CN114288962A - Device and method for synthesizing nano nitride powder by thermal plasma - Google Patents
Device and method for synthesizing nano nitride powder by thermal plasma Download PDFInfo
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 119
- 239000000843 powder Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 17
- 239000007769 metal material Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims description 35
- 239000002184 metal Substances 0.000 claims description 35
- 239000007789 gas Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 16
- 229910002601 GaN Inorganic materials 0.000 description 9
- 238000005245 sintering Methods 0.000 description 7
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 6
- 229910052581 Si3N4 Inorganic materials 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 238000005121 nitriding Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005261 decarburization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of thermal plasma application, and particularly relates to a device and a method for synthesizing nano nitride powder by thermal plasma, wherein the device comprises a nitride crucible, a metal material input port, a nitride steam outlet and a direct current arc thermal plasma torch, the top of the nitride crucible is provided with the metal material input port and the nitride steam outlet, an inner cavity of the nitride crucible is communicated with the metal material input port and the nitride steam outlet, and except the metal material input port and the nitride steam outlet, the top of the nitride crucible is closed; and a plurality of direct current arc plasma torches are uniformly arranged on the periphery of the nitride crucible. The invention effectively overcomes the technical bottleneck of the existing preparation process of the nitride powder material, and the nano nitride powder synthesized by the method has the advantages of average particle size below 200nm, spherical or linear appearance, high synthesis efficiency, low production cost and the like.
Description
Technical Field
The invention belongs to the technical field of thermal plasma application, and particularly relates to a device and a method for synthesizing nano nitride powder by thermal plasma.
Background
With the increasing development of high output of semiconductors, higher demands are being made on circuit boards for mounting semiconductors, and heat generated by dense circuits requires a board material having good heat conductivity, and at the same time, the substrate performance is also being required by the recent generation of semiconductor chips. The nitride ceramic material has excellent heat conducting performance, such as the theoretical value of the heat conductivity of the aluminum nitride is about 320W/m.K, and the nitride ceramic material is regarded as a new generation of electronic packaging material, is particularly suitable for packaging microwave vacuum tubes and hybrid power switches, and is an ideal substrate material for large-scale integrated circuit substrates. The nitride powder is the premise and key of excellent performance of the ceramic product, for example, the fine powder of AlN powder in the sintering process can enhance the sintering activity and the sintering driving force and accelerate the sintering process.
Research shows that when the particle size of AlN powder is 20 times fine, the sintering rate can be increased by 147 times, and for preventing secondary recrystallization, the particle size is also required to be fine and uniform, and if the particles are too large or unevenly distributed, abnormal growth or growth of crystal grains is easy to occur, so that dense sintering and the like are avoided, and therefore, the excellent performance of the nitride ceramic product (such as a high-power LED packaging heat dissipation substrate, a thin film printed circuit for an IGBT power module and the like) has a direct relation with the performance of the raw material powder.
At present, the preparation methods of high-performance nitride powder, such as carbothermic method, self-propagating high-temperature synthesis method, chemical vapor deposition method, sol-gel method and the like, have respective defects, and have the defects of high cost, uneven particle size and the like. Although the carbothermic method is easy to form and sinter, the synthesized powder needs secondary decarburization, the cost is high, the reaction speed of the self-propagating high-temperature synthesis and the sol-gel method is high, the cost is low, the particle size of the powder is difficult to control in the reaction process, the process of the chemical vapor deposition method is controllable, but the use of alkyl substances is expensive, and the industrial batch production is not facilitated.
Therefore, it is desired to develop a method for preparing synthetic high-performance nitride powder, which can effectively overcome the above-mentioned defects in the prior art.
Disclosure of Invention
The invention aims to provide a device and a method for synthesizing nano nitride powder by thermal plasma, which effectively overcome the technical bottleneck of the existing preparation process of nitride powder materials, and the nano nitride powder synthesized by the method has the characteristics of average particle size of below 200nm, spherical or linear shape, high synthesis efficiency, low production cost and the like.
The technical scheme for realizing the purpose of the invention is as follows:
a device for synthesizing nano nitride powder by thermal plasma comprises a nitride crucible, a metal material feeding port, a nitride steam outlet and a direct current arc thermal plasma torch, wherein the top of the nitride crucible is provided with the metal material feeding port and the nitride steam outlet; and a plurality of direct current arc plasma torches are uniformly arranged on the periphery of the nitride crucible.
The nitride crucible is a ceramic crucible prepared from a metal nitride ceramic to be synthesized.
A method of thermal plasma synthesis of a nano-nitride powder, the method comprising the steps of:
step 1, placing metal raw materials;
step 2, vacuumizing to perform bottom replacement of the inner cavity of the nitride crucible;
step 4, cooling the metal nitride steam after the metal and the nitrogen fully react;
step 5, carrying out particle size grading treatment on the metal nitride powder formed after condensation;
step 6, collecting and packaging the metal nitride powder subjected to grading treatment and separation;
and 7, turning off the whole plasma synthesis nitridation system.
The vacuum degree of the vacuum pumping in the step 2 is less than 3 multiplied by 10-3Pa。
The power of the plasma torch is adjusted to 70-90kW in the step 3.
In the step 3, both the plasma working gas and the protective gas are N2。
And the flow ratio of the plasma working gas to the protective gas in the step 3 is 1:1-3: 1.
The temperature for heating the metal material in the nitride crucible in the step 3 is 1200-1600 ℃.
The invention has the beneficial technical effects that:
1. the invention adopts a direct current arc plasma torch to synthesize the nano nitride powder in a thermal plasma mode, the thermal plasma has the characteristics of high temperature, high enthalpy and the like, and the central temperature of the plasma generated by the direct current arc reaches 104The catalyst has various active particles above the temperature, can provide high-temperature reaction atmosphere for most chemical reactions which are difficult to realize at normal temperature, has the characteristics of high reaction rate, complete reaction and the like, and has wide application prospect in the fields of plasma environmental protection, material preparation and the like.
2. The invention adopts the direct current arc thermal plasma torch technology to directly nitride metal powder or blocks to synthesize the nitride ceramic powder material, solves the problems of complex process, high cost and the like of the traditional nitride ceramic powder preparation process, has the characteristics of short process flow, thorough reaction and the like, and can realize high productivity and efficiency, low cost and continuous production on the premise of ensuring the performance of nitride.
The traditional methods for synthesizing nitride powder materials are more, but the problems of higher cost, secondary treatment of reaction products and the like exist mainly, for example, the powder synthesized by the carbothermic method needs secondary decarburization, the granularity of the self-propagating synthesis method and the sol-gel method is difficult to control in the reaction process, the process difficulty is high, expensive gas is needed in the reaction process of the chemical synthesis method, and the like, and the defects limit the large-scale popularization and application of the powder materials. By utilizing the high-temperature and high-enthalpy characteristics of the thermal plasma, metal powder (or blocks) is directly vaporized into metal steam under the high-temperature action of the plasma, and the metal steam reacts with nitrogen under the high-temperature action to be condensed to form nano nitride powder.
3. The nitride powder synthesized by the method has fine and uniform particle size distribution, has important significance for sintering molding and performance improvement of the nitride powder, and has the advantages of easy industrialization, low production cost and certain industrialization capability.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for synthesizing nitride nanopowder by thermal plasma according to the present invention;
in the figure: 1-a nitride crucible; 2-belongs to a material input port; a 3-nitride vapor outlet; 4-a direct current arc thermal plasma torch; 5-metal material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, the present invention provides an apparatus for synthesizing nano nitride powder by thermal plasma, comprising: nitride crucible 1, metal material input port 2, nitride steam outlet 3, and DC electric arc thermal plasma torch 4. The nitride crucible 1 is a ceramic crucible prepared from metal nitride ceramics to be synthesized, the top of the nitride crucible 1 is provided with a metal material input port 2 and a nitride steam outlet 3, and the top of the nitride crucible 1 is closed except the metal material input port 2 and the nitride steam outlet 3, so that the heat loss is reduced, and the reaction efficiency is improved; the nitride crucible 1 is provided with an inner cavity communicated with a metal material feeding port 2 and a nitride steam outlet 3 and is used for synthesizing nitride; the periphery of the nitride crucible 1 is uniformly provided with a plurality of direct current arc plasma torches for heating the metal material in the nitride crucible. The device and the method have the advantages of simple structure and process synthesis, high temperature and speed of plasma jet, high reaction speed of nitridation synthesis and the like.
Example 1
In this embodiment, nanometer aluminum nitride AlN is used as a nanometer nitride to synthesize nanometer aluminum nitride powder, which specifically includes the following steps:
step 1, placing metal raw materials
Aluminum powder with the particle size of 2-5 mu m is put into a crucible prepared from aluminum nitride through a metal material feeding port of the nitride crucible.
In the embodiment of the present invention, as shown in fig. 1, the plasma furnace crucible is made of an aluminum nitride crucible, and 3 100kW dc arc plasma torches are uniformly distributed around the aluminum nitride crucible.
Step 2, vacuumizing to perform bottom replacement of inner cavity of nitride crucible
After the aluminum powder material is put into the plasma synthetic nitridation system, all valves of the plasma synthetic nitridation system are closed, a vacuum pump group is opened, and the vacuum degree of the system is pumped to be less than 3 multiplied by 10-3Pa, to reach 2-3 × 10-3Pa is charged into the hearth2To atmospheric pressure, in order to remove oxygen from the cavity of the nitride crucible and to prevent the metal material from being oxidized during the nitriding process.
Respectively starting 3 direct current arc plasma torches, adjusting the power to 80kW, and using plasma working gas (N)2) And protective gas (N)2) The flow rates are respectively set to 5m3H and 2m3Heating the metal material in the nitride crucible to over 1400 ℃ to provide a high enough temperature for the nitridation reaction.
Step 4, cooling the metal nitride steam after the metal and the nitrogen fully react
Waiting for Al powder metal and N2After fully reacting for 10min, starting a vacuum pump set to introduce AlN steam generated by the reaction into a condenser for cooling.
Step 5, grading the particle size of the metal nitride powder formed after condensation
And sending the AlN powder formed after condensation into a cyclone separator for conventional cyclone separation particle size grading treatment so as to collect the nitride powder materials in different particle size ranges.
Step 6, collecting and packaging the metal nitride powder after grading treatment and separation
And collecting and packaging the AlN powder separated by the cyclone separator.
And 7, turning off the whole plasma synthesis nitridation system.
Example 2
This example uses nano Si3N4As a nano nitride, nano Si is carried out3N4The synthesis of the powder specifically comprises the following steps:
step 1, placing metal raw materials
Silicon powder with the granularity of 2-5 mu m is put into a crucible prepared from silicon nitride through a metal material feeding port of the nitride crucible.
In the embodiment of the present invention, as shown in fig. 1, the plasma furnace crucible is made of a silicon nitride crucible, and 3 100kW dc arc plasma torches are uniformly distributed around the silicon nitride crucible.
Step 2, vacuumizing to perform bottom replacement of inner cavity of nitride crucible
After the silicon powder material is put into the plasma synthetic nitridation system, all valves of the plasma synthetic nitridation system are closed, a vacuum pump set is opened, and the vacuum degree of the system is pumped to be less than 3 multiplied by 10-3Pa, to reach 2-3 × 10-3Pa is charged into the hearth2To atmospheric pressure, in order to remove oxygen from the cavity of the nitride crucible and to prevent the metal material from being oxidized during the nitriding process.
Respectively starting 3 direct current arc plasma torches, adjusting the power to 80kW, and using plasma working gas (N)2) And protective gas (N)2) Flow rates are respectively set to5m3H and 2m3Heating the metal material in the nitride crucible to over 1400 ℃ to provide a high enough temperature for the nitridation reaction.
Step 4, cooling the metal nitride steam after the metal and the nitrogen fully react
To be silicon powder metal and N2After fully reacting for 10min, starting a vacuum pump set to react generated Si3N4The steam is introduced into a condenser for cooling.
Step 5, grading the particle size of the metal nitride powder formed after condensation
For Si formed after condensation3N4The powder is sent into a cyclone separator to carry out conventional cyclone separation particle size classification treatment so as to collect the nitride powder materials in different particle size ranges.
Step 6, collecting and packaging the metal nitride powder after grading treatment and separation
For Si separated by a cyclone separator3N4And collecting and packaging the powder.
And 7, turning off the whole plasma synthesis nitridation system.
Example 3
In this embodiment, the synthesis of the nano GaN powder with nano GaN as the nano nitride specifically includes the following steps:
step 1, placing metal raw materials
Gallium powder with the granularity of 2-5 mu m is put into a crucible prepared from gallium nitride through a metal material feeding port of the nitride crucible.
In the present embodiment, as shown in fig. 1, the plasma furnace crucible used for synthesizing gallium nitride powder is made of a gallium nitride crucible, and 3 100kW dc arc plasma torches are uniformly distributed around the gallium nitride crucible.
Step 2, vacuumizing to perform bottom replacement of inner cavity of nitride crucible
After the gallium powder material is put into the plasma synthesis nitridation system, all valves of the plasma synthesis nitridation system are closed, a vacuum pump set is opened, and the vacuum degree of the plasma synthesis nitridation system is pumped to be less than 3 multiplied by 10-3Pa, to reach 2-3 × 10-3Pa is charged into the hearth2To atmospheric pressure, in order to remove oxygen from the cavity of the nitride crucible and to prevent the metal material from being oxidized during the nitriding process.
Respectively starting 3 direct current arc plasma torches, adjusting the power to 80kW, and using plasma working gas (N)2) And protective gas (N)2) The flow rates are respectively set to 5m3H and 2m3Heating the metal material in the nitride crucible to over 1400 ℃ to provide a high enough temperature for the nitridation reaction.
Step 4, cooling the metal nitride steam after the metal and the nitrogen fully react
Metal to be gallium powder and N2After the reaction is carried out for 10min, a vacuum pump set is started to introduce GaN steam generated by the reaction into a condenser for cooling.
Step 5, grading the particle size of the metal nitride powder formed after condensation
And feeding the condensed GaN powder into a cyclone separator for conventional cyclone separation particle size grading treatment so as to collect the nitride powder materials in different particle size ranges.
Step 6, collecting and packaging the metal nitride powder after grading treatment and separation
And collecting and packaging the GaN powder separated by the cyclone separator.
And 7, turning off the whole plasma synthesis nitridation system.
The particle size of the nano nitride powder prepared by the invention is in the nano particle size range, and the method comprises the following steps:
with the combination of the embodiments 1-3, the average particle size of the nano nitride powder prepared by the method of the present invention is less than 100nm, and the thermal plasma has the advantages of high temperature and enthalpy, fast plasma jet speed, fast reaction rate, etc.
The present invention has been described in detail with reference to the drawings and examples, but the present invention is not limited to the examples, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The prior art can be adopted in the content which is not described in detail in the invention.
Claims (8)
1. The device for synthesizing the nano nitride powder by the thermal plasma is characterized by comprising a nitride crucible (1), a metal material feeding port (2), a nitride steam outlet (3) and a direct-current arc thermal plasma torch (4), wherein the top of the nitride crucible (1) is provided with the metal material feeding port (2) and the nitride steam outlet (3), an inner cavity of the nitride crucible (1) is communicated with the metal material feeding port (2) and the nitride steam outlet (3), the metal material feeding port (2) and the nitride steam outlet (3) are removed, and the top of the nitride crucible (1) is closed; a plurality of direct current arc plasma torches are uniformly arranged on the periphery of the nitride crucible (1).
2. The apparatus for thermal plasma synthesis of nano-nitride powder according to claim 1, characterized in that the nitride crucible (1) is a ceramic crucible prepared from the metal nitride ceramic to be synthesized.
3. A method for synthesizing nano nitride powder by using thermal plasma, which is an apparatus for synthesizing nano nitride powder by using thermal plasma according to claim 1, comprising the following steps:
step 1, placing metal raw materials;
step 2, vacuumizing to perform bottom replacement of the inner cavity of the nitride crucible;
step 3, starting the direct current arc plasma torch to heat the metal material in the nitride crucible;
step 4, cooling the metal nitride steam after the metal and the nitrogen fully react;
step 5, carrying out particle size grading treatment on the metal nitride powder formed after condensation;
step 6, collecting and packaging the metal nitride powder subjected to grading treatment and separation;
and 7, turning off the whole plasma synthesis nitridation system.
4. The method for synthesizing nanometer nitride powder by using thermal plasma as claimed in claim 3, wherein the vacuum degree of the vacuum pumping in the step 2 is less than 3 x 10-3Pa。
5. A method for thermal plasma synthesis of nano nitride powder according to claim 3, characterized in that the power of the plasma torch is adjusted to 70-90kW in step 3.
6. The method for synthesizing nanometer nitride powder by using thermal plasma as claimed in claim 3, wherein the plasma working gas and the shielding gas in step 3 are both N2。
7. The method for synthesizing nano nitride powder by using thermal plasma as claimed in claim 3, wherein the flow ratio of the plasma working gas to the shielding gas in the step 3 is 1:1-3: 1.
8. The method as claimed in claim 3, wherein the temperature for heating the metal material in the nitride crucible in step 3 is 1200-1600 ℃.
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Application publication date: 20220408 |
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