JPH0987857A - Carbide coating method by plasma cvd - Google Patents
Carbide coating method by plasma cvdInfo
- Publication number
- JPH0987857A JPH0987857A JP7274681A JP27468195A JPH0987857A JP H0987857 A JPH0987857 A JP H0987857A JP 7274681 A JP7274681 A JP 7274681A JP 27468195 A JP27468195 A JP 27468195A JP H0987857 A JPH0987857 A JP H0987857A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- plasma
- carbide
- methane
- electromagnetic wave
- 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
- 238000000576 coating method Methods 0.000 title claims description 11
- 239000000843 powder Substances 0.000 claims abstract description 33
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 150000004706 metal oxides Chemical class 0.000 claims description 7
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000008246 gaseous mixture Substances 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000010453 quartz Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 108010085603 SFLLRNPND Proteins 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- -1 etc. Inorganic materials 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002065 inelastic X-ray scattering Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、チタニア,ジルコニア
等の金属酸化物粉末粒子の表面を炭化物でコーティング
する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for coating the surface of metal oxide powder particles such as titania and zirconia with a carbide.
【0002】[0002]
【従来の技術】ダイヤモンド膜やダイヤモンド状炭素膜
は、高硬度,耐摩耗性,低摩擦抵抗等の優れた特性を呈
することから、切削材料,半導体保護膜等として広範な
分野で使用されている。ダイヤモンド膜,ダイヤモンド
状炭素膜等の合成には、プラズマCVD法が多用されて
いる。2. Description of the Related Art Diamond films and diamond-like carbon films are used in a wide range of fields as cutting materials, semiconductor protective films, etc. because they exhibit excellent characteristics such as high hardness, wear resistance, and low friction resistance. . A plasma CVD method is often used for synthesizing a diamond film, a diamond-like carbon film and the like.
【0003】[0003]
【発明が解決しようとする課題】プラズマCVDでは、
ダイヤモンド膜やダイヤモンド状炭素膜を基板上で合成
しているが、金属酸化物粉体をコーティング対象とした
例はない。しかし、金属酸化物の粉末にダイヤモンド膜
やダイヤモンド状炭素膜をコーティングするとき、酸化
物粉体に新たに表面特性を付与できることが考えられ
る。本発明は、このような要求に応えるべく案出された
ものであり、電子密度や電離度が高く、長時間の安定性
に優れた低温プラズマCVD法を使用することにより、
酸化物粉体の表面を炭化物でコーティングし、高機能粉
末粒子を得ることを目的とする。In plasma CVD,
Although a diamond film and a diamond-like carbon film are synthesized on a substrate, there is no example in which metal oxide powder is used as a coating target. However, when coating a metal oxide powder with a diamond film or a diamond-like carbon film, it is considered that new surface characteristics can be imparted to the oxide powder. The present invention has been devised to meet such a demand, and has a high electron density and ionization degree, and by using a low temperature plasma CVD method excellent in stability for a long time,
The purpose is to obtain high-performance powder particles by coating the surface of oxide powder with carbide.
【0004】[0004]
【課題を解決するための手段】本発明のコーティング方
法は、その目的を達成するため、金属酸化物の粉体を収
容した容器を真空引きし、前記容器を回転させながらメ
タンと水素との混合ガスを供給すると共に、前記粉体に
電磁波を照射してプラズマを発生させ、該プラズマによ
りメタンを分解して得られる炭素と前記粉体中の格子状
酸素とを置換し、前記粉体の粒子表面に炭化物を付着さ
せることを特徴とする。金属酸化物の粉体を収容した容
器を毎分20〜100回転の速度で回転させるとき、個
々の粉末粒子にプラズマが均等に照射され、均一な炭化
物のコーティングが施される。また、メタンを効率よく
分解させて繊維状の炭素系物質を得る上では、照射する
電磁波の周波数を1MHz〜10GHzの範囲に維持す
ることが好ましい。In order to achieve the object, the coating method of the present invention is to evacuate a container containing a powder of metal oxide and to mix methane and hydrogen while rotating the container. While supplying gas, the powder is irradiated with electromagnetic waves to generate plasma, and carbon obtained by decomposing methane by the plasma is replaced with lattice oxygen in the powder, and particles of the powder are obtained. Characterized by depositing carbide on the surface. When the container containing the powder of the metal oxide is rotated at a speed of 20 to 100 revolutions per minute, the individual powder particles are uniformly irradiated with plasma, and a uniform carbide coating is applied. Further, in order to efficiently decompose methane to obtain a fibrous carbon-based substance, it is preferable to maintain the frequency of the electromagnetic wave to be irradiated within the range of 1 MHz to 10 GHz.
【0005】本発明では、たとえば図1に示す設備構成
の電磁波プラズマ加熱装置が使用される。電磁波発振器
1から発振された電磁波は、アイソレータ2を経て送り
出され、パワーモニター3で出力が測定される。次い
で、スリースタブチューナ4を経て反応室5に送り込ま
れる。反応室5の下部には、プランジャー6が設けられ
ている。プランジャー6の上方に、処理される粉体を収
容した石英製反応管7が配置されている。石英製反応管
7は、スターラ8によって回転可能になっている。石英
製反応管7の内部は、トラップ9を介して接続された真
空ポンプによって真空引きされ、真空ゲージ11によっ
て内圧が測定される。処理される粉体には、チタニア,
ジルコニア等の外にSc,Y,ランタノイド元素,H
f,V,Nb,Ta等の酸化物や複合酸化物等が使用さ
れる。粉体粒子の粒径は、使用目的にもよるが、1〜2
000μmの範囲にあることが好ましい。In the present invention, for example, an electromagnetic wave plasma heating device having the equipment structure shown in FIG. 1 is used. The electromagnetic wave oscillated from the electromagnetic wave oscillator 1 is sent out through the isolator 2 and the output is measured by the power monitor 3. Then, it is fed into the reaction chamber 5 via the three-stub tuner 4. A plunger 6 is provided below the reaction chamber 5. Above the plunger 6, a quartz reaction tube 7 containing the powder to be treated is arranged. The quartz reaction tube 7 is rotatable by a stirrer 8. The inside of the quartz reaction tube 7 is evacuated by a vacuum pump connected via a trap 9, and the internal pressure is measured by a vacuum gauge 11. The powder to be treated includes titania,
In addition to zirconia, etc., Sc, Y, lanthanoid element, H
An oxide such as f, V, Nb, or Ta, a complex oxide, or the like is used. The particle size of the powder particles depends on the purpose of use, but is 1-2.
It is preferably in the range of 000 μm.
【0006】適宜の混合ガス給気管が石英製反応管7に
接続されており、この給気管を介しメタンと水素の混合
ガスが石英製反応管7の内部に送り込まれる。混合ガス
としては、水素に対して0.1〜10体積%のメタンを
混合したものが好ましい。メタンは、分解によって炭素
系物質となるものであり、1体積%に達しないと有効な
炭素系物質のコーティングが得られない。しかし、10
体積%を超える配合比率では、その分だけ水素分圧が不
足し、雰囲気に含まれている酸素や水分の悪影響が現れ
易い。電磁波発振器1では、周波数1MHz〜10GH
zの電磁波を発生させる。この電磁波を石英製反応管7
に収容されている粉体に照射すると、粉体粒子が内部か
ら加熱され、粒子の表面が活性化される。また、石英製
反応管7の内部雰囲気に含まれているメタンが分解し、
活性度の高い炭素が生成する。この炭素が粉体粒子の格
子状酸素と置換し、電気伝導性に優れた炭化物コーティ
ング層を形成する。An appropriate mixed gas feed pipe is connected to the quartz reaction pipe 7, and a mixed gas of methane and hydrogen is fed into the quartz reaction pipe 7 through this feed pipe. The mixed gas is preferably a mixture of hydrogen and 0.1 to 10% by volume of methane. Methane becomes a carbon-based substance by decomposition, and an effective coating of the carbon-based substance cannot be obtained unless it reaches 1% by volume. But 10
When the blending ratio exceeds volume%, the partial pressure of hydrogen is insufficient and the adverse effects of oxygen and water contained in the atmosphere are likely to appear. In the electromagnetic wave oscillator 1, the frequency is 1 MHz to 10 GH
Generates an electromagnetic wave of z. This electromagnetic wave causes the quartz reaction tube 7
When the powder contained in the powder is irradiated, the powder particles are heated from the inside, and the surfaces of the particles are activated. Further, methane contained in the internal atmosphere of the quartz reaction tube 7 is decomposed,
Highly active carbon is produced. This carbon replaces the lattice-like oxygen of the powder particles to form a carbide coating layer having excellent electrical conductivity.
【0007】このようにして粉体粒子の表面に形成され
た炭化物コーティング層を観察すると、コーティング層
は、緻密で均一な層構造をもっており、母材に対する密
着性に優れ、硬質で熱伝導性にも優れている。コーティ
ング層を備えた粒子は、表面に導電性が発現して半導体
特性が向上するため、光触媒,ガスセンサー等として使
用される。Observing the carbide coating layer formed on the surface of the powder particles in this way, the coating layer has a dense and uniform layer structure, is excellent in adhesion to the base material, is hard and has high thermal conductivity. Is also excellent. The particles provided with a coating layer are used as a photocatalyst, a gas sensor, etc. because the surface exhibits conductivity and semiconductor characteristics are improved.
【0008】[0008]
【実施例】平均粒径20〜60メッシュのアナターゼ型
チタニア粉末を原料として使用し、チタニア粉末10g
を容量200ccの石英製反応管7に収容した。真空ポ
ンプで系内を排気した後、500Wで電磁波を照射しな
がらテスラーコイルによってプラズマを発生させた。そ
して、所定の混合比になるようにマスフロメータで流量
を30cc/分に調整したCH4 1%−H2 混合ガスを
所定の圧力で導入し、石英反応管7を70rpmで回転
させながら処理を開始した。所定時間(2時間)反応さ
せた後、電磁波照射を止め、処理を終了した。なお、ガ
ス圧は、1,10,20,30,40トールに設定し
た。雰囲気圧1トールで発生したプラズマは、図2
(a)に示す発光スペクトルをもっており、活性度の高
い分解生成物−CHが生成していた。このときのプラズ
マガスの温度は、約1000℃であった。プラズマの発
光スペクトルは、図2で(b),(c)として示すよう
に雰囲気圧に応じて変化した。EXAMPLE Anatase type titania powder having an average particle size of 20 to 60 mesh was used as a raw material, and 10 g of titania powder was used.
Was stored in a quartz reaction tube 7 having a capacity of 200 cc. After evacuating the system with a vacuum pump, plasma was generated with a Tesler coil while irradiating an electromagnetic wave at 500 W. Then, a CH 4 1% -H 2 mixed gas whose flow rate was adjusted to 30 cc / min by a mass flow meter so as to have a predetermined mixing ratio was introduced at a predetermined pressure, and the treatment was started while rotating the quartz reaction tube 7 at 70 rpm. did. After reacting for a predetermined time (2 hours), the electromagnetic wave irradiation was stopped and the treatment was completed. The gas pressure was set to 1, 10, 20, 30, 40 Torr. The plasma generated at an atmospheric pressure of 1 Torr is shown in FIG.
It has an emission spectrum shown in (a), and a highly active decomposition product -CH was produced. The temperature of the plasma gas at this time was about 1000 ° C. The emission spectrum of the plasma changed according to the atmospheric pressure as shown in FIGS. 2 (b) and 2 (c).
【0009】プラズマ処理した試料を、粉末X線回折法
(XRD)及びラマン分光法で物性評価した。また、プ
ラズマ中に発生した活性種を発光分光分析法(OES)
で測定した。アナターゼ型のチタニアをメタン水素プラ
ズマ処理したところ、表面のみが灰色になった。また、
ラマン分光法による分光結果を示す図3にみられるよう
に、チタニア表面に炭化チタンが形成されていることが
確認された。この結果は、TiO2 の酸素格子にCH4
の炭素が置換することにより生じたものと推察される。
そこで、炭化チタン合成の最適条件を調査するため、反
応条件のうちでガス圧力を変化させて反応を行わせた。Physical properties of the plasma-treated sample were evaluated by powder X-ray diffraction (XRD) and Raman spectroscopy. In addition, active species generated in plasma are analyzed by optical emission spectroscopy (OES).
It was measured at. When anatase type titania was treated with methane hydrogen plasma, only the surface became gray. Also,
As seen in FIG. 3, which shows the result of spectroscopy by Raman spectroscopy, it was confirmed that titanium carbide was formed on the titania surface. This result indicates that CH 4 is attached to the oxygen lattice of TiO 2.
It is presumed that it was caused by the substitution of the carbons of.
Therefore, in order to investigate the optimal conditions for titanium carbide synthesis, the gas pressure was changed under the reaction conditions to carry out the reaction.
【0010】その結果、1トールで処理した試料では表
面全体が灰色になったのに対し、40トールで処理した
試料では表面の一部のみが灰色になっていることを目視
観察によっても確認できた。チタニア表面に形成された
炭化チタンをラマン分光法で定量したところ、図4に示
すようにガス圧の上昇に応じて炭化チタンのラマンピー
クが減少していた。本来、電磁波電力を一定にしてもガ
ス圧力が高くなるに従ってプラズマ域が狭くなり、電力
が集中し、試料温度が上昇する。そのため、ガス圧力を
高くした方が膜の生成速度が早くなると予想されるが、
本実施例では全く逆の結果が得られた。そこで、プラズ
マ中の気相反応で重要な役割を果していると考えられて
いるラジカルやイオン等の活性種がガス圧の変化によっ
てどのような影響を受けるかを発光分光分析で調査し
た。調査結果は、前掲した図2に示されているように、
1トールのガス圧力ではCH(420nm),Hα(6
60nm),Hβ(486nm),H2 (600nm付
近)に基づく発光ピークが明確に確認された。しかし、
ガス圧力が20トール,40トールと高くなるに従っ
て、全ての発光強度が激減した。このことは、圧力の増
加によってガスの電離が抑制され、プラズマ中の活性種
の濃度が減少したことを示す。すなわち、ガス圧力の増
加は、炭化チタンの生成を減少させる一番の原因といえ
る。As a result, it can be confirmed by visual observation that the entire surface of the sample treated with 1 Torr is gray, whereas the sample treated with 40 Torr is gray only in a part of the surface. It was When the titanium carbide formed on the titania surface was quantified by Raman spectroscopy, the Raman peak of titanium carbide decreased with increasing gas pressure, as shown in FIG. Originally, even if the electromagnetic wave power is kept constant, the plasma region becomes narrower as the gas pressure becomes higher, the power is concentrated, and the sample temperature rises. Therefore, it is expected that the higher the gas pressure, the faster the film formation rate.
In this example, the exact opposite result was obtained. Therefore, we investigated by emission spectroscopy how the active species such as radicals and ions, which are considered to play an important role in the gas phase reaction in plasma, are affected by the change in gas pressure. The survey results, as shown in Figure 2 above,
At a gas pressure of 1 torr, CH (420 nm), Hα (6
The emission peaks based on 60 nm), Hβ (486 nm), and H 2 (near 600 nm) were clearly confirmed. But,
As the gas pressure increased to 20 Torr and 40 Torr, all the emission intensity decreased drastically. This indicates that the increase in pressure suppressed the ionization of gas and decreased the concentration of active species in plasma. That is, it can be said that the increase in gas pressure is the primary cause of reducing the production of titanium carbide.
【0011】次いで、表面を炭化したチタニアをアセト
アルデヒドの光分解に使用し、光触媒としての性能を調
査した。試験には、チタンテトライソプロポキシドを加
水分解し、水洗・濾過後、空気中で500℃に2時間焼
成したアナターゼ型のチタニアを試料Aとして使用し
た。また、試料Aを1トールの減圧雰囲気中でCH4 1
%−H2 混合ガスを流量30ml/分で供給しながら5
00Wで2時間プラズマ処理した試料Bを使用した。試
験は、アセトアルデヒド濃度1000ppm,反応器容
積2リットル,試料表面における紫外線強度2.0mW
/cm2 の条件下で行った。試験結果を示す図5にみら
れるように、プラズマ処理で表面をTiCコーティング
した試料Bは、試料Aに比較して2倍のアルデヒド光分
解性能を示した。Next, titania whose surface was carbonized was used for the photolysis of acetaldehyde, and the performance as a photocatalyst was investigated. In the test, anatase-type titania which was obtained by hydrolyzing titanium tetraisopropoxide, washed with water, filtered, and calcined in air at 500 ° C. for 2 hours was used as a sample A. Further, CH 4 1 Sample A in 1 Torr vacuum atmosphere
While supplying the% -H 2 mixed gas at a flow rate of 30 ml / min, 5
A sample B plasma-treated with 00W for 2 hours was used. The test was conducted with acetaldehyde concentration of 1000 ppm, reactor volume of 2 liters, and UV intensity of 2.0 mW on the sample surface.
It was performed under the condition of / cm 2 . As shown in FIG. 5, which shows the test results, Sample B, the surface of which was coated with TiC by plasma treatment, showed twice the aldehyde photodegradation performance as Sample A.
【0012】[0012]
【発明の効果】以上に説明したように、本発明において
は、電磁波で誘導されたプラズマで金属酸化物の粉体粒
子を処理することにより、粒子表面を炭化物コーティン
グしている。形成されたコーティング層は、硬質で電気
伝導性,熱伝導性等に優れているため、粉体粒子に高機
能が付与され、しかも耐摩耗性が改善されていることか
ら、寿命の長い触媒等の機能材料として使用できる。As described above, in the present invention, the surface of the particles is coated with carbide by treating the metal oxide powder particles with the plasma induced by the electromagnetic wave. The formed coating layer is hard and has excellent electrical conductivity, thermal conductivity, etc., so high functionality is given to the powder particles, and abrasion resistance is improved. It can be used as a functional material.
【図1】 本発明で使用する電磁波プラズマ加熱装置FIG. 1 is an electromagnetic wave plasma heating apparatus used in the present invention.
【図2】 メタン−水素混合ガスに電磁波を照射して発
生させたプラズマの発光スペクトルに及ぼすガス圧の影
響FIG. 2 Effect of gas pressure on emission spectrum of plasma generated by irradiating methane-hydrogen mixed gas with electromagnetic wave
【図3】 チタニアと炭化チタンのラマンスペクトルFIG. 3 Raman spectra of titania and titanium carbide
【図4】 雰囲気圧に応じたラマンスペクトルの変化FIG. 4 Changes in Raman spectrum depending on atmospheric pressure
【図5】 プラズマ処理の有無がチタニアの光触媒機能
に及ぼす影響FIG. 5: Effect of presence or absence of plasma treatment on photocatalytic function of titania
1:電磁波発振器 2:アイソレータ 3:パワー
モニター 4:スリースタブチューナ 5:反応室 6:プラ
ンジャー 7:石英製反応管 8:スターラ 9:トラップ
10:真空ポンプ 11:真空ゲージ1: Electromagnetic wave oscillator 2: Isolator 3: Power monitor 4: Three-stub tuner 5: Reaction chamber 6: Plunger 7: Quartz reaction tube 8: Stirrer 9: Trap
10: Vacuum pump 11: Vacuum gauge
Claims (3)
引きし、前記容器を回転させながらメタンと水素との混
合ガスを供給すると共に、前記粉体に電磁波を照射して
プラズマを発生させ、該プラズマによりメタンを分解し
て得られる炭素と前記粉体中の格子状酸素とを置換し、
前記粉体の粒子表面に炭化物を付着させることを特徴と
するプラズマCVDによる炭化物コーティング方法。1. A vacuum is applied to a container containing a powder of metal oxide, a mixed gas of methane and hydrogen is supplied while the container is rotated, and a plasma is generated by irradiating the powder with an electromagnetic wave. By replacing the carbon obtained by decomposing methane by the plasma with the lattice oxygen in the powder,
A method for coating a carbide by plasma CVD, which comprises depositing a carbide on the particle surface of the powder.
回転の速度で回転させる炭化物コーティング方法。2. The container according to claim 1 at a rate of 20 to 100 per minute.
A carbide coating method of rotating at a rotation speed.
照射する請求項1記載の炭化物コーティング方法。3. The carbide coating method according to claim 1, wherein electromagnetic waves having a frequency of 1 MHz to 10 GHz are irradiated.
Priority Applications (1)
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JP7274681A JPH0987857A (en) | 1995-09-27 | 1995-09-27 | Carbide coating method by plasma cvd |
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JP7274681A JPH0987857A (en) | 1995-09-27 | 1995-09-27 | Carbide coating method by plasma cvd |
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Family
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JP7274681A Pending JPH0987857A (en) | 1995-09-27 | 1995-09-27 | Carbide coating method by plasma cvd |
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