CN112719276A - Preparation method of nanoscale tin powder - Google Patents

Preparation method of nanoscale tin powder Download PDF

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Publication number
CN112719276A
CN112719276A CN202011598342.XA CN202011598342A CN112719276A CN 112719276 A CN112719276 A CN 112719276A CN 202011598342 A CN202011598342 A CN 202011598342A CN 112719276 A CN112719276 A CN 112719276A
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China
Prior art keywords
tin
tin powder
cooling
powder
evaporation chamber
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CN202011598342.XA
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Chinese (zh)
Inventor
柴立新
汪艳春
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Jiangsu Boqian New Materials Co Ltd
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Jiangsu Boqian New Materials Co Ltd
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Priority to CN202011598342.XA priority Critical patent/CN112719276A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention discloses a preparation method of nano-grade tin powder, relating to the technical field of powder preparation, and the key point of the technical scheme comprises the following steps: step 1, filling a tin material into a tin melting furnace, vacuumizing an evaporation chamber to be less than or equal to 10kPa, introducing nitrogen, and controlling the pressure to be 110-120 kPa; step 2, pre-filling a tin material in the evaporation chamber, starting a plasma gun in the evaporation chamber to form a plasma arc, melting the tin material, and controlling the current of the plasma arc to be less than 500A and the voltage to be less than 140V; step 3, after the tin material is completely melted, adjusting the plasma arc current to 500-600A and the voltage to 140-160V until the melted tin material is evaporated; step 4, guiding the tin liquid in the tin melting furnace into an evaporation chamber, and controlling the liquid level height of the molten tin material to be stable; step 5, crystallizing and nucleating the evaporated tin material in a condensing tube, and then cooling the tin material in a cooling chamber to 40-60 ℃ to obtain a tin powder solution; and 6, separating the tin powder solution to obtain the tin powder. The invention has the effect of improving the quality of the nano tin powder.

Description

Preparation method of nanoscale tin powder
Technical Field
The application relates to the technical field of powder preparation, in particular to a method for preparing nanoscale tin powder.
Background
In conductive fillers such as micro-capacitive materials and electronic paste, metallic nickel powder is generally used. The metallic nickel powder generally comprises a matrix resin and conductive filler, i.e., conductive particles, as main components, and the conductive particles are bonded together by the bonding action of the matrix resin to form a conductive path, thereby realizing conductive connection of the bonded material. In the capacitor firing process, certain nano tin powder is added on the surfaces of metal and ceramic, so that the sintering temperature of powder metallurgy products and high-temperature ceramic products is greatly reduced, and the performance of the capacitor is improved.
At present, the tin powder preparation method mainly comprises an aerosol method, a water mist method, a centrifugal atomization method and the like.
The gas mist method is a method in which molten tin is impacted with high-pressure nitrogen gas to pulverize the molten tin into fine droplets, and the fine droplets are condensed into powder by contact with the nitrogen gas. Present tin powder gas atomization bucket, including the atomizing bucket, the top of atomizing bucket is equipped with the small bag that communicates with the atomizing bucket, and one side of atomizing bucket is equipped with the air pump, is connected with the trachea on the air pump, trachea and atomizing bucket intercommunication. When the tin melting tank is used, the heated tin melt in a molten state is injected into the atomizing barrel, and then high-pressure nitrogen is injected into the atomizing barrel, so that the tin melt forms fine liquid drops, and the tin melt is rapidly condensed through the nitrogen to form fine tin powder.
The centrifugal atomization method is to throw molten tin outwards by using the centrifugal force of a centrifugal barrel so that the molten tin forms a sphere in the air and forms tin powder after cooling.
Therefore, the liquid tin in the tin powder prepared by the aerosol method has different pressures at the center and the periphery of the atomizing barrel to form a pressure difference, so that tin powder particles are unevenly distributed after atomization, part of fine particles are adhered to form conjoined particles, and the surface of the powder has poor sphericity and dispersibility. Due to the pressure limitation of the high-pressure nitrogen, the grain diameter of the atomized tin powder is often more than 5 u. The centrifugal atomization method requires that tin melt needs to be condensed to form tin powder, so that the influence of the ambient temperature outside a centrifugal barrel on the tin powder in the forming process is large, and the quality of the prepared tin powder is uneven. And the grain diameter of the formed tin powder is often more than 5um, and the tin powder below 0.5u required by micro-capacitance is difficult to produce.
In conclusion, the existing tin powder preparation method has the problems of large particle size, uneven distribution and poor dispersibility of the obtained tin powder, and further influences the quality of the nano tin powder and needs to be improved.
Disclosure of Invention
In view of this, an object of the present application is to provide a method for preparing nano-tin powder, so as to achieve the purpose of significantly improving the quality of nano-tin powder. The specific scheme is as follows:
a method for preparing nano-grade tin powder comprises the steps of adopting a preparation device which is formed by sequentially connecting a tin melting furnace, a tin feeding pipe, an evaporation chamber, a condensation pipe, a cooling chamber, a gas-liquid separator and a settling tank, and obtaining the tin powder by a wet cooling method; the wet cooling method comprises the following steps:
step 1, filling a tin material into a tin melting furnace, vacuumizing an evaporation chamber to be less than or equal to 10kPa, introducing nitrogen, and controlling the pressure in a preparation device to be 110-120 kPa;
step 2, pre-filling a tin material in the evaporation chamber, starting a plasma gun in the evaporation chamber to form a plasma arc between the evaporation chamber and the tin material, so that the tin material is molten, and controlling the current of the plasma arc to be less than 500A and the voltage to be less than 140V;
step 3, after the tin material is completely melted, adjusting the plasma arc current to 500-600A and the voltage to 140-160V until the melted tin material is evaporated;
step 4, guiding the tin liquid in the tin melting furnace into an evaporation chamber, and controlling the liquid level height of the molten tin material to be stable;
step 5, after crystallizing and nucleating the evaporated tin material in a condensing tube, allowing the tin material to enter a cooling chamber through the condensing tube and cooling the tin material to 40-60 ℃ to obtain a tin powder solution;
and 6, separating the tin powder solution to obtain the tin powder.
Preferably: the settling tank is connected with a centrifugal pump, and one end of the centrifugal pump is connected with the cooling chamber; and the top of the cooling chamber is provided with a spray header connected with the centrifugal pump.
Preferably: and cooling liquid is introduced into the cooling chamber, and the cooling liquid is deionized water.
Preferably: and an oxygen concentration adjusting unit is arranged in the condensing pipe.
Preferably: the preparation device is internally sealed integrally and is provided with nitrogen.
Preferably: and heating and melting the tin material in the tin melting furnace.
Preferably: the tin powder is spherical and has a particle size of 30-1500 nm.
Preferably: the oxygen content of the tin powder is 0.5-20%.
According to the scheme, the application provides the preparation method of the nano-grade tin powder, and the preparation method of the nano-grade tin powder has the following beneficial effects:
1. the growth speed of tin powder particles is controlled by adjusting the air flow, so that the tin powder with the particle size of 30-1500nm is effectively obtained.
2. The operability is improved by controlling the oxygen concentration of the condensation pipe, and the oxygen content of the tin powder is effectively controlled to be 0.5-20%.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a nano-scale tin powder preparation apparatus disclosed in the present application.
Description of reference numerals: 1. a tin melting furnace; 2. feeding a tin tube; 3. an evaporation chamber; 4. a condenser tube; 5. a shower head; 6. a cooling chamber; 7. a settling tank; 8. a centrifugal pump; 9. a vapor-liquid separator.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The following is a detailed description of the method for preparing nano-sized tin powder according to the embodiment of the present invention:
as shown in fig. 1, a nano-grade tin powder preparation device comprises a tin melting furnace 1, a tin feeding pipe 2, an evaporation chamber 3, a condensation pipe 4, a cooling chamber 6, a gas-liquid separator and a settling tank 7 which are connected in sequence.
Wherein, the tin melting furnace 1 is used for heating and melting metallic tin materials; the tin feeding pipe 2 guides the molten tin material in the tin melting furnace 1 into a crucible of the evaporation chamber 3; the condenser tube 4 is used for crystallization and nucleation of the evaporated tin material; the cooling chamber 6 is used for cooling and obtaining tin powder; the gas-liquid separator plays a role in effectively separating gas and solution containing tin powder; and after the solution is led into the settling tank 7, the tin powder can be primarily separated from the solution through settling separation. It should be mentioned that a centrifugal pump 8 is connected to the bottom of the settler 7. One end of the centrifugal pump 8 is connected with the cooling chamber 6, and the spray header 5 connected with the centrifugal pump 8 is arranged at the top of the cooling chamber 6, so that cooling liquid is guided into the cooling chamber 6 through the centrifugal pump 8 under the action of the spray header 5, and an effective cooling circulation effect is achieved. It should be noted that the cooling liquid is deionized water, so as to effectively avoid the influence of metal ions and non-metal ions on the preparation quality of the tin powder. And the preparation device is internally sealed integrally and is provided with nitrogen as protective gas so as to achieve the purpose of preventing tin powder from being oxidized in the preparation process. Meanwhile, an oxygen concentration adjusting unit is provided in the condensation duct 4. The oxygen concentration adjusting unit can improve the operability while adjusting the oxygen concentration of the gas entering the condensing pipe 4, and can effectively control the oxygen content of the tin powder to be 0.5-20%.
A nanometer tin powder preparation method, through adopting by melting the tin stove 1, send the tin tube 2, the evaporation chamber 3, the condenser pipe 4, the cooling chamber 6, the vapour-liquid separator and preparation facilities that the settling tank 7 connects sequentially, get the tin powder with the method of wet cooling; the wet cooling method comprises the following steps:
step 1, filling a tin material into a tin melting furnace 1, vacuumizing an evaporation chamber 3 to be less than or equal to 10kPa, introducing nitrogen, and controlling the pressure in a preparation device to be 110-120 kPa;
step 2, pre-filling tin materials in the evaporation chamber 3, starting a plasma gun in the evaporation chamber 3 to form a plasma arc between the tin materials, melting the tin materials, and controlling the current of the plasma arc to be less than 500A and the voltage to be less than 140V;
step 3, after the tin material is completely melted, adjusting the plasma arc current to 500-600A and the voltage to 140-160V until the melted tin material is evaporated;
step 4, guiding the tin liquid in the tin melting furnace 1 into the evaporation chamber 3, and controlling the liquid level height of the molten tin material to be stable;
step 5, after the evaporated tin material is crystallized and nucleated in the condensing tube 4, the evaporated tin material enters the cooling chamber 6 through the condensing tube 4 to be cooled to 40-60 ℃ to obtain a tin powder solution;
and 6, separating the tin powder solution to obtain the tin powder.
It is to be mentioned that the tin powder obtained is spherical and has a particle size of 30-1500 nm; wherein the oxygen content of the tin powder is controllable and is 0.5-20%.
Example one
As shown in fig. 1, a nano-grade tin powder preparation device comprises a tin melting furnace 1, a tin feeding pipe 2, an evaporation chamber 3, a condensation pipe 4, a cooling chamber 6, a gas-liquid separator and a settling tank 7 which are connected in sequence.
Wherein, the tin melting furnace 1 is used for heating and melting metallic tin materials; the tin feeding pipe 2 guides the molten tin material in the tin melting furnace 1 into a crucible of the evaporation chamber 3; the condenser tube 4 is used for crystallization and nucleation of the evaporated tin material; the cooling chamber 6 is used for cooling and obtaining tin powder; the gas-liquid separator plays a role in effectively separating gas and solution containing tin powder; and after the solution is led into the settling tank 7, the tin powder can be primarily separated from the solution through settling separation. It should be mentioned that a centrifugal pump 8 is connected to the bottom of the settler 7. One end of the centrifugal pump 8 is connected with the cooling chamber 6, and the spray header 5 connected with the centrifugal pump 8 is arranged at the top of the cooling chamber 6, so that cooling liquid is guided into the cooling chamber 6 through the centrifugal pump 8 under the action of the spray header 5, and an effective cooling circulation effect is achieved. It should be noted that the cooling liquid is deionized water, so as to effectively avoid the influence of metal ions and non-metal ions on the preparation quality of the tin powder. And the preparation device is internally sealed integrally and is provided with nitrogen as protective gas so as to achieve the purpose of preventing tin powder from being oxidized in the preparation process. Meanwhile, an oxygen concentration adjusting unit is provided in the condensation duct 4. The oxygen concentration adjusting unit can improve the operability while adjusting the oxygen concentration of the gas entering the condensation pipe 4, and the purpose of effectively controlling the oxygen content of the tin powder at 0.5% is achieved.
A nanometer tin powder preparation method, through adopting by melting the tin stove 1, send the tin tube 2, the evaporation chamber 3, the condenser pipe 4, the cooling chamber 6, the vapour-liquid separator and preparation facilities that the settling tank 7 connects sequentially, get the tin powder with the method of wet cooling; the wet cooling method comprises the following steps:
step 1, filling a tin material into a tin melting furnace 1, vacuumizing an evaporation chamber 3 to be less than or equal to 10kPa, introducing nitrogen, and controlling the pressure in a preparation device to be 110 kPa;
step 2, pre-filling tin materials in the evaporation chamber 3, starting a plasma gun in the evaporation chamber 3 to form a plasma arc between the plasma gun and the tin materials, melting the tin materials, and controlling the current of the plasma arc to be 250A and the voltage to be 80V;
step 3, after the tin material is completely melted, adjusting the plasma arc current to 500A and the voltage to 140V until the melted tin material is evaporated;
step 4, guiding the tin liquid in the tin melting furnace 1 into the evaporation chamber 3, and controlling the liquid level height of the molten tin material to be stable;
step 5, after the evaporated tin material is crystallized and nucleated in the condensing tube 4, the evaporated tin material enters the cooling chamber 6 through the condensing tube 4 to be cooled to 40-60 ℃ to obtain a tin powder solution;
and 6, separating the tin powder solution to obtain the tin powder.
It is to be mentioned that the tin powder obtained is spherical and has a particle size of 30-1500 nm; wherein the oxygen content of the tin powder is controllable and is 0.5 percent.
Example two
The difference between the second example and the first example is that the pressure in the production apparatus in the second example was 115 kPa.
EXAMPLE III
The difference between the third example and the first example is that the pressure in the production apparatus in the third example was 120 kPa.
Example four
The difference between the fourth embodiment and the first embodiment is that in the step 2 of the fourth embodiment, the plasma arc current is 300A and the voltage is 60V.
EXAMPLE five
The difference between the fifth embodiment and the first embodiment is that in the step 2 of the fifth embodiment, the plasma arc current is 400A and the voltage is 120V.
EXAMPLE six
The difference between the sixth embodiment and the first embodiment is that in step 2 of the sixth embodiment, the plasma arc current is 550A and the voltage is 150V.
EXAMPLE seven
The difference between the seventh embodiment and the first embodiment is that in the step 2 of the seventh embodiment, the plasma arc current is 600A and the voltage is 160V.
Example eight
The difference between the eighth embodiment and the first embodiment is that the oxygen content of the tin powder in the eighth embodiment is controllable and 10%.
Example nine
The difference between the ninth embodiment and the first embodiment is that the oxygen content of the tin powder in the ninth embodiment is controllable and is 20%.
In conclusion, the growth speed of tin powder particles is controlled by adjusting the gas flow, so that the tin powder with the particle size of 30-1500nm is effectively obtained; meanwhile, operability is improved through oxygen concentration controllability of the condensation pipe 4, and the oxygen content of the tin powder is effectively controlled to be 0.5-20%. Therefore, the obtained tin powder has a high quality effect.
References in this application to "first," "second," "third," "fourth," etc., if any, are intended to distinguish between similar elements and not necessarily to describe a particular order or sequence. It will be appreciated that the data so used may be interchanged under appropriate circumstances such that the embodiments described herein may be practiced otherwise than as specifically illustrated or described herein. Furthermore, the terms "comprises" and "comprising," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, or apparatus.
It should be noted that the descriptions in this application referring to "first", "second", etc. are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present application.
The principle and the implementation of the present application are explained herein by applying specific examples, and the above description of the embodiments is only used to help understand the method and the core idea of the present application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (8)

1. A preparation method of nano-grade tin powder is characterized in that the tin powder is obtained by a wet cooling method by adopting a preparation device which is formed by sequentially connecting a tin melting furnace, a tin conveying pipe, an evaporation chamber, a condensation pipe, a cooling chamber, a gas-liquid separator and a settling tank; the wet cooling method comprises the following steps:
step 1, filling a tin material into a tin melting furnace, vacuumizing an evaporation chamber to be less than or equal to 10kPa, introducing nitrogen, and controlling the pressure in a preparation device to be 110-120 kPa;
step 2, pre-filling a tin material in the evaporation chamber, starting a plasma gun in the evaporation chamber to form a plasma arc between the evaporation chamber and the tin material, so that the tin material is molten, and controlling the current of the plasma arc to be less than 500A and the voltage to be less than 140V;
step 3, after the tin material is completely melted, adjusting the plasma arc current to 500-600A and the voltage to 140-160V until the melted tin material is evaporated;
step 4, guiding the tin liquid in the tin melting furnace into an evaporation chamber, and controlling the liquid level height of the molten tin material to be stable;
step 5, after crystallizing and nucleating the evaporated tin material in a condensing tube, allowing the tin material to enter a cooling chamber through the condensing tube and cooling the tin material to 40-60 ℃ to obtain a tin powder solution;
and 6, separating the tin powder solution to obtain the tin powder.
2. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: the settling tank is connected with a centrifugal pump, and one end of the centrifugal pump is connected with the cooling chamber; and the top of the cooling chamber is provided with a spray header connected with the centrifugal pump.
3. The method for preparing nano-sized tin powder according to claim 2, wherein the method comprises the following steps: and cooling liquid is introduced into the cooling chamber, and the cooling liquid is deionized water.
4. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: and an oxygen concentration adjusting unit is arranged in the condensing pipe.
5. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: the preparation device is internally sealed integrally and is provided with nitrogen.
6. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: and heating and melting the tin material in the tin melting furnace.
7. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: the tin powder is spherical and has a particle size of 30-1500 nm.
8. The method for preparing nano-sized tin powder according to claim 1, wherein the method comprises the following steps: the oxygen content of the tin powder is 0.5-20%.
CN202011598342.XA 2020-12-29 2020-12-29 Preparation method of nanoscale tin powder Pending CN112719276A (en)

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