CN207435028U - The preparation system of the plasma-activated quick-fried synthesis nitridation aluminum nanopowder of nitrogen source zygomite - Google Patents
The preparation system of the plasma-activated quick-fried synthesis nitridation aluminum nanopowder of nitrogen source zygomite Download PDFInfo
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- CN207435028U CN207435028U CN201721149026.8U CN201721149026U CN207435028U CN 207435028 U CN207435028 U CN 207435028U CN 201721149026 U CN201721149026 U CN 201721149026U CN 207435028 U CN207435028 U CN 207435028U
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Abstract
The utility model discloses a kind of preparation system of the plasma-activated quick-fried synthesis nitridation aluminum nanopowder of nitrogen source zygomite, including plasma-activated device, high voltage power supply, discharge electrode, reactor and particulate cascade retracting device.The activation of the utility model using plasma is directly synthesized with reference to electric detonation method, electric energy is converted into reaction energy, process safety is nontoxic, pollution-free product withdraw, easy to operate, can quickly and efficiently produce at any time.The methods of compared to traditional carbothermic method, vapor phase method, organic salt cracking, the utility model reaction process less more directly, reduces the generation of consumption of raw materials and by-product, more economical environmental protection；Compared to existing method, the utility model due in reaction process environment it is pure, the oxygen content of product is low, more reduces the introducing of impurity metal components, can obtain high-purity, low oxygen content high-quality powder.
Description
Technical field
The utility model belongs to technical field of material, and in particular to a kind of plasma-activated quick-fried conjunction of nitrogen source zygomite
Into the preparation system of aluminum nitride nanometer powder.
Background technology
Aluminium nitride (AlN) ceramics have thermal conductivity height, coefficient of thermal expansion is small, dielectric constant is low, intensity in ceramic material
The advantages of high, chemical property is stablized is generally acknowledged high density, the preferable material of high-power and high speed integrated electrical base board and encapsulation
Material, has a bright future in fields such as national defence aviation, communication, electronic components.And the preparation process and practical performance of AlN ceramic material
It is directly affected be subject to powder characteristics, to obtain high performance AlN ceramic, it is necessary to have the powder that purity is high, sintering activity is good
As raw material.
AlN ceramic is very sensitive to metal impurities and oxygen impurities, will containing metals such as Si, Fe, the Mg for having more than 0.02%
Reduce the thermal conductivity and insulation performance of AlN.Oxygen impurities in powder influence maximum to thermal conductivity, and impurity oxygen is (with Al2O3Form)
AlN lattices (be dissolved oxygen presence) are diffused under high temperature and reduce thermal conductivity.
The manufacturing process high energy consumption of existing aluminium nitride powder, of high cost, therefore the application of aluminium nitride ceramics is also limited
System.Therefore, how with relatively low cost and the technique stablized the uniform superfine powder of high-purity, low oxygen content, dynamics is prepared,
It is a key link of the excellent AlN ceramic of processability.
The synthetic method of AlN powders has very much, and most study has 5 kinds at present：Aluminium powder direct nitridation method, self-propagating high-temperature
Method, carbothermic method, vapor phase method, organic salt cracking process etc..
Al powder is heated reaction by traditional aluminium powder direct nitridation method in nitrogen, and not only production cost is high, but also is nitrogenized
Aluminium powder purity is low, product easily lumps, it is incomplete to react, it is difficult to epigranular, high-purity, fine-grained powder are made, it can not
Meet the requirement for preparing high-performance AlN ceramic to raw material powder, be gradually eliminated.
Pulse Power Techniques are to be compressed energy on room and time, and substantial amounts of energy is discharged within the extremely short time
Amount, to generate specific physically or chemically effect.Using Pulse Power Techniques, the high current generated using moment makes aluminium wire moment
Gasification, with the nitrogen source haptoreaction after plasma-activated, being condensed into the silk explosion technique of particle rapidly becomes a kind of feasible
Direct-Nitridation new approaches.
The content of the invention
In view of above-mentioned, the utility model provides a kind of quick-fried synthesis nitridation aluminum nano of plasma-activated nitrogen source zygomite
The preparation system of body, not only environmental friendliness and no harm, and can reduce reaction step, reduces cost, prepares the low granularity of high-purity
AlN powder.
A kind of preparation system of the quick-fried synthesis nitridation aluminum nanopowder of plasma-activated nitrogen source zygomite, including plasma
Activate device, high voltage power supply, discharge electrode, reactor and particulate cascade retracting device；Wherein：
The plasma-activated device is connected by gas circuit with reactor, is used to carry out discharge treatment to nitrogen source, be made
Its ionization is passed through after activating into the nitrogen plasma containing active particle in reactor；
The high voltage power supply is loaded onto the microsecond or ns high voltage pulse at discharge electrode both ends for generating；
The discharge electrode is arranged in reactor, is used in the short time for Pulsed current injection to be located at the aluminium among electrode
Silk is vaporized, and the aluminium steam formed after gasification chemically reacts in the reactor with nitrogen plasma, and is rapidly condensed into
The nano-powder of aluminium nitride；
The particulate cascade retracting device is arranged in reactor the nano powder for before gas outlet, being used to collect aluminium nitride
Body, gas outlet are connected with air pump by gas circuit, and for emptying the foreign gas in reactor as early as possible, providing suitable air pressure will
It asks；
The reactor is used to providing the reaction compartment of proper air pressure, the rate and free path of control product condensation so as to
Control diameter of particle.
Further, the discharge electrode is aluminum electrode, to avoid incorporation foreign metal.
Further, it is equipped in the reactor automatically into silk device, is used for motor cooperation periodically by aluminium wire
It send to electrode, continues aluminium wire to be sent into electric field after ensureing each electric detonation reaction so that once taking out deflation course can be in a steady stream
Constantly electric detonation aluminium wire improves production efficiency.
Further, air distributor is equipped in the reactor around discharge electrode, is used to adjusting air-flow and causes silk
Quick-fried scope interior air-flow is uniformly distributed, and aluminium wire is made to come into full contact with to react with nitrogen plasma.
Further, the high voltage power supply uses nanosecond pulse power supply or microsecond pulse power supply, and electric voltage frequency is adjustable, with
Meet the requirement of energy sedimentation rate.
Further, the aluminium wire is high-purity aluminium wire, diameter ＜ 1mm and Al content >=99%.
Further, the nitrogen source is nitrogen, ammonia or nitrogen ammonia gaseous mixture.
Further, the ambient pressure in the reactor can be less than, greater than or equal to standard atmospheric pressure；Preferably,
Ambient pressure≤1 standard atmospheric pressure, it is safer compared to hyperbaric environment.
Compared with prior art, the advantageous effects of the utility model are as follows：
(1) the utility model using plasma activation quick-fried direct synthesis technique of nitrogen source zygomite, compared to traditional carbon heat also
The methods of former method, vapor phase method, organic salt cracking, reaction process less more directly, reduces the life of consumption of raw materials and by-product
Into more economical environmental protection；Compared to existing method, the utility model due in reaction process environment it is pure, the oxygen content of product is low,
More reduce the introducing of impurity metal components, high-purity, low oxygen content high-quality powder can be obtained.
(2) the utility model uses discharge-induced explosion method, electric energy is converted into reaction energy, process safety is nontoxic, no dirt
Product withdraw is contaminated, it is easy to operate, it can quickly and efficiently produce at any time.
(3) the utility model using plasma technology activation nitrogen source, aluminium nitride is effectively increased compared to traditional blasting
The conversion ratio of synthesis improves the accounting of aluminium nitride powder in product.
(4) the utility model is using continuously into the method for silk, compared to the method for a fixed electric detonation of filament length, electric detonation process can
To recur at intervals, production efficiency is improved, has saved cost, more economically practicality.
Description of the drawings
Fig. 1 is the structure diagram of 1 nano-powder preparation system of the utility model embodiment, wherein：1-high-voltage charging electricity
Source, 2-charging capacitor, 3-pulse switch, 4-discharge electrode, 5-aluminium wire, 6-automatically into silk device, 7-air distributor,
8-reactor, 9-air distributing device, 10-plasma-activated device, 11-vacuum seal, the recycling of 12-particulate cascade
Device, 13-vacuum seal, 14-air pump.
Fig. 2 is the structure diagram of 2 nano-powder preparation system of the utility model embodiment, wherein：1-high-voltage charging electricity
Source, 2-charging capacitor, 3-Low ESR are artificially formed line, 4-discharge electrode, 5-aluminium wire, 6-automatically into silk device, 7-gas
Flow distributor, 8-reactor, 9-air distributing device, 10-plasma-activated device, 11-vacuum seal, 12-particulate matter
It is classified retracting device, 13-vacuum seal, 14-air pump.
Fig. 3 is the structure diagram of 3 nano-powder preparation system of the utility model embodiment, wherein：1-high-voltage charging electricity
Source, 2-charging capacitor, 3-pulse-forming line, 4-discharge electrode, 5-aluminium wire, 6-automatically into silk device, 7-air flow method
Device, 8-reactor, 9-air distributing device, 10-plasma-activated device, 11-vacuum seal, 12-particulate cascade return
Receiving apparatus, 13-vacuum seal, 14-air pump.
Specific embodiment
In order to more specifically describe the utility model, below in conjunction with the accompanying drawings and specific embodiment is to the utility model
Technical solution is described in detail.
Embodiment 1：
As shown in Figure 1, the quick-fried directly synthesis nitridation aluminum nanopowder of the plasma-activated nitrogen source zygomite of the utility model
Preparation system, including distribution and plasma-activated unit, pulse energy input unit, vacuum continuous sample introduction reaction member and
Grain object stage unit；Wherein：
DC high-voltage is converted to DC pulse signal by pulse energy input unit, is added to 4 both ends of discharge electrode；Centainly
Length, the aluminium wire 5 of diameter are located among electrode, and when pulse switch 3 is connected, charging capacitor 2 starts to discharge, big electricity in the short time
Stream flows into aluminium wire 5, when energy input gasifies required energy more than aluminium wire 5,5 Quick-gasifying of aluminium wire；High temperature aluminum after gasification
Steam runs into the nitrogen, ammonia or the N being ionized of activation in reactor 8+、N*It is fast after chemically reacting during isoreactivity particle
Nanoparticle is formed in rapid hardening, and collected by particulate cascade retracting device 12, product main component is aluminium nitride and aluminum nano
Body.
Pulse energy input unit includes high voltage charging power supply 1, charging capacitor 2, pulse switch 3 and discharge electrode 4；It puts
Electrode 4 is aluminum, is placed in reactor 8, is insulated with 8 interface of reactor using insulator, and need to ensure that device is airtight
Property is good；Pulse switch 3 can be used but be not limited to gas switch, semiconductor switch, frequency-adjustable；High voltage charging power supply 1 can be adopted
With DC sources such as high-voltage DC power supply, constant-current supply or high frequency switch powers；Supply line requires as far as possible small loop inductance, and
There is larger capacitance to improve yield obtained by impulse discharge, entire circuit connection is preferably rationally distributed, reduces stray electrical as far as possible
Sense and stray resistance.
Vacuum continuous sample introduction reaction member is included automatically into silk device 6, air distributor 7, reactor 8, vacuum seal
11＆13 and air pump 14；The system provides place, suitable air pressure and atmosphere for the quick-fried reaction of silk；Automatically into silk device 6 periodically
Ground wire feed improves production efficiency between discharge electrode 4, realizing that single extraction gas continuous fibers are quick-fried；Air distributor 7 ensures silk
Quick-fried scope interior air-flow is uniformly distributed, and the nitrogen plasma after aluminium wire 5 and activation is made to come into full contact with to react；Air pump 14 can be used but
Mechanical pump and molecular pump are not limited to, meets and empties foreign gas, the requirement that suitable air pressure is provided as early as possible, remove the impurity such as oxygen
Gas obtains pure nano-powder.
Distribution and plasma-activated unit include air distributing device 9 and plasma-activated device 10；Wherein air distributing device 9
It can be used but be not limited to cyclinder gas mixing, each component gas content is adjustable；Plasma-activated device 10 is to the raw material of proportioning
Gas carries out discharge treatment, and gas is ionized activation into the nitrogen plasma containing active particle, is injected into the quick-fried space of silk, completely
Wrap up aluminium wire 5, the high temperature aluminum steam reaction with the quick-fried generation of silk.
It is solidifying properly to collect apart from the suitable distance in the quick-fried space of silk positioned at the particulate cascade unit of 8 inner wall of reactor
Poly- nano-powder, and the loss of product powder is avoided, exporting front end in reactor 8 sets particulate cascade retracting device
12, for collecting the powders such as the airborne dust taken up by air-flow, the blocking aging of air pump 14 is avoided while improving yield；Particulate matter point
Grade retracting device 12 can be used but be not limited to molecular sieve filter, electric precipitation etc..
When preparing nano-powder, between aluminium wire 5 first is positioned over discharge electrode 4, particulate cascade retracting device 12 has been debugged
Position.8 import of reactor is closed, and device air pressure is down to 1 × 10 by air pump 142Below Pa is then shut off exporting.Again will
The unstripped gas (nitrogen, ammonia or its gaseous mixture) that air distributing device 9 configures is passed through plasma-activated device 10 and is activated.It beats
8 air inlet of reactor is opened, the nitrogen plasma after activation spurts into reactor 8, and import is closed when rising to suitable air pressure.It opens
High voltage charging power supply 1, while start automatically into silk device 6, particulate cascade retracting device 12 starts to receive product；It relates in the process
And the reaction arrived is as follows：
Al→Al*
N2→2N
Al*+N→AlN
Al*+NH2 *→AlN+H*
It waits after the completion of reacting, is passed through protection gas to standard atmospheric pressure, opens reactor 8, take out product；Continuing production only needs
Aluminium wire 5 is loaded, repeats above step.
Embodiment 2：
As shown in Fig. 2, system still inputs list by distribution and plasma-activated unit, pulse energy in the embodiment
Member, vacuum continuous sample introduction reaction member and four part of particulate cascade unit are formed.
Pulse current formation is artificially formed line 3 by charging capacitor 2 and Low ESR and forms in present embodiment, and charging can be with one
Straight row makes circuit be in charged state.When preparing powder, unstripped gas is sent into reaction by air distributing device 9 according to certain proportioning
In device 8 in-situ activation or through plasma-activated device 10 carry out discharge treatment after spurt into reactor 8；Aluminium wire 5 is by automatic
It is automatically fed into silk device 6, reaches gap discharge during apart from 4 a certain distance of discharge electrode, it can while playing on-off action
To activate nitrogen source, switch is eliminated.
Embodiment 3：
As shown in figure 3, system still inputs list by distribution and plasma-activated unit, pulse energy in the embodiment
Member, vacuum continuous sample introduction reaction member and four part of particulate cascade unit are formed.
Pulse forming unit is that the artificial form wire formed on conductor is arranged in by multiple capacitance profiles in present embodiment,
The adoptable dielectric of the pulse-forming line can be but be not limited to sky gas and water, oil and ceramics etc..When preparing powder, raw material
Gas is put by air distributing device 9 according to in-situ activation in certain proportioning feeding reactor 8 or through plasma-activated device 10
It is spurted into after electric treatment in reactor 8；Aluminium wire 5 is automatically fed by automatic wire feeding device 6, is reached certain apart from discharge electrode 4
Distance Time gap is discharged, and nitrogen source can be activated while playing on-off action, eliminates switch.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this practicality
It is new.Person skilled in the art obviously can easily make above-described embodiment various modifications, and illustrating herein
General Principle be applied in other embodiment without having to go through creative labor.Therefore, the utility model is not limited to above-mentioned
Embodiment, those skilled in the art's announcement according to the present utility model, the improvement made for the utility model and modification all should
It should be within the scope of protection of the utility model.
Claims (8)
- A kind of 1. preparation system of the quick-fried synthesis nitridation aluminum nanopowder of plasma-activated nitrogen source zygomite, which is characterized in that bag Include plasma-activated device, high voltage power supply, discharge electrode, reactor and particulate cascade retracting device；Wherein：The plasma-activated device is connected by gas circuit with reactor, is used to carry out discharge treatment to nitrogen source, makes its electricity From activation into being passed through in reactor after the nitrogen plasma containing active particle；The high voltage power supply is loaded onto the microsecond or ns high voltage pulse at discharge electrode both ends for generating；The discharge electrode is arranged in reactor, is used in the short time make the aluminium wire that Pulsed current injection is located among electrode It gasifies, and the aluminium steam formed after gasification chemically reacts in the reactor with nitrogen plasma, and is rapidly condensed into nitridation The nano-powder of aluminium；The particulate cascade retracting device is arranged in reactor before gas outlet, is used to collect the nano-powder of aluminium nitride, is gone out Gas port is connected with air pump by gas circuit, for emptying the foreign gas in reactor as early as possible, provides suitable air pressure requirement；The reactor is used to provide the reaction compartment of proper air pressure, and rate and the free path of product condensation is controlled to control Diameter of particle.
- 2. preparation system according to claim 1, it is characterised in that：The discharge electrode is aluminum electrode.
- 3. preparation system according to claim 1, it is characterised in that：It is equipped in the reactor automatically into silk device, It is used to periodically send aluminium wire to electrode with motor cooperation.
- 4. preparation system according to claim 1, it is characterised in that：Air-flow is equipped in the reactor around discharge electrode Distributor is used to adjust air-flow so that the quick-fried scope interior air-flow of silk is uniformly distributed.
- 5. preparation system according to claim 1, it is characterised in that：The high voltage power supply uses nanosecond pulse power supply or micro- Pulse per second (PPS) power supply, electric voltage frequency are adjustable.
- 6. preparation system according to claim 1, it is characterised in that：The aluminium wire be high-purity aluminium wire, Al content >= 99%.
- 7. preparation system according to claim 1, it is characterised in that：The nitrogen source is nitrogen, ammonia or nitrogen ammonia gaseous mixture.
- 8. preparation system according to claim 1, it is characterised in that：Ambient pressure≤1 standard in the reactor Atmospheric pressure.
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|---|---|---|---|
| CN201721149026.8U CN207435028U (en) | 2017-09-08 | 2017-09-08 | The preparation system of the plasma-activated quick-fried synthesis nitridation aluminum nanopowder of nitrogen source zygomite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461884A (en) * | 2020-12-07 | 2021-03-09 | 中国计量大学 | Nano powder dispersing method and device based on ion flow control |
| CN112872348A (en) * | 2020-12-31 | 2021-06-01 | 广东省科学院稀有金属研究所 | Method for improving nitriding efficiency of rare earth-iron alloy |
-
2017
- 2017-09-08 CN CN201721149026.8U patent/CN207435028U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461884A (en) * | 2020-12-07 | 2021-03-09 | 中国计量大学 | Nano powder dispersing method and device based on ion flow control |
| CN112872348A (en) * | 2020-12-31 | 2021-06-01 | 广东省科学院稀有金属研究所 | Method for improving nitriding efficiency of rare earth-iron alloy |
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