JPS62212205A - Layered boron nitride intercalation compound and production thereof - Google Patents
Layered boron nitride intercalation compound and production thereofInfo
- Publication number
- JPS62212205A JPS62212205A JP5207686A JP5207686A JPS62212205A JP S62212205 A JPS62212205 A JP S62212205A JP 5207686 A JP5207686 A JP 5207686A JP 5207686 A JP5207686 A JP 5207686A JP S62212205 A JPS62212205 A JP S62212205A
- Authority
- JP
- Japan
- Prior art keywords
- layered
- boron nitride
- intercalation compound
- layered boron
- reaction
- 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
- 150000001875 compounds Chemical class 0.000 title claims abstract description 24
- 238000009830 intercalation Methods 0.000 title claims abstract description 20
- 230000002687 intercalation Effects 0.000 title claims abstract description 20
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 18
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000004020 conductor Substances 0.000 abstract description 2
- 239000000314 lubricant Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000011229 interlayer Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 235000001537 Ribes X gardonianum Nutrition 0.000 description 8
- 235000001535 Ribes X utile Nutrition 0.000 description 8
- 235000016919 Ribes petraeum Nutrition 0.000 description 8
- 244000281247 Ribes rubrum Species 0.000 description 8
- 235000002355 Ribes spicatum Nutrition 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000007872 degassing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000001683 neutron diffraction Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は新規物質である層状窒化ほう素層間化合物およ
びその製造法に関する。該化合物は潤滑剤、Ｘ線または
中性子線回折格子、導電性材料。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a novel material, a layered boron nitride intercalation compound, and a method for producing the same. The compounds are lubricants, X-ray or neutron diffraction gratings, conductive materials.
電池電橋材料、高誘電率材料、半導体拡散用材料。Battery bridge materials, high dielectric constant materials, semiconductor diffusion materials.
化学触媒等として有効なものである。It is effective as a chemical catalyst, etc.
従来技術
従来黒鉛層間化合物は知られているが、層状窒化ほう素
の眉間化合物は知られていない。Prior Art Conventionally, graphite intercalation compounds are known, but intercalation compounds of layered boron nitride are not known.
発明の目的
本発明の目的は有効で新規な層状窒化ほう素層間化合物
を提供するにある。OBJECTS OF THE INVENTION It is an object of the present invention to provide an effective and novel layered boron nitride intercalation compound.
発明の構成
常圧下で合成された窒化ほう素はＢとＮとからなる原子
網面の積重なりよりできているので層状−窒」ヒほう素
と呼ばれている。これにはＢ、Ｎの原１：Ｆ１７面の積
重なり方が二層周期の場合の六方晶゛ｍ；Ｈ＜以下ｈＢ
Ｎと記載する）、三層周期の場合Ｊ）４面体晶ＢＮ（以
下ｒＢＮと記載する、）周期性がなく層が乱れている場
合の乱層構造ＢＮ（以下ｔＢＮと記載する）とがある、
また熱分解沈積によって合成されたちのく以下ｐＢＮと
記載する）にも同様にＢＮがある。Structure of the Invention Since boron nitride synthesized under normal pressure is made up of stacked atomic networks consisting of B and N, it is called layered nitride. This is a hexagonal crystal when the stacking of the original 1:F17 planes of B and N has a two-layer periodicity.
J) Tetrahedral BN (hereinafter referred to as rBN) in the case of a three-layer periodic structure, and turbostratic structure BN (hereinafter referred to as tBN) in which there is no periodicity and the layers are disordered. ,
There is also BN in chinoku (hereinafter referred to as pBN), which is synthesized by pyrolysis deposition.
本発明においては、前記のものを総称して層状ＢＮと呼
ぶ、これらの層間隔は約３．３Ａであるため、従来の黒
鉛等におけると同様に層間に異種の原子や分子（以下イ
ンクカーラントと言う）を挿入結合させて新しい眉間化
合物を作−るべく試みられてきたが、未だ完成されたも
のはない。In the present invention, the above-mentioned materials are collectively referred to as layered BN. Since the spacing between these layers is approximately 3.3A, different atoms and molecules (hereinafter referred to as ink currant) are present between the layers, as in conventional graphite, etc. Attempts have been made to create a new glabellar compound by inserting and bonding the glabellar compounds, but nothing has been completed yet.
本発明者らは層状ＢＮの眉間化合物を得べく鋭意研究を
重ねた結果、インクカーランドとしてＢ１Ｃ１ｚ （
以下、これらをインクカーラントと記載する）を用い、
母結晶としてｒＢＮ、ｈＢＮ。As a result of intensive research to obtain a glabellar compound of layered BN, the present inventors found B1C1z (
Hereinafter, these are referred to as ink currants),
rBN and hBN as mother crystals.
ｔＢＮ、ｐＢＮ等の層状ＢＮを用いて反応温度。Reaction temperature using layered BN such as tBN and pBN.
インクカーラントと母結晶との加熱温度差１反応一時１
間を制御すると、容易に層状ＢＮ層間化合物を召１′成
し得られることを見出した。この知見に基いて、一本発
明を完成した。Heating temperature difference between ink currant and mother crystal 1 Reaction 1
It has been found that a layered BN intercalation compound can be easily formed by controlling the distance between the two layers. Based on this knowledge, the present invention was completed.
体発明の要旨は
層状窒化ほう素層間にＢ１Ｃ１５を挿入結合させた層状
窒化ほう素層間化合物にある。The gist of the present invention is a layered boron nitride intercalation compound in which B1C15 is inserted and bonded between layered boron nitride layers.
該層状窒化ほう素層間化合物としては、インクカーラン
トが層状ＢＨの各層に挿入結合されたもの（これを第１
ステージと言う）、一層飛びこえて挿入結合されたもの
（これを第２ステージと言う）またｎ層飛びこえて挿入
結合されたもの（これを第ｎステージと言う）とがある
、これは反応温度、インクカーランドと母結晶との加熱
温度差。The layered boron nitride intercalation compound is one in which an ink currant is inserted and bonded to each layer of the layered BH (this is the first layer).
There are two types of reaction. Temperature, heating temperature difference between ink car land and mother crystal.
反応時間によって制御される。Controlled by reaction time.
本発明の層状窒化ほう素層間化合物は、インタカーラン
トと層状ＢＮを同一の反応管に入れ、真空中または不活
性ガス中で１５０〜４５０℃で加熱する。この場合、イ
ンタカーラントと層状ＢＮとは、混合して同一場所に置
いても、また、両者を間隔を置いて別々に加熱してもよ
い。その具体的方法を−示すと、次の方法がある。To prepare the layered boron nitride intercalation compound of the present invention, intercalant and layered BN are placed in the same reaction tube and heated at 150 to 450° C. in vacuum or inert gas. In this case, the intercalant and layered BN may be mixed and placed in the same place, or they may be heated separately at intervals. The specific methods are as follows.
（１） 封管法
層状ＢＮとインクカーラントとを同容量混合した混合物
を一端が開放し他端が封じられた反応管に入れ、真空ポ
ンプで開放端から脱気した後開放部を封する。これを電
気炉で１５０〜５００℃好ましくは２６０〜４５０℃で
加熱し、反応後、封管を冷却する方法。(1) Sealing tube method A mixture of layered BN and ink currant in equal volumes is placed in a reaction tube with one end open and the other end sealed, and after degassing from the open end with a vacuum pump, the open part is sealed. . A method in which this is heated in an electric furnace at 150 to 500°C, preferably 260 to 450°C, and after the reaction, the sealed tube is cooled.
（２） 温度差封管法
層状ＢＮとインタカーラントとを一端が開放し、他端が
封じられた反応管内の別位置に配置し、真空ポンプで開
放端から脱気した後、開放部を封する。これを電気炉に
いれて、層状ＢＮ部とインクカーラント部（低温）とを
温度差をつけて１５０〜５００℃の範囲内で加熱し、反
応後封管を冷却する方法。(2) Temperature difference sealing tube method Layered BN and intercalant are placed in different positions in a reaction tube with one end open and the other end sealed, and after degassing from the open end with a vacuum pump, the open end is closed. Seal. A method of putting this in an electric furnace, heating the layered BN part and the ink currant part (low temperature) within a range of 150 to 500°C with a temperature difference, and cooling the sealed tube after the reaction.
（３） 開管法
層状ＢＮとインタカーラントとを両端開放の反応管内の
別位置に配置し、反応管を層状ＢＮ部とインタカーラン
ト部とを温度差をつけて加二熱、シ、インタカーラント
の置かれた側から不活−Ｗｌ、％ガス例えばアルゴンガ
ス、 Ｎｌガスを流してイノ；タカ−ラントの蒸気を層
状ＢＮに接触させてデ応させ、反応後冷却する方法。(3) Open tube method Layered BN and intercalant are placed in different positions in a reaction tube with both ends open, and the reaction tube is heated with a temperature difference between the layered BN part and the intercalant part. A method in which an inert Wl,% gas such as argon gas or Nl gas is flowed from the side where the intercalant is placed, and the vapor of the intercalant is brought into contact with the layered BN to cause de-reaction, and after the reaction is cooled.
なお、いずれの方法においても、冷却後反応管から層状
ＢＮ層間化合物を取出し、耐着したインクカーラントを
溶剤例えばメチルアルコール、エチルアルコールで溶解
除去することが好ましい。In either method, it is preferable to take out the layered BN intercalation compound from the reaction tube after cooling, and dissolve and remove the adhered ink curlant with a solvent such as methyl alcohol or ethyl alcohol.
発明の効果
本発明の層状ＢＮ層間化合物は、Ｂ１Ｃ１５をインクカ
ーランドとした場合、層状ＢＮの電気抵抗がＩＱ１４Ω
以上の良好な絶縁性を有するが、電気抵抗は１０桁以上
低下し、電導性を発現する。またステージの制御によっ
てＢＮ部ｑ面の繰返し周期を３．３Ａから数１ＯＡまで
の広い範囲のものとなし得る。これによりＸ線、中性子
線回折格子へ利用し得られる。Effects of the Invention In the layered BN intercalation compound of the present invention, when B1C15 is used as an ink car land, the electric resistance of the layered BN is IQ14Ω.
Although it has the above-mentioned good insulation properties, the electrical resistance is lowered by more than 10 orders of magnitude, and it exhibits electrical conductivity. Furthermore, by controlling the stage, the repetition period of the BN part q-plane can be set in a wide range from 3.3 A to several 1 OA. This allows it to be used for X-ray and neutron beam diffraction gratings.
実施例１゜
層状ＢＮとＢｉＣｌ３ との同容量の混合物を一端を封
じ他端を開放した反応管（ガラス管）に入れ、開１角端
より脱気して真空にした後、開放端を封じた・４．、こ
れを電気炉中に入れて３１５℃に加熱した。Example 1 A mixture of the same volume of layered BN and BiCl3 was placed in a reaction tube (glass tube) with one end sealed and the other open, and after degassing from the open corner end to create a vacuum, the open end was sealed.・4. This was placed in an electric furnace and heated to 315°C.
反ご応１時間はｒＢＮ、ｈＢＮの場合では数日、ｐ ’
Ｂ Ｈの場合は２ケ月位、反応させた０反応、１，７後
、急冷して開封し、次のいずれかの方法で：Ｊ！Ｉ 状
ＢＮ層間化合物を分離した。In the case of rBN and hBN, one hour of reaction takes several days, and p'
In the case of BH, react for about 2 months, after 0 reaction, 1, 7, quench, open, and use one of the following methods: J! The I-shaped BN intercalation compound was separated.
延
（１１反応管の両端に温度をつけてＢ１Ｃ１２の蒸気−
圧差を利用して未反応Ｂ１Ｃ１５を分離する方法。(11 Heat the both ends of the reaction tube and let the steam of B1C12 -
A method of separating unreacted B1C15 using a pressure difference.
（２） 生成物をメチルアルコールまたはエチルアル
コールで処理してＢ１Ｃ１５を溶解し、分離する方法。(2) A method of treating the product with methyl alcohol or ethyl alcohol to dissolve and separate B1C15.
得られた層状ＢＮ層間化合物の電気抵抗は１０’Ω値で
あった。またＢＮ部１４面の眉間繰返し周期は、第１ス
テージの時 ７．３Ａ、 ８．８ Ａ。The electrical resistance of the obtained layered BN intercalation compound was 10'Ω. In addition, the repetition period between the eyebrows on the 14th side of the BN section was 7.3A and 8.8A at the first stage.
第２ステージの時 １０．６３ Ａ、 １２．１Ａ。During the second stage 10.63 A, 12.1 A.
第５ステージの時 ２０．６Ａ、 ２２．１Ａ。At the 5th stage 20.6A, 22.1A.
であった。Met.
実施例２゜
実施例１の方法における層状ＢＮとインクカーラントと
の混合に代え、反応管内の離れた位置に配π）、層状Ｂ
Ｎ部を例えば３３０〜３７０℃に、インクどカーラント
部例えば３１０ ℃と温度差をつけて加、熱夷た。この
温度差を制御することにより層状ＢＮ層間化合物のステ
ージ数を制御し得た。Example 2 Instead of mixing layered BN and ink currant in the method of Example 1, layered B
The N part was heated to, for example, 330 to 370°C, and the ink and currant part was heated to a temperature of, for example, 310°C. By controlling this temperature difference, the number of stages of the layered BN intercalation compound could be controlled.
以下実施例１と同様にして層状ＢＮ層間化合物を分離し
た。Thereafter, the layered BN intercalation compound was separated in the same manner as in Example 1.
実施例３゜
実施例２とは異なり、両端が開放された反応管を使用し
、真空処理を施すことな（、Ｂ１Ｃ１５の置かれた側か
ら層状ＢＮの置かれた方に不活性ガス例えばアルゴンガ
ス、 Ｎｔガスを流してＢｉＣｌ３を層状ＢＮに接触さ
せ反応させた。この反応時間により層状ＢＮ層間化合物
のステージ数を制御し得た。Example 3: Unlike Example 2, a reaction tube with both ends open was used, and no vacuum treatment was applied (an inert gas such as argon was applied from the side where the B1C15 was placed to the side where the layered BN was placed). BiCl3 was brought into contact with the layered BN and reacted by flowing Nt gas.The number of stages of the layered BN intercalation compound could be controlled by this reaction time.
Claims (1)
せた層状窒化ほう素層間化合物。 ２、層状窒化ほう素とＢｉＣｌ＿３とを、混合あるいは
別個に反応管内に配置し、反応温度、加熱温度差、また
はおよび反応時間を制御しながら加熱反応させることを
特徴とする層状窒化ほう素層間化合物の製造法。[Claims] 1. A layered boron nitride intercalation compound in which BiCl_3 is inserted and bonded between layers of layered boron nitride. 2. A layered boron nitride intercalation compound characterized in that layered boron nitride and BiCl_3 are mixed or placed separately in a reaction tube, and heated and reacted while controlling the reaction temperature, heating temperature difference, and reaction time. manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5207686A JPS62212205A (en) | 1986-03-10 | 1986-03-10 | Layered boron nitride intercalation compound and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5207686A JPS62212205A (en) | 1986-03-10 | 1986-03-10 | Layered boron nitride intercalation compound and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62212205A true JPS62212205A (en) | 1987-09-18 |
Family
ID=12904726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5207686A Pending JPS62212205A (en) | 1986-03-10 | 1986-03-10 | Layered boron nitride intercalation compound and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62212205A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5021368A (en) * | 1988-09-29 | 1991-06-04 | The Dow Chemical Company | Novel ceramic-metal compounds |
| US5436372A (en) * | 1991-04-09 | 1995-07-25 | Nippon Soken, Inc. | Solid state displacement elements |
-
1986
- 1986-03-10 JP JP5207686A patent/JPS62212205A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5021368A (en) * | 1988-09-29 | 1991-06-04 | The Dow Chemical Company | Novel ceramic-metal compounds |
| US5436372A (en) * | 1991-04-09 | 1995-07-25 | Nippon Soken, Inc. | Solid state displacement elements |
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