CN114345524A - Improved preparation method of nano composite thermoelectric material - Google Patents

Improved preparation method of nano composite thermoelectric material Download PDF

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Publication number
CN114345524A
CN114345524A CN202210013673.5A CN202210013673A CN114345524A CN 114345524 A CN114345524 A CN 114345524A CN 202210013673 A CN202210013673 A CN 202210013673A CN 114345524 A CN114345524 A CN 114345524A
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China
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plate
grinding cylinder
powder
fixedly connected
grinding
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Inventor
陈哲
胡瑞
徐国栋
何翠群
付凯
何雪龙
徐芳
宦鹤波
华瑶
邹沛
张俊红
喻雪峰
周憬
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Nanchang Institute of Technology
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Nanchang Institute of Technology
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Priority to CN202210013673.5A priority Critical patent/CN114345524A/en
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Abstract

The invention discloses an improved preparation method of a nano composite thermoelectric material, belonging to the technical field of nano thermoelectric material preparation, comprising the following steps: smelting the Cu, Se and La block raw materials into ingots by adopting induction smelting equipment; s powder weighed according to the chemical formula proportion and a broken ingot thermoelectric material are loaded into a ball milling device, and the ball milling device is used for milling the S powder and the ingot thermoelectric material; in the grinding process, the ball milling device can fully grind the substandard cast ingots and powder, and the substandard powder can be sent into a graphite die by the ball milling device; then placing the graphite mould loaded with the primary ball milling powder into a discharge plasma sintering cavity, and sintering the graphite mould into a block in a vacuum atmosphere; crushing the sintered block, and performing secondary ball milling in a nitrogen atmosphere; then sintering under vacuum atmosphere; the invention can lead the S powder and the broken cast ingot to be ground more quickly and the efficiency to be higher.

Description

Improved preparation method of nano composite thermoelectric material
Technical Field
The invention relates to the technical field of nano thermoelectric material preparation, in particular to an improved preparation method of a nano composite thermoelectric material.
Background
The thermoelectric material can realize the interconversion between heat energy and electric energy, does not need mechanical moving parts in the conversion process, has no noise and abrasion, has a simple mechanism, has no pollution to the environment, and is considered to be one of the main ways for solving the energy crisis.
The prior art discloses an invention patent in the technical field of partial nano thermoelectric material preparation, wherein the invention patent with the application number of CN201910253459.5 discloses a preparation method of a nano composite thermoelectric material, which comprises the following steps: (1) smelting the Cu, Se and La block raw materials into ingots by adopting induction smelting equipment; (2) then, putting S powder weighed according to the chemical formula ratio and the crushed cast ingot into a ball milling tank, and carrying out primary ball milling in a nitrogen atmosphere by adopting mechanical ball milling equipment; (3) then placing the graphite mould loaded with the primary ball milling powder into a discharge plasma sintering cavity, and sintering the graphite mould into a block in a vacuum atmosphere; (4) crushing the sintered block, and performing secondary ball milling in a nitrogen atmosphere; (5) and then sintered under a vacuum atmosphere.
The prior art is when carrying out the ball-milling to broken ingot casting, what adopt is the ball mill, current ball mill need carry out the grinding repeatedly to the material of grinding, the material can appear partially grind thoroughly when grinding in the ball mill and partially grind incomplete circumstances, grind not thorough granule can be adulterated in the powder after grinding thoroughly, the powder that grinds thoroughly can play the cushioning effect to the steel ball, the effort that can lead to the steel ball to act on when granule reduces greatly, can lead to the granular material need carry out a lot of grinds just can grind thoroughly, and when powder increases granular material gradually and reduces gradually, granular material can be more and more difficult to grind thoroughly, can lead to grinding time long, the grinding efficiency is low.
Based on this, the invention designs an improved preparation method of the nano composite thermoelectric material to solve the problems.
Disclosure of Invention
The present invention is directed to an improved method for preparing a nanocomposite thermoelectric material, which solves the above-mentioned problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: an improved method for preparing a nanocomposite thermoelectric material, the method comprising the steps of:
the method comprises the following steps: smelting the Cu, Se and La block raw materials into ingots by adopting induction smelting equipment;
step two: s powder weighed according to the chemical formula proportion and a broken ingot thermoelectric material are loaded into a ball milling device, and the ball milling device is used for milling the S powder and the ingot thermoelectric material;
step three: in the grinding process, the ball milling device can fully grind the substandard cast ingots and powder, and the substandard powder can be sent into a graphite die by the ball milling device;
step four: then placing the graphite mould loaded with the primary ball milling powder into a discharge plasma sintering cavity, and sintering the graphite mould into a block in a vacuum atmosphere;
step five: crushing the sintered block, and performing secondary ball milling in a nitrogen atmosphere; and then sintered under a vacuum atmosphere.
The ball milling device comprises a bottom plate, two first mounting plates are fixedly connected to the top of the bottom plate, a first grinding cylinder and a second grinding cylinder are arranged between the two first mounting plates, the second grinding cylinder is positioned at the lower right part of the first grinding cylinder, a feeding pipe is rotatably connected to the first grinding cylinder, the feeding pipe is fixedly connected with the first mounting plate at the front side, the second grinding cylinder is rotatably connected with the first mounting plate, a driving assembly and a conveying assembly are arranged between the first grinding cylinder and the second grinding cylinder, the driving assembly is used for driving the first grinding cylinder and the second grinding cylinder to synchronously rotate so as to drive the first grinding cylinder and the second grinding cylinder to grind S powder and cast ingots, and the conveying assembly is used for conveying the powder after the primary grinding in the first grinding cylinder to the second grinding cylinder for secondary grinding;
the conveying assembly comprises a plurality of discharge holes, a plurality of feed holes and a third material guide plate; the plurality of discharge holes are arranged on the first grinding cylinder in a circumferential array, and the side edges of the discharge holes are provided with first material guide plates fixedly connected to the inner wall of the first grinding cylinder; the plurality of feeding holes are arranged on the second grinding cylinder in a circumferential array, and the side edges of the feeding holes are provided with second material guide plates fixedly connected to the inner wall of the second grinding cylinder; the third material guide plate consists of two cylinders and an inclined plate; the two cylinders are respectively sleeved on the first grinding cylinder and the second grinding cylinder and are positioned at the outer sides of the first grinding cylinder and the second grinding cylinder, and the inclined plate is used for fixedly connecting the two cylinders together; the inclined plate is provided with a material guide hole which can be in butt joint with the discharge hole and the feed hole; the bottom of the cylinder on the right side is provided with a discharge hole, and a second filter plate is fixedly connected in the discharge hole.
As a further aspect of the present invention, the driving assembly includes a first rotating wheel and a second rotating wheel, the first rotating wheel is fixedly connected to a rotating shaft of the first grinding cylinder, the second rotating wheel is fixedly connected to a rotating shaft of the second grinding cylinder, the first rotating wheel and the second rotating wheel are connected through a belt, a motor is disposed outside the second rotating wheel, the motor is fixedly connected to the front first mounting plate, and an output shaft of the motor is fixedly connected to the rotating shaft of the second grinding cylinder.
As a further scheme of the present invention, a fixed plate is fixedly connected to the first material guiding plate, a first filter plate is rotatably connected to the fixed plate, the first filter plate is disposed in an inclined manner, and the first filter plate, the fixed plate and the first material guiding plate shield the discharge hole on the inner sides thereof.
As a further scheme of the invention, the front side and the rear side of the first grinding cylinder are respectively and rotatably connected with a second mounting plate, and the second mounting plates are positioned on the outer side of the first filter plate; rear side the second mounting panel is with the first mounting panel fixed connection of rear side, the front side second mounting panel and inlet pipe fixed connection, the second mounting panel is close to the rubber block that fixedly connected with a plurality of was circumference array distribution on the lateral wall of first filter plate, and is a plurality of the rubber block is spherical, the rubber block distributes in the right side below of second mounting panel, the rubber block can act on the vibrations of first filter plate, the first spring of the common fixedly connected with of first filter plate and fixed plate.
As a further scheme of the invention, a shielding plate is connected to the inclined plate in a sliding manner, the shielding plate is arranged obliquely relative to the inclined plate, and a second spring for resetting the shielding plate is fixedly connected to the shielding plate; the shielding plate passes through fixed block fixedly connected with rack bar, rack bar and swash plate outer wall sliding connection, the rack bar meshing has incomplete gear, fixedly connected with third runner in the axis of rotation of incomplete gear, the third runner rotates with first mounting panel to be connected, the third runner is connected with belt drive.
As a further scheme of the invention, a buffer groove is formed in the inclined plate, the shielding plate is located in the buffer groove, a sealing plate is arranged above the buffer groove, the sealing plate is slidably connected with the inclined plate, the sealing plate is slidably connected with the shielding plate, a third spring is fixedly connected to the side wall of the sealing plate, and the right end of the third spring is fixedly connected with the inclined plate.
As a further scheme of the invention, the top of the bottom plate is fixedly connected with a collecting box, and the collecting box is positioned below the inclined plate and the discharge hole.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the first grinding cylinder, the second grinding cylinder and the conveying assembly, powder and particles ground to a certain degree in the first grinding cylinder can be conveyed into the second grinding cylinder by the conveying assembly, so that the powder and the particles ground to a certain degree can not obstruct the grinding of larger particles, the particles in the first grinding cylinder can be crushed to a certain degree more quickly, the powder and the particles ground to a certain degree can be ground better and finer in the second grinding cylinder, the completely ground powder in the second grinding cylinder can automatically fall off, and the completely ground powder can be ensured not to obstruct the grinding of the particles; through setting up first grinding vessel and second grinding vessel into the grinding of different fineness, not only can the grinding speed of greatly increased granule, can also not need to grind the granule repeatedly, long when can significantly reduce the granule and grind, efficiency that can greatly increased granule ground.
2. According to the invention, through the arrangement of the fixing plate and the first filter plate, the first filter plate which is obliquely arranged can replace the first guide plate to work, when the first filter plate drives the steel ball to move upwards, the steel ball cannot be contacted with the side wall of the first filter plate, and the first filter plate which is obliquely arranged can enable particles and powder which are crushed to a certain degree to better fall into the discharge hole, so that the possibility that the particles and the powder fall into the first grinding cylinder again can be greatly reduced, the particles and the powder which are ground to a certain degree can quickly move into the second grinding cylinder for fine grinding, the grinding speed of the particles can be greatly increased, the grinding time of the particles can be greatly reduced, and the grinding efficiency of the particles can be greatly increased.
3. According to the invention, through the arrangement of the second mounting plate, the rubber block and the first spring, when the first filter plate is driven by the first grinding cylinder to rotate from the lowest point to the rightmost side, the rubber block and the first spring act on the first filter plate together to vibrate the first filter plate, particles staying between small-diameter steel balls can fall under the vibration effect due to the vibration of the first filter plate, and then enter the discharge hole from the first filter plate, so that the particles can move into the second grinding cylinder more quickly and better for fine grinding, the grinding speed of the particles can be greatly increased, the grinding duration of the particles can be greatly reduced, and the grinding efficiency of the particles can be greatly increased.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a schematic diagram of the overall structure of the present invention;
FIG. 3 is a schematic cross-sectional view of the connection and position of the first grinding cylinder, the drum, the feeding tube and the second mounting plate according to the present invention;
FIG. 4 is a schematic cross-sectional view illustrating the connection relationship and the position relationship of the first polishing barrel, the second polishing barrel and the third material guiding plate according to the present invention;
FIG. 5 is an enlarged view of a portion A of FIG. 4;
FIG. 6 is a partial enlarged view of FIG. 4 at B;
FIG. 7 is an enlarged view of a portion of FIG. 4 at C;
FIG. 8 is a schematic view showing the connection and position of the shielding plate, the rack bar, the incomplete gear and the third pulley according to the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
the grinding device comprises a bottom plate 1, a first mounting plate 2, a first grinding cylinder 3, a second grinding cylinder 4, a feeding pipe 5, a discharging hole 6, a first guide plate 7, a plurality of feeding holes 8, a second guide plate 9, a third guide plate 10, a cylinder 101, an inclined plate 102, a guide hole 11, a first rotating wheel 12, a second rotating wheel 13, a belt 14, a motor 15, a fixing plate 16, a first filter plate 17, a second mounting plate 18, a rubber block 19, a first spring 20, a shielding plate 21, a second spring 22, a rack rod 23, an incomplete gear 24, a third rotating wheel 25, a buffer groove 26, a sealing plate 27, a third spring 28, a discharging hole 29, a second filter plate 30 and a collecting box 31.
Detailed Description
Referring to fig. 1-8, the present invention provides a technical solution: an improved method for preparing a nanocomposite thermoelectric material, the method comprising the steps of:
the method comprises the following steps: smelting the Cu, Se and La block raw materials into ingots by adopting induction smelting equipment;
step two: s powder weighed according to the chemical formula proportion and a broken ingot thermoelectric material are loaded into a ball milling device, and the ball milling device is used for milling the S powder and the ingot thermoelectric material;
step three: in the grinding process, the ball milling device can fully grind the substandard cast ingots and powder, and the substandard powder can be sent into a graphite die by the ball milling device;
step four: then placing the graphite mould loaded with the primary ball milling powder into a discharge plasma sintering cavity, and sintering the graphite mould into a block in a vacuum atmosphere;
step five: crushing the sintered block, and performing secondary ball milling in a nitrogen atmosphere; and then sintered under a vacuum atmosphere.
As a further scheme of the invention, the ball milling device comprises a bottom plate 1, two first mounting plates 2 are fixedly connected to the top of the bottom plate 1, a first grinding cylinder 3 and a second grinding cylinder 4 are arranged between the two first mounting plates 2, the second grinding cylinder 4 is positioned at the lower right part of the first grinding cylinder 3, a feeding pipe 5 is rotatably connected to the first grinding cylinder 3, the feeding pipe 5 is fixedly connected with the first mounting plate 2 at the front side, the second grinding cylinder 4 is rotatably connected with the first mounting plate 2, a driving assembly and a conveying assembly are arranged between the first grinding cylinder 3 and the second grinding cylinder 4, the driving assembly is used for driving the first grinding cylinder 3 and the second grinding cylinder 4 to synchronously rotate so as to drive the first grinding cylinder 3 and the second grinding cylinder 4 to grind the S powder and the cast ingot, the conveying assembly is used for conveying the powder after the primary grinding in the first grinding cylinder 3 to the second grinding cylinder 4 for grinding again.
The conveying assembly comprises a plurality of discharge holes 6, a plurality of feed holes 8 and a third material guide plate 10; the discharge holes 6 are arranged on the first grinding cylinder 3 in a circumferential array, and the side edges of the discharge holes 6 are provided with first material guide plates 7 fixedly connected to the inner wall of the first grinding cylinder 3; the plurality of feeding holes 8 are arranged on the second grinding cylinder 4 in a circumferential array, and the side edges of the feeding holes 8 are provided with second material guide plates 9 fixedly connected to the inner wall of the second grinding cylinder 4; the third material guide plate 10 consists of two cylinders 101 and an inclined plate 102; the two cylinders 101 are respectively sleeved on the first grinding cylinder 3 and the second grinding cylinder 4 and are positioned at the outer sides of the first grinding cylinder 3 and the second grinding cylinder 4, and the inclined plate 102 is used for fixedly connecting the two cylinders 101 together; the inclined plate 102 is provided with a material guide hole 11 which can be butted with the discharge hole 6 and the feed hole 8; the bottom of the cylinder 101 on the right side is provided with a discharge port 29, and a second filter plate 30 is fixedly connected in the discharge port 29.
When the scheme is put into practical use, firstly, S powder weighed according to the chemical formula proportion and a crushed cast ingot are loaded into a first grinding cylinder 3 from a feeding pipe 5, and then a driving assembly is started to drive the first grinding cylinder 3 and a second grinding cylinder 4 to synchronously rotate in the same direction; the first grinding cylinder 3 rotates, meanwhile, the first guide plate 7 can take steel balls loaded with different diameters in the first grinding cylinder 3, the first guide plate 7 can fall down after the steel balls move to a certain height, the steel balls can grind and crush S powder and crushed cast ingots, the S powder and the crushed cast ingots can be deposited at the bottom of the first grinding cylinder 3 after the cast ingots are crushed to a certain degree, the first guide plate 7 can drive the steel balls, the powder and the cast ingots to move upwards together while rotating, the powder and the cast ingots crushed to a certain degree can fall into the discharge hole 6, and when the discharge hole 6 rotates to be in butt joint with the guide hole 11, the powder and the cast ingots crushed to a certain degree in the discharge hole 6 can enter the guide hole 11; when the feeding hole 8 rotates to be in butt joint with the material guide hole 11, powder and cast ingots enter the feeding hole 8 along the material guide hole 11, and when the feeding hole 8 rotates to a certain angle, the powder and the cast ingots fall into the second grinding cylinder 4; the diameter of the largest steel ball in the second grinding cylinder 4 is far smaller than that of the largest steel ball in the first grinding cylinder 3; the powder and the cast ingot which are crushed to a certain degree are secondarily rolled by the steel balls in the second grinding cylinder 4, the size of the steel balls in the second grinding cylinder 4 is similar to the size of the powder and the cast ingot particles, and the steel balls are more easily collided with each other to roll the powder and the cast ingot, so that the powder and the cast ingot can be more quickly and better crushed; the completely ground powder in the second grinding cylinder 4 falls out from the discharge port 29 and the second filter plate 30, and then the completely ground powder can be collected; according to the invention, through the arrangement of the first grinding cylinder 3, the second grinding cylinder 4 and the conveying assembly, powder and particles ground to a certain degree in the first grinding cylinder 3 can be conveyed into the second grinding cylinder 4 by the conveying assembly, so that the powder and the particles ground to a certain degree can not obstruct the grinding of larger particles, the particles in the first grinding cylinder 3 can be crushed to a certain degree more quickly, the powder and the particles ground to a certain degree can be ground better and finer in the second grinding cylinder 4, the powder thoroughly ground in the second grinding cylinder 4 can automatically fall off, and the completely ground powder can be ensured not to obstruct the grinding of the particles; through setting up first grinding vessel 3 and second grinding vessel 4 to the grinding of different fineness, not only can the grinding speed of greatly increased granule, can also not need to grind the granule repeatedly, long time that can significantly reduce the granule and grind, efficiency that can greatly increased granule ground.
As a further aspect of the present invention, the driving assembly includes a first rotating wheel 12 and a second rotating wheel 13, the first rotating wheel 12 is fixedly connected to the rotating shaft of the first grinding cylinder 3, the second rotating wheel 13 is fixedly connected to the rotating shaft of the second grinding cylinder 4, the first rotating wheel 12 and the second rotating wheel 13 are in transmission connection through a belt 14, a motor 15 is disposed outside the second rotating wheel 13, the motor 15 is fixedly connected to the front first mounting plate 2, and an output shaft of the motor 15 is fixedly connected to the rotating shaft of the second grinding cylinder 4.
Above-mentioned drive assembly is at the actual work time, needs drive assembly to carry out the during operation, and the starter motor 15 earlier makes motor 15 drive second runner 13 rotate, and second runner 13 can drive the 4 anticlockwise rotations of second grinding vessel, and second runner 13 can drive first runner 12 synchronous rotations through belt 14, and first runner 12 can drive the 3 anticlockwise rotations of first grinding vessel.
As a further aspect of the present invention, a fixed plate 16 is fixedly connected to the first material guiding plate 7, a first filter plate 17 is rotatably connected to the fixed plate 16, the first filter plate 17 is disposed in an inclined manner, and the first filter plate 17, the fixed plate 16 and the first material guiding plate 7 shield the discharge hole 6 at the inner side thereof.
Consider that first stock guide 7 carries the steel ball and smashes to the ingot of certain degree after anticlockwise rotation to a take the altitude, the steel ball of major diameter can drive the part when falling downwards and smash the ingot of certain degree and fall first grinding vessel 3 once more in, can lead to smashing to the ingot of certain degree and need remove many times just can fall in second grinding vessel 4, above-mentioned problem is solved to above-mentioned scheme, and concrete working process is as follows: the first grinding cylinder 3 can drive the first material guide plate 7 to rotate while rotating, the first material guide plate 7 can drive the fixed plate 16 and the first filter plate 17 to rotate, at the moment, the first material guide plate 7 does not drive the steel balls, the powder and the particles to move upwards any more, and the first filter plate 17 can drive the steel balls, the powder and the particles to move upwards; the steel balls with large diameters cannot contact with the side wall of the first filter plate 17, and then powder and particles fall onto the first filter plate 17 from gaps among the steel balls and then fall into the discharge hole 6 from the first filter plate 17; according to the invention, through the arrangement of the fixed plate 16 and the first filter plate 17, the first filter plate 17 which is obliquely arranged can replace the first guide plate 7 to work, when the first filter plate 17 drives the steel ball to move upwards, the steel ball cannot be contacted with the side wall of the first filter plate 17, and the first filter plate 17 which is obliquely arranged can enable particles and powder which are crushed to a certain degree to better fall into the discharge hole 6, so that the possibility that the particles and the powder fall into the first grinding cylinder 3 again can be greatly reduced, the particles and the powder which are ground to a certain degree can rapidly move into the second grinding cylinder 4 for fine grinding, the grinding speed of the particles can be greatly increased, the grinding duration of the particles can be greatly reduced, and the grinding efficiency of the particles can be greatly increased.
As a further scheme of the present invention, the front side and the rear side of the first grinding cylinder 3 are both rotatably connected with a second mounting plate 18, and the second mounting plate 18 is located outside the first filter plate 17; rear side second mounting panel 18 and the first mounting panel 2 fixed connection of rear side, the front side second mounting panel 18 and 5 fixed connection of inlet pipe, second mounting panel 18 is close to rubber block 19 that a plurality of fixedly connected with was circumference array distribution on the lateral wall of first filter plate 17, and is a plurality of rubber block 19 is the sphere, rubber block 19 distributes in the right side below of second mounting panel 18, rubber block 19 can act on the vibrations of first filter plate 17, the first spring 20 of the common fixedly connected with of first filter plate 17 and fixed plate 16.
When the scheme is put into practical use, the second mounting plate 18 is in a static state when the first grinding cylinder 3 rotates, the first guide plate 7, the fixed plate 16 and the first filter plate 17 are driven by the first grinding cylinder 3 to rotate, the first filter plate 17 is in contact with the spherical rubber block 19, the spherical rubber block 19 drives the first filter plate 17 to vibrate, the vibrated first filter plate 17 can drive the small-diameter steel balls on the outer side of the first filter plate to vibrate together, particles staying among the small-diameter steel balls can fall under the action of vibration, then enter the discharge hole 6 from the first filter plate 17, and after the first filter plate 17 and the rubber block 19 are staggered, the first spring 20 can drive the first filter plate 17 to recover to the initial position and vibrate the first filter plate 17 again, so that the particles can fall better; according to the invention, through the arrangement of the second mounting plate 18, the rubber block 19 and the first spring 20, when the first filter plate 17 is driven by the first grinding cylinder 3 to rotate from the lowest point to the rightmost side, the rubber block 19 and the first spring 20 jointly act on the first filter plate 17, so that the first filter plate 17 vibrates, particles staying between the small-diameter steel balls can fall under the vibration effect of the first filter plate 17, and then enter the discharge hole 6 from the first filter plate 17, so that the particles can better and more quickly move into the second grinding cylinder 4 for fine grinding, the grinding speed of the particles can be greatly increased, the grinding time of the particles can be greatly reduced, and the grinding efficiency of the particles can be greatly increased.
As a further aspect of the present invention, a shielding plate 21 is slidably connected to the sloping plate 102, the shielding plate 21 is disposed obliquely with respect to the sloping plate 102, and a second spring 22 for resetting the shielding plate 21 is fixedly connected to the shielding plate 21; the shielding plate 21 is connected with the rack rod 23 through the fixed block fixedly, the rack rod 23 is connected with the outer wall of the inclined plate 102 in a sliding mode, the rack rod 23 is meshed with the incomplete gear 24, the third rotating wheel 25 is fixedly connected with the rotating shaft of the incomplete gear 24 and is connected with the first mounting plate 2 in a rotating mode, and the third rotating wheel 25 is connected with the belt 14 in a transmission mode.
When the scheme is put into practical use, the bottom of the inclined plate 102 needs to be set into a filter plate powder and particles which can filter completely crushed powder, and the filter plate powder and the particles can slide down along the inclined plate 102 to the lower right after falling into the material guide hole 11 from the material discharge hole 6, the qualified powder can fall down from the inclined plate 102, and when the particles impact the shielding plate 21, the shielding plate 21 can rebound the particles, so that the particles can shake off a small amount of completely crushed powder adhered to the particles, and then the powder can fall off from the filter plate at the bottom of the inclined plate 102; the second pulley 13 rotates and simultaneously drives the third pulley 25 to rotate through the belt 14. The third rotating wheel 25 can drive the incomplete gear 24 to rotate, when the incomplete gear 24 is meshed with the rack bar 23, the incomplete gear 24 can drive the rack bar 23 to move upwards, the rack bar 23 can drive the shielding plate 21 to move upwards synchronously, and then particles on the left side of the shielding plate 21 can enter the second grinding cylinder 4 from the material guide hole 11 to be ground; according to the invention, through the arrangement of the shielding plate 21, particles can enter the material guide hole 11 from the material outlet 6 and can stay in the material guide hole 11 for a short time, then thoroughly crushed powder can fall from the bottom of the inclined plate 102, and the particles can vibrate under the action of the shielding plate 21 when impacting the shielding plate 21, so that the particles can shake off the thoroughly crushed powder adhered to the particles, the thoroughly crushed powder amount in the second grinding cylinder 4 can be reduced, and the particles can be better crushed after entering the second grinding cylinder 4.
As a further aspect of the present invention, a buffer groove 26 is formed on the inclined plate 102, the shielding plate 21 is located in the buffer groove 26, a sealing plate 27 is disposed above the buffer groove 26, the sealing plate 27 is slidably connected to the inclined plate 102, the sealing plate 27 is slidably connected to the shielding plate 21, a third spring 28 is fixedly connected to a side wall of the sealing plate 27, and a right end of the third spring 28 is fixedly connected to the inclined plate 102; during operation, through the setting of buffer slot 26, can make shielding plate 21 slightly rock in buffer slot 26, can make the better effect that acts on of shielding plate 21 granule vibrations to through the setting of closing plate 27, can prevent that the granule from overflowing from buffer slot 26.
As a further scheme of the invention, a collecting box 31 is fixedly connected to the top of the bottom plate 1, and the collecting box 31 is positioned below the inclined plate 102 and the discharge hole 29; during operation, the powder after thorough crushing can be better collected through the arrangement of the collection box 31.
The working principle is as follows: firstly, S powder weighed according to the chemical formula proportion and a broken ingot are loaded into a first grinding cylinder 3 from a feeding pipe 5, and then a driving assembly is started to drive the first grinding cylinder 3 and a second grinding cylinder 4 to synchronously rotate in the same direction; the first grinding cylinder 3 rotates, meanwhile, the first guide plate 7 can take steel balls loaded with different diameters in the first grinding cylinder 3, the first guide plate 7 can fall down after the steel balls move to a certain height, the steel balls can grind and crush S powder and crushed cast ingots, the S powder and the crushed cast ingots can be deposited at the bottom of the first grinding cylinder 3 after the cast ingots are crushed to a certain degree, the first guide plate 7 can drive the steel balls, the powder and the cast ingots to move upwards together while rotating, the powder and the cast ingots crushed to a certain degree can fall into the discharge hole 6, and when the discharge hole 6 rotates to be in butt joint with the guide hole 11, the powder and the cast ingots crushed to a certain degree in the discharge hole 6 can enter the guide hole 11; when the feeding hole 8 rotates to be in butt joint with the material guide hole 11, powder and cast ingots enter the feeding hole 8 along the material guide hole 11, and when the feeding hole 8 rotates to a certain angle, the powder and the cast ingots fall into the second grinding cylinder 4; the diameter of the largest steel ball in the second grinding cylinder 4 is far smaller than that of the largest steel ball in the first grinding cylinder 3; the powder and the cast ingot which are crushed to a certain degree are secondarily rolled by the steel balls in the second grinding cylinder 4, the size of the steel balls in the second grinding cylinder 4 is similar to the size of the powder and the cast ingot particles, and the steel balls are more easily collided with each other to roll the powder and the cast ingot, so that the powder and the cast ingot can be more quickly and better crushed; the completely ground powder in the second grinding cylinder 4 falls out from the discharge port 29 and the second filter plate 30, and then the completely ground powder can be collected; according to the invention, through the arrangement of the first grinding cylinder 3, the second grinding cylinder 4 and the conveying assembly, powder and particles ground to a certain degree in the first grinding cylinder 3 can be conveyed into the second grinding cylinder 4 by the conveying assembly, so that the powder and the particles ground to a certain degree can not obstruct the grinding of larger particles, the particles in the first grinding cylinder 3 can be crushed to a certain degree more quickly, the powder and the particles ground to a certain degree can be ground better and finer in the second grinding cylinder 4, the powder thoroughly ground in the second grinding cylinder 4 can automatically fall off, and the completely ground powder can be ensured not to obstruct the grinding of the particles; through setting up first grinding vessel 3 and second grinding vessel 4 to the grinding of different fineness, not only can the grinding speed of greatly increased granule, can also not need to grind the granule repeatedly, long time that can significantly reduce the granule and grind, efficiency that can greatly increased granule ground.

Claims (8)

1. An improved method for preparing a nanocomposite thermoelectric material, the method comprising the steps of:
the method comprises the following steps: smelting the Cu, Se and La block raw materials into ingots by adopting induction smelting equipment;
step two: s powder weighed according to the chemical formula ratio and the ingot thermoelectric material crushed in the step one are loaded into a ball milling device, so that the ball milling device grinds the S powder and the ingot thermoelectric material;
step three: in the grinding process, the ball milling device can fully grind the substandard cast ingots and powder, and the substandard powder can be sent into a graphite die by the ball milling device;
step four: placing the graphite mould loaded with the primary ball milling powder into a discharge plasma sintering cavity, and sintering into a block in a vacuum atmosphere;
step five: crushing the sintered block, and performing secondary ball milling in a nitrogen atmosphere; then sintering under vacuum atmosphere; the ball milling device is characterized in that the ball milling device in the second step and the third step comprises a base plate (1), two first mounting plates (2) are fixedly connected to the top of the base plate (1), a first grinding cylinder (3) and a second grinding cylinder (4) are arranged between the two first mounting plates (2), the second grinding cylinder (4) is positioned at the lower right part of the first grinding cylinder (3), a feeding pipe (5) is rotatably connected to the first grinding cylinder (3), the feeding pipe (5) is fixedly connected with the first front-side mounting plate (2), the second grinding cylinder (4) is rotatably connected with the first mounting plate (2), a driving assembly and a conveying assembly are arranged between the first grinding cylinder (3) and the second grinding cylinder (4), and the driving assembly is used for driving the first grinding cylinder (3) and the second grinding cylinder (4) to synchronously rotate so as to drive the first grinding cylinder (3) and the second grinding cylinder (4) to grind S powder and cast ingots, the conveying assembly is used for conveying the powder after the primary grinding in the first grinding cylinder (3) to the second grinding cylinder (4) for grinding again.
2. The improved process of claim 1 for the preparation of a nanocomposite thermoelectric material, wherein: the conveying assembly comprises a plurality of discharge holes (6), a plurality of feed holes (8) and a third material guide plate (10); the discharge holes (6) are arranged on the first grinding cylinder (3) in a circumferential array, and the side edges of the discharge holes (6) are provided with first material guide plates (7) fixedly connected to the inner wall of the first grinding cylinder (3); the plurality of feeding holes (8) are arranged on the second grinding cylinder (4) in a circumferential array, and the side edges of the feeding holes (8) are provided with second material guide plates (9) fixedly connected to the inner wall of the second grinding cylinder (4); the third material guide plate (10) consists of two cylinders (101) and an inclined plate (102); the two cylinders (101) are respectively sleeved on the first grinding cylinder (3) and the second grinding cylinder (4) and are positioned at the outer sides of the first grinding cylinder (3) and the second grinding cylinder (4), and the inclined plate (102) is used for fixedly connecting the two cylinders (101) together; the inclined plate (102) is provided with a material guide hole (11) which can be butted with the discharge hole (6) and the feed hole (8); a discharge port (29) is formed in the bottom of the right cylinder (101), and a second filter plate (30) is fixedly connected in the discharge port (29).
3. The improved process of claim 2 for the preparation of a nanocomposite thermoelectric material, wherein: the drive assembly comprises a first rotating wheel (12) and a second rotating wheel (13), the first rotating wheel (12) is fixedly connected to the rotating shaft of the first grinding cylinder (3), the second rotating wheel (13) is fixedly connected to the rotating shaft of the second grinding cylinder (4), the first rotating wheel (12) and the second rotating wheel (13) are connected through a belt (14) in a transmission mode, a motor (15) is arranged on the outer side of the second rotating wheel (13), the motor (15) is fixedly connected to the first front-side mounting plate (2), and the output shaft of the motor (15) is fixedly connected to the rotating shaft of the second grinding cylinder (4).
4. The improved process of claim 3 for the preparation of a nanocomposite thermoelectric material, wherein: the material discharging device is characterized in that a fixing plate (16) is fixedly connected onto the first material guiding plate (7), a first filter plate (17) is rotatably connected onto the fixing plate (16), the first filter plate (17) is arranged in an inclined mode, and the first filter plate (17), the fixing plate (16) and the first material guiding plate (7) shield the material discharging hole (6) on the inner sides of the first filter plate, the fixing plate and the first material guiding plate.
5. The improved process of claim 4 for the preparation of a nanocomposite thermoelectric material, wherein: the front side and the rear side of the first grinding cylinder (3) are respectively and rotatably connected with a second mounting plate (18), and the second mounting plates (18) are positioned on the outer side of the first filter plate (17); rear side second mounting panel (18) and the first mounting panel of rear side (2) fixed connection, the front side second mounting panel (18) and inlet pipe (5) fixed connection, fixedly connected with a plurality of rubber block (19) that are the circumference array and distribute on second mounting panel (18) are close to the lateral wall of first filter plate (17), and is a plurality of rubber block (19) are the sphere, rubber block (19) distribute in the right side below of second mounting panel (18), rubber block (19) can act on first filter plate (17) vibrations, first filter plate (17) and the first spring (20) of the common fixedly connected with of fixed plate (16).
6. The improved process of claim 5 for the preparation of a nanocomposite thermoelectric material, wherein: a shielding plate (21) is connected onto the inclined plate (102) in a sliding manner, the shielding plate (21) is obliquely arranged relative to the inclined plate (102), and a second spring (22) for resetting the shielding plate (21) is fixedly connected with the shielding plate; shutter (21) are through fixed block fixedly connected with rack bar (23), rack bar (23) and swash plate (102) outer wall sliding connection, rack bar (23) meshing has incomplete gear (24), fixedly connected with third runner (25) in the axis of rotation of incomplete gear (24), third runner (25) rotate with first mounting panel (2) and are connected, third runner (25) are connected with belt (14) transmission.
7. The improved process of claim 6, wherein: the improved structure of the sealing plate is characterized in that a buffer groove (26) is formed in the inclined plate (102), the shielding plate (21) is located in the buffer groove (26), a sealing plate (27) is arranged above the buffer groove (26), the sealing plate (27) is in sliding connection with the inclined plate (102), the sealing plate (27) is in sliding connection with the shielding plate (21), a third spring (28) is fixedly connected to the side wall of the sealing plate (27), and the right end of the third spring (28) is fixedly connected with the inclined plate (102).
8. The improved process of claim 7 for the preparation of a nanocomposite thermoelectric material, wherein: the top of the bottom plate (1) is fixedly connected with a collecting box (31), and the collecting box (31) is positioned below the inclined plate (102) and the discharge hole (29).
CN202210013673.5A 2022-01-06 2022-01-06 Improved preparation method of nano composite thermoelectric material Pending CN114345524A (en)

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