KR101666924B1 - System for detail analysis of powder with metal foreign substance - Google Patents

System for detail analysis of powder with metal foreign substance Download PDF

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Publication number
KR101666924B1
KR101666924B1 KR1020150063700A KR20150063700A KR101666924B1 KR 101666924 B1 KR101666924 B1 KR 101666924B1 KR 1020150063700 A KR1020150063700 A KR 1020150063700A KR 20150063700 A KR20150063700 A KR 20150063700A KR 101666924 B1 KR101666924 B1 KR 101666924B1
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metal
stick
magnetic
powder
mixing device
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KR1020150063700A
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Korean (ko)
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이상익
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이상익
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G01N1/18—Devices for withdrawing samples in the liquid or fluent state with provision for splitting samples into portions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G01N2001/1006—Dispersed solids

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  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Hydrology & Water Resources (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention relates to system for a high-precision analysis of powder with a metallic foreign substance comprising: a mixing device (100); a dissolving device (200); a heating device (300); an ICP analyzer (400); and a moving device (500). According to the present invention, highly precise ICP analysis is able to be performed by increasing a magnetic property and increasing an area having a high magnetic property, and preventing a separation of metallic foreign substances adhered due to an impact.

Description

In this paper, we propose a new system for the analysis of metals in powdery materials.

The present invention relates to a method for detecting an ICP mass, a spectroscopy, a luminescence, and the like by detecting water using a magnet stick and an acidic solution, the metal reacting with magnetism contained in a powder such as a secondary battery material whose performance deteriorates when a metal is contained in water To a high-precision analytical system through which a magnetic stick can be analyzed in a PPB unit or less by forming a structure having a high magnetic force.

When metal particles are present in the secondary battery material, non-lithium metal ions are ionized to move to the cathode during charging, and the migrated metal ions are deposited on the separator while growing into metallic particles on the surface of the cathode, Thereby forming a path.

This causes the capacity failure of the secondary battery in the initial stage, and when the short path formation is accelerated, ignition or explosion occurs.

In addition, when metal particles are contained in the powder during the manufacture of various foods such as infant formula, confectionery, etc., the harmful influence to the human body may be adversely affected.

In order to prevent such problems, it is necessary to remove the metal if it is contained in the powder, or to filter the metal so as not to contain the metal.

The quality control department of the inspection organization or the product production line accurately analyzes whether the metal is contained in the powder through ICP analysis method such as ICP mass spectrometry or ICP spectrometry.

A method for detecting the content of metal particles in the same powder as the secondary battery raw material to a unit of ppb is disclosed in Korean Patent Laid-Open Publication No. 10-2014- 0048370 discloses a method of separating a suspended material by generating bubbles in a suspension in which a material for a secondary battery containing a non-magnetic metal particle is dispersed, selectively dissolving the non-magnetic metal particles in the suspended material, Contents for analyzing the contents using an ICP analyzing device such as ICP-AES and ICP-MS are disclosed.

In Patent Document 1, contents for separating magnetic metal particles through a magnetic separator are disclosed.

However, since the magnetic substance used in the present high-precision analysis is made of a general magnet, the magnetic force is weak and the surface area of the steel magnetic force is small, so that the adhesion force of the metal foreign substance in the powder is lowered, There is a problem in that the analytical performance is deteriorated even if it is used.

KR 10-2014-0048370 (April 24, 2014)

The present invention provides a water high precision analytical system for a metal powder to solve the problems of the prior art as described above. The magnet stick has a plurality of magnets connected side by side, The surface of the N pole and the S pole is formed larger than the surface of the N pole and the S pole in the direction perpendicular to the surface, thereby maximizing the magnetic force so that the magnetic metal can improve the trapping ability of the water.

Particularly, a bottom separating member is provided at both ends of the magnet stick to prevent the magnet stick from contacting the bottom surface in the mixing device, so that the metal attached through mixing and stirring in the mixing device such as a ball mill, And to prevent the collection ability from being detached due to impact or the like.

In addition, a heating device for heating the acid solution in the dissolving device for dissolving the metal water is provided, and the surface of the magnet stick is formed with a heat-resistant coating layer, thereby preventing the decrease of magnetism due to heating, So that a precise content analysis in units of ppb can be performed through the analyzer.

In addition, since the magnet is provided between the adjacent magnets to increase the magnetic force, the magnetic force can be improved to enhance the adhesion of the magnetic metal.

As a result, it is aimed to increase the magnetism and to increase the area of the magnetically high portion, and to prevent the water from escaping from the metal due to the impact, so that a highly accurate ICP analysis can be performed.

In order to solve the above problem, a pretreatment magnet stick for high precision analysis of metal in powder of the present invention is characterized in that a plurality of magnets 11 having N poles 11a and S poles 11b are connected to each other, The adjacent magnets 11 are made of the same polarity and the anode surface 10a in which the N poles 11a and the S poles 11b are located is disposed on an orthogonal plane The magnet stick 10 having an area larger than that of the magnetic stick 10b and the powder 20 containing the metal water 21 are mixed and stirred so that the metal 21 reacting with the magnet is immersed in the magnet stick 10), a mixing device 100 made of a ball mill; The magnetic sticks 10 to which the metal 21 is adhered are introduced by mixing and stirring in the mixing device 100 and the metal sticks 10 attached to the magnet stick 10 A dissolution apparatus (200) for dissolving the foreign matter (21) in the acidic solution (210); A heating device 300 for heating the contents of the dissolution apparatus 200; An ICP analyzer 400 for analyzing the acid solution by supplying the acid solution 210 in which the metal 21 is dissolved in the dissolution apparatus 200; A rail 510 installed on the upper side of the mixing apparatus 100 and the dissolving apparatus 200, a moving member 520 moving along the rail, a hydraulic or pneumatic cylinder 530 And a pulling hook 540 installed on the arm of the cylinder 530 for pulling the magnetic stick 10 and the magnet stick 10 is fixed to the magnet 11 And the outer circumference of the bottom spacer 12 is larger than the circumference of the side surface of the magnet stick 10, The surface of the magnetic stick 10 is spaced apart from the inner circumferential surface of the mixing device 100 so that the metal in the powder 20 adheres to the surface of the magnet stick 10 in the state where the water 21 is attached to the surface of the magnet stick 10 Is prevented from colliding with or contacting with the inner circumferential surface of the mixing apparatus 100, 1 is not separated and a heat resistant coating layer 13 is formed on the surface and a magnet 14 is provided between the magnets 11 adjacent to each other to increase the magnetic force. The pulling hook 540 is fastened And a ring is provided.

According to the present invention, a plurality of magnets are connected side by side in a magnetic stick, and the portions where the adjacent magnets are in contact with each other are made to have the same magnetic property so that the magnetic property is increased. Thereby maximizing the magnetic force. As a result, the magnetic metal can improve the trapping ability of water and analyze it.

Particularly, a bottom separating member is provided at both ends of the magnet stick to prevent the magnet stick from contacting the bottom surface in the mixing device, so that the metal attached through mixing and stirring in the mixing device such as a ball mill, It is possible to prevent the collection ability from being reduced due to the impact or the like.

In addition, a heating device for heating the acid solution in the dissolving device for dissolving the metal water is provided, and the surface of the magnet stick is formed with a heat-resistant coating layer, thereby preventing the decrease of magnetism due to heating, A precise content analysis in units of ppb can be performed through the analyzer.

In addition, since the magnetic iron is provided between the adjacent magnets to increase the magnetic force, the magnetic force can be further improved and the magnetic metal can increase the adhesion of water.

As a result, the magnetism is increased, the area of the high magnetic portion is increased, and the metal sticking due to the impact prevents the water from escaping, so that a highly precise ICP analysis can be performed.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a partially cut exploded perspective view showing one embodiment of a magnetic stick for high precision analysis of water in a powder in the present invention. FIG.
2 to 7 are schematic views sequentially showing an embodiment of a pretreatment process for an ICP analysis experiment using the magnet stick of the present invention.

The magnetic stick for high precision analysis of metal in the powder of the present invention is put into a mixing device 100 composed of a ball mill together with the powder 20 as shown in FIG. 2 and mixed and stirred, The attached metal 21 is dissolved in the acidic solution 210 in the dissolution apparatus 200 and then the acidic solution 210 in which the metal 21 is dissolved is introduced into the analysis apparatus 400) is used for analysis systems.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will now be described in detail with reference to the accompanying drawings.

The magnetic stick for high-precision analysis of metal in powder of the present invention is constituted by connecting a plurality of magnets 11 having N pole 11a and S pole 11b side by side as shown in FIG.

In this configuration, the adjacent magnets 11 have the same polarity at the portions where they are in contact with each other.

Particularly, the anode surface 10a in which the N poles 11a and the S poles 11b having high magnetic forces are located is larger than the orthogonal surface 10b in the direction orthogonal to the anode surface 10a .

Specifically, the upper magnet 11 in FIG. 1 has the N pole 11a at the lower portion and the S pole 11b at the upper portion. The lower magnet 11 has the S pole 11b at the lower portion and the N pole The magnetic pole 10a of the magnet stick 10 is formed on the upper surface and the lower surface of the magnet stick 10 as compared with the orthogonal surface 10b formed on the side orthogonal to the upper surface. The area of the portion having a high density of the magnetic force lines is large, so that a large amount of metal can adhere to the water 21.

This is because the area of the anode surface 10a on which the magnetic lines of force are concentrated is large and the magnets are disposed adjacent to each other to increase the magnetic force.

This is because as shown in FIGS. 2 and 3, when the metal contained in the powder 20 is adhered to the surface of the powder 20 through mixing and stirring in the mixing device 100, The magnetic force is increased as compared with other portions, so that the water 21 is adhered to the maximum amount of metal present in the powder 20, thereby maximizing the precision of the experiment.

In addition, as shown in the figure, the magnet 14 is provided between the two magnets 11 to further increase the magnetic force, so that the magnetic force of the thin layer can be increased.

Particularly, as shown in the figure, the magnet stick 10 is attached with the bottom spacer 12 at both ends in a direction perpendicular to the direction in which the magnets 11 are connected to each other, and the outer diameter of the bottom spacer 12 And the surface of the magnetic stick 10 is spaced apart from the inner circumferential surface of the mixing device 100 in the mixing device 100. [

The metal in the powder 20 is prevented from colliding with or contacting with the inner circumferential surface of the mixing device 100 while the water 21 is attached to the surface of the magnet stick 10, 21 can be prevented from being separated well so that the detection rate of the metal 21 can be maximized.

Particularly, as shown in the figure, the bottom separating member 12 has a circular shape and moves smoothly while rolling inside the mixing device 100 during mixing and stirring of the mixing device 100 such as a ball mill, So that the foreign object 21 can be attached to the magnetic stick 10 as much as possible.

The powder 20 to be inspected and the magnetic stick 10 are inserted into the mixing device 100 such as a ball mill and mixed and stirred so that the metal in the powder 20 reacts with the water 21 To the surface of the magnetic stick 10 can be maximized.

In this case, a heat-resistant coating layer 13 may be formed on the outer circumferential surface of the magnet stick 10 in order to prevent the magnetic force from being lowered due to heating.

The heat-resistant coating layer 13 may be formed of Teflon, molybdenum coating or the like as a coating layer for preventing the magnetic force of the magnet 11 from being lowered due to generation of a high temperature according to heating.

Hereinafter, an embodiment of the analyzing system and analyzing method using the magnetic stick for water high precision analysis in the present invention having the above-described structure will be described.

2, the mixing apparatus 100 includes a magnetic stick 10 and a powder 20 to be analyzed, which are mixed and stirred therein.

The oil and air pressure actuator 120 is shown in FIG. 2 as a configuration for mixing and stirring. However, it is only an embodiment of mixing and stirring, and an agitator equipped with an impeller may be installed therein.

Preferably, the mixing device 100 itself is composed of a vibrating and rotating body such as a ball mill, and the powder 20 and the magnetic stick 10 are mixed and stirred.

As shown in the drawing, the dissolving apparatus 200 stores an acidic solution 210 such as hydrochloric acid, sulfuric acid, and nitric acid, which is capable of dissolving the water 21 with a metal having magnetism to be detected therein.

The metal stick 21 is attached to the magnet stick 10 by mixing and stirring in the mixing apparatus 100 and the metal attached to the magnet stick 10 is immersed in the acid solution 210 ). ≪ / RTI >

The water 21 dissolved in the acid solution 210 in the dissolving apparatus 200 is supplied to the ICP analyzer together with the acidic solution 210 to perform a high-precision analysis.

1, a heating device 300 for heating the contents of the dissolution apparatus 200 is further provided, and the magnet stick 10 may be formed with a heat-resistant coating layer 13 on the surface thereof have.

The heating device 300 may be composed of a heater or the like made of a normal heating wire.

With such a heating device 300, the metal 21 can dissolve the water 21 as quickly as possible, and a high-precision analysis can be performed more easily.

The heat-resistant coating layer 13 may be formed of Teflon, molybdenum or the like as a coating layer for preventing the magnetic force of the magnet 11 from being lowered due to the high temperature generated by the operation of the heating device 300.

A supply pipe 220 and a supply valve 221 connected to the ICP analyzer 400 are installed on the dissolution apparatus 200 to supply the acid solution 210 in the dissolution apparatus 200 to the analysis apparatus 400 And a drain pipe 230 and a drain valve 231 may be installed at the lower part so as to dispose of the remaining acidic solution 210.

2, the magnetic stick 10 may be inserted into and discharged from the mixing device 100 by the mixing device 100 and the dissolving device 200, And a moving device 500 for moving the magnet stick 10 to and from the dissolving apparatus 200, and drawing the magnet stick 10 into and out of the dissolving apparatus 200.

The embodiment of the drawing shows that the rail 510 is installed on the upper side of the mixing apparatus 100 and the melting apparatus 200 and the moving member 520 moving along the rail is provided. A pneumatic cylinder 530 is provided and the arm of the cylinder 530 is provided with a pulling hook 540 capable of pulling the magnet stick 10.

At this time, a hook is formed so that the pulling hook 540 can be fastened to the magnet stick 10.

At this time, although the rail 510 is illustrated as moving in only one side in the horizontal direction in the figure, it may be configured to move along the X axis and the Y axis.

In addition, the moving member 520 may be constructed to be movable along the rail 510 with a wheel and a motor built therein.

At this time, an unillustrated control device for controlling the operation of the mobile device 500 may be configured to be electrically connected to the mobile device 500 to control the operation of the mobile device 500.

At this time, in the mixing device 100, the opening and closing door 110 is opened so that the inside of the mixing device 100 can be opened or closed before or after the time when the magnetic stick 10 is inserted or withdrawn by the pulling hook 540 3, the opening / closing door 110 is connected to a pneumatic / pneumatic cylinder whose hinge portion is not shown. The cylinder is electrically connected to the control device and is controlled by the control device to open / close the door 110 May be configured to operate.

The analytical method using the magnetic stick for high-precision water analysis in the powder of the present invention will be described as follows.

2, a magnetic stick 10 is connected to a pulling hook 540 of a moving device 500, and a powder 20 containing a metal and water 21 is supplied to the mixing device 100 The magnetic stick 10 is inserted into the mixing device 100 as shown in FIG. 3 by using the moving device 500.

At this time, of course, the opening and closing door 110 takes an opened state as shown.

Then, as shown in FIG. 4, the moving device 500 is operated to move the pulling hook 540 to be positioned outside the mixing device 100, and then the mixing device 100 is reciprocally moved using the actuator 120 So that the metal 21 adheres to the surface of the magnetic stick 10 as shown in FIG.

Thereafter, the magnetic stick 10 to which the metal 21 is attached is connected to the pulling hook 540 as shown in FIG. 5 by using the moving device 500, and then the moving device 500 The magnetic stick 10 is put into the dissolution apparatus 200 in which the acid solution 210 is stored.

7, the metal 21 is dissolved by the acidic solution to become the state shown in FIG. 7. In this state, the acidic solution moves to the analysis device 400 by opening the supply valve 221, Analysis is performed.

After the analysis is completed, the remaining acidic solution 210 is discharged through the discharge pipe 230 by the opening of the discharge valve 231 and is disposed of.

This structure is advantageous in that the magnetic stick 10 has a structure in which the magnet 11 is continuously arranged and the area of the anode portion associated with the arrangement of the magnets 11 is increased, ) Of the powder 21 by increasing the metal deposition rate of the metal 21 by preventing the metal 21 from being separated again by the vibration of the mixing device 100 of the water 21 It is possible to collect the water 21 as much as possible in the dissolving apparatus 200 and the metal dissolving apparatus 200 using the acidic solution improves the dissolving efficiency by using the dissolving and heating apparatus 300, Due to the structure of preventing the magnetic force from being lowered by the coating layer 13, the water detection and analysis experiment can be continuously performed with high precision.

The magnetic stick for high-precision water analysis of metal in the powder of the present invention can be used for quality control experiments and experiment analysis facilities of various manufacturing facilities using high-purity powders as well as raw materials for secondary batteries and food materials as described above.

In some cases, it may be applied to other magnetic separation facilities.

10: magnet stick 10a: positive pole face
10b: orthogonal plane 11: magnet
11a: N pole 11b: S pole
12: bottom separating member 13: heat-resistant coating layer
14: Metric 20: Powder
21: metal water 100: dissolution apparatus
110: opening / closing door 120: actuator
200: dissolution apparatus 210: acid solution
220: supply pipe 221: supply valve
230: discharge pipe 231: discharge valve
300: Heating device 400: Analyzer
500: Mobile device 510: Rail
520: moving member 530: cylinder
540: Tow hook

Claims (5)

In a metal-in-water high-precision analytical system,
A plurality of magnets 11 having N poles 11a and S poles 11b are connected in parallel to each other and adjoining magnets 11 are made of the same poles. Wherein the positive pole face 10a in which the pole 11b is located is larger than the perpendicular face 10b in the direction orthogonal to the positive pole face 10a; A mixing device 100 composed of a ball mill so that the powder 20 contained therein is mixed and stirred so that the metal 21 reacting with magnetism adheres to the surface of the magnetic stick 10;
The magnetic sticks 10 to which the metal 21 is adhered are introduced by mixing and stirring in the mixing device 100 and the metal sticks 10 attached to the magnet stick 10 A dissolution apparatus (200) for dissolving the foreign matter (21) in the acidic solution (210);
A heating device 300 for heating the contents of the dissolution apparatus 200;
An ICP analyzer 400 for analyzing the acid solution by supplying the acid solution 210 in which the metal 21 is dissolved in the dissolution apparatus 200;
A rail 510 installed on the upper side of the mixing apparatus 100 and the dissolving apparatus 200, a moving member 520 moving along the rail, a hydraulic or pneumatic cylinder 530 And a pulling hook 540 installed on the arm of the cylinder 530 for pulling the magnetic stick 10,
The magnet stick 10 has a bottom spacer 12 at both ends in a direction perpendicular to the direction in which the magnets 11 are connected to each other. The surface of the magnetic stick 10 is separated from the inner circumferential surface of the mixing device 100 in the mixing device 100 so that the water 21 in the powder 20 is mixed with the magnetic stick 10, The metal sticks are prevented from being separated from each other by preventing the magnet stick 10 from colliding with or contacting the inner circumferential surface of the mixing device 100 in a state of being attached to the surface and the heat resistant coating layer 13 is formed on the surface , A yoke (14) for increasing the magnetic force between adjacent magnets (11) is provided, and a hook is provided for fastening the pulling hook (540)
High - precision analytical system for water in metal powders. delete delete delete delete
KR1020150063700A 2015-05-07 2015-05-07 System for detail analysis of powder with metal foreign substance KR101666924B1 (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0373591A (en) * 1989-08-11 1991-03-28 Elna Co Ltd Manufacture of printed board
JP2003080107A (en) * 2001-09-11 2003-03-18 Magnetec Japan Ltd Magnetic filter and its manufacturing method
JP2008145305A (en) * 2006-12-11 2008-06-26 Olympus Corp Container with stirring mechanism and autoanalyzer
JP2008145246A (en) * 2006-12-08 2008-06-26 Denki Kagaku Kogyo Kk Method of measuring number of magnetized particles in nonmagnetic metal oxide powder
KR20140048370A (en) 2012-10-10 2014-04-24 삼성에스디아이 주식회사 Method for detecting non-magnetic metal particles contained in secondary battery materials

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0373591A (en) * 1989-08-11 1991-03-28 Elna Co Ltd Manufacture of printed board
JP2003080107A (en) * 2001-09-11 2003-03-18 Magnetec Japan Ltd Magnetic filter and its manufacturing method
JP2008145246A (en) * 2006-12-08 2008-06-26 Denki Kagaku Kogyo Kk Method of measuring number of magnetized particles in nonmagnetic metal oxide powder
JP2008145305A (en) * 2006-12-11 2008-06-26 Olympus Corp Container with stirring mechanism and autoanalyzer
KR20140048370A (en) 2012-10-10 2014-04-24 삼성에스디아이 주식회사 Method for detecting non-magnetic metal particles contained in secondary battery materials

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