JP6717086B2 - Particle measuring device - Google Patents

Description

The present invention relates to a particle measuring device for measuring a physical quantity of a sample particle such as a particle size distribution of the sample particle, a surface state, a particle constituent element and the like (hereinafter referred to as “particle size distribution”).

Generally, when confirming properties, quality, etc. at the time of development or production of a powder product, physical quantities relating to sample particles such as particle size distribution of powder are measured. For example, in the measurement of particle size distribution, a laser scattering/diffraction method or an image analysis method is used. In the laser scattering/diffraction method, a particle size distribution is calculated by irradiating a sample particle with a parallel light beam such as a laser beam, and measuring and analyzing a pattern of light diffracted and scattered by the sample particle. In the image analysis method, a particle size distribution is calculated by photographing a sample particle group with a CCD camera or the like and analyzing the image.

An image analysis type particle size distribution measuring device is described in Patent Document 1, for example. Patent Document 1 describes an apparatus that images a falling sample particle group with a CCD camera or the like to perform image analysis and to measure a particle size distribution using a statistical method. With such an image analysis type particle size distribution measuring apparatus, it has become possible to perform highly accurate measurement by increasing the speed of a computer and increasing the resolution of an image capturing apparatus.

In the image analysis method, the outer diameter, shape, etc. of the sample particles are measured from the captured image, so that the plurality of sample particles are prevented from overlapping at the time of capturing. Specifically, when the particle concentration of the turbid liquid (slurry) as a dispersion containing the sample particles as the dispersoid is high, it is necessary to sufficiently dilute the slurry to disperse the sample particles to be measured. ..

As a method of supplying the sample particles to be measured, there are an off-line method in which the particles previously taken out from the powder manufacturing apparatus are sent to the particle size distribution measuring apparatus, and an in-line method in which the slurry is directly taken out from the powder manufacturing apparatus and sent to the particle size distribution measuring apparatus. is there.

The in-line method is advantageous for early measurement of the particle size distribution in the particle manufacturing process. On the other hand, the particle size distribution measuring device is expensive, and it is not desirable to provide it for each powder manufacturing device. In addition, the particle size distribution measuring device is often not suitable for the surrounding environment of the powder manufacturing device (for example, an environment with a lot of dust and mist). Therefore, in many cases, a particle size distribution measuring device is installed in a room different from the powder manufacturing device and the particle size distribution is measured by an off-line method. In the case of such a separate room arrangement, when trying to measure the particle size distribution by the in-line method to increase the measurement frequency, it is necessary to install a long transfer pipe for transferring the slurry sample from the powder manufacturing apparatus to the particle size distribution measuring apparatus. There is.

JP, 11-258141, A

In the in-line method, it is necessary to transfer each slurry sample to the particle size distribution measuring device through a transfer pipe or the like in order to obtain the slurry samples from one or a plurality of powder manufacturing devices and sequentially perform the measurement with one particle size distribution measuring device. There is. In particular, when a slurry containing high-concentration and heavy sample particles is transferred while switching the transfer tube, the previously measured slurry is mixed, the sample particles are often precipitated in the transfer tube, and the longer the transfer distance is, the more slurry is generated. There are problems that the slurry is required to be deposited on the transfer pipe switching portion, that it takes time to clean the transfer pipe when switching the transfer pipe, and the like.

Furthermore, when the particle size distribution measuring device is installed in a separate room away from the powder manufacturing equipment and with a small amount of mist, dust, etc., the transfer pipe for transferring a high-concentration slurry sample becomes long and the transfer pipe is clogged with slurry. Such problems may occur. Therefore, in order to prevent clogging of the transfer pipe due to accumulation of slurry and the like, maintenance such as frequent cleaning and replacement of the transfer pipe is required.

Therefore, an object of the present invention is to provide a particle measuring device that more efficiently measures the particle size distribution of particles in a slurry sample. Such an apparatus is, for example, in order to efficiently grasp the particle size distribution of the particles in the slurry sample from each of the one or more powder manufacturing apparatuses, in order to efficiently grasp the particle size of the previously measured slurry, sample particles, etc. It is desirable to satisfy the conditions such as not remaining on the transfer pipe, the pipe connecting member and the like, and that the amount of slurry required for measurement is small even if the transfer distance is long. In addition, it is additional to provide a particle measuring device in which a part of the main body is installed near a powder manufacturing device where mist, dust, etc. exist and another part such as measurement control device is installed in another room. To aim.

The particle measuring device according to the embodiment of the present invention is a transfer unit that transfers the slurry of the first container to the second container by using a diluting liquid, and dilutes the slurry with the diluting liquid in the second container. A diluting unit that generates a diluting liquid, a data acquiring unit that acquires data regarding particles in the diluting liquid, an arithmetic unit that calculates a physical quantity regarding the particles using the data acquired by the data acquiring unit, and the second have a, and a discharge portion for discharging the diluent from the container, the transfer unit includes a first pipe connecting the said second container and the first container, a third container in which the dilution liquid has entered the A second pipe connecting the first pipe and a pipe connecting member connecting the first pipe and the second pipe, wherein the first pipe is between the pipe connecting member and the second container. By pushing the slurry drawn into a part of the pipe portion with the dilution liquid, the slurry drawn into the pipe portion is transferred to the second container .

By the above-described means, it is possible to provide a particle measuring device that more efficiently measures the particle size distribution of particles in the slurry sample.

It is a figure showing the example of composition of the particle measuring device concerning the embodiment of the present invention. It is an enlarged view of the periphery of a slurry pump. It is an enlarged view of the periphery of a slurry pump. It is an enlarged view of the periphery of a slurry pump. It is an enlarged view of the periphery of a slurry pump. It is a figure which shows another structural example of the particle measuring device which concerns on embodiment of this invention.

A particle measuring device 100 according to an embodiment of the present invention will be described with reference to the drawings. FIG. 1 is a schematic diagram showing a configuration example of the particle measuring apparatus 100, and shows a mode in which the slurry 21 is sampled from the slurry tank 38 of one powder manufacturing apparatus. The slurry 21 exists in the slurry tank 38 as the first container in a state of being dispersed by stirring. The solid arrow in FIG. 1 indicates the rotation direction of the pump.

The in-line type particle measuring device 100 mainly includes a main body unit 1, a calculation unit 5, a transfer unit 7, and the like. In the example of FIG. 1, the main body 1 is installed in the same room as the powder manufacturing apparatus, and the arithmetic unit 5 is installed in a separate room 6 such as an office that is not affected by mist, dust and the like. The transfer section 7 is installed in the immediate vicinity of the slurry tank 38.

The sample particles to be measured are, for example, metal-based particles having a relatively large specific gravity. The particle size is generally 0.1 μm to several hundreds μm. The sample particles to be measured may be inorganic powder containing a ceramic material. In the following, metal particles will be described as an example. The slurry 21 is obtained by mixing a predetermined amount of a dispersion medium or the like with the metal-based particles as the dispersoid. There are no particular restrictions on the measurement items for sample particles. Physical quantities relating to the sample particles, such as the particle size distribution of the sample particles, the surface state of the sample particles, the constituent elements (for example, the ratio of constituent elements) of the sample particles, can be measured. For example, in the case of particle size distribution, measurement using a laser scattering/diffraction measuring device, measurement by analysis of an image photographed by a CCD camera or the like is performed. In particular, in image analysis, not only the particle size distribution, but also the outer diameter, area, angle of the protrusion on the contour, center of gravity, circumference, etc. can be measured from the captured image. Therefore, the measurement of the particle size distribution using image analysis will be described below as an example.

The particle measuring device 100 automatically measures the particle size distribution of the sample particles collected from the slurry 21.

The main body 1 mainly includes a diluting unit 2, a measuring unit 3, a discharging unit 4, and the like. The diluting unit 2 includes one or a plurality of diluting liquid pumps 2a and one or a plurality of diluting tanks 2b, and dilutes the slurry 21 to about 1/100 to 1/40000 to generate a diluting liquid 23.

The diluting liquid pump 2a pumps out the diluting liquid 22 from the diluting liquid tank 39, and supplies the diluting liquid 22 through the diluting pipe C1 that connects the diluting tank 2b as the second container and the diluting liquid tank 39 as the third container. Is transferred to the dilution tank 2b.

As the diluting liquid 22, the same liquid as the dispersion medium of the slurry 21 is used. The diluting liquid 22 may be pure water or the like. An example in which pure water is used as the diluting liquid 22 will be described below.

The measurement unit 3 is a data acquisition unit that acquires data regarding particles in the diluting liquid and, for example, acquires data necessary for measuring the particle size distribution of sample particles in the diluting liquid 23. In FIG. 1, an image analysis method will be described as an example, in which the time required for measurement is relatively short and the particle shape and the like can be analyzed from image data.

The measurement unit 3 includes a circulation pump 3a, a camera 35, a flow cell 36, and a lighting device 37.

The circulation pump 3a pumps out the diluting liquid 23 from the diluting tank 2b, and circulates the diluting liquid 23 in the circulation pipe C2 that returns from the diluting tank 2b to the diluting tank 2b via the flow cell 36.

The camera 35 is a photographing device that outputs an image obtained by photographing the sample particles contained in the fluid flowing in the flow cell 36, and is composed of a photographing device such as CCD or CMOS. In the example of FIG. 1, the camera 35 is arranged on the opposite side of the lighting device 37 with respect to the flow cell 36 so as to face the lighting device 37. The camera 35 also has a lens 35a. The lens 35a is, for example, a telecentric lens. The telecentric lens has an effect that the size of the image of the sample particle in the captured image does not change even if the distance between the sample particle to be captured and the lens 35a in the direction of the optical axis of the camera 35 changes.

The flow cell 36 is an optical cell through which a fluid containing sample particles flows. In the example of FIG. 1, the surface facing the camera 35 and the surface facing the lighting device 37 are configured to be optically transparent.

The illumination device 37 is a device that irradiates the flow cell 36. In the example of FIG. 1, the lighting device 37 is arranged on the opposite side of the camera 35 with respect to the flow cell 36 so as to face the camera 35. As the lighting device 37, for example, a surface emitting type light emitting diode is adopted.

In addition, the lighting device 37 may control the light emission timing by the calculation unit 5, or may constantly emit light. In the example of FIG. 1, the calculation unit 5 causes the lighting device 37 to emit strobe light in synchronization with the shooting timing of the camera 35. The camera 35 can take a particle image of sample particles in the diluting liquid 23 in the flow cell 36 by receiving the light transmitted through the flow cell 36.

The discharge unit 4 is composed of a discharge pump 4a that discharges the diluent 23 from the dilution tank 2b. The discharge pump 4a pumps out the diluting liquid 23 in the diluting tank 2b and discharges the diluting liquid 23 to the outside through a discharge pipe C3 extending from the diluting tank 2b to the outside.

The calculation unit 5 is a functional element that executes various calculations. In the example of FIG. 1, the calculation unit 5 is a computer including a CPU, a volatile storage device, a nonvolatile storage device, an input/output interface, and the like, and is separated from the main body unit 1, the calculation unit 5, the transfer unit 7, and the like. It is installed in the separate room 6.

The calculation unit 5 processes, for example, the image captured by the camera 35 to calculate and save data necessary for measuring the particle size distribution of the sample particles, and calculates and saves the particle size distribution of the sample particles based on the data. To do. In addition, the calculation unit 5 outputs the calculated particle size distribution and the like using an output device such as a speaker and a display.

The transfer unit 7 is a functional element that transfers various fluids. In the example of FIG. 1, the transfer unit 7 includes a slurry pump 10, a supply pump 11, a diluting liquid pump 12, and the like. The supply pump 11 and the diluting liquid pump 12 form a sampling pump unit.

The slurry pump 10 pumps out the slurry 21 in the slurry tank 38, circulates the slurry 21 in a circulation pipe C10 which returns from the slurry tank 38 to the outside and then returns to the slurry tank 38.

In the example of FIG. 1, the slurry pump 10 is constantly rotated during the operation of the particle measuring device 100 to circulate the slurry 21 in the slurry tank 38 in the circulation conduit C10. The sample particles to be measured contained in the slurry 21 are metal particles having a relatively large specific gravity, and will easily precipitate unless they are circulated at a certain flow rate. Further, the sample particles to be measured may be partially solidified by drying. The slurry pump 10 is continuously rotated in order to prevent such precipitation or solidification of sample particles to be measured.

The supply pump 11 pumps out the slurry 21 from the slurry tank 38 and transfers the slurry 21 to the dilution tank 2b through a pipe C11 serving as a first pipe connecting the slurry tank 38 and the dilution tank 2b. In the example of FIG. 1, the pipe C11 is connected to the circulation pipe C10 on the downstream side of the slurry pump 10 in the circulation pipe C10. Therefore, during the sampling operation for measuring the particle size distribution, the supply pump 11 can draw the slurry 21 circulating in the circulation pipe C10 into the pipe C11 and transfer the drawn slurry 21 to the dilution tank 2b.

The circulation line C10 and the pipe C11 are connected using a pipe connecting member 31. The pipe connection member 31 is, for example, three-way cheese, and constitutes a connection point where the pipe C11 is connected to the circulation pipe line C10.

The diluting liquid pump 12 pumps out the diluting liquid 22 from the diluting liquid tank 39, and transfers the diluting liquid 22 into the pipe C11 through a pipe C12 as a second pipe connecting the diluting liquid tank 39 and the pipe C11. ..

The pipe C11 and the pipe C12 are connected using the pipe connecting member 32. The pipe connecting member 32 is, for example, three-way cheese, and constitutes a connection point where the pipe C12 is connected to the pipe C11.

The pumps used in particle measurement device 100 are all tube pumps, which provide a constant delivery rate at a constant rotational speed. Further, when each pump is stopped, the tube (tube) attached to each pump is completely closed in the tube pump, and the flow of fluid in the tube is stopped.

Next, the operation of the particle measuring device 100 will be described with reference to FIGS. 2 to 5 are enlarged views of the periphery of the slurry pump 10 of FIG. 2 shows a state in which a part of the pipe C11 is washed with the diluting liquid 22, and FIG. 3 shows a state in which the remaining part of the pipe C11 is washed with the diluting liquid 22. Further, FIG. 4 shows a state in which the slurry 21 is sampled, and FIG. 5 shows a state in which the slurry 21 in the pipe C11 is pushed by the diluting liquid 22 and transferred to the diluting tank 2b. 2 to 5, the slurry 21 is represented by dot hatching, and the diluting liquid 22 is represented by diagonal hatching. Further, the arrow drawn in the slurry pump 10 represents the rotation direction of the slurry pump 10, and the arrow drawn in the pipe and the pipe connecting member represents the flow direction of the fluid.

[Washing process]

The particle measuring device 100 cleans the pipe C11 before sampling the slurry 21. During cleaning, the diluting liquid pump 12 is operated with the supply pump 11 stopped. As shown in FIG. 2, the diluting liquid pump 12 transfers the diluting liquid 22 from the diluting liquid tank 39 to the pipe connecting member 32 through the pipe C12.

When the diluting liquid 22 reaches the pipe connecting member 32, the diluting liquid 22 passes through the pipe portion C11a between the pipe connecting member 32 and the pipe connecting member 31 in the pipe C11, and further, the circulation pipe C10 on the discharge side of the slurry pump 10. To the slurry tank 38 through the pipe portion C10b. The diluting liquid 22 does not flow into the pipe portion C11b of the pipe C11. This is because the supply pump 11 is stopped.

By this operation, the slurry 21 remaining in the pipe portion C11a is pushed out by the diluting liquid 22, flows into the pipe portion C10b, and returns to the slurry tank 38. The slurry 21 remaining in the pipe portion C11a has flowed into the pipe portion C11a during the previous sampling operation, for example.

The length of the pipe portion C11a between one end of the pipe C11 and the pipe connecting member 32, that is, the distance D1 between the pipe connecting member 31 and the pipe connecting member 32 should be as short as possible. This is because the amount of the diluting liquid 22 required for cleaning the pipe C11 and the amount of the slurry 21 consumed in the sampling operation can be reduced. The distance D1 is preferably 0.05 meters or less, for example. When the length of the pipe portion C11a is 0.05 meters, the amount of the slurry 21 in the pipe portion C11a is, for example, 0.63 ml.

After that, when a predetermined time (for example, 0.5 to 2 seconds) has elapsed, the particle measuring device 100 sets the supply pump 11 so that the discharge flow rate of the supply pump 11 and the discharge flow rate of the diluting liquid pump 12 become the same. And, the diluting liquid pump 12 is simultaneously operated. For example, if the discharge flow rate per rotation of the supply pump 11 and the discharge flow rate per rotation of the dilution liquid pump 12 are the same, the supply pump 11 and the dilution liquid pump 12 are operated at the same rotation speed. As a result, the diluting liquid 22 in the pipe C12 flows into the pipe portion C11b at the pipe connecting member 32 toward the dilution tank 2b, as shown in FIG.

During this time, the slurry pump 10 is operating, but when the diluting liquid pump 12 and the supply pump 11 are operating at the same discharge flow rate, the slurry 21 circulating in the circulation pipe C10 is in the pipe C11. Is hardly drawn in. This is because the flow rate of the diluting liquid 22 in the pipe C11 provided by the supply pump 11 and the flow rate of the diluting liquid 22 in the pipe C12 provided by the diluting liquid pump 12 are substantially equal.

This operation is continued until, for example, the diluting liquid 22 that has flowed into the pipe C11 at the pipe connecting member 32 reaches the diluting tank 2b, and a sufficient amount of the diluting liquid 22 is transferred. As a result, even when the slurry 21 remains in the pipe C11, the slurry 21 can be reliably pushed out into the diluting tank 2b.

Further, in the particle measuring apparatus 100, the diluting liquid pump 2a may be operated to transfer the diluting liquid 22 pumped from the diluting liquid tank 39 to the diluting tank 2b to wash the diluting tank 2b. The diluting liquid pump 2a transfers the diluting liquid 22 to the diluting tank 2b at a discharge flow rate that is four times the discharge flow rate of the supply pump 11 and the diluting liquid pump 12, for example.

The diluting liquid 22 in the diluting tank 2b used for cleaning the pipe C11 and the diluting tank 2b is discharged to the outside of the particle measuring apparatus 100 by the discharging unit 4. This cleaning operation is performed plural times, and the slurry 21 sampled last time is discharged to the outside of the main body 1.

In this way, the particle measuring device 100 can switch the path through which the diluting liquid 22 flows by controlling the operation of the plurality of pumps without providing a valve for switching the path through which the diluting liquid 22 flows. ..

[Sampling process]

Next, the particle measuring device 100 operates the supply pump 11 with the dilution liquid pump 12 stopped. As a result, as shown in FIG. 4, the flow of the diluting liquid 22 in the pipe C12 is stopped, and the slurry 21 in the circulation pipe C10 is drawn into the pipe C11 at the pipe connecting member 31. This is because the diluting solution 22 in the pipe C11 is continuously transferred to the diluting tank 2b. Then, the particle measuring device 100 continues this operating state for a predetermined time (for example, about 1 to 6 seconds). This is for the slurry 21 to be drawn into the pipe portion C11b beyond the pipe connection member 32.

Next, the particle measuring device 100 operates the diluting liquid pump 12. As a result, as shown in FIG. 5, the dilution liquid 22 transferred in the pipe C12 by the dilution liquid pump 12 flows into the pipe portion C11b at the pipe connection member 32 and is drawn into the pipe portion C11b. While pressing the slurry 21, it flows in the pipe portion C11b toward the dilution tank 2b. The slurry 21 drawn into the pipe portion C11b is transferred to the diluting tank 2b while being diluted with the diluting liquid 22 as a slurry sample.

When the supply pump 11 and the diluting liquid pump 12 operate at substantially the same discharge flow rate, the slurry 21 circulated in the circulation conduit C10 is almost drawn into the pipe C11 (particularly in the pipe portion C11b). I can't.

In this way, the particle measuring apparatus 100 dilutes the slurry 21 by pushing only the slurry 21 drawn into the pipe portion C11b as the slurry sample with the dilution liquid 22 when the supply pump 11 is stopped and the dilution liquid pump 12 is stopped. Transfer to tank 2b.

The particle measuring apparatus 100 may operate the discharge pump 4a until just before the slurry sample enters the dilution tank 2b, and continue discharging the dilution liquid 22 in the dilution tank 2b to the outside. This is because when the slurry 21 drawn into the pipe portion C11b is transferred to the diluting tank 2b, the diluting liquid 22 existing in the pipe portion C11b precedes the slurry 21 and is discharged to the outside.

Then, the particle measuring apparatus 100 stops the discharge pump 4a immediately before the slurry sample enters the diluting tank 2b, and collects the diluting liquid 23 in the diluting tank 2b until the diluting liquid 23 containing the slurry sample reaches a desired amount. The diluting liquid 22 may be transferred to the diluting tank 2b using the diluting liquid pump 2a.

When the amount of the diluting liquid 23 containing the slurry sample reaches a desired amount, the particle measuring device 100 stops the supply pump 11 and the diluting liquid pump 12 at the same time, and moves the diluting liquid tank 39 to the diluting tank 2b. The transfer of the diluting liquid 22 is stopped. When the diluting liquid pump 2a is operating, the diluting liquid pump 2a is also stopped.

The operating time of the supply pump 11 and the diluting liquid pump 12 for transferring the slurry sample is calculated from the inner diameter, length, etc. of the pipe C11. The diluting liquid 23 containing the slurry sample is diluted with the diluting liquid 22 in the diluting tank 2b until the slurry concentration becomes suitable for particle size distribution measurement.

[Photographing and particle size distribution measurement process]

After that, the particle measuring apparatus 100 operates the circulation pump 3a to circulate the diluent 23 containing the slurry sample diluted in the dilution tank 2b through the circulation conduit C2. Then, the diluted liquid 23 passing through the flow cell 36 is photographed by the camera 35. The camera 35 repeats photographing at a predetermined interval (for example, several times per second) for a predetermined time (for example, 6 minutes), and sends the photographed image to the calculation unit 5.

The calculation unit 5 acquires and records the particle measurement information such as the outer diameter, the area, the angle of the protrusion on the contour, the center of gravity, and the perimeter of each particle in the captured image by image processing. In order to obtain a highly accurate particle size distribution, it is desirable that approximately 4000 or more pieces of particle measurement information be acquired. During this time, the diluent 23 circulates in the circulation line C2.

[Discharging process]

After the image capturing, the particle measuring device 100 operates the discharge pump 4a to discharge the diluent 23 in the dilution tank 2b to the outside.

[Viewing particle size distribution results]

The above-mentioned washing process, sampling process, photographing/particle size distribution measurement process, and discharge process are sequentially and repeatedly executed, and the particle size distribution measurement result is stored in the calculation unit 5.

A user terminal such as a personal computer can communicate with the arithmetic unit 5 via a computer network such as a LAN, draw a graph using the particle size distribution measurement result, and calculate an aggregate value such as an average particle size. .. The calculation unit 5 may have a web server function. In this case, the user terminal can confirm the particle size distribution measurement result on the web browser. Moreover, the calculation unit 5 may be configured to automatically update and present the transition of the average particle size over a predetermined time (for example, several hours).

[Sampling from multiple powder manufacturing equipment]

Next, with reference to FIG. 6, a particle measuring device 100S that measures the particle size distribution of sample particles by sampling the slurries 21 and 21S from the respective slurry tanks 38 and 38S of the two powder manufacturing devices will be described. FIG. 6 is a schematic diagram showing a configuration example of the particle measuring device 100S.

The particle measuring apparatus 100S is different from the particle measuring apparatus 100 of FIG. 1 mainly in that it has a transfer section 7S, but it is common in other points. Therefore, in the following, a description of common parts will be omitted, and different parts will be described in detail.

The transfer unit 7 includes a slurry pump 10, a supply pump 11, a diluting liquid pump 12, and the like, like the transfer unit 7 in the particle measuring apparatus 100 of FIG.

The transfer unit 7S includes a slurry pump 10S, a supply pump 11S, a diluting liquid pump 12S, and the like, like the transfer unit 7. The configurations of the slurry pump 10S, the supply pump 11S, and the diluting liquid pump 12S are the same as the configurations of the transfer unit 7 and the transfer unit 7 of FIG.

The particle measuring device 100S sequentially transfers the slurry 21 in the slurry tank 38 and the slurry 21S in the slurry tank 38S to the dilution tank 2b to measure the particle size distribution of the sample particles. In the example of FIG. 6, the slurry pump 10 continuously operates during operation of the particle measuring device 100S. This is to maintain the circulation of the slurry 21 in the circulation pipe C10. Similarly, the slurry pump 10S continuously operates. This is for maintaining the circulation of the slurry 21S in the circulation pipe C10S.

As in the case of the particle measuring device 100 of FIG. 1, the particle measuring device 100S sequentially and repeatedly executes the cleaning process, the sampling process, the photographing/particle size distribution measuring process, and the discharging process. For example, the particle measuring device 100S samples the slurry 21 from the slurry tank 38 in the sampling process, executes the photographing/particle size distribution measuring process, the discharging process, and the cleaning process, and then performs the slurry 21S from the slurry tank 38S in the next sampling process. To sample.

Further, the particle measuring device 100S may simultaneously perform cleaning of the pipe C11 and the pipe C11S. In this case, the particle measuring device 100S can reduce the time required for the cleaning process as a whole.

In addition, the particle measuring device 100S operates by switching between the transfer unit 7 and the transfer unit 7S to operate the two slurry tanks 38, 38S using one set of the measurement unit 3, the discharge unit 4, and the calculation unit 5. The particle size distribution of the sample particles collected from the respective slurries 21 and 21S can be measured.

With this configuration, the particle measuring device 100S draws the slurry sample into the pipes C11 and C11S by the supply pumps 11 and 11S corresponding to the slurry tanks 38 and 38S, respectively, without providing a valve for switching the flow path of the fluid. be able to. Further, the slurry samples in the pipes C11 and C11S can be pushed toward the dilution tank 2b by the dilution liquids 22 and 22S pumped out by the dilution liquid pumps 12 and 12S. Therefore, the slurry sample can be transferred to the diluting tank 2b while cleaning the pipes C11 and C11S. This function realizes the effect that the heavy particles in the slurries 21 and 21S are less likely to remain in the tubes C11 and C11S, and that the cleaning time of the tubes C11 and C11S can be shortened. Even if the tubes C11 and C11S are long, the consumption amount of the slurries 21 and 21S during the sampling operation does not increase. This is because it is not necessary to push the slurry sample in the pipes C11 and C11S into the diluting tank 2b with the slurries 21 and 21S. Further, the particle measuring device 100S can efficiently dilute the diluting liquid 23 containing the slurry sample by directly transferring the diluting liquid 22 pumped by the diluting liquid pump 2a to the diluting tank 2b.

Thereafter, the particle measuring device 100S operates the circulation pump 3a to circulate the diluent 23 containing the slurry sample diluted in the diluting tank 2b through the circulation conduit C2, as in the particle measuring device 100 of FIG. The camera 35 sends an image of the diluted liquid 23 passing through the flow cell 36 to the calculation unit 5. The calculation unit 5 records and analyzes the received image and measures the particle size distribution of the sample particles.

In this way, the particle measuring device 100S can measure a particle size distribution of sample particles by acquiring a small amount of a slurry sample from each of the slurry tanks 38 and 38S of the two powder manufacturing devices. Note that another particle measuring device according to the embodiment of the present invention may be configured to acquire a small amount of a slurry sample from each of three or more slurry tanks and measure the particle size distribution of sample particles. In this case, the particle measuring device may include the same number of transfer units as the number of slurry tanks. With this configuration, the particle measuring apparatus 100S can reduce the cost burden related to the particle size distribution measurement per powder manufacturing apparatus.

Further, in the particle measuring device 100S, the total length of the pipe C11 and the pipe C11S can be reduced by installing the main body portion 1 at approximately the middle of the two slurry tanks 38, 38S. The same applies when there are three or more slurry tanks.

Although the embodiments for carrying out the present invention have been described in detail above, the present invention is not limited to the specific embodiments as described above, and is within the scope of the gist of the present invention described in the claims. In, various modifications and changes are possible.

For example, in the above-described embodiment, the supply pump 11 and the diluting liquid pump 12 are installed in the main body 1, but the present invention is not limited to this configuration. For example, the supply pump 11 and the diluting liquid pump 12 may be installed outside the main body 1.

Next, a first embodiment will be described with reference to FIGS. In Example 1, an in-line type particle measuring device 100 will be described in which the slurry 21 is sampled from the slurry tank 38 and the particle size distribution of sample particles is regularly measured in one step of the Ni powder manufacturing process.

The slurry 21 contains Ni particles, and the diluting liquid 22 was pure water. First, the slurry pump 10 was installed near the slurry tank 38. Further, the main body 1 was installed at a position slightly away from the slurry tank 38. The main body 1 was provided with a diluting unit 2, a measuring unit 3, a discharging unit 4, a supply pump 11, and a diluting liquid pump 12. The computing unit 5 was installed in the office, which is a separate room 6 that is more than 10 meters away from the main unit 1.

A diluting liquid tank (pure water tank) 39 was installed on the suction side of the diluting liquid pump 12. The length D1 of the tube portion C11a of the tube C11 was 0.05 meters. Tube pumps were used as the slurry pump 10, the supply pump 11, and the diluting liquid pump 12.

Next, a washing step was performed prior to measuring the particle size distribution. First, the slurry pump 10 was operated, and then the diluting liquid pump 12 was operated for 2 seconds while the supply pump 11 was stopped to wash the pipe portion C11a. After that, the supply pump 11 and the diluting liquid pump 12 were simultaneously operated. The discharge flow rates of the supply pump 11 and the diluting liquid pump 12 were set to be the same, and pure water as the diluting liquid 22 was transferred to the diluting tank 2b through the pipe C12 and the pipe C11 to wash the pipe C11. The pure water accumulated in the diluting tank 2b was circulated in the circulation pipe C2 and then discharged by the discharge unit 4. This cleaning operation was performed 3 times.

Next, the supply pump 11 was operated with the dilution liquid pump 12 stopped. As a result, the slurry 21 from the slurry tank 38 was drawn into the pipe C11 as a slurry sample. This operation was performed for about 3 seconds so that about 5 milliliters of the slurry sample was drawn into the tube portion C11b. Next, the diluting liquid pump 12 was operated, and the pure water pushed the slurry sample in the pipe portion C11b to transfer the slurry sample to the diluting tank 2b. Then, the slurry sample in the diluting tank 2b was diluted about 10,000 times. Then, the diluted liquid 23, which is the diluted slurry sample, was transferred to the measuring unit 3 to measure the particle size distribution of the sample particles. The particle size distribution of the sample particles was measured by the image analysis method. Specifically, the diluent 23 was transferred to the flow cell 36, and the particles in the diluent 23 were photographed by the camera 35 while passing through the flow cell 36. The captured image data was transmitted to the calculation unit 5. The calculation unit 5 calculated the particle size distribution of the sample particles based on the received image data. The photographed diluent 23 was discharged to the outside using the discharge unit 4. Then, in order to measure the particle size distribution of the sample particles of the next slurry sample, a series of steps starting with the washing step was restarted.

In the second embodiment, the number of the slurry tanks 38 is 6, and the six transfer units 7 are prepared and arranged. That is, six slurry pumps 10, six supply pumps 11 and one diluting liquid pump 12 were prepared and arranged. The diluting unit 2, the measuring unit 3, the discharging unit 4, and the calculating unit 5 each have a single configuration. Then, the slurry samples were sequentially taken from the six slurry tanks 38 at intervals of about 10 minutes, and the particle size distribution of the sample particles of the slurry sample was automatically measured. That is, a slurry sample was taken from the same slurry tank about every hour, and the particle size distribution of sample particles in the slurry sample was automatically measured. The particle size distribution was measured by the same procedure as in Example 1.

In Example 1 and Example 2, the particle size distribution of sample particles could be continuously measured. During that time, problems such as remarkable accumulation of slurry and blockage in the pipe C11 did not occur. Moreover, the previously measured slurry sample was not mixed in, and particles were not left in the tubes, the tube connecting members 31, 32, or the like. As a result, the particle size distribution of the sample particles of the slurry sample collected from each of the one or more slurry tanks could be measured accurately and efficiently.

Further, in the sampling step, since the slurry sample in the pipe portion C11b is pushed toward the dilution tank 2b by the diluting liquid 22 instead of the slurry 21, the consumption amount of the slurry 21 does not increase even if the pipe portion C11b is long. .. Therefore, the amount of the slurry sample necessary for measuring the particle size distribution of the sample particles is about 1/100 or less (for example, the pipe portion C11b) as compared with the case where the slurry sample in the pipe portion C11b is pushed toward the dilution tank 2b by the slurry 21. The length is 5 m).

Moreover, by grasping the particle size distribution of the sample particles of the slurry sample collected from each of the one or more slurry tanks in a short time, the quality of the slurry could be frequently confirmed. Therefore, it was possible to contribute to the quality improvement of the Ni powder. In addition, since the consumption of the slurry required for measuring the particle size distribution of the sample particles is small, a cost reduction effect was obtained.

Further, by installing the calculation unit 5 in the separate chamber 6 apart from the powder manufacturing apparatus, it becomes possible to omit special measures against dust and the like. In addition, by separating the arithmetic unit 5 from the main body 1, the main body 1 can be downsized.

DESCRIPTION OF SYMBOLS 1... Body part 2... Diluting part 2a... Diluting liquid pump 2b... Diluting tank 3... Measuring part 3a... Circulation pump 4... Discharge part 4a... Discharge pump 5... Calculation part 6... Separate room 7, 7S... Transfer part 10, 10S... Slurry pump 11, 11S... Supply pump 12, 12S... Diluting liquid pump 21, 21S... Slurry 22, 22S... Diluting liquid 23... Diluting liquid 31, 32... Pipe connecting member C1... Diluting pipe C2... Circulating pipe C3... Discharging pipe C10, C10S...・Circulation pipelines C10a, C10b... Pipe portions C11, C11S... Pipes C11a, C11b... Pipe portions C12... Pipe 35... Camera 35a... Lens 36... Flow cell 37... -Illumination device 38, 38S... Slurry tank 39, 39S... Diluting liquid tank 100, 100S... Particle measuring device

Claims (5)

A transfer unit that transfers the slurry of the first container to the second container using the diluting liquid,
A diluting unit that dilutes the slurry with the diluting liquid in the second container to generate a diluting liquid,
A data acquisition unit for acquiring data on particles in the diluent,
A calculation unit that calculates a physical quantity regarding the particles using the data acquired by the data acquisition unit,
Have a, and a discharge portion for discharging the diluent from the second container,
The transfer unit includes a first pipe that connects the first container and the second container, a second pipe that connects the third container containing the diluting liquid and the first pipe, and the first pipe. A pipe connecting member for connecting the second pipe,
By pressing the slurry drawn into the pipe portion, which is a part of the first pipe between the pipe connecting member and the second container, with the diluting liquid, the slurry drawn into the pipe portion. Is transferred to the second container ,
Particle measuring device. The slurry prior Symbol first container is transferred to the second container through the first pipe,
The diluting liquid in the third container is transferred to the second container through the second pipe and a part of the first pipe,
The particle measuring device according to claim 1. The transfer unit transfers a slurry pump that pumps the slurry, a diluting liquid pump that pumps the diluting liquid, the slurry pumped by the slurry pump or the diluting liquid pumped by the diluting liquid pump. And a supply pump to
The particle measuring device according to claim 1 or 2. Having a plurality of the transfer units,
It has one each of the dilution unit, the data acquisition unit, the calculation unit, and the discharge unit,
The particle measuring device according to claim 1. Prior Symbol length between the pipe connecting member and one end of the first tube is less than 0.05 meters,
The particle measuring device according to claim 2.

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