JP4439101B2 - Attritor equipment - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an attritor apparatus used for producing intermetallic compound powder, alloy powder, ceramic powder or the like.
[0002]
[Prior art]
Intermetallic compounds are attracting attention as various functional materials because they have high temperature characteristics, shape memory characteristics, magnetic characteristics, and the like that cannot be obtained with conventional alloys.
As a method for producing an intermetallic compound powder, a method of casting an ingot of a predetermined component ratio, pulverizing the ingot, and powdering, a predetermined amount of the raw powder is blended, and this is solidified by a cold isostatic press, Next, a method is known in which this is melted and further gas atomized to form an intermetallic compound powder.
[0003]
In the method of pulverizing the ingot, the ductility at room temperature is reduced by the adsorption of oxygen, and the density of the sintered body is low because the powder particles are coarse and irregular in shape. Further, in the gas atomization method, there are problems of reduced ductility due to oxygen adsorption and non-uniform structure.
[0004]
As a method for solving the above problems, there is known a mechanical alloying method in which material powder and steel balls are put in a ceramic mill, and the mill is rotated to repeat mixing, friction, diffusion, and pulverization and alloying. However, the production of intermetallic compound powder by this mechanical alloying method takes a long time (several weeks in a laboratory or the like). Therefore, an attritor apparatus disclosed in Japanese Patent Laid-Open No. 5-148513 is known as an apparatus for improving the mechanical alloying method and producing a uniform intermetallic compound powder in a short time (about 50 to 100 hours). ing. This attritor device inserts a shaft with a stirring blade into a sealed container containing a steel ball and rotates the shaft to alloy the material contained in the sealed container by collision or abrasion with the steel ball. It has a structure that becomes.
[0005]
[Problems to be solved by the invention]
The attritor device usually takes 50 to 100 hours to alloy the raw material powder. During this time, the temperature of the container, the stirring shaft, the stirring blade, etc. rises significantly due to the collision of the steel balls and the reaction heat of the raw material powder. In particular, a stirring shaft and a stirring blade that are difficult to form a water jacket or the like may be buckled or deformed by this temperature rise. In addition, the seal with which the stirring shaft is in sliding contact is also deteriorated or broken by heat, and a clearance is generated, so that air (oxygen) enters the container and hinders alloying, or material powder is removed from the part of the generated clearance from the container. May leak.
[0006]
In particular, when producing intermetallic compound powder, etc., if a solvent is used, carbides and nitrides are generated, and mechanical properties after firing are deteriorated. Therefore, mixing in a vacuum atmosphere or an inert gas atmosphere is necessary. Therefore, this is a disadvantageous condition for cooling.
[0007]
In addition, in the attritor device disclosed in Japanese Patent Laid-Open No. 5-148513, in order to know when the production of the compound is completed, a temperature sensor is attached to the stirring blade, and the time point when the surface temperature of the powder changes rapidly. I try to detect it. However, since the stirring blade rotates at high speed and repeatedly collides with the steel ball, even if a temperature sensor is provided on the stirring blade, there is a high possibility that the sensor and the cord are damaged.
[0008]
[Means for Solving the Problems]
In order to solve the above problems, the attritor apparatus according to the present invention is configured to forcibly cool the stirring shaft provided with the stirring blade for stirring the raw material powder in the sealed container by the cooling mechanism.
[0009]
In order to effectively cool the stirring shaft, a cooling fin is provided on a portion of the stirring shaft that is outside the sealed container, and a cooling mechanism that blows a cooling medium onto the cooling fin is disposed outside the cooling fin. preferable. Examples of the cooling medium include cold air or cooling water. Moreover, it can cool more effectively by making the said stirring shaft hollow.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is an overall view of an atomizer device according to the present invention, FIG. 2 is a cross-sectional view taken along line AA of FIG. 1, and the attritor device includes a sealed container 1 and a stirring shaft 20.
[0012]
The sealed container 1 is composed of a container body 2 and a lid 3, and a steel ball 4 for abrading material is stored in the sealed container 1, and a water jacket 5 is formed in the side wall of the container body 2. By circulating the cooling water through the cooling water supply pipe 6 and the discharge pipe 7 in the jacket 5, the temperature in the sealed container 1 is not extremely increased by the energy generated by the collision of the steel balls 4. .
[0013]
An opening 8 is formed at the bottom of the hermetic container 1, and a filter 9 is provided in the opening 8 to block the permeation of the steel balls 4 and pass the manufactured intermetallic compound powder. A recovery pot 10 for receiving intermetallic compound powder and the like that has passed through the filter 9 is attached below, and an intake / exhaust pipe for replacing the air in the pot with an inert gas such as nitrogen gas or argon gas. 11 is connected.
[0014]
Further, a temperature sensor 12 is embedded at the bottom of the sealed container 1 at the side of the opening 8, and a signal line 13 connected to the temperature sensor 12 is drawn out along the collection pot 10. As described above, in this embodiment, the temperature sensor 12 is provided at a place where it is difficult to be damaged, and when the temperature in the sealed container 1 becomes abnormally high, the operation is immediately stopped and the maximum flow rate is supplied to the water jacket. The cooling water is made to flow.
[0015]
On the other hand, the lid 3 is provided with a seal member 14 with which the stirring shaft 20 is slidably contacted. A water jacket 15 is formed inside the lid 3, and a cooling water supply pipe 16 and a discharge pipe 17 are formed in the water jacket 15. By circulating the cooling water through, not only the inside of the sealed container 1 but also the seal member 14 is cooled.
[0016]
The lid 3 is connected with an exhaust pipe 18 for decompressing the inside of the sealed container 1 and a supply pipe 19 for supplying an inert gas such as nitrogen gas or argon gas into the sealed container 1 so that the inside of the sealed container 1 is inert. It is structured to replace with gas.
[0017]
The stirring shaft 20 has a hollow shape with the lower end closed, and an upper end portion of the stirring shaft 20 is attached to a rotating shaft 22 of the motor 21 in an exchangeable manner, and the motor 21 is fixed to the frame 23.
[0018]
The lower half of the stirring shaft 20 is inserted into the sealed container 1, and a scraping arm 24 for circulating the steel balls 4 in the sealed container 1 is provided at the lower end of the stirring shaft 20. Is provided with a stirring blade 25.
[0019]
A cooling fin 26 is formed along the axial direction in the upper half of the stirring shaft 20 protruding upward from the sealed container 1. The cooling fins 26 may be formed not only in the axial direction but also in the circumferential direction.
[0020]
And the cooling mechanism 30 is arrange | positioned so that the cooling fin 26 may be enclosed. The cooling mechanism 30 is attached to the frame 23 via an arm 31 so that the vertical position can be adjusted, and a temperature sensor 32 is provided through the cooling mechanism 30.
[0021]
As shown in FIG. 2, the cooling mechanism 30 has a cylindrical shape and a hollow inside, and supplies an extremely low temperature cold air from a cold air supply source (not shown) into the hollow portion, and a stirring shaft from a jet port 33 formed on the inner peripheral surface. Cold air is blown toward 20 (cooling fins 26) to suppress the temperature rise of the stirring shaft 20, and the deformation of the stirring shaft 20 and the deterioration and breakage of the seal member 14 due to heat are prevented.
[0022]
Here, it is conceivable to spray cooling water instead of cold air, but cold air is preferable because water may fall and adhere to the material. In the embodiment, the cooling fin 26 is provided and the stirring shaft 20 is hollowed to enhance the cooling effect, but the present invention is not limited to these.
[0023]
For example, as shown in FIG. 3, the motor 21 is hollow, a cooling air supply pipe 40 is inserted into the stirring shaft 20 so as to penetrate the motor 21, and a cold air outlet 41 formed in the supply pipe 40. Further, a configuration in which cooling is forcibly applied by applying cold air toward the inner surface of the stirring shaft 20 is also possible.
[0024]
In the above description, for example, a case where a TiAl metal compound powder is manufactured as a raw material will be described. A raw material powder prepared by mixing Ti powder and Al powder so as to have an atomic weight ratio of 51:49 is prepared. And put into the sealed container 1.
At the same time, the steel balls 4 are introduced into the sealed container 1 so that the weight ratio to the raw material powder is 25 to 75 times (for example, 50 times).
[0025]
Thereafter, the inside of the sealed container 1 is replaced with argon gas, the stirring shaft 20 is rotated, and the material powder is crushed, compressed, diffused, and worn by collision between the steel balls 4 or between the steel balls 4 and the inner surface of the container. To obtain a TiAl intermetallic compound.
[0026]
【The invention's effect】
As described above, according to the present invention, since the agitator shaft of the attritor device is forcibly cooled, even if the temperature in the container rises due to the collision of the steel balls in the sealed container, the stirring is performed. The shaft temperature can be kept low to some extent.
[0027]
If the temperature of the agitation shaft is kept low, the seal member will not be damaged due to the temperature of the agitation shaft, and thus the confidentiality in the sealed container can be maintained. If confidentiality in the sealed container can be maintained, high quality intermetallic compound powder, alloy powder or ceramic powder can be stabilized without air (oxygen) entering the container and without forming an oxide film on the material surface. Can be obtained on condition.
[0028]
Further, since the temperature rise of the stirring shaft can be suppressed, it is possible to operate for a long time, and it is also possible to produce a powder of difficult-to-form intermetallic compounds that could not be produced conventionally.
[0029]
Moreover, since the sealing member can be directly cooled by providing the water jacket also on the lid of the sealed container, the production efficiency of intermetallic compound powder and the like is further improved.
[0030]
Furthermore, by providing a temperature sensor for measuring the temperature of the material powder at the bottom of the sealed container, the operation can be stopped immediately in the event of abnormal temperature rise, and the sensor itself is damaged compared to when it is embedded in the stirring blade. Very unlikely.
[Brief description of the drawings]
FIG. 1 is an overall view of an atomizer device according to the present invention. FIG. 2 is a cross-sectional view taken along line AA in FIG. 1. FIG. 3 is a view similar to FIG.
DESCRIPTION OF SYMBOLS 1 ... Sealed container, 2 ... Container main body, 3 ... Cover body, 4 ... Steel ball, 5 ... Water jacket, 6 ... Cooling water supply pipe, 7 ... Cooling water discharge pipe, 8 ... Opening, 9 ... Filter, 10 DESCRIPTION OF SYMBOLS ... Recovery pot, 11 ... Intake / exhaust pipe, 12 ... Temperature sensor, 13 ... Signal line, 14 ... Seal member, 15 ... Water jacket, 16 ... Cooling water supply pipe, 17 ... Cooling water discharge pipe, 18 ... Exhaust pipe, DESCRIPTION OF SYMBOLS 19 ... Inert gas supply pipe, 20 ... Stirring shaft, 21 ... Motor, 22 ... Motor rotating shaft, 23 ... Frame, 24 ... Scraping arm, 25 ... Stirring blade, 26 ... Cooling fin, 30 ... Cooling mechanism, 31 DESCRIPTION OF SYMBOLS ... Arm, 32 ... Temperature sensor, 33 ... Cold air outlet, 40 ... Cooling air supply pipe, 41 ... Cold air outlet.

Claims (3)

Via a sealing member in a sealed container and insert the stirring shaft rotatably, only setting the stirring blade at a portion facing the sealed container of the stirring shaft, before Symbol brought forcibly cooled through the cooling mechanism stirring shaft in Rua door writer device,
Cooling fins are provided on the part of the stirring shaft that protrudes from the sealed container. An attritor device characterized in that a jet port is formed, and cool air is blown from the jet port toward the stirring shaft and the cooling fin . 2. The attritor apparatus according to claim 1 , wherein the seal member is provided on a lid of a sealed container, and a water jacket for cooling the seal member is formed on the lid. 3. The attritor apparatus according to claim 1, wherein a temperature sensor is provided at the bottom of the sealed container.

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