Ａ
Ｉ）（Ｃ，Ｎ）系固溶体の焼結体を提供しようとするも
のである。The present invention was made in view of these circumstances, and its purpose is to create a (Ti, AI) (C, N)-based solid solution with high hardness and excellent oxidation resistance and thermal conductivity. It is intended to be provided as a powder, and another purpose is to easily obtain such a powder solid solution. The purpose of this study is to establish a method by which (Ti, A
I) The present invention aims to provide a sintered body of a (C,N)-based solid solution.
［課題を解決するための手段］
上記課題を解決することのできた本発明に係る固溶体粉
末とは、
（Ｔ １ ＋ −ｘ Ａ １１１） （Ｃｙ Ｎｔ Ｏ
□−ｙ−ｔ） ａ［但し、０≦ｘ≦０．７．０≦ｙ≦１
．０≦ｚ≦１ 、０．ｆｉ ＜ａ＜１．０ ］の化化学
酸を有し、ＮａＣｌ型結晶構造を有するセラミック固溶
体粉末からなるところに要旨を有するものであり、この
セラミック固溶体粉末は、ＴｉＯ２粉末とＡｌ２Ｏ３粉
末よりなる混合粉末またはＡｌ２ＴｉＯ５粉末、あるい
はＡ １２ Ｔ ｔ Ｏ、粉末と、ＴｉＯ２粉末および
／もしくはＡｌ２Ｏ３粉末との混合粉末を、還元性霊囲
気下で窒化および／もしくは炭化する過程で固溶化する
ことによって製造することができ、またこのセラミック
固溶体粉末を圧粉成形して焼結すると、高硬度で耐酸化
性および熱伝導性等の優れた任意形状の焼結体を得るこ
とができる。[Means for Solving the Problems] The solid solution powder according to the present invention that can solve the above problems is (T 1 + -x A 111) (Cy Nt O
□-y-t) a[However, 0≦x≦0.7.0≦y≦1
．． 0≦z≦1, 0. fi < a < 1.0 ], and consists of a ceramic solid solution powder having a NaCl type crystal structure. This ceramic solid solution powder is a mixture of TiO2 powder and Al2O3 powder. Producing a powder or Al2TiO5 powder, or a mixed powder of A 12 T t O, powder, and TiO2 powder and/or Al2O3 powder by solid solutioning it in the process of nitriding and/or carbonizing under a reducing atmosphere. When this ceramic solid solution powder is compacted and sintered, a sintered body of any shape with high hardness and excellent oxidation resistance and thermal conductivity can be obtained.
［作用］
前述の如＜ＴｉＮとＡＩＮは結晶構造が全く異なるもの
であるから、これらを混合溶融しあるいは粉末焼結した
としても（ＴｉＡ１）Ｎよりなる固溶体粉末を得ること
ができず、またこの処理系にＣ源を共存させたとしても
（Ｔ ｉ 、 Ａ Ｉ）（Ｃ。[Function] As mentioned above, since TiN and AIN have completely different crystal structures, even if they are mixed and melted or powder sintered, a solid solution powder consisting of (TiA1)N cannot be obtained; Even if a C source coexists in the processing system, (T i , A I) (C.
Ｎ）よりなる固溶体粉末を得ることはできない。It is not possible to obtain a solid solution powder consisting of N).
一方、ＴｉおよびＡ１の酸化物であるＴ ｉ Ｏ２とＡ
ｌ２Ｏ３はいずれも結晶構造がＮａＣｌ型で類似してお
り、これらの混合物を加熱処理するとＡｌ２ＴｉＯ５よ
りなる固溶体を容易に得ることができる。そこで本発明
者らは出発原料としてＮａＣ’ｌ型結晶構造のＴｉＯ２
およびＡｌ２Ｏ３を用いてこれをＡ１２ＴｉＯＢ固溶体
に代え、或は出発原料としてＡ１ｚＴｉＯＢ粉末を使用
し、これを還元窒化して窒化物および／もしくは炭化物
に変えれば、粉末状の（Ｔｉ、ＡＩ）（Ｃ。On the other hand, T i O2, which is an oxide of Ti and A1, and A
Both l2O3 have similar crystal structures of the NaCl type, and a solid solution of Al2TiO5 can be easily obtained by heat-treating a mixture of these. Therefore, the present inventors used TiO2 with NaC'l type crystal structure as a starting material.
If this is replaced with an A12TiOB solid solution by using and Al2O3, or by using A1zTiOB powder as a starting material and reducing and nitriding it to convert it into a nitride and/or carbide, powdered (Ti, AI) (C) can be obtained.
Ｎ、Ｏ）固溶体が得られるのではないかと考え、研究を
進めた。We thought that it might be possible to obtain a solid solution (N, O), and proceeded with our research.
その結果、ＴｉＯ２粉末とＡｌ２Ｏ３粉末よりなる混合
粉末またはＡ１２Ｔｉ０６粉末、あるいはＡｌ２ＴｉＯ
５粉末とＴ ｉ Ｏ２粉末および／もしくはＡｌ２Ｏ３
粉末との混合粉末を、還元性雰囲気下で窒化および／も
しくは炭化すると共に、該窒化および／もしくは炭化す
る過程で固溶化すれば（Ｔｉ、ＡＩ）（’Ｃ，Ｎ、、Ｏ
）よりなるＮａＣｌ型結晶構造の固溶体が粉末状物とし
て容易に得られることを知った。As a result, a mixed powder consisting of TiO2 powder and Al2O3 powder, A12Ti06 powder, or Al2TiO
5 powder and T i O2 powder and/or Al2O3
If the mixed powder with powder is nitrided and/or carbonized in a reducing atmosphere and made into a solid solution during the nitriding and/or carbonizing process, (Ti, AI) ('C, N,, O
) was found to be easily obtained as a powder with a NaCl-type crystal structure.
尚、本発明においては、固溶体粉末の化学組成を
（Ｔ ｉ （−８Ａ Ｉ ＋１） （Ｃｙ Ｎ ｚ
Ｏ＋−ｙ−ｚ）ａ ・・・［１］但し、０＜ｘ≦０．
７
０≦ｙ≦１
０≦ｚ≦１
０．９≦ （ｙ＋ｚ） ≦１．０
ｏ、６＜ ａ ＜ １．０
に特定するが、上記化学組成の設定理由は次の通りであ
る。In the present invention, the chemical composition of the solid solution powder is (T i (-8A I +1) (Cy N z
O+-y-z)a ... [1] However, 0<x≦0.
7 0≦y≦1 0≦z≦1 0.9≦(y+z)≦1.0 o, 6<a<1.0 The reason for setting the above chemical composition is as follows.
まず［＋１式においてＸがＯであるものは、金属成分中
にＡＩが含まれていないことを意味するものであって、
当然のことながら複合セラミック固溶体としての特性が
発揮されない。しかしＸが０．７を超えると、固溶体中
のＡＩが固溶限界を超えることになり、原料であるＡｌ
２Ｏ３が残留して希望物性が低下する。First, in the formula [+1, X is O, which means that AI is not included in the metal component,
Naturally, the properties as a composite ceramic solid solution are not exhibited. However, when X exceeds 0.7, AI in the solid solution exceeds the solid solution limit, and the raw material Al
2O3 remains and desired physical properties deteriorate.
次にｙと２は０〜１の全範囲に及び得るものであり、０
．９≦（ｙ＋ｚ）≦１．０の要件を満たす限りあらゆる
組合せが可能である。たとえば（Ｃ１Ｎ、０）の実現可
能な組合せとしては、ＮおよびＯが零でＣが１００％を
占めるものＣおよび０が零でＮが１００％を占めるもの
０が零で（Ｃ＋Ｎ）が１００％を占めるもの０が零以上
０．１以下で（Ｃ＋Ｎ）が０．９〜１．０であるもの
が挙げられ、これらのうちどの要件に当てはまるもので
あってもよい。しかしくｙ＋ｚ）が０．９未満であるも
のは必然的に０が０．１を超えるものとなり、固溶体中
にＴｉｏ２．Ａｌ２Ｏ，またはＡｌ２ＴｉＯ５の酸化物
が残留することになるので、（Ｃ＋Ｎ’）は０．９以上
となる様に残留酸素量を抑えなければならない。Next, y and 2 can span the entire range from 0 to 1, and 0
．． Any combination is possible as long as the requirement of 9≦(y+z)≦1.0 is satisfied. For example, possible combinations of (C1N, 0) include: N and O are zero and C occupies 100%; C and 0 are zero and N occupies 100%; 0 is zero and (C+N) is 100%. Examples include those in which 0 is 0 or more and 0.1 or less, and (C+N) is 0.9 to 1.0, and any of these requirements may be met. However, if y+z) is less than 0.9, 0 will inevitably exceed 0.1, and Tio2. Since oxides of Al2O or Al2TiO5 will remain, the amount of residual oxygen must be suppressed so that (C+N') is 0.9 or more.
またａが０．６以下であるものは、固溶体中にフリーの
ＴｉやＡＩが残存し、一方１．０以上になるとＴｉＯ２
やＡｌ２Ｏ３が残留したりフリーカーボンが析出してく
る。In addition, when a is 0.6 or less, free Ti and AI remain in the solid solution, while when a is 1.0 or more, TiO2
and Al2O3 remain and free carbon precipitates.
従って本発明のセラミック固溶体粉末を製造するに当た
っては、上記［１，１式の化学、組成を満たす様にＴｉ
Ｏ２粉末、Ａｌ２Ｏ３粉末もしくはＡ１２ＴｉＯ，粉末
の配合量を設定すると共に、添加するＣ量を設定し、且
つ炭・窒化条件を適正にコントロールしなければならな
い、。尚、炭・窒化の為の炭素源としてはカーボンブラ
ック等が最も一般的であり、窒素源としては窒素ガスが
最も一般的である。従って本発明方法を実施するに当た
っては、上記の酸化物粉末に適量のカーボンブラック等
を配合し、これを窒素ガス雰囲気下で１０００〜２００
０℃程度に加熱して酸化物を炭・窒化物に変換すると共
に固溶化させればよく、該炭・窒化条件（炭素配合量、
加熱温度、窒素圧力等）をうまく制御して残存酸素量を
前述の許容範囲以下に低減することにより、目的とする
セラミック固溶体粉末を得ることができる。このとき前
記［＋１式におけるＣとＮの組成比率は、酸化物粉末中
に混入されるＣ源の添加量によって調整すればよい。
かくして得られる固溶体はＮａＣｌ型の結晶構造を有す
る粉末であり、この粉末はＴｉＮに比べて耐酸化性、熱
伝導性および硬度の非常に優れたものである。しかもこ
の粉末は圧粉成形後焼結することによって任意の形状に
加工することができるので、その優れた特徴を様々の分
野に亘って幅広く活用することが可能となる。Therefore, in producing the ceramic solid solution powder of the present invention, Ti
It is necessary to set the blending amount of O2 powder, Al2O3 powder or A12TiO powder, set the amount of C to be added, and appropriately control the carbonization and nitriding conditions. The most common carbon source for carbonization and nitriding is carbon black, and the most common nitrogen source is nitrogen gas. Therefore, when carrying out the method of the present invention, an appropriate amount of carbon black, etc. is blended with the above oxide powder, and this is mixed with 1,000 to 200
It is sufficient to heat the oxide to about 0°C to convert the oxide to carbon/nitride and make it a solid solution, and the carbon/nitriding conditions (carbon content,
The desired ceramic solid solution powder can be obtained by skillfully controlling the heating temperature, nitrogen pressure, etc. to reduce the amount of residual oxygen below the above-mentioned allowable range. At this time, the composition ratio of C and N in the formula [+1] may be adjusted by the amount of the C source mixed into the oxide powder.
The solid solution thus obtained is a powder having a NaCl type crystal structure, and this powder has much better oxidation resistance, thermal conductivity, and hardness than TiN. Moreover, since this powder can be processed into any shape by compacting and sintering, its excellent characteristics can be widely utilized in various fields.
以下、実施例を挙げて本発明を具体的に説明するが、本
発明はもとより下記実施例によって制限を受けるもので
はない。EXAMPLES Hereinafter, the present invention will be specifically explained with reference to examples, but the present invention is not limited by the following examples.
［実、施例］
ゑ】■１１
ＴｉＯ、粉末とＡ、１２０３粉−末を第１表、に示す比
率で配合し、こガ・にカーボンブラックを２０重量％添
加した後、笹媒中で湿式混合し乾燥した。[Examples] E]■11 TiO, powder and A, 1203 powder were blended in the ratio shown in Table 1, and after adding 20% by weight of carbon black to Koga, in a bamboo medium. Wet mixed and dried.
得られた混合粉末を、窒素雰囲気下１６００℃で２時間
加熱することにより還元、窒化を行なった。The obtained mixed powder was reduced and nitrided by heating at 1600° C. for 2 hours in a nitrogen atmosphere.
得られた各粉末の結晶構造をＸ線回折法により調べると
共に、各粉末を窒素雰囲気中１７００℃で３０分ホット
プレスして焼結成形体とし硬度を調べた。結果は第１表
に一括して示す通りであり、いずれもＮａＣｌ型結晶構
造のＢｌ型固溶体単相であって高い硬度を有しているこ
とが分かる。The crystal structure of each of the obtained powders was examined by X-ray diffraction, and each powder was hot-pressed at 1700° C. for 30 minutes in a nitrogen atmosphere to form a sintered compact, and its hardness was examined. The results are summarized in Table 1, and it can be seen that all of the samples were single-phase Bl-type solid solutions with an NaCl-type crystal structure and had high hardness.
上記実験Ｎ０１３で得た粉末のＸ線回折チャートを代表
して第１図に示す、また該固溶体粉末の化学分析結果は
第２表に示す通りであり、（Ｔｉｏ、ａ。ＡＩｏ、４゜
） （ｃ ０．４゜Ｎｏ、６゜）。９８の化学組成を有
するものであった。The X-ray diffraction chart of the powder obtained in the above experiment No. 13 is shown in FIG. 1 as a representative, and the chemical analysis results of the solid solution powder are as shown in Table 2. (Tio, a. AIo, 4°) (c 0.4°No, 6°). It had a chemical composition of 98.
１
夾直■ｌ
Ｔｉ０ｚ粉末とＡｌ２Ｏ３粉末を第３表に示す比率で配
合し、溶媒中で湿式混合した後乾燥した。この混合粉末
を大気雰囲気中１３００℃で２時間焼成した。この焼結
粉末は、Ｘ線回折分析の結果Ａ１．ＴｉＯ舊相とＴｉ１
２相の２相であることが確認された。1. TiOz powder and Al2O3 powder were mixed in the ratio shown in Table 3, wet mixed in a solvent, and then dried. This mixed powder was fired at 1300° C. for 2 hours in an air atmosphere. The result of X-ray diffraction analysis of this sintered powder was A1. TiO 舊phase and Ti1
It was confirmed that there were two phases.
上記で得た焼結粉末にカーボンブラックを２０重量％配
合して溶媒中で湿式混合した後乾燥し、次いで窒素雰囲
気中１６００℃で２時間加熱して還元窒化を行なりた。20% by weight of carbon black was blended into the sintered powder obtained above, wet mixed in a solvent, dried, and then heated at 1600° C. for 2 hours in a nitrogen atmosphere to perform reductive nitridation.
得られた還元窒化粉末をＸ線回折により構成相の同定を
行なうと共に、該粉末を窒素雰囲気下に１７００℃×３
０分でホットプレスして得た焼結体の硬度を測定し、第
３表に示す結果を得た。The constituent phases of the obtained reduced nitrided powder were identified by X-ray diffraction, and the powder was heated at 1700°C x 3 in a nitrogen atmosphere.
The hardness of the sintered body obtained by hot pressing for 0 minutes was measured, and the results shown in Table 3 were obtained.
比較例１．２
Ｔ ｉ ０２粉末とＡｌ２Ｏ，粉末を第４表に示す比率
で混合し、これにカーボンブラックを２０重量％添加し
た後、実施例１または実施例２と同様にして還元窒化処
理を行なった。Comparative Example 1.2 Ti02 powder, Al2O, and powder were mixed in the ratio shown in Table 4, and 20% by weight of carbon black was added thereto, followed by reduction nitriding treatment in the same manner as in Example 1 or Example 2. I did this.
得られた粉末の構成相同定結果と、実施例１と同様にし
て得た焼結体の硬度を第４．５表に示す。The results of identifying the constituent phases of the obtained powder and the hardness of the sintered body obtained in the same manner as in Example 1 are shown in Table 4.5.
第４．５表からも明らかである様に、配合原料中のＡ１
成分が多過ぎる場合は、得られる固溶体のＡｌ固溶限界
を超えて系中にＡｌ２Ｏ５が残留し、目的とするＢｌ型
固溶体単相のものが得られなくなる。As is clear from Table 4.5, A1 in the blended raw materials
If there are too many components, Al2O5 will remain in the system exceeding the Al solid solution limit of the resulting solid solution, making it impossible to obtain the desired single-phase Bl type solid solution.
５
［発明の効果］
本発明は以上の様に構成されており、従来は薄膜状でし
か得ることのできなかった（Ｔｉ。5 [Effects of the Invention] The present invention is configured as described above, and conventionally it could only be obtained in the form of a thin film (Ti.
ＡＩ）（Ｃ，Ｎ）系のセラミック固溶体を粉末状として
得ることができ、圧粉成形後焼結することによって任意
の形状に加工することができるので、ＴｉＮ系セラミッ
クの耐酸化性、熱伝導性および硬度を改善したものとし
て、冒頭で示した様な種々の用途に亘って幅広く活用し
得ることになった。AI) (C,N)-based ceramic solid solution can be obtained in powder form, and can be processed into any shape by compacting and sintering, which improves the oxidation resistance and thermal conductivity of TiN-based ceramics. As a product with improved properties and hardness, it can now be used in a wide variety of applications as mentioned at the beginning.
Claims (5)
＿１＿−ｙ＿−＿ｚ）＿ａ［但し、０≦ｘ≦０．７，０
≦ｙ≦１，０≦ｚ≦１，０．９＜（ｙ＋ｚ）≦１．０，
０．６＜ａ＜１．０］ の化学組成を有し、ＮａＣｌ型結晶構造を有するもので
あることを特徴とするセラミック固溶体粉末。(1) (Ti_1_-_xAl_x) (C_yN_zO
_1_-y_-_z)_a [However, 0≦x≦0.7,0
≦y≦1,0≦z≦1,0.9<(y+z)≦1.0,
A ceramic solid solution powder having a chemical composition of 0.6<a<1.0] and a NaCl type crystal structure.
合粉末を、還元性雰囲気下で窒化および／もしくは炭化
する過程で固溶化し、請求項（１）記載のセラミック固
溶体粉末を得ることを特徴とするセラミック固溶体粉末
の製法。(2) A ceramic solid solution characterized in that a mixed powder of TiO_2 powder and Al_2O_3 powder is made into a solid solution in the process of nitriding and/or carbonizing in a reducing atmosphere to obtain the ceramic solid solution powder according to claim (1). Powder manufacturing method.
化および／もしくは炭化する過程で固溶化し、請求項（
１）記載のセラミック固溶体粉末を得ることを特徴とす
るセラミック固溶体粉末の製法。(3) Al_2TiO_5 powder is made into a solid solution in the process of nitriding and/or carbonizing in a reducing atmosphere, and
1) A method for producing a ceramic solid solution powder, which is characterized by obtaining the ceramic solid solution powder as described above.
／もしくはＡｌ＿２Ｏ＿３粉末との混合粉末を、還元性
雰囲気下で窒化および／もしくは炭化する過程で固溶化
し、請求項（１）記載のセラミック固溶体粉末を得るこ
とを特徴とするセラミック固溶体粉末の製法。(4) A mixed powder of Al_2TiO_5 powder and TiO_2 powder and/or Al_2O_3 powder is made into a solid solution in the process of nitriding and/or carbonizing in a reducing atmosphere to obtain the ceramic solid solution powder according to claim (1). Characteristic manufacturing method of ceramic solid solution powder.
セラミック固溶体粉末焼結体。(5) A ceramic solid solution powder sintered body obtained by sintering the solid solution powder according to claim (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1325342A JPH03187976A (en) | 1989-12-14 | 1989-12-14 | Ceramic solid solution powder, its production and ceramic solid solution powder sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1325342A JPH03187976A (en) | 1989-12-14 | 1989-12-14 | Ceramic solid solution powder, its production and ceramic solid solution powder sintered compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03187976A true JPH03187976A (en) | 1991-08-15 |
Family
ID=18175739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1325342A Pending JPH03187976A (en) | 1989-12-14 | 1989-12-14 | Ceramic solid solution powder, its production and ceramic solid solution powder sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03187976A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102094165A (en) * | 2010-12-27 | 2011-06-15 | 北京工业大学 | Highly wear-resistant mechanical seal moving ring and manufacturing method thereof |
-
1989
- 1989-12-14 JP JP1325342A patent/JPH03187976A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102094165A (en) * | 2010-12-27 | 2011-06-15 | 北京工业大学 | Highly wear-resistant mechanical seal moving ring and manufacturing method thereof |
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