JP3207850B2 - Method for producing alkali titanate whiskers - Google Patents
Method for producing alkali titanate whiskersInfo
- Publication number
- JP3207850B2 JP3207850B2 JP33005090A JP33005090A JP3207850B2 JP 3207850 B2 JP3207850 B2 JP 3207850B2 JP 33005090 A JP33005090 A JP 33005090A JP 33005090 A JP33005090 A JP 33005090A JP 3207850 B2 JP3207850 B2 JP 3207850B2
- Authority
- JP
- Japan
- Prior art keywords
- alkali
- titanate
- source
- firing
- alkali titanate
- 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 - Lifetime
Links
- 239000003513 alkali Substances 0.000 title claims description 40
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 238000010304 firing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 230000004907 flux Effects 0.000 claims description 8
- 150000004820 halides Chemical class 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- -1 alkali metal titanate Chemical class 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 10
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 238000007716 flux method Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 239000011698 potassium fluoride Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000003270 potassium fluoride Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910010280 TiOH Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はチタン酸アルカリウィスカー、詳しくは例え
ばプラスチックス等の補強材、イオン吸着剤、イオン交
換材、分子吸着材、摩擦材、過材、触媒担体、断熱材
その他種々の用途に供される繊維状特にアスペクト比の
高い繊維状チタン酸アルカリウィスカーの製造方法に関
する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to alkali titanate whiskers, specifically, for example, reinforcing materials such as plastics, ion adsorbents, ion exchange materials, molecular adsorbents, friction materials, excess materials, The present invention relates to a method of producing a fibrous alkali titanate whisker having a high aspect ratio, particularly a catalyst carrier, a heat insulating material and various other uses.
従来のチタン酸アルカリの製造方法としては、例えば
原料混合物を焼成し、固相反応により合成する焼成法
（特開昭53−26298）、融剤と共に溶融し、融剤中でチ
タン酸アルカリの結晶を育成し、冷却後融剤を溶出除去
してチタン酸アルカリを得る融剤法（フラックス法）
（特特昭51−122700）、主として化学量論的に調合され
た混合物を溶融しこれを冷却固化して結晶化させる溶融
法（特開昭51−89900）、溶媒を用いて水の臨界点以上
の高温高圧下で合成する水熱法（特開昭50−64526号）
等があげられる。As a conventional method for producing alkali titanate, for example, a firing method in which a raw material mixture is fired and synthesized by a solid-phase reaction (Japanese Patent Application Laid-Open No. 53-26298), melting with a flux, and crystallization of alkali titanate in the flux Flux method to obtain alkali titanate by leaching and removing flux after cooling (flux method)
(JP-B-51-122700), a melting method in which a stoichiometrically prepared mixture is melted, cooled, solidified and crystallized (JP-A-51-89900), the critical point of water using a solvent Hydrothermal method synthesized under the above high temperature and high pressure (Japanese Patent Laid-Open No. 50-64526)
And the like.
上記のような従来の焼成法においては結晶性が低く得
られる繊維は数μｍの短繊維であり、フラックス法では
フラックスを除去する水洗工程が必要であり、かつフラ
ックスの回収設備を必要としコスト高となる。また溶融
法は結晶が互いに密着したまま成長するので解離処理が
困難であり、かつ得られる繊維は径が太くアスペクト比
が低く強度の点で補強材として好ましくない。In the conventional calcination method as described above, the fiber obtained with low crystallinity is a short fiber of several μm, and the flux method requires a water washing step for removing the flux, and requires equipment for collecting the flux, resulting in high cost. Becomes In addition, the melting method is difficult to perform the dissociation treatment because the crystals grow while keeping the crystals in close contact with each other, and the obtained fiber is not preferable as a reinforcing material because of its large diameter, low aspect ratio, and strength.
更に水熱法は、高圧下で高アルカリ溶液中で合成操作
が行われるものであるから保安装置を必要とし設備全体
として費用が高くなり、またAg等の特殊材質を必要と
し、かつ連続操業が難しい。従来法にはそれぞれ上記の
ような問題点があり、かついずれもアスペクト比の高い
ウィスカーを得ることはできない。Furthermore, the hydrothermal method requires a safety device because the synthesis operation is performed in a high-alkaline solution under high pressure, which increases the cost of the entire equipment, requires special materials such as Ag, and requires continuous operation. difficult. Each of the conventional methods has the above-mentioned problems, and none of them can obtain a whisker having a high aspect ratio.
本発明者らは高度のアスペクト比を有する高品質のチ
タン酸アルカリウィスカーを得る方法について鋭意研究
の結果、ハロゲン化アルカリと炭素とを粉末状で共存せ
しめたチタン源とアルカリ源の混合粉体を焼成するとア
スペクト比の高いチタン酸アルカリウィスカーが容易に
得られることを見出し本発明を完成した。The present inventors have conducted intensive studies on a method of obtaining a high-quality alkali titanate whisker having a high aspect ratio.As a result, a mixed powder of a titanium source and an alkali source in which an alkali halide and carbon coexisted in a powder form was obtained. The inventors have found that an alkali titanate whisker having a high aspect ratio can be easily obtained by firing, thereby completing the present invention.
本発明の目的は、直線状でアスペクト比が高く、従来
のチタン酸アルカリ繊維にみられるような欠陥がない高
品質のチタン酸アルカリウィスカーを高収率で得ること
ができ、成形、水洗その他従来法のような特定の前後処
理工程を要することなく短縮化された工程により効率よ
く製造する方法を提供するにある。An object of the present invention is to obtain a high-quality alkali titanate whisker having a high linearity and a high aspect ratio without defects such as those found in conventional alkali titanate fibers, and forming, washing and other conventional methods. It is an object of the present invention to provide a method for manufacturing efficiently by a shortened step without requiring a specific pre-processing and post-processing step.
上記目的を達成するため、本発明の方法は、チタン源
とアルカリ源の混合物を焼成して繊維状のチタン酸アル
カリを製造するに当り、M2O・nTiO2（但しＭはアルカリ
金属）で示されるチタン酸アルカリ金属に相当する組成
を形成するチタン源とアルカリ源の原料混合物中に、炭
素原料及びチタン酸アルカリの結晶成長のフラックスと
して作用し焼成時に蒸発するハロゲン化アルカリを、そ
れぞれ0.1〜20重量％共存せしめて焼成することを特徴
とするものである。In order to achieve the above object, the method according to the present invention employs M 2 O · nTiO 2 (where M is an alkali metal) in firing a mixture of a titanium source and an alkali source to produce a fibrous alkali titanate. In a raw material mixture of a titanium source and an alkali source forming a composition corresponding to the alkali metal titanate shown, a carbon raw material and an alkali halide which acts as a flux for crystal growth of the alkali titanate and evaporates during firing are each 0.1 to 0.1%. It is characterized by firing in the presence of 20% by weight.
チタン源としては例えばTiO2、TiOH4等があげられ、
アルカリ源としては例えばM2CO3（但しＭはアルカリ金
属）があげられる。炭素原料としては主成分を炭素とす
る原料であればよく、例えばカーボンブラック（チャン
ネルブラック、サーマルブラック、ファーネスブラック
等）、グラファイト活性炭などがあげられ、特に限定さ
れるものではないが、灰分やその他の不純物等が少いも
のが純度の高い製品を得るためには好ましい。Examples of titanium sources include TiO 2 , TiOH 4 and the like,
Examples of the alkali source include M 2 CO 3 (where M is an alkali metal). The carbon raw material may be any raw material containing carbon as a main component, and examples thereof include carbon black (channel black, thermal black, furnace black, etc.), graphite activated carbon, and the like. It is preferable to obtain a high-purity product with few impurities and the like.
ハロゲン化アルカリとしては、KCl、KF、NaCl、NaF等
があげられ１種又は２種以上を用いることができ、焼成
により蒸発するものを用いることにより純度の高い製品
が得られる。通常これらの原料は通常粉状で混合して焼
成する。As the alkali halide, KCl, KF, NaCl, NaF and the like can be mentioned, and one or more kinds can be used, and a product having a high purity can be obtained by using one that evaporates by firing. Usually, these raw materials are usually mixed in powder form and fired.
チタン源とアルカリ源の混合比は好ましくは酸化チタ
ン（TiO2）、酸化アルカリ（R2O）換算モル比でTiO2/R2
O＝２〜８を主原料として、炭素原料及びハロゲン化ア
ルカリをそれぞれ0.1〜20重量％添加混合して900〜1200
℃で焼成する。The mixing ratio of the titanium source and the alkali source is preferably TiO 2 / R 2 in terms of a molar ratio in terms of titanium oxide (TiO 2 ) and alkali oxide (R 2 O).
O = 2 to 8 as main raw materials, carbon raw materials and alkali halides are added and mixed at 0.1 to 20% by weight, respectively, and 900 to 1200
Bake at ℃.
焼成により形成されるTiO2粒子と溶融アルカリとの固
液界面反応が重要であるとの知見を基に研究を重ねた結
果本発明に到達したものであり、本発明における炭素原
料の役割は、瞬間的な燃焼と発生するCOガスの還元雰囲
気が固液界面反応を促進するものと推定される。又焼成
物を多孔質化しウィスカーの成長を助長するすなわち極
く少いハロゲン化アルカリでありながら、その作用はハ
ロゲン化アルカリをチタン酸アルカリの結晶成長のフラ
ックスとして働かせ、反応育成を促し径方向への成長を
抑制し高アスペクト比化させるものである。Based on the finding that the solid-liquid interface reaction between the TiO 2 particles formed by firing and the molten alkali is important, the present inventors have arrived at the present invention as a result of repeated studies, and the role of the carbon material in the present invention is as follows. It is presumed that the instantaneous combustion and the reducing atmosphere of the generated CO gas promote the solid-liquid interface reaction. It also makes the fired product porous and promotes the growth of whiskers. That is, while the amount of alkali halide is extremely small, the action of the alkali halide acts as a flux for crystal growth of alkali titanate, which promotes reaction growth and promotes radial growth. This suppresses the growth of GaN and increases the aspect ratio.
M2O・nTiO2（Ｍはアルカリ金属）で示されるチタン酸
アルカリ金属に相当する組成を形成するチタン源とアル
カリ源の原料に加える炭素原料及びハロゲン化アルカリ
の量は、焼成条件により蒸発可能な添加量で行うことに
より、焼成物はチタン酸アルカリのみであるから水洗工
程は必要としないものである。The amount of the carbon source and alkali halide added to the titanium source and alkali source materials forming the composition corresponding to the alkali metal titanate represented by M 2 O · nTiO 2 (M is an alkali metal) can be evaporated depending on the firing conditions By performing the addition in a small amount, the calcined product is only the alkali titanate, so that the washing step is not required.
なお、この焼成に当ってはトンネル炉等が使用できる
ので、連続焼成を行なうことができる。In addition, since a tunnel furnace or the like can be used for this firing, continuous firing can be performed.
〔実施例１〕 炭酸カリウム1.15kg、酸化チタン4.00kg、カーボンブ
ラック、0.36kg、塩化カリウム0.40kgを、20ヘンシェ
ルミキサーで混合し、1100℃で２時間焼成した。焼成物
をＸ線回折で同定したところ、六チタン酸カリウムであ
った。又、走査型電子顕微鏡で拡大してみると、平均繊
維径0.7μｍ、平均繊維長30μｍの単繊維状態にある高
アスペクト比のものであった。Example 1 1.15 kg of potassium carbonate, 4.00 kg of titanium oxide, 0.36 kg of carbon black, and 0.40 kg of potassium chloride were mixed with a 20 Henschel mixer, and fired at 1100 ° C. for 2 hours. When the calcined product was identified by X-ray diffraction, it was potassium hexatitanate. When enlarged by a scanning electron microscope, it was a single fiber having an average fiber diameter of 0.7 μm and an average fiber length of 30 μm and a high aspect ratio.
〔実施例２〕 炭酸ナトリウム0.88kg、酸化チタン4.00kg、人造黒鉛
0.70kg、塩化ナトリウム0.20kg、弗化カリウム0.40kg混
合し、1100℃で1.5時間焼成した。Ｘ線回折で、得られ
た生成相は、六チタン酸ナトリウムで、平均繊維径0.8
μｍ、平均繊維長40μｍの単繊維状態の高アスペクト比
のものである。[Example 2] 0.88 kg of sodium carbonate, 4.00 kg of titanium oxide, artificial graphite
0.70 kg, 0.20 kg of sodium chloride and 0.40 kg of potassium fluoride were mixed and calcined at 1100 ° C. for 1.5 hours. The product phase obtained by X-ray diffraction was sodium hexatitanate with an average fiber diameter of 0.8.
It has a high aspect ratio in a single fiber state having an average fiber length of 40 μm.
〔実施例３〕 炭酸カリウム1.72kg、酸化チタン3.97kg、カーボンブ
ラック0.03kg、弗化カリウム0.02kgの混合物を、1000℃
で30分間焼成、得られた生成相は、四チタン酸カリウム
で、平均繊維径0.5μｍ、平均繊維長50μｍの単繊維状
態の高アスペクト比のものである。Example 3 A mixture of 1.72 kg of potassium carbonate, 3.97 kg of titanium oxide, 0.03 kg of carbon black, and 0.02 kg of potassium fluoride was heated at 1000 ° C.
The resulting phase is potassium tetratitanate having a high aspect ratio in a single fiber state with an average fiber diameter of 0.5 μm and an average fiber length of 50 μm.
〔比較例１〕 炭酸カリウム1.15kg、酸化チタン4.00kgを実施例１と
同様に、混合、焼成を行ない、評価を行なった。Comparative Example 1 1.15 kg of potassium carbonate and 4.00 kg of titanium oxide were mixed and fired in the same manner as in Example 1, and evaluated.
生成相は、六チタン酸カリウムであるが、平均繊維径
1.5μｍ、平均繊維長2.0μｍの棒状が焼結した塊状のも
のである。The produced phase is potassium hexatitanate, but the average fiber diameter is
It is a lump obtained by sintering a rod having an average fiber length of 1.5 μm and an average fiber length of 2.0 μm.
〔比較例２〕 炭酸カリウム1.15kg、酸化チタン4.00kg、カーボンブ
ラック0.36kgを同様の混合、焼成を行ない評価した。[Comparative Example 2] 1.15 kg of potassium carbonate, 4.00 kg of titanium oxide, and 0.36 kg of carbon black were similarly mixed and fired, and evaluated.
生成相は、六チタン酸カリウムであるが、平均繊維径
1.3μｍ、平均繊維長2.5μｍの棒状が焼結した塊状のも
のである。The produced phase is potassium hexatitanate, but the average fiber diameter is
It is a lump obtained by sintering a rod having a diameter of 1.3 μm and an average fiber length of 2.5 μm.
〔比較例３〕 炭酸カリウム1.15kg、酸化チタン4.00kg、塩化カリウ
ム0.40kgを同様の混合、焼成を行ない評価した。Comparative Example 3 1.15 kg of potassium carbonate, 4.00 kg of titanium oxide, and 0.40 kg of potassium chloride were similarly mixed and fired, and evaluated.
生成相は、六チタン酸カリウムであるが、平均繊維径
1.0μｍ、平均繊維長５μｍの棒状が焼結した塊状のも
のである。The produced phase is potassium hexatitanate, but the average fiber diameter is
It is a lump obtained by sintering a rod having an average fiber length of 1.0 μm and an average fiber length of 5 μm.
以上、説明した様に本発明により、得られるチタン酸
アルカリは、その応用として、利用されやすい高アスペ
クト比の繊維形状として容易に得られるものである。As described above, the alkali titanate obtained by the present invention can be easily obtained as a fiber shape having a high aspect ratio which is easily used as an application thereof.
又、本発明によるチタン酸アルカリウィスカーは、欠
陥の少ない高品質のものとして得られるのも特徴であ
る。第１図は、本実施例１で得られたものの透過型電子
顕微鏡写真である。従来のフラックス法で得られたもの
は、第２図のように転位、欠陥がみられるが、本発明で
得られたものは、結晶欠陥はほとんどみられない。Further, the alkali titanate whisker according to the present invention is characterized in that it can be obtained as a high quality product having few defects. FIG. 1 is a transmission electron micrograph of the product obtained in Example 1. As shown in FIG. 2, dislocations and defects are observed in the one obtained by the conventional flux method, but almost no crystal defects are observed in the one obtained in the present invention.
本発明によれば、従来の方法では得られなかった直線
状でアスペクト比が極めて高い高品質のチタン酸アルカ
リウィスカーが、焼成後水中での水洗工程又は水中での
解離操作等特別の後処理を必要とせずに高収率に得ら
れ、工程も簡単で短縮され、低コストで製造できるので
極めて有益である。また数ミリ以上の長繊維の製造も可
能であり、利用分野の拡大が可能となる。According to the present invention, high-quality alkali titanate whiskers having a linear and aspect ratio extremely high, which could not be obtained by the conventional method, undergo a special post-treatment such as a washing step in water or a dissociation operation in water after firing. It is extremely beneficial because it can be obtained in high yield without the need, the process is simple and short, and it can be manufactured at low cost. In addition, it is possible to manufacture long fibers of several millimeters or more, and it is possible to expand the application field.
図面は透過型電子顕微鏡写真で、第１図は本発明方法で
得られたチタン酸アルカリウィスカーであり、第２図は
従来のフラックス法で得られたチタン酸アルカリ繊維で
ある。The drawing is a transmission electron micrograph. FIG. 1 shows an alkali titanate whisker obtained by the method of the present invention, and FIG. 2 shows an alkali titanate fiber obtained by a conventional flux method.
Claims (2)
繊維状のチタン酸アルカリを製造するに当り、 M2O・nTiO2（但しＭはアルカリ金属）で示されるチタン
酸アルカリ金属に相当する組成を形成するチタン源とア
ルカリ源の原料混合物中に、炭素原料及びチタン酸アル
カリの結晶成長のフラックスとして作用し焼成時に蒸発
するハロゲン化アルカリを、それぞれ0.1〜20重量％共
存せしめて焼成することを特徴とするチタン酸アルカリ
ウィスカーの製造方法。1. A method for producing a fibrous alkali titanate by firing a mixture of a titanium source and an alkali source, which corresponds to an alkali metal titanate represented by M 2 O.nTiO 2 (where M is an alkali metal). In the raw material mixture of the titanium source and the alkali source that forms the composition to be formed, 0.1 to 20% by weight of an alkali halide which acts as a flux for crystal growth of the carbon raw material and the alkali titanate and evaporates at the time of firing is coexistent and fired. A method for producing an alkali titanate whisker.
タン（TiO2）、酸化アルカリ（R2O）換算モル比でTiO2/
R2O＝２〜８である請求項１記載のチタン酸アルカリウ
ィスカーの製造方法。2. A mixing ratio of a titanium source and an alkali source is TiO 2 / TiO 2 in terms of molar ratio in terms of titanium oxide (TiO 2 ) and alkali oxide (R 2 O).
R 2 O = 2 to 8 in which the production method of the alkali metal titanate whiskers according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33005090A JP3207850B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali titanate whiskers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33005090A JP3207850B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali titanate whiskers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04202099A JPH04202099A (en) | 1992-07-22 |
| JP3207850B2 true JP3207850B2 (en) | 2001-09-10 |
Family
ID=18228220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33005090A Expired - Lifetime JP3207850B2 (en) | 1990-11-30 | 1990-11-30 | Method for producing alkali titanate whiskers |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3207850B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4755738B2 (en) * | 2005-05-31 | 2011-08-24 | 学校法人日本大学 | Piezoelectric material and synthesis method thereof |
| CN107614438B (en) * | 2015-06-02 | 2020-03-06 | 东邦钛株式会社 | Alkali metal titanates and friction materials |
-
1990
- 1990-11-30 JP JP33005090A patent/JP3207850B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04202099A (en) | 1992-07-22 |
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