JPS6159243B2 - - Google Patents
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- Publication number
- JPS6159243B2 JPS6159243B2 JP56140778A JP14077881A JPS6159243B2 JP S6159243 B2 JPS6159243 B2 JP S6159243B2 JP 56140778 A JP56140778 A JP 56140778A JP 14077881 A JP14077881 A JP 14077881A JP S6159243 B2 JPS6159243 B2 JP S6159243B2
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- sio
- cao
- ammonia
- showed
- 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
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- 229910052582 BN Inorganic materials 0.000 claims description 35
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 17
- 229910010293 ceramic material Inorganic materials 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 229910021540 colemanite Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910052918 calcium silicate Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000008262 pumice Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- VLCLHFYFMCKBRP-UHFFFAOYSA-N tricalcium;diborate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]B([O-])[O-].[O-]B([O-])[O-] VLCLHFYFMCKBRP-UHFFFAOYSA-N 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- YKAIJSHGJPXTDY-CBDGTLMLSA-N α-cao Chemical compound C([C@@H](N(CC1)C)C23C=CC4([C@H](C3)N(CCCl)CCCl)OC)C3=CC=C(O)C5=C3[C@@]21[C@H]4O5 YKAIJSHGJPXTDY-CBDGTLMLSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- NBUGSEZNBDVRPG-UHFFFAOYSA-N B([O-])([O-])[O-].[Ca+2].[Ca+2] Chemical compound B([O-])([O-])[O-].[Ca+2].[Ca+2] NBUGSEZNBDVRPG-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 235000019402 calcium peroxide Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
【発明の詳細な説明】
本発明は窒化硼素（BN）を含むセラミツク物
質の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing ceramic materials containing boron nitride (BN).
周知の如く、窒化硼素は耐火性・耐蝕性等の優
れたセラミツク物質である。かかる窒化硼素の製
造方法としては、従来、硼酸又は硼酸塩とアンモ
ニアガスとの反応による方法、或いは三塩化硼素
とアンモニアガスとの反応による方法が知られて
いる。しかしながら、これら方法にあつては、
得られた窒化硼素の含有窒素量は低く（化学純度
の低い）、無定形、乱層構造のものとなり易く純
度や結晶化度を高めるために1800〜2000℃で再熱
処理を施す必要がある副生物中に耐火性の低い
物質が生成され、そのままでは窒化硼素を含む耐
火性セラミツク物質としては使用できない等の欠
点があつた。 As is well known, boron nitride is a ceramic material with excellent fire resistance and corrosion resistance. Conventionally known methods for producing boron nitride include a reaction between boric acid or a borate and ammonia gas, or a reaction between boron trichloride and ammonia gas. However, with these methods,
The resulting boron nitride has a low nitrogen content (low chemical purity), tends to be amorphous and has a turbostratic structure, and requires reheat treatment at 1800 to 2000°C to increase purity and crystallinity. There were drawbacks such as the formation of substances with low fire resistance in living organisms, which could not be used as is as a fire-resistant ceramic material containing boron nitride.
このようなことから、本発明は鋭意研究を重ね
た結果、自然に産するコレマナイト鉱を高温度下
でアンモニアと反応させることによつて、結晶化
度が高い窒化硼素を多量含むセラミツク物質を容
易に製造し得る方法を見い出した。 Therefore, as a result of extensive research, the present invention was developed to easily produce ceramic materials containing a large amount of boron nitride with a high degree of crystallinity by reacting naturally occurring colemanite ore with ammonia at high temperatures. We have discovered a method that can be manufactured.
以下、本発明を詳細に説明する。 The present invention will be explained in detail below.
まず、コレマナイト鉱（一般的な組成を挙げる
と、B2O3；40〜46％、CaO；25〜27％、SiO2；
３〜５％、MgO；１％以下、Fe2O3；0.5％以
下、Na2O＋K2O；0.3％以下、Ａ2O3；１％以
下、Ig、Loss；22〜26％、付着水；１〜２％か
らなる）のCaOに対するSiO2のモル比が0.5≦
SiO2／CaO≦1.0の範囲となるようにシリカ分を
調整したものを原料として用意する。こうした原
料の調整は、主に珪石やフラツタリーサンド等の
SiO2を主成分とする粉末を添加することにより
なされる。 First, colemanite (general compositions are B2O3 ; 40-46% , CaO; 25-27%, SiO2 ;
3 to 5%, MgO; 1% or less, Fe 2 O 3 ; 0.5% or less, Na 2 O + K 2 O; 0.3% or less, A 2 O 3 ; 1% or less, Ig, Loss; 22 to 26%, attached water The molar ratio of SiO 2 to CaO (consisting of 1 to 2%) is 0.5≦
A raw material with a silica content adjusted so that SiO 2 /CaO≦1.0 is prepared. The adjustment of these raw materials is mainly done using silica stone, flattery sand, etc.
This is done by adding powder whose main component is SiO2 .
次いで、前記原料を所定温度で脱水処理して多
孔質の軽石状物を作る。つづいて、この軽石状物
を適当な大きさに粉砕して1000℃以上の温度下で
アンモニアと反応させる。こうした反応により窒
化硼素、α−珪酸−カルシウム（α−CaO・
SiO2）、α′−珪酸二カルシウム（α′−2CaO・
SiO2）が生成され、窒化硼素を含むセラミツク物
質が得られる。 Next, the raw material is dehydrated at a predetermined temperature to produce a porous pumice-like material. Next, this pumice-like material is crushed into an appropriate size and reacted with ammonia at a temperature of 1000°C or higher. These reactions produce boron nitride, α-calcium silicate (α-CaO・
SiO 2 ), α′-dicalcium silicate (α′-2CaO・
SiO 2 ) is produced and a ceramic material containing boron nitride is obtained.
前記コレマナイト鉱のSiO2／CaOモル比を上
記範囲に限定した理由は、そのモル比を0.5未満
にすると、アンモニアとの反応時に窒化硼素、
α′−珪酸二カルシウムの他に硼酸三カルシウム
（3CaO・B2O3）が生成され、窒化されない硼素成
分が増大してセラミツク物質中の窒化硼素量が低
下する。一方、前記SiO2／CaOのモル比が１を
越えると、アンモニアとの反応時に窒化硼素、α
−ケイ酸−カルシウムの他に酸洗浄での溶出が困
難なシリカが残留し、アンモニウムの反応後のセ
ラミツク物質から窒化硼素のみを得る場合の障害
となる。なお、これらの窒化硼素、α′−珪酸二
カルシウム、硼酸三カルシウム、α−ケイ酸−カ
ルシウムはＸ線回折図形により同定される。 The reason why the SiO 2 /CaO molar ratio of the colemanite ore is limited to the above range is that if the molar ratio is less than 0.5, boron nitride,
In addition to α'-dicalcium silicate, tricalcium borate (3CaO.B 2 O 3 ) is produced, and the unnitrided boron component increases, reducing the amount of boron nitride in the ceramic material. On the other hand, if the molar ratio of SiO 2 /CaO exceeds 1, boron nitride, α
- Silicate - In addition to calcium, silica, which is difficult to be eluted by acid washing, remains and becomes an obstacle when only boron nitride is obtained from the ceramic material after the ammonium reaction. Note that these boron nitride, α'-dicalcium silicate, tricalcium borate, and α-calcium silicate are identified by X-ray diffraction patterns.
前記アンモニアの反応温度を限定した理由は、
その温度を1000℃未満にすると窒化硼素の他の硼
酸二カルシウム（2CaO・B2O3）、硼酸−カルシ
ウム（CaO・B2O3）が生成して得られたセラミツ
ク物質中の窒化硼素の含有量が低下するからであ
る。反応させるアンモニアは、必ずしもアンモニ
ア単独にしなくてもよく、不活性ガスで希釈され
たアンモニアを使用してもよい。 The reason for limiting the ammonia reaction temperature is as follows:
When the temperature is lower than 1000°C, dicalcium borate (2CaO・B 2 O 3 ) and calcium borate (CaO・B 2 O 3 ) other than boron nitride are formed, and boron nitride in the ceramic material obtained is This is because the content decreases. The ammonia to be reacted does not necessarily need to be ammonia alone, and ammonia diluted with an inert gas may be used.
この様にして得られたセラミツク物質を微粉砕
して酸洗滌後、濾過水洗を繰りかえすとα′−珪
酸二カルシウム、α−珪酸一カルシウム、その他
の微量不純物は溶出され純度の高い窒化硼素が得
られる。しかしながら酸洗滌では遊離シリカは溶
出除去できないので窒化硼素だけを得る場合は
SiO2／CaOのモル比を1.0以下にする必要があ
る。 After pulverizing the ceramic material thus obtained and washing with acid, repeated filtration and washing with water dissolves α'-dicalcium silicate, α-monosilicate, and other trace impurities, yielding highly pure boron nitride. It will be done. However, free silica cannot be eluted and removed by pickling, so if only boron nitride is obtained,
The molar ratio of SiO 2 /CaO needs to be 1.0 or less.
しかして、本発明によれば以下に示す種々の効
果を発揮できる。 According to the present invention, various effects shown below can be achieved.
(イ) 原料（コレマナイト鉱）中の硼素分をほぼ完
全に窒化することができる。(a) The boron content in the raw material (colemanite ore) can be almost completely nitrided.
(ロ) 高温再処理を行なわずに結晶化度の高い窒化
硼素を含むセラミツク物質を得ることができ
る。このものはそのまま耐火性セラミツク材料
として使用できる。(b) A ceramic material containing boron nitride with a high degree of crystallinity can be obtained without performing high-temperature reprocessing. This product can be used as is as a refractory ceramic material.
(ハ) 簡単な酸溶出処理により純粋な窒化硼素を得
ることができる。(c) Pure boron nitride can be obtained by simple acid elution treatment.
(ニ) 自然に産するコレマナイト鉱を原料とするた
め、窒化硼素を含むセラミツク物質の製造コス
トを大巾に低減できる。(d) Since naturally occurring colemanite ore is used as a raw material, the manufacturing cost of ceramic materials containing boron nitride can be greatly reduced.
次に、本発明の実施例を説明する。 Next, examples of the present invention will be described.
実施例 １
B2O341.6％、CaO26.76％、SiO24.00％、
MgO0.89％、Fe2O30.04％、Na2O0.05％、
K2O0.003％、Ａ2O30.09％、IgLoss24.29％、付
着水1.37％を含むコレマナイト鉱200ｇに
SiO299.9％を含むフラツタリーサンド18.8ｇを加
え、容量１のポリエチレン製ポツトミル中で４
時間乾式混合した。この混合粉末を760℃で30分
間加熱乾燥して多孔性軽石状物167.8ｇを作つ
た。この軽石状物を粒状物に粉砕した後、このう
ちの99.4ｇをカーボン板に載せ、内径95mmのムラ
イト管に装填した。つづいて、管内雰囲気をアン
モニアガスで置換し、同管内にアンモニアガスを
0.53／minの流量で供給しながら、300℃／min
の昇温速度で1160℃まで昇温し、１時間保持した
後、直ちにアンモニアガスの供給を停止し、代わ
りにアルゴンガスを供給しながら自然放冷して反
応生成物84.4ｇを得た。Example 1 B2O3 41.6 %, CaO26.76%, SiO2 4.00%,
MgO0.89%, Fe2O30.04 %, Na2O0.05 % ,
200 g of colemanite ore containing 0.003% K 2 O, 0.09% A 2 O 3 , 24.29% IgLoss, and 1.37% attached water.
Add 18.8 g of flattery sand containing 99.9% SiO 2 and mix in a polyethylene pot mill with a capacity of 4.
Dry mixed for an hour. This mixed powder was dried by heating at 760° C. for 30 minutes to produce 167.8 g of porous pumice. After pulverizing this pumice-like material into granules, 99.4 g of the granules were placed on a carbon plate and loaded into a mullite tube with an inner diameter of 95 mm. Next, replace the atmosphere inside the tube with ammonia gas, and add ammonia gas into the tube.
300℃/min while supplying at a flow rate of 0.53/min
The temperature was raised to 1160° C. at a heating rate of 1,160° C. and held for 1 hour, and then the supply of ammonia gas was immediately stopped, and instead, argon gas was supplied while allowing the mixture to cool naturally to obtain 84.4 g of a reaction product.
得られた生成物を粉末Ｘ線回折法にて分析した
ところ、BNとα′−2CaO・SiO2だけの回折ピー
クを示した。生成物のうち6.2ｇをカーボンルツ
ボに取り、窒素気流中で1800℃の温度下で加熱し
たが、溶融した形態もなく、かつその回折結果も
BNとα′−2CaO・SiO2のピークを示し高い耐火
性を付することが確認された。 When the obtained product was analyzed by powder X-ray diffraction, it showed diffraction peaks of only BN and α'-2CaO.SiO 2 . 6.2g of the product was placed in a carbon crucible and heated at 1800℃ in a nitrogen stream, but no molten form was found, and the diffraction results also showed that
The peaks of BN and α′-2CaO・SiO 2 were observed, and it was confirmed that the material had high fire resistance.
また、残りの生成物78.2ｇを振動ミルで微粉砕
し、4NのHC360c.c.に入れて充分酸溶出した
後、吸引濾過、水洗を６回繰り返し、更に80℃で
１日夜乾燥して白色粉末を得た。この白色粉末を
Ｘ線回折で分析したところ窒化硼素のみのピーク
を示した。また、白色粉末の重量は32.0ｇでBN
の理論生成量（32.25ｇ）の99.2％にあたり、良
好な生成収率を示した。また、Warrenの式；0.9
×λ／Bcos〔但し、λはCuKα線の波長（1.542
Å）、Ｂは半値巾の補正値B2√M ２−S ２ここ
でＢMは窒化硼素（002）の半値巾、ＢSはシリコ
ン（111）の半値巾、は窒化硼素の回折角を示
す〕より結晶子のＣ軸方向の厚みＬCを測定した
結果、460Åであり、かなりの結晶化が進んでい
ることが確認された。 In addition, 78.2 g of the remaining product was finely pulverized with a vibrating mill, put into 4N HC360c.c., and thoroughly eluted with acid, followed by suction filtration and washing with water 6 times, and then dried at 80℃ for 1 day and night to produce a white color. A powder was obtained. When this white powder was analyzed by X-ray diffraction, it showed only a peak of boron nitride. Also, the weight of the white powder is 32.0g and BN
This was 99.2% of the theoretical production amount (32.25 g), indicating a good production yield. Also, Warren's equation; 0.9
×λ／Bcos [However, λ is the wavelength of CuKα ray (1.542
Å), B is the half-width correction value B2√ M 2 − S 2 where B M is the half-width of boron nitride (002), B S is the half-width of silicon (111), and B is the diffraction angle of boron nitride. ], the thickness L C of the crystallite in the C-axis direction was measured to be 460 Å, confirming that crystallization had progressed considerably.
実施例 ２
実施例１で作つた多孔性軽石状物の残り68.4ｇ
をカーボン板に載せ、内径95mmのムライト管に装
填した。つづいて、管内雰囲気をアンモニアガス
で置換し、同管内にアンモニアガスを0.53／
minの流量で供給しながら、300℃／minの昇温速
度で1160℃まで昇温し、１時間保持した後、直ち
にアンモニアガスの供給を停止し、代わりに窒素
ガスを0.03／min供給しながら1250℃に上げ４
時間保持し、その後窒素ガスを流しながら自然放
冷して反応生成物57.7ｇを得た。得られた生成物
は粉末Ｘ線回折法で分析したところBNとα′−
2CaO・SiO2だけの回折ピークを示した。この生
成物を実施例１と同様に粉砕、酸溶出濾過、水
洗、乾燥をして白色粉末を得た。この白色粉末は
Ｘ線回折でBNだけのピークを示した。また白色
粉末の重量は23.5ｇでBNの理論生成量（23.8
ｇ）の98.7％に当たり良好な生成収率を示した。
またＬC（002）は1029.9Åで非常に高い結晶化度
を有している事が確認された。Example 2 Remaining porous pumice material made in Example 1: 68.4g
was placed on a carbon plate and loaded into a mullite tube with an inner diameter of 95 mm. Next, the atmosphere inside the tube was replaced with ammonia gas, and the ammonia gas was added to the tube at 0.53%
The temperature was raised to 1160°C at a rate of 300°C/min while supplying at a flow rate of 0.03 min, and after holding for 1 hour, the supply of ammonia gas was immediately stopped, and nitrogen gas was supplied at 0.03/min instead. Raise to 1250℃ 4
The mixture was maintained for a certain period of time, and then allowed to cool naturally while flowing nitrogen gas to obtain 57.7 g of a reaction product. The obtained product was analyzed by powder X-ray diffraction and was found to be BN and α′-
It showed a diffraction peak only for 2CaO・SiO 2 . This product was pulverized, filtered with acid elution, washed with water, and dried in the same manner as in Example 1 to obtain a white powder. This white powder showed only a BN peak in X-ray diffraction. The weight of the white powder is 23.5g, and the theoretical production amount of BN (23.8
g) showed a good production yield of 98.7%.
Furthermore, it was confirmed that L C (002) had a very high degree of crystallinity at 1029.9 Å.
実施例 ３
まず、B2O345.58％、CaO25.42％、SiO23.66
％、MgO0.88％、Fe2O30.49％、Na2O0.06％、
K2O0.21％、Ａ2O30.88％、IgLoss22.8％及び付
着水1.29％を含むコレマナイト鉱を用意し、これ
をポツトミルにて粉砕した。つづいて、この粉砕
コレマナイト鉱200ｇとSiO299.9％を含むフラツ
タリーサンド47.2ｇとを混合した後、760℃、30
分間加熱乾燥して多孔性軽石状物200.8ｇを作つ
た。このうちの100ｇを取りアンモニアとの反応
温度を1240℃に変えた他は実施例１と同一条件で
処理して反応生成物85.6ｇを得た。Example 3 First, B 2 O 3 45.58%, CaO2 5.42%, SiO 2 3.66
%, MgO0.88%, Fe 2 O 3 0.49%, Na 2 O 0.06%,
Colemanite ore containing 0.21% K 2 O, 0.88% A 2 O 3 , 22.8% IgLoss and 1.29% attached water was prepared and ground in a pot mill. Next, 200 g of this crushed colemanite ore and 47.2 g of flattery sand containing 99.9% SiO 2 were mixed and heated at 760°C for 30 minutes.
The mixture was heated and dried for 200.8 g of porous pumice. 100g of this was taken and treated under the same conditions as in Example 1 except that the reaction temperature with ammonia was changed to 1240°C to obtain 85.6g of a reaction product.
得られた生成物を粉末Ｘ線回折で分析したとこ
ろ、BNとα−CaO・SiO2だけのピークを示し
た。この生成物を実施例１と同条件で粉砕、酸溶
出、乾燥を行なつたところ白色粉末を得た。この
白色粉末をＸ線回折で分析したところ、BNだけ
の回折ピークを示した。白色粉末の重量は29.5ｇ
でBNの理論生成量（32.4ｇ）の91.0％に相当し
た。また、ＬC（002）の測定値は370Åで結晶化
がかなり進んでいることが確認された。 When the obtained product was analyzed by powder X-ray diffraction, it showed only peaks of BN and α-CaO·SiO 2 . This product was pulverized, acid eluted and dried under the same conditions as in Example 1 to obtain a white powder. When this white powder was analyzed by X-ray diffraction, it showed a diffraction peak only for BN. The weight of the white powder is 29.5g
This corresponded to 91.0% of the theoretical production amount of BN (32.4 g). Furthermore, the measured value of L C (002) was 370 Å, which confirmed that crystallization had progressed considerably.
実施例 ４
実施例３で作つた多孔性軽石状物の残り100.8
ｇを取りアンモニアとの反応を1240℃、１時間に
変えた他は実施例２と同一条件で反応、熱処理し
反応生成物86.1ｇを得た。Example 4 Remaining porous pumice material made in Example 3 100.8
86.1 g of a reaction product was obtained by reaction and heat treatment under the same conditions as in Example 2, except that the reaction with ammonia was changed to 1240° C. for 1 hour.
得られた生成物はBNとα−CaO・SiO2だけの
Ｘ線回折ピークを示した。この生成物を実施例１
と同一条件で粉砕、酸溶出、濾過、水洗、乾燥を
行なつたところ白色粉末を得た。この粉末はBN
だけのＸ線回折ピークを示した。白色粉末の重量
は30.3ｇでBNの理論生成量（32.6ｇ）の92.8％に
相当した。またＬC（002）の測定値は712.1Åで
結晶化がかなり進んでいる事が確認された。 The obtained product showed X-ray diffraction peaks of only BN and α-CaO·SiO 2 . This product was prepared in Example 1.
After pulverization, acid elution, filtration, washing with water, and drying under the same conditions as above, a white powder was obtained. This powder is BN
showed only one X-ray diffraction peak. The weight of the white powder was 30.3 g, which corresponded to 92.8% of the theoretical production amount of BN (32.6 g). Furthermore, the measured value of L C (002) was 712.1 Å, which confirmed that crystallization had progressed considerably.
Claims (1)
SiO2のモル比が0.5≦SiO2／CaO≦1.0となるよう
にシリカ分を調整したものを原料とし、この原料
を1000℃以上の温度下でアンモニアと反応させる
ことを特徴とする窒化硼素を含むセラミツク物質
の製造方法。1 Regarding CaO of naturally occurring colemanite ore
Boron nitride is produced by using a raw material whose silica content is adjusted so that the molar ratio of SiO 2 is 0.5≦SiO 2 /CaO≦1.0, and reacting this raw material with ammonia at a temperature of 1000°C or higher. A method of manufacturing a ceramic material comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56140778A JPS5841706A (en) | 1981-09-07 | 1981-09-07 | Preparation of ceramic substance containing boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56140778A JPS5841706A (en) | 1981-09-07 | 1981-09-07 | Preparation of ceramic substance containing boron nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5841706A JPS5841706A (en) | 1983-03-11 |
| JPS6159243B2 true JPS6159243B2 (en) | 1986-12-15 |
Family
ID=15276522
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56140778A Granted JPS5841706A (en) | 1981-09-07 | 1981-09-07 | Preparation of ceramic substance containing boron nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5841706A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0526939U (en) * | 1991-09-17 | 1993-04-06 | 村田機械株式会社 | Roll paper storage device |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6256307A (en) * | 1985-09-05 | 1987-03-12 | Tokuyama Soda Co Ltd | Production of powder mixed with boron nitride |
| FR2817855B1 (en) * | 2000-12-11 | 2003-09-05 | Saint Gobain Ct Recherches | BORON NITRIDE POWDER AND PROCESS FOR ITS PREPARATION |
| US7297317B2 (en) | 2004-12-28 | 2007-11-20 | Momentive Performance Materials Inc. | Process for producing boron nitride |
| DE112013007154B4 (en) * | 2013-06-14 | 2018-10-31 | Yeditepe Universitesi | Production process for boron nitride nanotubes |
| JP6516594B2 (en) * | 2015-07-01 | 2019-05-22 | 株式会社トクヤマ | Hexagonal boron nitride particles and method for producing the same |
-
1981
- 1981-09-07 JP JP56140778A patent/JPS5841706A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0526939U (en) * | 1991-09-17 | 1993-04-06 | 村田機械株式会社 | Roll paper storage device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5841706A (en) | 1983-03-11 |
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