Classifications

• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D3/00—Charging; Discharging; Manipulation of charge
  • F27D3/0025—Charging or loading melting furnaces with material in the solid state
  • F27D3/0026—Introducing additives into the melt

Definitions

• the present invention relates to a method for producing an alloy or a metal compound which produces an exothermic reaction, and particularly to a method for producing a large amount of an alloy or an intermetallic compound which produces a large amount of heat during alloying or synthesis. It relates to a method of melting while avoiding splash and other obstacles caused by heat generation.
• the melting method of adding an additive element that remains in the melt of some of the constituent elements constituting the system is widely practiced, but a large amount of heat is generated during the addition.
• implementation is difficult. This is basically because the exothermic reaction causes a flash, which causes a decrease in yield, a change in composition and temperature, and the like.
• the smelting method differs from the sintering method and the like in that large and high-density products can be produced easily and in large quantities.
• Polysilicon has conventionally been used as an electrode or a line of a semiconductor device, particularly as a gate of a MOS / LSI.
• the polysilicon has been used.
• the propagation delay due to the resistance of the gate electrode has become an issue.
• the gate electrode, source electrode, and gate electrode have been used to facilitate the formation of the MOS element by the cell ferrule method. It is desired to use a material having a high melting point as the electrode. Under these circumstances, research on high bran point metal gate electrodes, source electrodes, and drain electrodes with lower resistivity than polysilicon will be conducted.
• Research on refractory metal silicide electrodes with compatibility as the first is being actively pursued. Promising practical examples of such refractory metal silicides are titanium silicides, and moreover, molybdenum silicides and tungsten stainless silicides. is there.
• a method effective for forming a titanium silicide thin film for an electrode of a semiconductor device or a K line there are a sputtering method and an electron beam evaporation method.
• the spark method metal is released by colliding an argon ion with a target plate, and the released metal is infested on a substrate facing the target plate.
• the electron beam evaporation method is a method in which an ingot evaporation source is dissolved by an electron beam to perform evaporation.
• the purity and other properties of the resulting film depend on the purity, composition, and spatability of the target plate or evaporation source (hereinafter collectively referred to as the target). Depends on the tuning characteristics.
• titanium silicide target high-purity titanium powder and silicon powder are mixed at a predetermined mixing ratio, molded, vacuum-sintered, and then mixed with a desired target.
• the sintering method and the melting method of handing out silicon and titanium of a specified blend in a crucible are known, but the sintering method does not produce high-density products, so large quantities are required. There are problems such as target leakage, contamination, etc. originating from the voids. Therefore, there is an interest in producing titanium silicide by the smelting method.
• titanium silicide by the conventional smelting method was as follows: In a vacuum or argon reduced pressure atmosphere, a high frequency induction furnace or a resistance heating furnace was used. Dissolve silicon in aluminum crucible. A predetermined amount of titanium small pieces or powder is weighed into a container, the container is charged into a furnace, and the titanium pieces or powder are poured into the silicon from above the molten silicon bath. Titanium silicide is produced by dissolving titanium in silicon.
• This method has the following problems:
• splashing is more likely to occur due to charging a cold charge into a high-temperature bath and dropping small pieces of titanium from above the bath.
• an object of the present invention is to establish a quenching method in which an alloy or a metal rust compound involved in an exothermic reaction can be obtained under good operations and under stable operation.
• the entire lower end surface of the rod is not always in contact with the melt, and the lower end surface of the rod is not flat after immersion and causes local melting, that is, after a part is melted, It is thought that the melting progressed while repeating the process of preferential melting partly.
• the descending rods were preheated by ripening, the submersion by cold material charging No flushing occurs, loss due to powder or small pieces input and severe fluctuations in the surface are inevitable To be avoided. In the case of bars, the control of the descending speed is easy, and the optimum melting operation is guaranteed from the start to the end of melting.
• the additives are supplied in the form of a soil capsule filled with powder as a rod or in a power vessel made of bath components.
• a small amount of the initial reaction, which reacts exothermically, is less likely to react to the exothermic reaction, and the amount of the reaction is gradually increased as the reaction stops. It was found that the ash could effectively control.
• the shape and descending speed of the rod or the capsule in accordance with the amount of dissolution, stable configuration work becomes possible.
• the present inventors have conducted repeated tests on the possibility of establishing a dimensional form that does not cause slush, scattering, etc. Adding the additive in the form of a ret in the melt led to a haze that this problem could be solved.
• the present invention provides an alloy or an intermetallic compound system which causes an exothermic reaction at the time of alloying or synthesizing, by adding at least one component element remaining in at least one melting bath to constitute the system.
• smelting by adding
• Disclosed is a method for producing an alloy or a metal-compound system involved in an exothermic reaction characterized by gradually dissolving the additive element.
• the term wire refers to a wire having a diameter of 5 ⁇ I or less. Descending in the form of a wire means that the wire is being bathed from above the bath! : Includes the state of blossoming as a monotonic state or multiple straight lines or as a spiral line. * The term bar is more than the diameter Sia Is referred to. Its: the upper limit is determined Ri by the diameter and volume of the crucible, generally under that it 1 5 less crucible diameter co emissions collected by filtration Lumpur has been lowering speed can scan blanking rats shoe suppression is there.
• the descent includes not only a case where the vehicle always moves downward, but also a descent operation in which a stop or a pull-up operation is intermittently taken in.
• FIG. 1 is a schematic view of an example of a smelting apparatus for carrying out the present invention.
• FIG. 2 is a sectional view of a capsule for adding powder.
• BEST MODE FOR CARRYING OUT THE INVENTION First, a description will be given of an example of the production of 5_ titanium silicide.
• FIG. 1 is a schematic diagram of a melting furnace 1 for dissolving a titanium rod in a silicon bath.
• the melting furnace any type capable of melting under reduced pressure of vacuum or argon (inert gas) may be used.
• argon inert gas
• the furnace is equipped with an exhaust port and observation port.
• the vacuum is generally between 10 -4 and 10 " 5 Torr, and the elimination of argon is generally between 10 Q and 30 Q Torr. It is.
• silicon is first melted by the heater S in the crucible 2.
• silicon source As a raw material silicon source,
• the crucible it is preferable to use a high-density crucible that can damage the crucible due to heat generation and avoid trouble with holes.
• a high-purity material it is preferable to use a high-purity material to avoid product contamination due to elution of impurities from the crucible.
• High-purity aluminum crucibles, high-purity quartz crucibles, high-purity ceramic crucibles, etc. are used. High purity with a density ratio of 100%
• Rina Lurup is a crucible manufactured by compressing high-purity aluminum to the theoretical density. Rip 'cast rubbish It is commercially available. It is even better to use a quartz crucible to avoid contamination of A1. Also useful are double wraps, such as quartz on the inside and graphite on the outside.
• the wire After dissolving the silicon, the wire is placed in the silicon bath, (2) titanium rod, (3) titanium appropriately tapered so that the cross-sectional area gradually increases from the sharp tip. Rod, (4) a filled tube fitted with titanium particles in a silicon tube and appropriately tapered so that the cross-section building is added from the tip or (5) 1-5 Titanium particles or pellets having a straight diameter are added through the lowering means or adding means provided in the furnace. * It is needless to say that titanium is also of high purity. None ⁇ Fig. 1 illustrates the tapered titanium rod (4). The tapered titanium rod 4 slowly descends. Here, titanium 4 is suspended from the top of the furnace, and is shown to be lowered at a speed controlled by a low-speed motor M. Take the configuration o
• Titanium wire For example, a titanium wire is wound around a reel, and is dropped straight down into the bath. Depending on the crucible diameter, crucible capacity, wire diameter, etc., multiple titanium buns may be simultaneously lowered. The reel is rotated by a variable speed motor and controls the descending speed of the titanium wire. The rate of descent is such that the initial exothermic reaction is less vigorous and the rate of reaction increases as the reaction gradually subsides. To install.
• the titanium wire dipped * into a spiral or other shape within a range well within the crucible For example, a spiral wound titanium wire is suspended from the furnace top ⁇ and descends at a controlled speed. By doing so, the immersion point in the bath moves in a circular shape, avoiding the interesting fever caused by intensive immersion in one place. It is also favorable in terms of achieving a uniform reaction. Use not only a spiral shape but also an arbitrary bent or wound form. The descent speed can be controlled here as well ⁇
• the rate of descent may be selected depending on the diameter and shape of the titanium wire and the diameter and volume of the crucible, or generally ranges from 2Q0 to 5Q0Qan.
• Titanium rods are suspended via a suitable means, for example, on a shaft connected to a low-speed motor as shown in Fig. 1 and lowered at a controlled speed.
• the rate of descent may be a constant and slow rate, or the amount of reaction may be reduced as the exothermic reaction is intense during the long period of time and the reaction is gradually increased as the reaction progresses.
• Rolling may be performed, or a relatively high descent speed and a low descent speed may be alternately employed. Alternatively, the descent may be stopped intermittently.
• the rod end may be intermittently pulled up to just above the surface of the molten metal using a reversible motor.
• the descending speed is selected depending on the diameter of the titanium rod and the diameter and capacity of the rod, and furthermore, depending on the condition of the molten metal. It is in the range of 10 to 200 «/ min.
• the entire lower end of the titanium rod is not completely dissolved at a time.
• the melt is mixed and the surface is slightly moved. Therefore, the melt contacts the melt only locally.
• the rod end undergoes melting with repeated local preferential melting here and there. ⁇ Therefore, even with a very large diameter titanium rod, the lower speed is properly controlled. If rolled, it will dissolve without generating splash.
• Taper-equipped titanium rods The form of the titanium rods reduces the amount of the initial exothermic reaction and increases the amount of the reaction as the reaction gradually subsides. Anything will be used. Normally, a titanium rod having a tapered portion tapered from a sharp tip to a certain size range may be used. The titanium rod slowly descends to avoid a sudden reaction. The descent speed is determined depending on the titanium rod dimensions, the shape, the rippling capacity, etc., but is between 5 and 10 OuaZ.
• Titanium grains or pellets are coated with a diameter of 1 to 5 j Avenue If the diameter is less than 1 ⁇ » the addition will cause scattering or loss due to evacuation No. On the other hand, if it exceeds 5 am, the drop impact becomes large, so that when the metal is added, large fluctuations or slush of the molten metal surface are likely to occur.
• the method of addition is basically to drop from the container holding the titanium granules or pellets into the crucible, but to minimize the flash, use a method such as 3 ⁇ 4 It is also beneficial to use strategies:
• titanium particles or pellets added in this way also have a high purity.
• T i S i x is generally selected the target composition from the scope of the t 5 ⁇ ⁇ ⁇ 2 ⁇ 7 .
• Adjustment of the bath temperature during melting depends on the heat of reaction between the silicon and titanium (ie, the titan, size and descent rate, titanium particle or pellet addition rate) and furnace heat. It is brought about by adjusting the input power of the In the present invention, since there is no sudden generation of heat of reaction, it is very easy to control the bath temperature.
• the titanium rod gradually dissolves in the silicon bath to form titanium silicide.
• Moribden Zen or Tungsten rods are made from high-purity Molybdenum or Tungsten powder in the form of rods, or high-purity Molybdenum or Tungsten rods. Any of those processed into a predetermined shape can be used.
• snacks have been established to produce such extremely pure molybdenum or tungsten powders or ingots.
• high-purity molybdenum or tungsten is added to a high-purity silicon melt, an exothermic reaction occurs in a stunning manner. However, the exothermic reaction can be buried sufficiently. Also, high melting point metals such as molybdenum and tungsten can be easily dissolved.
• the smelting of Fe-Co-rare earth elements (at least species such as Tb, Gd, Dy) Performed using c.
• the capsule c is made of pure iron, which is one of the components of the melt bath, and is a hollow body having a new area increasing from Shinjing, similar to the rod.
• the heavy rare earth element described above is compressed and filled in the capsule c so that the heavy rare earth element does not flow out as a powder or a granule during melting. Or (I) powder spillage, (H) powder fly, or powder accompanying the Na exhaust. This eliminates the situation of exhaust loss. Alternatively, 1-5 w heavy rare earth element particles or pellets are added to the Fe-Co melt.
• the present invention is not limited to such specific examples, and is applied to a situation where it is desired to control the initial explosive reaction progress particularly in the production of alloys and metal compound systems involved in the exothermic reaction.
• the yield can be reduced. improves.
• the target composition can be manufactured.
• the temperature of the silicon bath was initially set to 1 ⁇ 45O ⁇ C Power was maintained within 10 ot by adjusting power. Temperature control was easily performed, and stable melting operation was performed. A visual inspection was conducted on the rupu-no-hanabe after the dissolution of the port, but almost no deposits were found.
• the composition of the titanium silicide formed was as follows: TiSi ⁇ in the analysis, which was in line with the target value. Furthermore, the titanium wire contained 500 ppm of oxygen, but the product ⁇ oxygen content was reduced to 100 ppm.
• the silicon bath temperature was initially set at 1450 and was maintained within 1 ⁇ 0 ⁇ by adjusting the input power. Temperature control was easily performed, and stable melting work was performed. After the desolvation, the ⁇ side of the crucible was visually inspected, but almost no deposits were found. The composition of the generated titanium silicide is the result of the analysis.
• titanium silicide was melted under a vacuum atmosphere of 3 X 10 " 4 Torr.
• the crucibles were as follows: An ultra-high purity aluminum rupe with a density ratio of 100% was used, and the size of the rupe was 10 mm in inside diameter and 2 O ca in depth. The melt was melted in 2,000.Then, high-strength titanium zen (dimensions: 2 ca in diameter x 100, length, pointed to 100 an.) 1 »800 Descended into the silicon bath at a rate of 3 O wa, and finally made 1.705 ⁇ of titanium insoluble. The temperature of the silicon bath was Initially
• the composition of the titanium silicide formed was TiSi as a result of analysis. And it was on the street. In addition, the titanium bar contained 50 Qppm of oxygen, but the oxygen content of the product was reduced to 100 pm.
• titanium silicide was melted under a vacuum atmosphere of 3 X 10 " 4 Torr.
• the size of the rup was 1 O CTI X 20 deep.First, in a crucible? The N silicon mass was dissolved in 20000. Thereafter, a small amount of high-purity titanium particles (size 2 to 4 » « #) 105 was added and dissolved.
• the temperature of the silicon bath was initially set to t450, and was maintained within 100 degrees of input power regulation. The temperature could be easily adjusted, and stable melting operation could be performed.
• the composition of the titanium silicide formed was TiSim as a result of analysis, which was in line with the target value.
• the titanium particles contained 500 ppm of oxygen, but the oxygen content of the product was reduced by 100 ppm fc.
• an alloy or an intermetallic compound having a target composition can be stably melted in a high yield, and an appropriate exothermic reaction can be carried out, so that an effect of purifying harmful elements can be obtained.
• the present invention relates to a refractory metal silicide represented by titanium silicide, molybdenum silicide, tungsten silicide, and the like, and a tag material for a photothermal magnetic element. It is effectively applied to the field of melting of Fe-Co- direct rare earth element (at least one plant such as Tb, Gd. Dy) alloy known as.
• refractory metal sheet Li Sa I de (TiSi x which is Ri ⁇ by the present invention, MoSi x, WS i x :) is a semiconductor device electrode or Hai ⁇ , especially M 0 S ⁇ LSI Depai scan of Target for forming gate electrode, source electrode and drain electrode W

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• 1987
  • 1987-03-12 WO PCT/JP1987/000155 patent/WO1988005472A1/ja active Application Filing
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