JPH0135772B2 - - Google Patents
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- Publication number
- JPH0135772B2 JPH0135772B2 JP58236753A JP23675383A JPH0135772B2 JP H0135772 B2 JPH0135772 B2 JP H0135772B2 JP 58236753 A JP58236753 A JP 58236753A JP 23675383 A JP23675383 A JP 23675383A JP H0135772 B2 JPH0135772 B2 JP H0135772B2
- Authority
- JP
- Japan
- Prior art keywords
- acicular
- iron
- particles
- present
- iron oxide
- 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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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 41
- 239000002245 particle Substances 0.000 claims description 33
- 229910001567 cementite Inorganic materials 0.000 claims description 20
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 claims description 15
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 27
- 235000013980 iron oxide Nutrition 0.000 description 20
- 229910052799 carbon Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 229910001566 austenite Inorganic materials 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 229910052598 goethite Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910006540 α-FeOOH Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 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
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910006299 γ-FeOOH Inorganic materials 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Description
【発明の詳細な説明】
本発明は炭化鉄を含有する針状粒子の製法に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing acicular particles containing iron carbide.
炭化鉄を含有する針状粒子は高保磁力及び磁場
配向性を有し、磁性材料、特に磁気記録材料とし
て優れたものであり、このような針状粒子につい
て本出願人は既に特許出願（特願昭58−171765
号）している。 Acicular particles containing iron carbide have high coercive force and magnetic field orientation, and are excellent as magnetic materials, especially magnetic recording materials. Showa 58-171765
No.).
上記炭化鉄を含有する針状粒子は針状オキシ水
酸化鉄又は針状酸化鉄をCO又はこれとH2との混
合物と接触させて製造されるものであり、その好
適な接触温度は約300〜400℃であつた。 The iron carbide-containing acicular particles are produced by contacting acicular iron oxyhydroxide or acicular iron oxide with CO or a mixture thereof with H 2 , and the preferred contact temperature is about 300° C. It was ~400℃.
しかしながら、その後も継続して研究を行つた
結果、250〜300℃の温和な接触条件でも炭化鉄を
含有する針状粒子が製造できることを見い出し、
本発明を完成した。 However, as a result of continued research, it was discovered that acicular particles containing iron carbide could be produced even under mild contact conditions of 250 to 300°C.
The invention has been completed.
即ち本発明は、針状オキシ水酸化鉄又は針状酸
化鉄を250〜300℃でCO又はこれとH2との混合物
と接触させることを特徴とする炭化鉄を含有する
針状粒子の製法に係るものである。 That is, the present invention provides a method for producing acicular particles containing iron carbide, which is characterized by contacting acicular iron oxyhydroxide or acicular iron oxide with CO or a mixture of CO and H2 at 250 to 300°C. This is related.
本発明の方法によれば、より温和な条件で目的
とする炭化鉄を含有する針状粒子を製造すること
が可能で、工業的メリツトが大きい。 According to the method of the present invention, it is possible to produce the target acicular particles containing iron carbide under milder conditions, which has great industrial merits.
本発明において、針状オキシ水酸化鉄又は針状
酸化鉄は、平均軸比が３以上のものが通常であ
り、３〜20のものが好適であり、平均粒径（長
軸）は、通常2μｍ以下、好適には0.1〜2μｍ、最
適には0.1〜1.0μｍである。後にも述べるように、
製造される針状粒子は平均軸比及び平均粒径が、
これらの原料のそれらと比較して若干小さくなる
が殆ど変らず、本発明により製造される針状粒子
一般について通常このようなものが好適であるか
らである。 In the present invention, the acicular iron oxyhydroxide or acicular iron oxide usually has an average axis ratio of 3 or more, preferably 3 to 20, and the average particle diameter (long axis) is usually It is 2 μm or less, preferably 0.1 to 2 μm, most preferably 0.1 to 1.0 μm. As mentioned later,
The produced acicular particles have an average axial ratio and an average particle diameter of
This is because, although it is slightly smaller than those of these raw materials, there is almost no difference, and such particles are generally suitable for acicular particles produced by the present invention.
針状オキシ水酸化鉄は、針状α−FeOOH（ゲ
ーサイト）又は針状γ−FeOOH（レピドクサイ
ト）が好ましく、針状酸化鉄は、針状α−Fe2O3
（ヘマタイト）、針状γ−Fe2O3（マグヘマイト）
又は針状Fe3O4（マグネタイト）が好ましい。針
状オキシ水酸化鉄は、また表面のPHが５以上のも
のが好ましい。 The acicular iron oxyhydroxide is preferably acicular α-FeOOH (goethite) or acicular γ-FeOOH (lepidoxite), and the acicular iron oxide is acicular α-Fe 2 O 3
(hematite), acicular γ-Fe 2 O 3 (maghemite)
Or acicular Fe 3 O 4 (magnetite) is preferable. The acicular iron oxyhydroxide preferably has a surface pH of 5 or more.
上記の針状α−Fe2O3又は針状γ−Fe2O3とし
ては、例えば針状α−FeOOH又は針状γ−
FeOOHをそれぞれ約200〜350℃に加熱及び脱水
して得られたもの、あるいはこれらを更に約350
〜900℃に加熱して結晶の緻密化を図つた針状α
−Fe2O3等あらゆるものが用いられる。 As the above-mentioned acicular α-Fe 2 O 3 or acicular γ-Fe 2 O 3 , for example, acicular α-FeOOH or acicular γ-
Those obtained by heating and dehydrating FeOOH to approximately 200 to 350℃, or further heating and dehydrating FeOOH to approximately 350℃.
Acicular α heated to ~900℃ to densify the crystal
−Fe 2 O 3 , etc. can all be used.
前記の針状Fe3O4は、針状Fe3O4以外の針状酸
化鉄又は針状オキシ水酸化鉄をCO、H2又はこれ
らの混合物と接触させることによつて製造するこ
とができる。もつとも、前記の針状Fe3O4は、こ
の製法によつて製造されたものに限定されるもの
ではない。特別な場合として、CO又はこれとH2
との混合物を針状オキシ水酸化鉄又は針状Fe3O4
以外の針状酸化鉄と接触させて針状Fe3O4を製造
する場合、後述の接触条件と比較して、時間に関
する以外同一の接触条件にすることができる。そ
の場合は、針状Fe3O4の製造に引き続き同一条件
で接触を継続して目的とする本発明の針状粒子を
製造することができる。 The above-mentioned acicular Fe 3 O 4 can be produced by contacting acicular iron oxide or acicular iron oxyhydroxide other than acicular Fe 3 O 4 with CO, H 2 or a mixture thereof. . However, the acicular Fe 3 O 4 described above is not limited to that produced by this method. As a special case, CO or it and H 2
Mixture with acicular iron oxyhydroxide or acicular Fe 3 O 4
When producing acicular Fe 3 O 4 by contacting with other acicular iron oxides, the contact conditions can be the same except for time, compared to the contact conditions described below. In that case, the desired acicular particles of the present invention can be produced by continuing contact under the same conditions following the production of acicular Fe 3 O 4 .
また、本発明における針状オキシ水酸化鉄又は
針状酸化鉄は、形状が針状であり、主成分がオキ
シ水酸化鉄又は酸化鉄である限り、少量の銅、マ
グネシウム、マンガン、ニツケル、コバルト等の
酸化物、炭酸塩等の化合物及び／又は珪素等の酸
化物、カリウム塩、ナトリウム塩等の化合物を添
加して成るものであつてもよい。 In addition, the acicular iron oxyhydroxide or acicular iron oxide in the present invention is acicular in shape and contains a small amount of copper, magnesium, manganese, nickel, or cobalt, as long as the main component is iron oxyhydroxide or iron oxide. It may be formed by adding compounds such as oxides and carbonates of silicon, etc., and/or compounds such as oxides of silicon, potassium salts, sodium salts, etc.
CO又はこれとH2との混合物は、希釈してある
いは希釈せずに使用することができ、希釈剤とし
ては、例えばN2、CO2、アルゴン、ヘリウム等
を挙げることができる。COとH2との混合物を用
いるとき、その混合比は適宜に選択することがで
きるが、通常はCO／H2（容量比）＝１／0.05〜
１／５とするのが好ましい。また希釈率は任意に
選択できるが、10倍（容量比）にとどめるのが好
ましい。接触時間、CO又はこれとH2との混合物
の流速等の接触条件は、例えば針状オキシ水酸化
鉄又は針状酸化鉄の製造履歴、平均軸比、平均粒
径、比量面積、CO又はこれとH2との混合物の希
釈比等に応じ変動するため、適宜選択するのがよ
い。好ましい接触時間は、針状Fe3O4に対して約
１〜10時間、その他の針状酸化鉄又は針状オキシ
水酸化鉄に対してはFe3O4に還元された後、更に
約１〜10時間、好ましいCO又はこれとH2との混
合物の流速は、原料の針状オキシ水酸化鉄等１ｇ
当り約１〜1000mlS.T.P／分である。なお、接触
圧力は、希釈されたCO又はこれとH2との混合物
を用いる場合は希釈剤をも含めて、１〜２気圧が
常用されるが、特に制限はない。 CO or a mixture thereof with H 2 can be used diluted or undiluted, and diluents include, for example, N 2 , CO 2 , argon, helium, and the like. When using a mixture of CO and H2 , the mixing ratio can be selected as appropriate, but usually CO/ H2 (volume ratio) = 1/0.05~
It is preferable to set it to 1/5. Further, the dilution rate can be selected arbitrarily, but it is preferably kept at 10 times (volume ratio). Contact conditions such as contact time, flow rate of CO or a mixture of CO and H2, etc. are determined based on, for example, the manufacturing history of acicular iron oxyhydroxide or acicular iron oxide, average axial ratio, average particle diameter, specific area, CO or Since it varies depending on the dilution ratio of the mixture of this and H 2 , it is best to select it appropriately. The preferred contact time is about 1 to 10 hours for acicular Fe 3 O 4 , and about 1 hour for other acicular iron oxides or acicular iron oxyhydroxides after being reduced to Fe 3 O 4 . ~10 hours, the preferred flow rate of CO or its mixture with H2 is 1 g of raw material acicular iron oxyhydroxide, etc.
Approximately 1 to 1000 ml S.TP/min. In addition, when using diluted CO or a mixture of CO and H 2 , the contact pressure is usually 1 to 2 atmospheres including a diluent, but there is no particular restriction.
本発明で得られる粒子は、電子顕微鏡で観察す
ると、原料の針状オキシ水酸化鉄又は針状酸化鉄
の針状粒子と同形状で、これらの形骸粒子であ
り、これが一次粒子となつて存在している。ま
た、本発明で得られる針状粒子は、Ｘ線回折パタ
ーンにより炭化鉄を含有することが明らかであ
る。Ｘ線回折パターンは、面間隔が2.28、2.20、
2.08、2.05及び0.92Åを示す。かかるパターンは、
Fe5C2に相当し、本発明の炭化鉄は通常は主とし
てFe5C2からなるが、Fe2C、Fe20C9（Fe2、2C）、
Fe3C等が共存することがある。従つて本発明の
針状粒子に含有される炭化鉄は、FexC（２≦ｘ＜
３）と表示するのが適切である。 When observed with an electron microscope, the particles obtained in the present invention have the same shape as the acicular particles of the raw material acicular iron oxyhydroxide or acicular iron oxide, and are vestigial particles of these particles, which exist as primary particles. are doing. Furthermore, it is clear from the X-ray diffraction pattern that the acicular particles obtained in the present invention contain iron carbide. The X-ray diffraction pattern has interplanar spacings of 2.28, 2.20,
2.08, 2.05 and 0.92 Å are shown. Such a pattern is
Corresponding to Fe 5 C 2 , the iron carbide of the present invention usually mainly consists of Fe 5 C 2 , but also Fe 2 C, Fe 20 C 9 (Fe 2 , 2 C),
Fe 3 C etc. may coexist. Therefore, the iron carbide contained in the acicular particles of the present invention satisfies FexC (2≦x<
3) is appropriate.
また、炭化が不完全な場合、本発明で得られる
針状粒子は酸化鉄、主としてFe3O4をも含有す
る。一般に、残化鉄については、FeO、Fe3O4及
びγ−Fe2O3が構造的に関連があり、これら３者
とも酸素原子は立方最密詰込み構造を有してお
り、現実に存在するFe3O4は、これらの幅で変動
することから上記の酸化鉄は、FeOy（１＜ｙ≦
1.5）で示すのが適切である。 If carbonization is incomplete, the acicular particles obtained according to the invention also contain iron oxides, mainly Fe 3 O 4 . In general, with regard to residual iron, FeO, Fe 3 O 4 and γ-Fe 2 O 3 are structurally related, and oxygen atoms in these three have a cubic close-packed structure, and in reality Since the existing Fe 3 O 4 varies within these ranges, the above iron oxide is FeOy (1<y≦
1.5) is appropriate.
また、本発明で得られる針状粒子は、炭化鉄又
は場合により酸化鉄を含有するが、Ｃ、Ｈ及びＮ
の元素分析値を参照すると、通常、Ｘ線回析パタ
ーンで確認される炭化鉄の化学式で計算される炭
素量よりも炭素を過剰に含有する。かかる過剰の
炭素は、鉄と結合して存在するか遊離の炭素とし
て存在するか不明である。この意味において、前
記で得られる針状粒子には、元素炭素が存在する
ことがある。従つて、本発明で得られる粒子は、
一次粒子としての形状が平均軸比３以上の、実質
的に炭化鉄から成る針状粒子、又は炭化鉄と酸化
鉄及び／又は元素炭素である針状粒子である。 Further, the acicular particles obtained in the present invention contain iron carbide or iron oxide in some cases, but include C, H and N.
Referring to the elemental analysis value of , it usually contains more carbon than the amount of carbon calculated from the chemical formula of iron carbide confirmed by the X-ray diffraction pattern. It is unclear whether such excess carbon exists in combination with iron or as free carbon. In this sense, elemental carbon may be present in the acicular particles obtained above. Therefore, the particles obtained by the present invention are
These are acicular particles having an average axial ratio of 3 or more as primary particles and consisting essentially of iron carbide, or acicular particles consisting of iron carbide, iron oxide, and/or elemental carbon.
しかして、本発明で得られる針状粒子における
炭化鉄及び酸化鉄の含有量は、Ｘ線回折分析で検
出されるそれぞれの主成分であるFe5C2及び
Fe3O4を炭化鉄及び酸化鉄の化学式と定め、更に
元素分析及び均熱増量により求めることができ
る。炭化鉄の含有量は20重量％以上が好ましく、
50重量％以上が更に好ましい。また酸化鉄は70重
量％以下が好ましく、40重量％以下が更に好まし
い。 Therefore, the content of iron carbide and iron oxide in the acicular particles obtained by the present invention is determined by the respective main components Fe 5 C 2 and Fe 5 C 2 and iron oxide detected by X-ray diffraction analysis.
Fe 3 O 4 is defined as the chemical formula of iron carbide and iron oxide, and it can be further determined by elemental analysis and soaked weight increase. The content of iron carbide is preferably 20% by weight or more,
More preferably 50% by weight or more. Further, the iron oxide content is preferably 70% by weight or less, more preferably 40% by weight or less.
また、本発明で得られる針状粒子の平均軸比及
び平均粒径は、原料の針状オキシ水酸化鉄又は針
状酸化鉄のそれらと比較して若干小さくなるが殆
ど差はない。従つて、本発明で得られる針状粒子
の平均軸比は、通常３以上、好適には３〜20であ
り、平均粒径（長軸）は、通常2μｍ以下、好適
には0.1〜2μｍ、最適には0.1〜1.0μｍである。 Furthermore, the average axial ratio and average particle diameter of the acicular particles obtained in the present invention are slightly smaller than those of the raw material acicular iron oxyhydroxide or acicular iron oxide, but there is almost no difference. Therefore, the average axial ratio of the acicular particles obtained in the present invention is usually 3 or more, preferably 3 to 20, and the average particle diameter (long axis) is usually 2 μm or less, preferably 0.1 to 2 μm, The optimal thickness is 0.1 to 1.0 μm.
本発明において、炭化鉄が生成したことは、そ
の生成物のＸ線回折パターンを観察し、保磁力を
測定することによつて確認することができる。Ｘ
線回折パターンについては、標準チヤートと照合
すること、保磁力については、Fe3O4の保磁力を
越えていることにより炭化鉄の生成を確認するこ
とができる。 In the present invention, generation of iron carbide can be confirmed by observing the X-ray diffraction pattern of the product and measuring the coercive force. X
The formation of iron carbide can be confirmed by comparing the line diffraction pattern with a standard chart and by checking that the coercive force exceeds that of Fe 3 O 4 .
以下に実施例を挙げて詳しく説明する。 A detailed explanation will be given below with reference to examples.
実施例において、磁気特性は次の方法によつて
求めた。即ちホール素子を用いたガウスメーター
により試料充填率0.2で、測定磁場5kOeで、保磁
力Hcを測定する。 In the examples, magnetic properties were determined by the following method. That is, the coercive force Hc is measured using a Gaussmeter using a Hall element at a sample filling rate of 0.2 and a measurement magnetic field of 5 kOe.
実施例 １
平均粒径（長軸）0.6μｍ、平均軸比８の針状の
表面のPHが8.0のゲーサイト粒子２ｇを磁製ボー
トに入れて管状炉に挿入し、窒素を流して空気を
置換した後、250℃に昇温し、その温度でCOガス
を毎分200mlの流速で流しながら５時間処理し、
その後室温まで放冷して黒色の針状粉末を得た。Example 1 2 g of goethite particles with an average particle diameter (long axis) of 0.6 μm, an average axial ratio of 8, and a pH of 8.0 on the acicular surface were placed in a porcelain boat, inserted into a tube furnace, and nitrogen was flowed to remove air. After the substitution, the temperature was raised to 250°C, and the treatment was carried out at that temperature for 5 hours while flowing CO gas at a flow rate of 200ml per minute.
Thereafter, it was allowed to cool to room temperature to obtain a black acicular powder.
得られた針状粉末のＸ線回折スペクトルは面間
隔2.29、2.21、2.08、2.05及び1.92Åの各ピークを
有し、また針状粉末のHcは940Oeであつた。 The X-ray diffraction spectrum of the obtained acicular powder had peaks with interplanar spacings of 2.29, 2.21, 2.08, 2.05 and 1.92 Å, and the Hc of the acicular powder was 940 Oe.
実施例 ２〜３
接触温度を280℃及び300℃とした以外は、実施
例１と同様にして炭化鉄を含有する針状粉末を得
た。この針状粉末のHcはそれぞれ988及び945Oe
であつた。Examples 2-3 Acicular powder containing iron carbide was obtained in the same manner as in Example 1, except that the contact temperatures were 280°C and 300°C. The Hc of this acicular powder is 988 and 945 Oe, respectively.
It was hot.
Claims (1)
300℃でCO又はこれとH2との混合物と接触させ
ることを特徴とする炭化鉄を含有する針状粒子の
製法。1 Acicular iron oxyhydroxide or acicular iron oxide from 250 to
A method for producing acicular particles containing iron carbide, characterized by contacting with CO or a mixture thereof with H 2 at 300°C.
Priority Applications (8)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58236753A JPS60127212A (en) | 1983-12-14 | 1983-12-14 | Production of needlelike particle containing iron carbide |
| EP84104661A EP0123318B1 (en) | 1983-04-25 | 1984-04-25 | Acicular particulate material containing iron carbide |
| DE8484104661T DE3469820D1 (en) | 1983-04-25 | 1984-04-25 | Acicular particulate material containing iron carbide |
| KR1019840002220A KR900005686B1 (en) | 1983-04-25 | 1984-04-25 | A cicular particulate material containing iron carbide |
| BE0/213877A BE900884A (en) | 1983-11-17 | 1984-10-24 | Acicular particulate materials - contg. iron carbide useful as magnetic materials |
| CA000466189A CA1320033C (en) | 1983-11-17 | 1984-10-24 | Acicular particulate material containing iron carbide |
| US06/918,783 US4842759A (en) | 1983-04-25 | 1986-10-14 | Acicular process for producing particulate material |
| US07/327,461 US5151206A (en) | 1983-04-25 | 1989-03-22 | Acicular iron carbide particulate material and process for producing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58236753A JPS60127212A (en) | 1983-12-14 | 1983-12-14 | Production of needlelike particle containing iron carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60127212A JPS60127212A (en) | 1985-07-06 |
| JPH0135772B2 true JPH0135772B2 (en) | 1989-07-27 |
Family
ID=17005278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58236753A Granted JPS60127212A (en) | 1983-04-25 | 1983-12-14 | Production of needlelike particle containing iron carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60127212A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0729763B2 (en) * | 1987-10-13 | 1995-04-05 | ダイキン工業株式会社 | Iron carbide fine particles and method for producing the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6016808A (en) * | 1983-07-05 | 1985-01-28 | Daikin Ind Ltd | Magnetic material containing iron carbide |
-
1983
- 1983-12-14 JP JP58236753A patent/JPS60127212A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6016808A (en) * | 1983-07-05 | 1985-01-28 | Daikin Ind Ltd | Magnetic material containing iron carbide |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60127212A (en) | 1985-07-06 |
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