JPH0640954B2 - Fine particle heat treatment method and heat treatment apparatus - Google Patents
Fine particle heat treatment method and heat treatment apparatusInfo
- Publication number
- JPH0640954B2 JPH0640954B2 JP61200688A JP20068886A JPH0640954B2 JP H0640954 B2 JPH0640954 B2 JP H0640954B2 JP 61200688 A JP61200688 A JP 61200688A JP 20068886 A JP20068886 A JP 20068886A JP H0640954 B2 JPH0640954 B2 JP H0640954B2
- Authority
- JP
- Japan
- Prior art keywords
- region
- fine particles
- plasma
- carrier gas
- gas
- 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
- 239000010419 fine particle Substances 0.000 title claims description 77
- 238000010438 heat treatment Methods 0.000 title claims description 27
- 238000000034 method Methods 0.000 title claims description 7
- 239000007789 gas Substances 0.000 claims description 49
- 239000012159 carrier gas Substances 0.000 claims description 48
- 238000001816 cooling Methods 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 description 26
- 150000001875 compounds Chemical class 0.000 description 12
- 239000011261 inert gas Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910001566 austenite Inorganic materials 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000000112 cooling gas Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 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
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Description
【発明の詳細な説明】 本願発明は次に述べる問題点の解決を目的とする。DETAILED DESCRIPTION OF THE INVENTION The present invention aims to solve the following problems.
（産業上の利用分野）この発明は種々の原料の微粒子に
対し、それを変態させる熱処理を施すようにした微粒子
の熱処理方法及び熱処理装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fine particle heat treatment method and a heat treatment apparatus for subjecting fine particles of various raw materials to heat treatment for transforming them.
（従来の技術）微粒子に対し上記のような熱処理を施す
場合、従来は例えば加熱炉内に置いた容器内に多量の微
粒子を入れ、上記炉内の雰囲気ガスを高温化させること
により、そのガスによって上記微粒子を高温化して変態
させ、然る後上記炉内に冷却用ガスを導入して上記高温
化させた微粒子を冷却することが行なわれている。しか
しこのような手段によれば、上記容器内では微粒子同志
が接触している為、それらを高温化させている間に微粒
子相互の凝集が生じて粒径が極めて増大してししまう問
題点があった。また、冷却の場合、上記のように冷却用
のガスを導入しても、微粒子の周囲に存在している上記
高温化した雰囲気ガスの為に微粒子の冷却速度が比較的
ゆっくりとなり、その結果冷却を終えた段階では、上記
高温化により変態させた微粒子が元の状態に戻ってしま
う問題点もあった。(Prior Art) In the case of subjecting fine particles to the heat treatment as described above, for example, a large amount of fine particles are placed in a container placed in a heating furnace and the atmosphere gas in the furnace is heated to a high temperature so that the gas is heated. According to the method, the fine particles are heated to a high temperature to be transformed, and then a cooling gas is introduced into the furnace to cool the high temperature fine particles. However, according to such a means, since the fine particles are in contact with each other in the container, there is a problem in that the fine particles agglomerate with each other while the temperature of the fine particles is raised and the particle size is extremely increased. there were. Further, in the case of cooling, even if the cooling gas is introduced as described above, the cooling rate of the fine particles becomes relatively slow due to the above-mentioned high temperature atmosphere gas existing around the fine particles, and as a result, the cooling is performed. At the stage of finishing the above, there is also a problem that the fine particles transformed by the above-mentioned high temperature return to the original state.
（発明が解決しようとする問題点）この発明は上記従来
の問題点を除き、多数の微粒子を、その微粒子の形態を
保たせたまま熱処理でき、その上、その熱処理過程の冷
却の段階においては微粒子を急冷することができて、微
粒子を変態させたそのままの状態を保たせて冷却できる
ようにした微粒子の熱処理方法及び熱処理装置を提供し
ようとするものである。(Problems to be Solved by the Invention) Except for the above-mentioned conventional problems, the present invention can heat-treat a large number of fine particles while keeping the form of the fine particles, and further, in the cooling step of the heat treatment process, An object of the present invention is to provide a heat treatment method and a heat treatment apparatus for fine particles that can be rapidly cooled and can be cooled while keeping the transformed state of the fine particles.
本願発明の構成は次の通りである。The configuration of the present invention is as follows.
（問題点を解決する為の手段）本願発明は前記請求の範
囲記載の通りの手段を講じたものであってその作用は次
の通りである。(Means for Solving Problems) The invention of the present application is provided with the means as described in the claims, and its operation is as follows.
（作用）搬送ガスはプラズマ化領域を通って冷却領域に
至る。微粒子は上記プラズマ化領域を通る搬送ガスに浮
遊して、上記搬送ガスと共にプラズマ化領域を通って上
記冷却領域に至る。上記プラズマ化領域において、上記
微粒子は変態する温度にまで上記搬送ガスのプラズマに
よって高温化される。次に上記微粒子は、上記冷却領域
において上記搬送ガスによって急冷される。(Function) The carrier gas passes through the plasma region and reaches the cooling region. The fine particles are suspended in the carrier gas passing through the plasma region and reach the cooling region together with the carrier gas through the plasma region. In the plasma region, the fine particles are heated to a temperature at which they are transformed by the plasma of the carrier gas. Next, the fine particles are rapidly cooled by the carrier gas in the cooling region.
（実施例）以下本願の実施例を示す図面について説明す
る。第１図に示される熱処理装置において、Ａは微粒子
供給手段を示す。これにおいて、１は真空容器、２は吸
引口で真空ポンプに接続される。３は弁を示す。４はガ
ス受入口である。５は原料支持具を示し、容器１に固定
された導電材製の支柱６，６とその上端に取付けた原料
支持台７とから成る。原料支持台７はタングステンの板
体（タングステンボートと称される）を用いて形成され
ている。８は支持台７に乗せられた原料を示す。９は原
料の加熱手段として例示する通電加熱用の電源で、前記
支柱６に接続してある。(Embodiment) A drawing showing an embodiment of the present application will be described below. In the heat treatment apparatus shown in FIG. 1, A indicates a fine particle supply means. In this, 1 is a vacuum container and 2 is a suction port connected to a vacuum pump. 3 indicates a valve. 4 is a gas inlet. Reference numeral 5 denotes a raw material support, which is composed of columns 6 made of conductive material fixed to the container 1 and a raw material support base 7 attached to the upper ends thereof. The raw material support base 7 is formed using a tungsten plate body (referred to as a tungsten boat). Reference numeral 8 indicates the raw material placed on the support base 7. Reference numeral 9 is a power source for electric heating, which is exemplified as a heating means of the raw material, and is connected to the support column 6.
次に15は混合室で、弁12を介してガス受入口４に接続し
てある。10は搬送ガス供給手段、13は化合物形成用の反
応性ガスの供給手段で、これらは夫々供給量調整用の弁
11，14を介して混合室15に接続してある。Next, 15 is a mixing chamber, which is connected to the gas inlet 4 via the valve 12. 10 is a carrier gas supply means, 13 is a reactive gas supply means for compound formation, and these are valves for adjusting the supply amount, respectively.
It is connected to the mixing chamber 15 via 11 and 14.
次に16は容器１に接続した流通管で、管内のガスをプラ
ズマ化する為のマイクロ波エネルギーを管外から管内へ
通すことのできる材料例えばガラス管、石英管等でもっ
て形成される。31は流通管16内において設定したプラズ
マ化領域で、31ａはその入口、31ｂは出口を夫々示す。
32はプラズマ化領域31の出口31ｂに隣接して設けた冷却
領域を示す。Next, 16 is a flow pipe connected to the container 1, which is formed of a material such as a glass pipe or a quartz pipe that can pass microwave energy for converting the gas inside the pipe into plasma from outside the pipe. Reference numeral 31 denotes a plasma region set in the flow pipe 16, 31a indicates its inlet, and 31b indicates its outlet.
Reference numeral 32 denotes a cooling region provided adjacent to the outlet 31b of the plasma region 31.
次に17は、プラズマ化領域31に付設のプラズマ化手段と
して例示するマイクロ波印加装置である。これにおい
て、18は空洞共振器で、その大きさは内部においてマイ
クロ波の共振が生じそこに定在波が生ずることのできる
大きさ、例えばマイクロ波の波長と同程度乃至は２倍程
度の大きさに形成してある。20はパワーユニットで、マ
イクロ波発振器21やその発振器の出力を調節する為の出
力制御部22等が備わっている。上記マイクロ波発振器と
しては一例としてマグネトロンが用いてある。23はアイ
ソレータで、反射マイクロ波を吸収して発振器21の破損
を防止する為に設けられたものであり、水を矢印で示す
如く流通させ得るようになっている。24は電力モニタ
で、発振器21から流通管16の側に向かう入射波とその反
対方向に向かう反射波の夫々の電力を監視する為のもの
である。25は整合器（スリースタブチューナと称され
る）で、空洞共振器18における共振をとる為に設けられ
ている。尚マイクロ波発振器の発振周波数は例えば2.45
G Hzであり、又空洞共振器の共振モードは例えばＨ01で
ある。Next, 17 is a microwave application device exemplified as a plasma generating means attached to the plasma region 31. In this, 18 is a cavity resonator, the size of which is such that microwave resonance occurs inside and a standing wave is generated therein, for example, about the same as the wavelength of the microwave or twice as large. Is formed. Reference numeral 20 denotes a power unit, which includes a microwave oscillator 21 and an output control unit 22 for adjusting the output of the oscillator. As an example of the microwave oscillator, a magnetron is used. An isolator 23 is provided to absorb the reflected microwaves and prevent the oscillator 21 from being damaged, and allows water to flow as indicated by an arrow. Reference numeral 24 denotes a power monitor for monitoring the power of each of the incident wave traveling from the oscillator 21 toward the flow pipe 16 and the reflected wave traveling in the opposite direction. Reference numeral 25 is a matching unit (referred to as a stub tuner), which is provided to obtain resonance in the cavity resonator 18. The oscillation frequency of the microwave oscillator is 2.45, for example.
G Hz, and the resonance mode of the cavity is, for example, H 01 .
次に26は回収装置で、流通管16に連通させたケース27内
にフィルタ28を備えさせて構成してある。尚この回収装
置26としては従来より周知の任意の構成のものを用いる
ことができる。29は吸引口で、真空ポンプに接続され
る。30は弁を示す。Next, 26 is a recovery device, which is configured by providing a filter 28 in a case 27 communicating with the flow pipe 16. Incidentally, as the recovery device 26, any conventionally known structure can be used. 29 is a suction port, which is connected to a vacuum pump. 30 indicates a valve.
次に上記構成の熱処理装置による熱処理の一例として、
α−Feの微粒子をγ−Feの微粒子とする熱処理について
説明する。この場合、原料８として鉄が原料支持台７に
置かれ、搬送ガス供給手段10からの搬送ガスとしては、
アルゴン又はヘリウム等の不活性ガス若しくはそれらの
混合ガスが用いられる。次に熱処理の操作としては、先
ず弁12,30を閉じる一方弁３を開いて、真空容器１の内
部を真空ポンプにより真空排気する。次に所定の真空度
になったならば弁３を閉じる一方弁30を開いて、吸引口
29から真空ポンプによる吸引を行うと共に、弁11，12を
適切に開いて搬送ガス供給手段10から搬送ガスを真空容
器１の内部に連続的に供給する。すると、供給手段10か
ら送り出された搬送ガスは、微粒子供給手段Ａにおける
容器１内を通って流通管１６内へ入る。そしてプラズマ
化領域31をその入口31ａから出口31ｂへ向けて流通し、
更に冷却領域32を通って回収装置26へ至り、更にそこを
通って真空ポンプへと引かれる。尚上記搬送ガスの供給
量は、流通管16の内部での搬送ガスのガス圧が例えば１
〜数10Torrとなり、また流通管16の内部での搬送ガスの
流速が３〜30m/秒程度となるようにするのがよい。一
方、マイクロ波発振器21を作動させてアンテナ21ａから
空洞共振器18の内部にマイクロ波を与え、そのマイクロ
波を流通管16の内部のプラズマ化領域31に及ぼす。その
結果、プラズマ化領域31においては、そこを流通する上
記搬送ガスがプラズマ化される。尚本件明細書中におい
てはプラズマ化手段17からのマイクロ波エネルギーによ
って搬送ガスがプラズマ化される領域をプラズマ化領域
と呼ぶ。またその領域31において、搬送ガスの流通方向
に対してその最も上流側の箇所を入口31ａ、最も下流側
の箇所を出口31ｂと夫々呼ぶ。このプラズマ化領域31は
そこを流通するガスの種類、圧力や、プラズマ化手段17
から及ぼされるマイクロ波のエネルギーの大きさに応じ
て、その大きさが大きかったり小さかったりする。尚共
振器18の内部に与えるマイクロ波のエネルギーは、モニ
タ24で監視しながら制御部22を調節することにより、微
粒子を搬送ガスのプラズマによって後述の如き所定の温
度にまで高温化させられるような値にする。他方、電源
９から支柱６，６を介して原料支持台７に通電し、支持
台７をそれの有する電気抵抗によって発熱させて原料８
を加熱する。Next, as an example of heat treatment by the heat treatment apparatus having the above-mentioned configuration,
The heat treatment for converting the α-Fe fine particles into γ-Fe fine particles will be described. In this case, iron is placed on the raw material support 7 as the raw material 8, and the carrier gas from the carrier gas supply means 10 is
An inert gas such as argon or helium or a mixed gas thereof is used. Next, as a heat treatment operation, first, the valves 12 and 30 are closed and the valve 3 is opened, and the inside of the vacuum container 1 is evacuated by a vacuum pump. Next, when the predetermined vacuum level is reached, valve 3 is closed while valve 30 is opened and the suction port
The suction from 29 is performed by the vacuum pump, and the valves 11 and 12 are appropriately opened to continuously supply the carrier gas from the carrier gas supply means 10 into the vacuum container 1. Then, the carrier gas sent from the supply means 10 passes through the container 1 in the particle supply means A and enters the flow pipe 16. Then, the plasma region 31 flows from the inlet 31a toward the outlet 31b,
Further, it passes through the cooling region 32 to reach the recovery device 26, and further passes there through to the vacuum pump. The carrier gas is supplied at a gas pressure of, for example, 1 within the distribution pipe 16.
It is preferable that the flow rate of the carrier gas inside the flow pipe 16 is about 3 to 30 m / sec. On the other hand, the microwave oscillator 21 is operated to apply a microwave from the antenna 21a to the inside of the cavity resonator 18, and the microwave is applied to the plasma region 31 inside the flow pipe 16. As a result, in the plasma region 31, the carrier gas flowing therethrough is turned into plasma. In the present specification, a region in which the carrier gas is made into plasma by the microwave energy from the plasma forming means 17 is called a plasma region. Further, in the area 31, the most upstream portion in the flow direction of the carrier gas is called an inlet 31a, and the most downstream portion is called an outlet 31b. The plasma-generating region 31 has a type of gas flowing therethrough, a pressure, and plasma-generating means 17
Depending on the magnitude of the microwave energy that is transmitted from the microwave, the magnitude is large or small. The microwave energy applied to the inside of the resonator 18 can be raised to a predetermined temperature as described below by the plasma of the carrier gas by adjusting the control unit 22 while monitoring it with the monitor 24. Value. On the other hand, the raw material supporting base 7 is energized from the power source 9 through the columns 6 and 6, and the supporting base 7 is heated by the electric resistance of the raw material supporting base 7 to generate the raw material 8.
To heat.
上記のような操作を行うことにより原料８はそれが置か
れた場所（微粒子生成領域）において順次蒸発し、その
近傍でその原料８の微粒子が生成される。その生成され
た微粒子（α−Fe微粒子）は上記搬送ガスに乗って浮遊
状態で流通管16内に流れ込み、プラズマ化領域31に至
る。このプラズマ化領域31においては、そこに印加され
るマイクロ波によってプラズマ密度が所定の密度まで高
くされているから、上記α−Fe微粒子はそれが変態する
温度（910〜1390℃）にまで上記搬送ガスのプラズマに
よって加熱、高温化され、γ−Fe微粒子となる。この場
合、上記搬送ガスはプラズマ化領域31においてはプラズ
マ化されるが、ガス自体としてはさぼど高温化されてい
ない。尚実験装置によりそのガスの温度を測定した結果
の一例を示せば第２図に示される通りである。この第２
図において横軸の０mmはプラズマ化領域の中心位置を示
し、３０mm、６０mmは夫々の寸法だけ冷却領域32の側へ
寄った位置を示す。この図から明らかなように上記搬送
ガスは微粒子に比べればほとんど高温化されず低い温度
に保たれている。By performing the above operation, the raw material 8 is sequentially evaporated at the place where it is placed (fine particle generation region), and the fine particles of the raw material 8 are generated in the vicinity thereof. The generated fine particles (α-Fe fine particles) are carried by the carrier gas into the flow pipe 16 in a floating state, and reach the plasma region 31. In this plasma region 31, since the plasma density is increased to a predetermined density by the microwave applied thereto, the α-Fe fine particles are transported to the temperature (910 to 1390 ° C) at which they are transformed. It is heated and raised in temperature by the plasma of gas to become γ-Fe fine particles. In this case, the carrier gas is turned into plasma in the plasma-generated region 31, but the temperature of the gas itself is not so high. An example of the result of measuring the temperature of the gas by the experimental apparatus is as shown in FIG. This second
In the figure, 0 mm on the horizontal axis indicates the center position of the plasma region, and 30 mm and 60 mm indicate the positions shifted toward the cooling region 32 by the respective dimensions. As is clear from this figure, the carrier gas is maintained at a low temperature with almost no increase in temperature as compared with the particles.
次に上記のように変態してγ−Feとなった微粒子は、上
記搬送ガスに浮遊したままの状態で冷却領域32に至る。
該領域32においては上記搬送ガスはプラズマ化されてい
ない為、上記微粒子の加熱は行なわれず、微粒子は該領
域32に入るや否や、上記の如く比較的低い温度に保たれ
ていた上記の搬送ガスによって直ちに冷却される。従っ
て、上記γ−Fe微粒子は急冷されることになり、α−Fe
に戻ってしまうことなくγ−Feのままで冷却される。上
記のようにして冷却されたγ−Fe微粒子は、搬送ガスに
浮遊したまま次に回収装置26へ至り、そこに備えられた
フィルタ28によって捕捉される。尚残りのガスはフィル
タ28を通り吸引口29から真空ポンプに向けて引き抜かれ
る。Then, the fine particles transformed into γ-Fe as described above reach the cooling region 32 while being suspended in the carrier gas.
Since the carrier gas is not plasmatized in the region 32, the particles are not heated, and as soon as the particles enter the region 32, the carrier gas kept at a relatively low temperature as described above. Is immediately cooled by. Therefore, the γ-Fe fine particles are rapidly cooled, and
It is cooled in γ-Fe as it is without returning to. The γ-Fe fine particles cooled as described above reach the recovery device 26 while floating in the carrier gas, and are captured by the filter 28 provided therein. The remaining gas passes through the filter 28 and is drawn from the suction port 29 toward the vacuum pump.
上記のようにして回収された微粒子を電子顕微鏡で４万
倍に拡大した状態を示せば第３図に符号33で示す通りで
ある。A state in which the fine particles collected as described above are magnified 40,000 times with an electron microscope is shown by reference numeral 33 in FIG.
次に、上記のような手法によれば、Fe微粒子ならばγ化
の比率を非常に高くできる（例えば５割以上。これに対
し従来法では１〜２割程度）。しかし需要によってはよ
り低いγ化の比率で処理を行うようにしても良い。その
ような操作は、プラズマ化領域31での加熱温度、プラズ
マ化領域31を通る速度、或いは、搬送ガスのガス圧を変
えることによって行える。Next, according to the method as described above, the ratio of γ conversion can be made extremely high in the case of Fe fine particles (for example, 50% or more, while in the conventional method, about 10 to 20%). However, the processing may be performed at a lower γ conversion rate depending on demand. Such an operation can be performed by changing the heating temperature in the plasma conversion region 31, the speed through the plasma conversion region 31, or the gas pressure of the carrier gas.
次に、上記実施例では、搬送ガス供給手段10を微粒子供
給手段Ａを介してプラズマ化領域31に接続した例を示し
たが、搬送ガス供給手段10は第１図において符号Ｘで示
される箇所即ちプラズマ化領域31の入口31ａに直接に接
続し、そこからプラズマ化領域31に搬送ガスを直接に供
給してもよい。その場合、微粒子供給手段Ａにおけるガ
ス受入口４には、容器１内での雰囲気用及び、生成され
た微粒子を、上記搬送ガス供給手段からプラズマ化領域
に直接に供給される搬送ガスに乗せる為のガスを供給す
るようにすればよい。Next, in the above-mentioned embodiment, an example in which the carrier gas supply means 10 is connected to the plasma region 31 via the fine particle supply means A is shown, but the carrier gas supply means 10 is indicated by a symbol X in FIG. That is, it may be directly connected to the inlet 31a of the plasma region 31 and the carrier gas may be directly supplied to the plasma region 31 from there. In that case, the gas receiving port 4 of the particle supply means A is to carry the atmosphere and the generated particles in the container 1 onto the carrier gas directly supplied from the carrier gas supply means to the plasma region. It suffices to supply the above gas.
また第１図において符号Ｙで示される箇所に冷却用ガス
の供給手段を接続し、そこから微粒子の冷却用ガスを冷
却領域に付加的に送り込むようにしてもよい。Further, a cooling gas supply means may be connected to the portion indicated by the symbol Y in FIG. 1 and the cooling gas for the fine particles may be additionally fed into the cooling region from there.
次に、上記微粒子供給手段としては、夫々周知の高周波
加熱、プラズマアークによる加熱、アーク放電による加
熱、電子ビームによる加熱など任意の加熱手段を用いた
微粒子生成装置を利用できる。Next, as the above-mentioned fine particle supplying means, it is possible to use a fine particle generating apparatus using any known heating means such as high frequency heating, heating by plasma arc, heating by arc discharge, heating by electron beam, etc., respectively.
次に上記装置による熱処理の他の例を示せば次の第１表
の通りで、同表における原料を同表の搬送ガス及びマイ
クロ波エネルギーの条件のもとで前述と同様に熱処理す
ることによって、同表の製品を得ることができる。Next, another example of heat treatment by the above-mentioned apparatus is shown in Table 1 below. By performing heat treatment on the raw materials in the same table under the conditions of carrier gas and microwave energy in the same table as described above, , You can get the products in the table.
次に、上記第１図の装置を用いれば化合物の微粒子の製
造を行うことができる。その操作について以下に説明す
る。 Next, fine particles of the compound can be produced by using the apparatus shown in FIG. The operation will be described below.
前述と同様に操作により容器１内が所定の真空度になっ
たならば、弁３を閉じる一方弁30を開いて、吸引口29か
ら真空ポンプによる吸引を行うと共に、弁11，14，12を
開いて混合室15から不活性ガスと化合物形成用の反応ガ
スとの混合ガスを真空容器１の内部に連続的に送り込
む。尚その送り込む量は真空容器１の内部が所定の圧力
となるようにする。また不活性ガスと反応性ガスとは、
弁11，14により各々の供給手段10，13から混合室15に供
給される量を調節して適切な混合の割合になるようにす
る。次にマイクロ波発振器21の作動及び、原料８の加熱
を前述の場合と同様に行う。尚共振器18の内部に与える
マイクロ波のエネルギーは、化合物微粒子の製造に適し
た値となるようにする。上記のような操作を行うことに
より原料８はそれが置かれた場所（微粒子生成領域）に
おいて順次蒸発し、その近傍でその原料８の微粒子が生
成される。その生成された原料の微粒子は上記ガス受入
口４から送り込まれる混合ガスと共に流通管16内に流れ
込み、プラズマ化領域31に至る。このプラズマ化領域31
において、上記原料の微粒子は粒径が小さい（＜10nm）
が故にマイクロ波エネルギーを十分に吸収して自らの温
度が上昇すると共に、上記化合物形成用の反応性ガスは
上記マイクロ波によってプラズマ化され活性化する。そ
してそれらの原料の微粒子と活性化したガスとが反応
し、上記微粒子は化合物化されて化合物微粒子が生成さ
れる。この場合、上記原料の微粒子及びガスは夫々上記
のような状態となっている為、両者の反応は極めて促進
される。このようにして生成された化合物の微粒子は回
収装置26へ至り、そこに備えられたフィルタ28によって
捕捉される。尚残りのガスはフィルタ28を通り吸引口29
から真空ポンプに向けて引き抜かれる。When the inside of the container 1 has a predetermined degree of vacuum by the same operation as described above, the valve 3 is closed while the valve 30 is opened, suction is performed by the vacuum pump from the suction port 29, and the valves 11, 14, 12 are turned on. After opening, a mixed gas of an inert gas and a reaction gas for compound formation is continuously fed into the vacuum container 1 from the mixing chamber 15. In addition, the amount to be fed is set so that the inside of the vacuum container 1 has a predetermined pressure. In addition, the inert gas and the reactive gas,
The amount supplied from each supply means 10, 13 to the mixing chamber 15 by the valves 11, 14 is adjusted so as to obtain an appropriate mixing ratio. Next, the microwave oscillator 21 is operated and the raw material 8 is heated in the same manner as described above. The microwave energy applied to the inside of the resonator 18 is set to a value suitable for the production of compound fine particles. By performing the above operation, the raw material 8 is sequentially evaporated at the place where it is placed (fine particle generation region), and the fine particles of the raw material 8 are generated in the vicinity thereof. The generated fine particles of the raw material flow into the flow pipe 16 together with the mixed gas sent from the gas receiving port 4, and reach the plasma conversion region 31. This plasma region 31
In the above, the fine particles of the above raw material have a small particle size (<10 nm)
Therefore, the microwave energy is sufficiently absorbed to raise the temperature of itself, and the reactive gas for forming the compound is plasmaized and activated by the microwave. Then, the fine particles of these raw materials react with the activated gas, and the fine particles are compounded to produce compound fine particles. In this case, since the fine particles of the raw material and the gas are in the above-described states, respectively, the reaction between them is extremely promoted. The fine particles of the compound thus produced reach the recovery device 26 and are captured by the filter 28 provided therein. The remaining gas passes through the filter 28 and the suction port 29
Is pulled out toward the vacuum pump.
次に上記のようにして化合物微粒子の製造を行う場合、
プラズマ化領域31には上記反応性ガスのみならず不活性
ガスも一緒に通される為、広範囲なマイクロ波電力値及
び反応性ガスの広範囲なガス圧値において上記原料の微
粒子を全て化合物化することができる。その実験結果の
一例を示せば第４図の通りである。即ち、不活性ガスを
用いず化合物形成用の反応性ガス（この場合は窒素
Ｎ２）のみを上記原料（この場合はアルミニウムＡｌ）
の微粒子と共にプラズマ化領域31に通した場合には、マ
イクロ波電力及び反応性ガスのガス圧相互の条件が破線
（Ａ）よりも上方の範囲内に入るときにのみ、回収装置
26において回収される微粒子は全て化合物化された微粒
子であり、破線（Ａ）と（Ｂ）との間の範囲のときには
化合物化された微粒子と原料そのものの微粒子とが混在
しており、破線（Ｂ）よりも下の範囲では原料の微粒子
のみであった。一方前述の如く不活性ガス（この場合は
アルゴンＡｒ）と上記反応性ガスとの混合ガス（この場
合、全圧を10Torrにし、窒素及びアルゴンの分圧を図の
ように変えた）をプラズマ化領域に通した場合には、マ
イクロ波電力及び反応性ガスのガス圧相互の条件が実線
（Ｃ）よりも上方の範囲内に入る広い条件下において、
回収装置26には全て化合物化された微粒子を得ることが
できた。この実験結果から明らかなように、混合ガスを
用いた場合には、全ての微粒子を化合物化する為のマイ
クロ波電力や反応性ガスのガス圧の条件は、反応性ガス
を単独で用いた場合に比べて緩やかであり、従ってそれ
らの制御は容易である。Next, when the compound fine particles are produced as described above,
Since not only the reactive gas but also the inert gas is passed through the plasma region 31 together, all the fine particles of the raw material are compounded in a wide range of microwave power value and a wide range of gas pressure value of the reactive gas. be able to. An example of the experimental result is shown in FIG. That is, only the reactive gas for forming a compound (nitrogen N 2 in this case) is used without using an inert gas, and the raw material (aluminum Al in this case)
When passing through the plasmaization region 31 together with the fine particles of the above, only when the mutual conditions of the microwave power and the gas pressure of the reactive gas fall within the range above the broken line (A), the recovery device
All the fine particles collected in 26 are compounded fine particles, and in the range between the broken lines (A) and (B), the compounded fine particles and the fine particles of the raw material itself are mixed, and the broken line ( In the range below B), only the raw material fine particles were used. On the other hand, as mentioned above, a mixed gas of an inert gas (argon Ar in this case) and the above reactive gas (in this case, the total pressure was set to 10 Torr and the partial pressures of nitrogen and argon were changed as shown in the figure) was turned into plasma. When passing through the region, under a wide range of conditions in which the mutual conditions of the microwave power and the gas pressure of the reactive gas fall within the range above the solid line (C),
In the recovery device 26, all compounded fine particles could be obtained. As is clear from the results of this experiment, when a mixed gas is used, the conditions for the microwave power and the gas pressure of the reactive gas for compounding all the fine particles are the same when the reactive gas is used alone. They are slower than, and therefore their control is easy.
尚上記混合ガスの全圧は上記の値に限ることなく種々の
値で行うことができる。また不活性ガスと反応性ガスの
導入は、上記混合室15を用いることなく、図示の如く別
にもう一つの受入口32を任意の箇所に設け、受入口４，
32の一方から不活性ガス、他方から反応性ガスを夫々導
入してもよい。The total pressure of the mixed gas is not limited to the above value and can be various values. Further, for introducing the inert gas and the reactive gas, another receiving port 32 is separately provided at an arbitrary position as shown in the drawing without using the mixing chamber 15, and the receiving ports 4,
An inert gas may be introduced from one of the 32 and a reactive gas may be introduced from the other.
次に上記原料８として用いられる物質を元素記号で示せ
ば、Al、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、In、Si、
Feなどがある。Next, if the substances used as the raw material 8 are represented by element symbols, Al, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, In, Si,
Fe, etc.
上記化合物形成用の反応性ガスは製造すべき化合物の微
粒子に応じて種々のものが用いられる。例えば窒化物を
製造する場合には窒素、酸化物の場合には酸素、炭化物
の場合にはメタン（ＣＨ４）、硫化物の場合には硫化水
素（Ｈ２Ｓ）、ホウ化物の場合にはＢCl3、Ｂ２Ｈ６な
どが用いられる。上記のようにして製造される化合物の
微粒子としては次のようなものがある。Various kinds of reactive gas for forming the compound are used depending on the fine particles of the compound to be produced. For example, in the case of producing a nitride, nitrogen, in the case of an oxide, oxygen, in the case of a carbide, methane (CH 4 ), in the case of a sulfide, hydrogen sulfide (H 2 S), and in the case of a boride, BCl 3 , B 2 H 6 or the like is used. The fine particles of the compound produced as described above include the following.
（イ）窒化物：AlＮ、TiＮ、ZrＮ、HfＮ、ＶＮ、NbＮ、
Ta2Ｎ、CrＮ、Mo2Ｎ、W2Ｎ、InＮ、Si3、Ｎ４、Ｆｅ2-3
Ｎ、Ｆｅ４Ｎ （ロ）硫化物：TiＳ２ （ハ）ホウ化物：TiＢ２，ZrＢ２ （発明の効果）以上のように本発明であっては、微粒子
に熱処理を施す場合、微粒子を搬送ガスに浮遊させた状
態で高温化させ、その浮遊状態のまま冷却できるから、
微粒子の形態を保たせたままその熱処理ができ、従来の
問題点を解決できる効果がある。(A) Nitride: AlN, TiN, ZrN, HfN, VN, NbN,
Ta 2 N, CrN, Mo 2 N, W 2 N, InN, Si 3 , N 4 , Fe 2-3
N, Fe 4 N (b) Sulfide: TiS 2 (c) Boride: TiB 2 , ZrB 2 (Effect of the Invention) As described above, in the present invention, when heat treating fine particles, the fine particles are conveyed. Because it can be heated in the state of being suspended in gas and cooled in the suspended state,
The heat treatment can be performed while maintaining the form of the fine particles, and there is an effect that the conventional problems can be solved.
しかも上記微粒子をプラズマ化領域31で高温化させる場
合、搬送ガスをプラズマ化しそのプラズマによって微粒
子を高温化させるから、微粒子を変態させる高温度にま
で充分に加熱できる特長がある。Moreover, when the temperature of the fine particles is raised in the plasma-generating region 31, the carrier gas is turned into plasma and the temperature of the fine particles is raised by the plasma, so that the fine particles can be sufficiently heated to a high temperature for transformation.
しかも上記の場合、上記搬送ガスはプラズマ化するが、
ガス自体としてはさほど高温化されない特長がある。こ
のことは、その搬送ガスがプラズ化領域31から冷却領域
32に至った場合に、その搬送ガスを微粒子の冷却用のガ
スとして利用できる効果がある。Moreover, in the above case, the carrier gas becomes plasma,
The gas itself has the feature that it does not heat up so much. This means that the carrier gas from the plaza region 31 to the cooling region
When it reaches 32, there is an effect that the carrier gas can be used as a gas for cooling fine particles.
更に上記プラズマ化領域31で高温化した微粒子を冷却領
域32で冷却する場合、高温の微粒子が冷却領域に至るや
否や上記の搬送ガスによって直ちに冷却することがで
き、上記微粒子を変態させたそのままの状態を保たせて
冷却させられる効果がある。Further, when the fine particles whose temperature has been raised in the plasma conversion region 31 are cooled in the cooling region 32, as soon as the high temperature fine particles reach the cooling region, they can be immediately cooled by the carrier gas, and the fine particles are transformed as they are. It has the effect of keeping the state and cooling.
図面は本願の実施例を示すもので、第１図は熱処理装置
の縦断面略示図、第２図は搬送ガスの温度を示すグラ
フ、第３図は微粒子の拡大図、第４図はガス圧とマイク
ロ波電力と生成微粒子の種類との関係を示す図。 Ａ……微粒子供給手段、10……搬送ガス供給手段、31…
…プラズマ化領域、32……冷却領域。The drawings show an embodiment of the present application. FIG. 1 is a schematic vertical cross-sectional view of a heat treatment apparatus, FIG. 2 is a graph showing the temperature of carrier gas, FIG. 3 is an enlarged view of fine particles, and FIG. 4 is gas. The figure which shows the relationship between a pressure, microwave electric power, and the kind of produced | generated particle | grains. A ... Particle supply means, 10 ... Carrier gas supply means, 31 ...
… Plasmaization area, 32 …… cooling area.
Claims (2)
域を備え、搬送ガスを上記プラズマ化領域を通して上記
冷却領域に至らしめると共に、微粒子を上記プラズマ化
領域を通る搬送ガスに浮遊させて、該微粒子を上記搬送
ガスと共にプラズマ化領域を通して上記冷却領域に至ら
しめることにより、上記プラズマ化領域においては、搬
送ガスのプラズマによって上記微粒子を変態させる温度
にまで高温化させ、上記冷却領域においてはその高温化
した微粒子を上記搬送ガスによって急冷することを特徴
とする微粒子の熱処理方法。1. A plasmaization region and a cooling region adjacent to the plasmaization region are provided, and a carrier gas is introduced to the cooling region through the plasmaization region, and fine particles are suspended in the carrier gas passing through the plasmaization region, By bringing the particles together with the carrier gas to the cooling region through the plasmaization region, the plasmaization region raises the temperature to a temperature at which the particles of the carrier gas are transformed by the plasma of the carrier gas, and the high temperature in the cooling region. A method for heat treating fine particles, which comprises rapidly cooling the fine particles that have been turned into a carrier gas.
夫々備えるプラズマ化領域と、プラズマ化領域の出口に
隣接させた冷却領域とを備え、上記プラズマ化領域の入
口には、搬送ガス供給手段と、微粒子供給手段とを接続
し、さらに上記プラズマ化領域には、該プラズマ化領域
を通る搬送ガスをプラズマ化させその搬送ガスのプラズ
マによって上記微粒子を変態させる温度にまで高温化さ
せるようにしたプラズマ化手段を付設したことを特徴と
する微粒子の熱処理装置。2. A plasma-generating region having a gas inlet at one end and a gas outlet at the other end, and a cooling region adjacent to the outlet of the plasma-generating region, the inlet of the plasma-generating region comprising: The carrier gas supply means and the fine particle supply means are connected to each other, and the carrier gas passing through the plasma region is turned into plasma, and the temperature of the carrier gas is raised by the plasma of the carrier gas. A heat treatment apparatus for fine particles, characterized in that it is provided with a plasma generating means.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61200688A JPH0640954B2 (en) | 1985-10-28 | 1986-08-27 | Fine particle heat treatment method and heat treatment apparatus |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60241225 | 1985-10-28 | ||
| JP60-241225 | 1985-10-28 | ||
| JP61200688A JPH0640954B2 (en) | 1985-10-28 | 1986-08-27 | Fine particle heat treatment method and heat treatment apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62176537A JPS62176537A (en) | 1987-08-03 |
| JPH0640954B2 true JPH0640954B2 (en) | 1994-06-01 |
Family
ID=26512347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61200688A Expired - Lifetime JPH0640954B2 (en) | 1985-10-28 | 1986-08-27 | Fine particle heat treatment method and heat treatment apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0640954B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4545357B2 (en) * | 2001-07-23 | 2010-09-15 | 電気化学工業株式会社 | Method for producing aluminum nitride powder |
-
1986
- 1986-08-27 JP JP61200688A patent/JPH0640954B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62176537A (en) | 1987-08-03 |
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