JPS6256108B2 - - Google Patents
Info
- Publication number
- JPS6256108B2 JPS6256108B2 JP59162477A JP16247784A JPS6256108B2 JP S6256108 B2 JPS6256108 B2 JP S6256108B2 JP 59162477 A JP59162477 A JP 59162477A JP 16247784 A JP16247784 A JP 16247784A JP S6256108 B2 JPS6256108 B2 JP S6256108B2
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- magnesium
- boron nitride
- composite
- lithium
- 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.)
- Expired
Links
- 239000002131 composite material Substances 0.000 claims description 30
- 229910052582 BN Inorganic materials 0.000 claims description 22
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 20
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 20
- 229910052744 lithium Inorganic materials 0.000 claims description 20
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 8
- 150000004767 nitrides Chemical class 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 description 44
- 229910052749 magnesium Inorganic materials 0.000 description 39
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 32
- 238000000034 method Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- -1 alkaline earth metal nitride Chemical class 0.000 description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 10
- 229910052750 molybdenum Inorganic materials 0.000 description 10
- 239000011733 molybdenum Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 239000011575 calcium Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 235000012245 magnesium oxide Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical class [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
【発明の詳細な説明】
本発明は立方晶窒化ほう素焼結体製造用複合体
及びその製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a composite for producing a cubic boron nitride sintered body and a method for producing the same.
従来(1)立方晶窒化ほう素（以下cBNと記載す
る）の合成法として、六方晶窒化ほう素（以下
hBNと記載する）にアルカリ金属又はアルカリ土
類金属の窒化物あるいはほう窒化物を混合し、こ
れを高圧高温下で処理して製造する方法が知られ
ている。 Conventionally (1) cubic boron nitride (hereinafter referred to as cBN) has been synthesized using hexagonal boron nitride (hereinafter referred to as cBN).
A known method is to mix alkali metal or alkaline earth metal nitride or boron nitride with hBN and process the mixture under high pressure and high temperature.
また(2)cBN焼結体の製法として、hBNにマグネ
シウムのほう窒化物を混合して高圧高温下で焼結
する方法が本出願人により開発された（特願昭57
−57549号）。 (2) As a manufacturing method for cBN sintered bodies, the applicant has developed a method in which hBN is mixed with magnesium boronitride and sintered under high pressure and high temperature.
−57549).
これらの方法におけるアルカリ金属又はアルカ
リ土類金属のほう窒化物への混合は、従来機械的
な手段によつて行われている。機械的混合では、
アルカリ金属又はアルカリ土類金属のほう窒化物
を分散度が高く、また均一分散させることは非常
に困難であり、その上、均一に混合するため、長
時間混合すると、アルカリ金属、アルカリ土類金
属のほう窒化物（ただし、窒化ほう素マグネシウ
ムを除く）は湿気との反応性が強く活性を失い易
いので得られる物の品質低下を来す欠点があつ
た。 The mixing of alkali metals or alkaline earth metals into boronitrides in these methods has conventionally been carried out by mechanical means. In mechanical mixing,
Bonitrides of alkali metals or alkaline earth metals have a high degree of dispersion, and it is very difficult to disperse them uniformly. Boron nitrides (excluding magnesium boron nitride) have a drawback in that they are highly reactive with moisture and tend to lose their activity, resulting in a decrease in the quality of the products obtained.
そのため、高品位のcBNが得られなく、また、
cBN焼結体は透光性のものが得られるが、製品に
雲状、点状のくもりや、黄色の着色が見られる
等、良質なものが得られない欠点があつた。 Therefore, high-quality cBN cannot be obtained, and
Although cBN sintered bodies can be made translucent, they have drawbacks such as cloud-like or dot-like cloudiness or yellow coloring, which prevents the production of high-quality products.
本発明の目的は、機械的の混合によらず、hBN
焼結体にリチウム又はアルカリ土類金属のほう窒
化物あるいはこれらの混合物を均一に分散させた
立方晶窒化ほう素製造用複合体（以下BN複合体
という）及びその製造法を提供するにある。 The object of the present invention is to produce hBN without mechanical mixing.
The present invention provides a composite for manufacturing cubic boron nitride (hereinafter referred to as BN composite) in which lithium or alkaline earth metal boronitride or a mixture thereof is uniformly dispersed in a sintered body, and a method for manufacturing the same.
本発明者らは、前記目的を達成すべく研究の結
果、hBN焼結体と、リチウム又はアルカリ土類金
属、それらの窒化物もしくはほう窒化物あるいは
これらの混合物を接触下又は非接触下で加熱する
と、hBN焼結体中に拡散し、均一に分散されると
共に、リチウム又はアルカリ土類金属のほう窒化
物あるいはこれらの混合物を形成担持されること
を知見し得た。この知見に基いて本発明を完成し
た。 In order to achieve the above object, the present inventors conducted research and found that the hBN sintered body and lithium or alkaline earth metals, their nitrides or boronitrides, or mixtures thereof were heated in contact or non-contact. As a result, it was found that hBN was diffused and uniformly dispersed in the hBN sintered body, and that lithium or alkaline earth metal boronitride or a mixture thereof was formed and supported. The present invention was completed based on this knowledge.
本発明はhBN焼結体にリチウム又はアルカリ土
類金属あるいはこれらの混合物をほう窒化物とし
て拡散担持させたものからなる新しい焼結複合体
及びその製造法にある。 The present invention resides in a new sintered composite comprising an hBN sintered body in which lithium or an alkaline earth metal or a mixture thereof is diffusely supported as a boronitride, and a method for manufacturing the same.
その製造法はhBN焼結体と、リチウム又はアル
カリ土類金属、それらの窒化物もしくはほう窒化
物あるいはこれらの混合物を接触させて、非酸化
雰囲気中で加熱して、hBN焼結体にリチウム又は
アルカリ土類金属あるいはこれらの混合物を拡散
させてほう窒化物として担持させる方法。また、
hBN焼結体をるつぼに入れ、リチウム又はアルカ
リ土類金属、それらの窒化物もしくはほう窒化物
あるいはこれらの混合物を非酸化雰囲気下の加熱
によりるつぼ外からるつぼ内に拡散させて、hBN
焼結体にほう窒化物として担持させる方法があ
る。 The manufacturing method is to bring the hBN sintered body into contact with lithium or an alkaline earth metal, their nitride or boronitride, or a mixture thereof, and heat the mixture in a non-oxidizing atmosphere to inject lithium or alkaline earth metal into the hBN sintered body. A method in which alkaline earth metals or their mixtures are diffused and supported as boronitrides. Also,
The hBN sintered body is placed in a crucible, and lithium or alkaline earth metals, their nitrides, boron nitrides, or mixtures thereof are diffused from outside the crucible into the crucible by heating in a non-oxidizing atmosphere to form hBN.
There is a method in which boronitride is supported on a sintered body.
例えば、モリブデン製るつぼにリチウム又は
Mg、Ca、Ba、Sr等のアルカリ土類金属、それら
の窒化物もしくはほう窒化物あるいはこれらの混
合物を入れ、この中にBN焼結体を埋め込み加熱
する。 For example, lithium or
Alkaline earth metals such as Mg, Ca, Ba, and Sr, their nitrides or boronitrides, or mixtures thereof are placed, and a BN sintered body is embedded in the metal and heated.
hBN焼結体は酸素、炭素の不純物を除去して使
用する。例えばhBN焼結体を黒鉛発熱体を用いて
2100℃に加熱した後、モリブデン炉で更に同様に
加熱することによつて除去し得られる。また、
hBN焼結体としては多孔質（例えば気孔率約14
％）の焼結体であること、及びその大きさが余り
大きいとリチウム又はアルカリ土類金属（以下、
代表例としてマグネシウムとして記載する）を内
部まで均一に拡散分散させるのに長時間を要する
ので、必要最小限の大きさであることが望まし
い。 The hBN sintered body is used after removing oxygen and carbon impurities. For example, using an hBN sintered body with a graphite heating element,
After heating to 2100°C, it can be removed by further heating in a molybdenum furnace. Also,
The hBN sintered body is porous (for example, the porosity is about 14
%), and if the size is too large, lithium or alkaline earth metal (hereinafter referred to as
Since it takes a long time to uniformly diffuse and disperse magnesium (described as magnesium as a typical example) to the inside, it is desirable that the size is the minimum necessary.
マグネシウム等のアルカリ土類金属またはリチ
ウム（以下その代表としてマグネシウムと記載す
る。）粉末の粒径は、重要な要素ではない。しか
し大き過ぎると、マグネシウム粒間の隙間が大き
くなるため、hBN焼結体中へ浸入する気相成分が
るつぼ外への散逸が多くなるので好ましくない。
また微粒すぎると高純度品が得にくく、マグネシ
ウムの酸化物が悪影響を与えるので、粒径は約１
mm程度が望ましい。 The particle size of alkaline earth metal such as magnesium or lithium (hereinafter referred to as magnesium as a representative) powder is not an important factor. However, if it is too large, the gaps between the magnesium grains will become large, which is not preferable because the gas phase components that have entered the hBN sintered body will dissipate to the outside of the crucible.
Also, if the particles are too fine, it will be difficult to obtain a high-purity product, and magnesium oxides will have an adverse effect, so the particle size should be approximately 1.
Approximately mm is desirable.
加熱炉の部材は、マグネシウム、その窒化物も
しくはほう窒化物と反応を起さないものであれば
よく、例えばモリブデンを発熱体及び断熱材とし
て用いられる。 The heating furnace member may be any material as long as it does not react with magnesium, its nitride, or boronitride. For example, molybdenum may be used as a heating element and a heat insulating material.
加熱雰囲気は非酸化性雰囲気であることが必要
である。そうでないと本発明の窒化ほう素焼結複
合体は得られない。マグネシウムが金属単体であ
る場合には、窒素又はアンモニアの雰囲気である
ことが必要である。 The heating atmosphere needs to be a non-oxidizing atmosphere. Otherwise, the boron nitride sintered composite of the present invention cannot be obtained. When magnesium is an elemental metal, a nitrogen or ammonia atmosphere is required.
その製造に際しては、炉内を十分真空排気した
後、例えば窒素ガスを導入して窒素雰囲気とし、
高周波等で加熱する。昇温は徐々に行い、640℃
で２時間保持した後、800℃で５時間保持し、さ
らに1150℃で５時間保持するとBN複合体が得ら
れる。急激な昇温はマグネシウムの急激な溶融
（融点650℃）、蒸発（沸点1150℃）をまねき、さ
らには焼結体の表面に緻密なほう窒化マグネシウ
ム膜を形成し、内部へのマグネシウムの均一な拡
散が阻害されるので、hBN焼結体中にマグネシウ
ムが浸入拡散するに十分な温度までマグネシウム
を安定に存在させておくことが望ましい。前記の
640℃、800℃での保持はマグネシウムを窒化物と
して安定化するためである。この意味でマグネシ
ウム金属よりも窒化マグネシウム、ほう窒化マグ
ネシウムとして使用することが好ましい。 When manufacturing it, after thoroughly evacuating the inside of the furnace, for example, nitrogen gas is introduced to create a nitrogen atmosphere.
Heating with high frequency etc. The temperature was gradually increased to 640℃.
After holding at 800°C for 2 hours, holding at 800°C for 5 hours, and further holding at 1150°C for 5 hours, a BN composite is obtained. Rapid temperature rise causes rapid melting (melting point: 650℃) and evaporation (boiling point: 1150℃) of magnesium, and also forms a dense magnesium boronitride film on the surface of the sintered body, preventing the uniform distribution of magnesium inside. Since diffusion is inhibited, it is desirable to allow magnesium to stably exist up to a temperature sufficient for magnesium to infiltrate and diffuse into the hBN sintered body. the above
The purpose of holding at 640°C and 800°C is to stabilize magnesium as nitride. In this sense, it is preferable to use magnesium nitride or magnesium boronitride rather than magnesium metal.
最終的な加熱温度はBN複合体の使用目的に応
じたマグネシウムのほう窒化物の含有量及び濃度
分散の均一性を考慮して選べばよい。通常1000〜
1300℃である。cBN透明焼結体用では、1150℃で
５時間加熱することによつて十分な性能を持つ含
マグネシウムほう窒化物のBN焼結複合体が得ら
れる。 The final heating temperature may be selected in consideration of the content of magnesium boronitride and the uniformity of concentration distribution depending on the intended use of the BN composite. Usually 1000~
The temperature is 1300℃. For cBN transparent sintered bodies, a BN sintered composite of magnesium-containing boronitride with sufficient performance can be obtained by heating at 1150°C for 5 hours.
hBN焼結体が微細な場合は、これらとマグネシ
ウム粉末とを接触させて加熱すると、残存する窒
化マグネシウム粉末とBN複合体製品との分離が
困難である。このような場合には、粉末の代りに
塊状マグネシウムを用いるかあるいはhBN焼結体
をるつぼに入れ、これをマグネシウムを入れたる
つぼ中に入れて前記のように加熱すると、BN複
合体の分離が容易である。hBN焼結体を入れるる
つぼは、マグネシウム等のアルカリ土類金属又は
リチウムやBNと反応したり、あるいは加熱によ
り分解して障害とならないものであることが必要
である。そのるつぼ壁は多孔質でマグネシウム等
が拡散し易いものが望ましく、例えばBN焼結体
るつぼ、モリブデン等の金属るつぼが使用され
る。BN焼結体るつぼは窒化マグネシウムと反応
して一部ほう窒化マグネシウムとなるが、るつぼ
の形態を失わないので、その機能を損われること
はない。したがつてほう窒化物るつぼを使用する
ことも可能であるモリブデン等の金属るつぼは一
端を開放するか、多孔質のふたをすることによつ
て拡散させる。 When the hBN sintered bodies are fine, when they are brought into contact with magnesium powder and heated, it is difficult to separate the remaining magnesium nitride powder from the BN composite product. In such a case, the BN composite can be separated by using bulk magnesium instead of powder or by placing the hBN sintered body in a crucible containing magnesium and heating it as described above. It's easy. The crucible in which the hBN sintered body is placed needs to be one that does not react with alkaline earth metals such as magnesium, lithium, or BN, or decompose upon heating and cause problems. The wall of the crucible is preferably porous and allows easy diffusion of magnesium, for example, a BN sintered crucible or a metal crucible made of molybdenum or the like is used. The BN sintered crucible reacts with magnesium nitride to partially turn into magnesium boron nitride, but it does not lose its crucible form, so its functionality is not impaired. It is therefore also possible to use boronitride crucibles. Metal crucibles such as molybdenum can be diffused by being open at one end or by having a porous lid.
この方法では直接接触させる方法に較べて、マ
グネシウム等の濃度分布の均一なものが得られ、
特に低濃度に分布させる場合に有利である。 Compared to direct contact methods, this method provides a more uniform concentration distribution of magnesium, etc.
This is particularly advantageous when distributed at low concentrations.
マグネシウム以外のアルカリ土類金属及びリチ
ウムを使用する場合もほぼ同様にしてBN複合体
が得られるが、各元素の融点、沸点、反応性など
を考慮することがよい。例えばリチウムは融点が
179℃と低く、反応性が強く取扱いが困難である
ため、窒化リチウム又はほう窒化リチウムとして
使用することが好ましい。Ca、Ba、Srににおい
ても同様である。 When using an alkaline earth metal other than magnesium and lithium, a BN composite can be obtained in almost the same way, but it is better to consider the melting point, boiling point, reactivity, etc. of each element. For example, lithium has a melting point of
It is preferably used as lithium nitride or lithium boronitride because it is as low as 179°C and has strong reactivity and is difficult to handle. The same applies to Ca, Ba, and Sr.
BN複合体中におけるリチウム又はアルカリ土
類金属の担持形態は、主にMg3BN3、Mg3B2N4、
Ca3B2N4、Ba3B2N4、Sr3B2N4、Li3BN2等のほう
窒化物として担持される。 The supported forms of lithium or alkaline earth metals in the BN composite are mainly Mg 3 BN 3 , Mg 3 B 2 N 4 ,
It is supported as a boronitride such as Ca 3 B 2 N 4 , Ba 3 B 2 N 4 , Sr 3 B 2 N 4 and Li 3 BN 2 .
本発明のBN複合体は、cBN合成原料、cBN焼
結体の原料とするときは、優れたものが得られ、
特に透明なcBN焼結体が得られる。 When the BN composite of the present invention is used as a raw material for cBN synthesis or a raw material for cBN sintered bodies, an excellent product can be obtained.
A particularly transparent cBN sintered body can be obtained.
従来のBN粉末を用いて機械的に混合したもの
と、本発明のBN焼結複合体を使用した場合にお
ける光の透過率は第１図の通りであつた。 The light transmittances of the mechanically mixed conventional BN powder and the BN sintered composite of the present invention were as shown in FIG.
図において、１の曲線は本発明の複合体を使用
して得られたcBN焼結体の光透過率を示し、２の
曲線は機械的に混合したものを使用して得られた
cBN焼結体の光透過率を示す。すなわち、(1)が可
視部で(2)の約４倍もよくなつている。 In the figure, curve 1 shows the light transmittance of the cBN sintered body obtained using the composite of the present invention, and curve 2 shows the light transmittance of the cBN sintered body obtained using the composite of the present invention.
The light transmittance of cBN sintered body is shown. That is, (1) is about four times better than (2) in the visible part.
実施例 １
モリブデン製るつぼに、マグネシウム粒状粉末
を入れ、その中にhBN焼結体片（５mmφ、厚さ１
mm）を数十個埋込み、高周波加熱炉にセツトし
た。炉内を真空排気した後、窒素ガスを送入して
窒素ガス雰囲気とした。炉内温度を徐々に昇温し
て640℃で２時間保持した後、800℃で２時間保持
し、更に1150℃に昇温して５時間保持した。Example 1 Magnesium granular powder was placed in a molybdenum crucible, and a piece of hBN sintered body (5 mmφ, thickness 1
Several tens of mm) were embedded and placed in a high-frequency heating furnace. After the inside of the furnace was evacuated, nitrogen gas was introduced to create a nitrogen gas atmosphere. The temperature inside the furnace was gradually raised and held at 640°C for 2 hours, then held at 800°C for 2 hours, and further raised to 1150°C and held for 5 hours.
その後室温に冷却した後BN焼結体片を取り出
して周囲に付着した窒化マグネシウム粉末を取り
除いた。得られた含マグネシウムBN複合体は厚
さ約0.1mmの褐色のMg3B2N4に富んだ層に覆わ
れ、内部は淡黄色またはうぐいす色であつて、
Mgが0.1〜0.5重量％の濃度で連続的に分布して
いることがEPMA分析によつて確認され、Ｘ線回
折によりMgはほう窒化マグネシウムとして検出
された。 Thereafter, after cooling to room temperature, the BN sintered piece was taken out and the magnesium nitride powder adhering to its surroundings was removed. The obtained magnesium-containing BN composite is covered with a brown Mg 3 B 2 N 4 -rich layer with a thickness of about 0.1 mm, and the inside is pale yellow or greenish color.
It was confirmed by EPMA analysis that Mg was continuously distributed at a concentration of 0.1 to 0.5% by weight, and Mg was detected as magnesium boronitride by X-ray diffraction.
実施例 ２
マグネシウム粒状粉末の代りに窒化マグネシウ
ム粒状粉末を用いて実施例１と同様な試料構成に
て加熱した。昇温は徐々に行い、1150℃で５時間
保持し、実施例１と同様にしてBN複合体を製造
した。得られたBN複合体は実施例１のものとほ
ぼ同様なものであつた。Example 2 A sample configuration similar to that of Example 1 was heated using granular magnesium nitride powder instead of granular magnesium powder. The temperature was gradually raised and held at 1150°C for 5 hours, and a BN composite was produced in the same manner as in Example 1. The obtained BN composite was almost the same as that of Example 1.
実施例 ３
BN粉末及びhBN焼結体を入れたBNるつぼを、
モリブデン製るつぼに入れた窒化マグネシウム粉
中に埋込み、1200℃で５時間窒素気流中で加熱し
た。得られたBN複合体中には約0.2重量％のマグ
ネシウムが含まれていた。この方法によるときは
実施例１及び実施例２におけるようなBN複合体
の表面の褐色膜は見られなかつた。Example 3 A BN crucible containing BN powder and hBN sintered body was
It was embedded in magnesium nitride powder in a molybdenum crucible and heated at 1200°C for 5 hours in a nitrogen stream. The obtained BN composite contained about 0.2% by weight of magnesium. When this method was used, no brown film was observed on the surface of the BN composite as in Examples 1 and 2.
実施例 ４
hBN焼結体を入れたモリブデン製るつぼを窒化
マグネシウム粉末を入れたモリブデン製るつぼ中
に入れ、ふたをした後、実施例３と同様に加熱す
ることによりBN複合体を得た。Example 4 A molybdenum crucible containing the hBN sintered body was placed in a molybdenum crucible containing magnesium nitride powder, the crucible was covered, and the crucible was heated in the same manner as in Example 3 to obtain a BN composite.
前記実施例１〜４によつて得られたBN複合体
をモリブデン製容器に入れ、ベルト型高圧装置を
使用して5.7GPa、1550℃の条件下で約30分間保
持した後、急冷して取出した。モリブデン製容器
を熱王水による処理によつて除去し、緻密体を得
た。これは無色透明で、その表面及び破断面につ
いて化学的分析を行つた結果、不純物を含まない
cBN単一相であることが実証された。密度は理論
値と一致し、微小押込み硬さは5700Kg／mm2以上の
高い値であつた。この緻密体の可視紫外領域
（250〜800μｍ）の透過率はいずれも第１図の１
曲線に示す優れたものであつた。 The BN composites obtained in Examples 1 to 4 were placed in a molybdenum container, held at 5.7 GPa and 1550°C for about 30 minutes using a belt-type high-pressure device, and then rapidly cooled and taken out. did. The molybdenum container was removed by treatment with hot aqua regia to obtain a dense body. It is colorless and transparent, and chemical analysis of its surface and fractured surfaces revealed that it does not contain any impurities.
It was demonstrated that cBN is a single phase. The density matched the theoretical value, and the microindentation hardness was a high value of 5700 Kg/mm 2 or more. The transmittance of this dense body in the visible and ultraviolet region (250 to 800 μm) is 1 in Figure 1.
The results were excellent as shown in the curve.
実施例 ５
実施例２における窒化マグネシウムに代え窒化
リチウム、窒化カルシウムをそれぞれ使用し、実
施例２と同様にして、それぞれ、ほう窒化リチウ
ム、ほう窒化カルシウムを拡散担持したBN複合
体が得られた。Example 5 In the same manner as in Example 2, using lithium nitride and calcium nitride instead of magnesium nitride in Example 2, BN composites in which lithium boronitride and calcium boronitride were diffusely supported, respectively, were obtained.
このBN焼結体を前記と同様なベルト型高圧装
置を使用して、5.2GPa、1510℃で１時間保持
し、前記と同様にして緻密体を得た。この緻密体
は淡緑物または淡黄色に着色した透光性のcBN緻
密体であつた。微少押込み硬さは約6400Kg／mm2と
極めて高い値を示した。 This BN sintered body was held at 5.2 GPa and 1510° C. for 1 hour using the same belt-type high-pressure device as described above, and a dense body was obtained in the same manner as described above. This compact body was a translucent cBN compact colored pale green or pale yellow. The micro-indentation hardness showed an extremely high value of approximately 6400Kg/mm 2 .
第１図はhBN粉末と窒化マグネシウムとを機械
的に混合したものと本発明の方法で得られたほう
窒化マグネシウムを拡散担持したBN複合体を使
用して得られたcBN焼結体の光透過率を示すもの
である。
１の曲線は本発明の複合体の場合、２の曲線は
BN粉末とほう窒化マグネシウムとを機械的に混
合した場合を示す。
Figure 1 shows the optical transmission of a cBN sintered body obtained using a mechanical mixture of hBN powder and magnesium nitride and a BN composite in which magnesium boronitride is diffusely supported by the method of the present invention. It shows the rate. Curve 1 is for the composite of the present invention; curve 2 is for the composite of the present invention;
This shows a case where BN powder and magnesium boronitride are mechanically mixed.
Claims (1)
カリ土類金属をほう窒化物として拡散担持せしめ
たものからなる立方晶窒化ほう素焼結体製造用複
合体。 ２ 六方晶窒化ほう素焼結体と、リチウム又はア
ルカリ土類金属、それらの窒化物もしくはほう窒
化物あるいはこれらの混合物を接触下、非酸化雰
囲気中で加熱して、六方晶窒化ほう素焼結体にリ
チウム又はアルカリ土類金属あるいはこれらの混
合物をほう窒化物として拡散担持させることを特
徴とする立方晶窒化ほう素焼結体製造用複合体の
製造法。 ３ 六方晶窒化ほう素焼結体をるつぼに入れ、リ
チウム又はアルカリ土類金属、それらの窒化物も
しくはほう窒化物あるいはこれらの混合物を非酸
化雰囲気下の加熱によりるつぼ外からるつぼ内に
拡散させて、六方晶窒化ほう素焼結体にほう窒化
物として担持させることを特徴とする立方晶窒化
ほう素焼結体製造用複合体の製造法。[Scope of Claims] 1. A composite for producing a cubic boron nitride sintered body, which is made of a hexagonal boron nitride sintered body and lithium or an alkaline earth metal diffused thereon as a boron nitride. 2 Hexagonal boron nitride sintered body and lithium or alkaline earth metal, their nitrides or boron nitrides, or mixtures thereof are heated in a non-oxidizing atmosphere in contact with each other to form a hexagonal boron nitride sintered body. A method for producing a composite for producing a cubic boron nitride sintered body, which comprises diffusing and supporting lithium or an alkaline earth metal or a mixture thereof as a boronitride. 3. A hexagonal boron nitride sintered body is placed in a crucible, and lithium or an alkaline earth metal, their nitride or boron nitride, or a mixture thereof is diffused from outside the crucible into the crucible by heating in a non-oxidizing atmosphere, A method for producing a composite for manufacturing a cubic boron nitride sintered body, which comprises supporting the hexagonal boron nitride sintered body as a boron nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59162477A JPS6086077A (en) | 1984-07-31 | 1984-07-31 | Composite for manufacturing cubic boron nitride sintered body and method for manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59162477A JPS6086077A (en) | 1984-07-31 | 1984-07-31 | Composite for manufacturing cubic boron nitride sintered body and method for manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6086077A JPS6086077A (en) | 1985-05-15 |
| JPS6256108B2 true JPS6256108B2 (en) | 1987-11-24 |
Family
ID=15755359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59162477A Granted JPS6086077A (en) | 1984-07-31 | 1984-07-31 | Composite for manufacturing cubic boron nitride sintered body and method for manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6086077A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6436007U (en) * | 1987-08-26 | 1989-03-06 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2020009117A1 (en) * | 2018-07-03 | 2021-07-08 | 住友電工ハードメタル株式会社 | Cutting insert and its manufacturing method |
-
1984
- 1984-07-31 JP JP59162477A patent/JPS6086077A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6436007U (en) * | 1987-08-26 | 1989-03-06 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6086077A (en) | 1985-05-15 |
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