CN109809366A - The continuous producing method of laser evaporation Multicarity metal compound nano body - Google Patents
The continuous producing method of laser evaporation Multicarity metal compound nano body Download PDFInfo
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Abstract
The present invention relates to nano-powder production technical field, specifically a kind of laser evaporation Multicarity metal compound nano body continuous producing method.By utilizing laser evaporation Multicarity sodium rice powder preparation facilities, laser power is increased into target fusing power, passes through the control to laser power, to change the evaporation efficiency of anode, by the temperature gradient in control cavity, the nano-powder of different-grain diameter is formed, it can be achieved that continuous production.Preparation while a variety of heterogeneity powders can be achieved in the present invention, avoid the mutual pollution in powder preparation process, improve the purity of powder, production efficiency greatly improves, cost reduces, it industrially may be implemented constantly to switch between different cavitys, persistently evaporate the production effect of nano-powder, continuous production may be implemented under the premise of vacuum system satisfaction continues working.
Description
Technical field
The present invention relates to nano-powder production technical field, specifically a kind of metal compound nano body continuous production side
Method.
Background technique
DC arc plasma is to prepare nanoparticle, especially " core shell " type metal (alloy) nano-complex particle,
A kind of effective heat source of carbon associated materials and ceramic nano material tentatively realizes magnanimity production using the method at present, such as
Chinese patent application: a kind of multi-source direct-current arc automation nano-powder production system and method (201410189518.4), but
For large-scale industrial production, there is also many technical problems, be mainly manifested in how high efficiency, low cost, high-purity,
It is pollution-free, serialization to prepare nano-powder.
Existing metal compound nano body Preparation equipment and technique are mainly single in single-chamber body both for nano-powder
It generates in room and generates, classification, traps and handle, the powder Preparation equipment and technique of this single-chamber body have the following deficiencies:
1, production efficiency is lower, higher cost
Currently, the powder Preparation equipment and technique of single-chamber body, are protected completing vacuum drawn, powder generation and processing, vacuum
It holds in equal cyclic processes, the most of the time keeps with vacuum and recycle this process for vacuumizing, and is used in a preparation process
The time that this vacuum drawn and vacuum are kept accounts for 50%-70%, and the practical power production time is 15-20%, generally speaking,
Production efficiency is lower, simultaneously because vacuum drawn and vacuum keep and are iteratively repeated this process, will consume a large amount of energy, so that
Cost greatly increases.
2, purity is lower, there are cross contaminations
The powder Preparation equipment and technique of single-chamber body, after the nano-powder preparation of material always is completed in preparation, if again
The powder of other materials is prepared, at least there is the mutual pollution between 2 kinds of powders, to reduce the purity of nano-powder.
3, it cannot achieve continuous production truly
The powder Preparation equipment and technique of current single-chamber body, although the lasting feeding and confession of anode material can be passed through
It gives, realizes continuous production to a certain extent, but be limited by the size of anode material, continue feeding in material and supplied
Cheng Zhonghui there is a problem of not continuous enough, simultaneously because influence of the friction feeding to chamber vacuum degree, this method is extensive
Continuous production can not be realized under the premise of guaranteeing product quality in industrialized production, be phased out in the near future.
Currently, laser heat source is mainly used in field of material processing, increasing material manufacturing, such as China are realized by laser heat source
A kind of patent application: compound welding gun of laser-(201510144976.0).The present invention applies the production of laser realization nano-powder for the first time
Industry metaplasia produces, and realizes effective control of laser heat source, improves the production efficiency of nano-powder.Existing laser heat source evaporation
Type of laser specifically includes that CO2Gas laser beam, YAG Solid State Laser beam or diode laser beam, it is defeated using continuous or pulse
Mode out.
Summary of the invention
The purpose of the present invention is to provide laser evaporation Multicarity metal compound nano body continuous producing methods, with solution
Certainly the problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme: laser evaporation Multicarity metal compound nano
Body continuous producing method, it is characterised in that: the following steps are included:
(1), it places target: the monometallic of identical component or heterogeneity is installed on the target fixator of each individual cavity
Or metallic compound target, sealing installation GaAs glass at the cavity inner wall upper opening of the top of target, and to GaAs glass
Glass is cooled down；
(2), it vacuumizes: closing the hatch door of each individual cavity, open the vacuum valve of each individual cavity, to all cavitys
Vacuum degree is evacuated to not higher than 10-4Pa closes the vacuum valve of each individual cavity；
(3), it is filled with working gas: opening the air intake valve of each individual cavity, be passed through working gas according to the attribute of target:
When target is metallic compound, it is passed through working gas hydrogen；When target is monometallic, it is passed through working gas hydrogen and reaction gas
Body；
(4), laser is imported: by external laser light source by the way that in GaAs glass introduction chamber body, adjusting laser power is simultaneously right
Quasi- target；
(5), laser evaporation: laser power is increased into target fusing power, by the control to laser power, to change
The evaporation efficiency of anode；
(6), form powder: the temperature gradient in control cavity is 7000-14000K/m, forms the nano powder of different-grain diameter
Body；
(7), metal nano powder is collected: being consumed and is completed to any one anode target material, closes the cavity and correspond to laser
Light source collects the metal nano powder taken out in the cavity；
(8), it changes target: the cavity that powder taking-up is completed being cleared up, is put into before being put into the cavity
The identical monometallic of target material composition or metallic compound target are anode, close the cavity hatch door, open the vacuum valve of the cavity
Door is evacuated to vacuum degree not higher than 10 to the cavity-4Pa closes the vacuum valve of the cavity, opens the intake valve of the cavity
Door, is passed through working gas according to the attribute of target: when target is metallic compound, being passed through working gas hydrogen；Target is Dan Jin
When category, it is passed through working gas hydrogen and reaction gas；
(9), continuous production: repeating the processing step of above-mentioned (4)-(8), realizes continuous production.
GaAs thickness of glass is 3-5mm in the step (1).
It is 0.1 atmospheric pressure that hydrogen gas pressure is passed through in the step (3) or step (8), and reaction gas air pressure is 0.2-0.3
Atmospheric pressure.
The reaction gas being passed through in the step (3) or step (8) is oxygen, nitrogen, ammonia, alkanes gas or hydrogen sulfide
Gas.When reaction gas is oxygen, what is obtained is metallic oxide nano powder；When reaction gas is nitrogen or ammonia, obtain
Be metal nitride nano-powder；When reaction gas is alkanes gas, what is obtained is metal carbides nano-powder；Reaction gas
When body is hydrogen sulfide gas, what is obtained is nano metal sulfide powder.
It is 300-400W that laser power is adjusted in the step (4).
Target fusing power is 500-3000W in the step (5), and evaporation efficiency range changes between 0.1-0.8.It steams
Hair efficiency is defined as η=P/P0, according to different metals, range changes the range of η between 0.1-0.8, wherein magnesium, aluminium,
Calcium, zinc, tin 0.6-0.8, iron, cobalt, nickel 0.4-0.6, molybdenum, niobium, tantalum 0.1-0.4.
The partial size of step (6) nano-powder is 30-120nm.
The method of temperature gradient in the step (6) in control cavity is: by controlling the flow of cooling water or in chamber
Liquid nitrogen cooling tube is placed in body, to control cavity medium temperature degree gradient.
By controlling the flow of cooling water or placing liquid nitrogen cooling tube in cavity, to change temperature gradient in cavity, swash
The operative temperature of light and target material surface is 3000-5000K, and the temperature of cavity wall is 300K, temperature gradient 7000-14000K/
M, under different temperature gradients, diameter of nano particles is different, 7000-9000K/m, partial size 90-120nm, 9000-11000K/
M, partial size is 60-90nm, 110000-14000K/m, partial size 30-60nm.
Compared with prior art, the beneficial effects of the present invention are:
1, it realizes and is prepared while a variety of heterogeneity powders
It is mutually indepedent between multiple and different individual cavities, receiving for preparation heterogeneity can be evaporated in different cavitys
Rice flour body, the function of realizing different powders on one device while preparing.
2, the mutual pollution in powder preparation process is avoided, the purity of powder is improved
The nano-powder of same ingredient can be prepared in each individual cavity, it is therefore prevented that prepare different powder in a cavity
Body and the mutual pollution generated, further improve the purity of nano-powder.
3, production efficiency greatly improves, cost reduces
Multiple cavities use same set of pumped vacuum systems simultaneously, and vacuum system can not have to open and close repeatedly, significantly
The time vacuumized in production is reduced, production efficiency improves at least 30%, and production cost at least reduces 20%.
4, continuous production is realized
This continuous production technology of Multicarity, industrially may be implemented constantly to switch between different cavitys, persistently steam
Continuous production may be implemented under the premise of vacuum system satisfaction continues working in the production effect for sending out nano-powder.
Specific embodiment
Below in conjunction in the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1
Laser evaporation Multicarity metal compound nano body continuous producing method, comprising the following steps:
(1), it places target: the monometallic of identical component or heterogeneity is installed on the target fixator of each individual cavity
Or metallic compound target, at the cavity inner wall upper opening of the top of target sealing installation with a thickness of 3mm GaAs glass, and
GaAs glass is cooled down；
(2), it vacuumizes: closing the hatch door of each individual cavity, open the vacuum valve of each individual cavity, use mechanical pump pair
All cavitys are vacuumized not higher than 10-1Pa reuses molecular pump and vacuumizes not higher than 10-4Pa closes the true of each individual cavity
Empty valve；
(3), it is filled with working gas: opening the air intake valve of each individual cavity, be passed through working gas according to the attribute of target:
When target is metallic compound, it is passed through working gas hydrogen；When target is monometallic, it is passed through working gas hydrogen and reaction gas
Body；Being passed through hydrogen gas pressure is 0.1 atmospheric pressure, and reaction gas air pressure is 0.2 atmospheric pressure；
The reaction gas that is passed through is oxygen, and what is obtained is metallic oxide nano powder；
(4), it imports laser: being by GaAs glass introduction chamber body, adjusting laser power by external laser light source
300W is simultaneously directed at target；
(5), laser evaporation: by laser power increase to target fusing power: magnesium, aluminium, calcium, zinc 500-1500W, iron, cobalt,
Nickel 1500-2500W, molybdenum, niobium, tantalum 2500-3500W, by the control to laser power, come change the evaporation efficiency η of anode=
The range of P/P0, η change between 0.1-0.8 according to different metals, range: magnesium, aluminium, calcium, zinc 0.6-0.8, iron, cobalt, nickel
0.4-0.6, molybdenum, niobium, tantalum 0.1-0.4；
(6), powder is formed: by controlling the flow of cooling water or placing liquid nitrogen cooling tube in cavity, to change cavity
The operative temperature of middle temperature gradient, laser and target material surface is 3000K, and the temperature of cavity wall is 300K, and temperature gradient is
7000-9000K/m, partial size 90-120nm；
(7), metal nano powder is collected: being consumed and is completed to any one anode target material, closes the cavity and correspond to laser
Light source collects the metal nano powder taken out in the cavity；
(8), it changes target: the cavity that powder taking-up is completed being cleared up, is put into before being put into the cavity
The identical monometallic of target material composition or metallic compound target are anode, close the cavity hatch door, open the vacuum valve of the cavity
Door is evacuated to vacuum degree not higher than 10 to the cavity-4Pa closes the vacuum valve of the cavity, opens the intake valve of the cavity
Door, is passed through working gas according to the attribute of target: when target is metallic compound, being passed through working gas hydrogen；Target is Dan Jin
When category, it is passed through working gas hydrogen and reaction gas；
(9), continuous production: repeating the processing step of above-mentioned (4)-(8), realizes continuous production.
Embodiment 2
Laser evaporation Multicarity metal compound nano body continuous producing method, comprising the following steps:
(1), it places target: the monometallic of identical component or heterogeneity is installed on the target fixator of each individual cavity
Or metallic compound target, at the cavity inner wall upper opening of the top of target sealing installation with a thickness of 4mm GaAs glass, and
GaAs glass is cooled down；
(2), it vacuumizes: closing the hatch door of each individual cavity, open the vacuum valve of each individual cavity, use mechanical pump pair
All cavitys are vacuumized not higher than 10-1Pa reuses molecular pump and vacuumizes not higher than 10-4Pa closes the true of each individual cavity
Empty valve；
(3), it is filled with working gas: opening the air intake valve of each individual cavity, be passed through working gas according to the attribute of target:
When target is metallic compound, it is passed through working gas hydrogen；When target is monometallic, it is passed through working gas hydrogen and reaction gas
Body；Being passed through hydrogen gas pressure is 0.1 atmospheric pressure, and reaction gas air pressure is 0.25 atmospheric pressure；
The reaction gas being passed through is nitrogen or ammonia, and what is obtained is metal nitride nano-powder；
(4), it imports laser: being by GaAs glass introduction chamber body, adjusting laser power by external laser light source
350W is simultaneously directed at target；
(5), laser evaporation: by laser power increase to target fusing power: magnesium, aluminium, calcium, zinc 500-1500W, iron, cobalt,
Nickel 1500-2500W, molybdenum, niobium, tantalum 2500-3500W, by the control to laser power, come change the evaporation efficiency η of anode=
The range of P/P0, η change between 0.1-0.8 according to different metals, range: magnesium, aluminium, calcium, zinc 0.6-0.8, iron, cobalt, nickel
0.4-0.6, molybdenum, niobium, tantalum 0.1-0.4；
(6), powder is formed: by controlling the flow of cooling water or placing liquid nitrogen cooling tube in cavity, to change cavity
The operative temperature of middle temperature gradient, laser and target material surface is 4000K, and the temperature of cavity wall is 300K, and temperature gradient is
79000-11000K/m, partial size 60-90nm；
(7), metal nano powder is collected: being consumed and is completed to any one anode target material, closes the cavity and correspond to laser
Light source collects the metal nano powder taken out in the cavity；
(8), it changes target: the cavity that powder taking-up is completed being cleared up, is put into before being put into the cavity
The identical monometallic of target material composition or metallic compound target are anode, close the cavity hatch door, open the vacuum valve of the cavity
Door is evacuated to vacuum degree not higher than 10 to the cavity-4Pa closes the vacuum valve of the cavity, opens the intake valve of the cavity
Door, is passed through working gas according to the attribute of target: when target is metallic compound, being passed through working gas hydrogen；Target is Dan Jin
When category, it is passed through working gas hydrogen and reaction gas；
(9), continuous production: repeating the processing step of above-mentioned (4)-(8), realizes continuous production.
Embodiment 3
Laser evaporation Multicarity metal compound nano body continuous producing method, comprising the following steps:
(1), it places target: the monometallic of identical component or heterogeneity is installed on the target fixator of each individual cavity
Or metallic compound target, at the cavity inner wall upper opening of the top of target sealing installation with a thickness of 5mm GaAs glass, and
GaAs glass is cooled down；
(2), it vacuumizes: closing the hatch door of each individual cavity, open the vacuum valve of each individual cavity, use mechanical pump pair
All cavitys are vacuumized not higher than 10-1Pa reuses molecular pump and vacuumizes not higher than 10-4Pa closes the true of each individual cavity
Empty valve；
(3), it is filled with working gas: opening the air intake valve of each individual cavity, be passed through working gas according to the attribute of target:
When target is metallic compound, it is passed through working gas hydrogen；When target is monometallic, it is passed through working gas hydrogen and reaction gas
Body；Being passed through hydrogen gas pressure is 0.1 atmospheric pressure, and reaction gas air pressure is 0.3 atmospheric pressure；
The reaction gas being passed through is alkanes gas, and what is obtained is metal carbides nano-powder；
(4), it imports laser: being by GaAs glass introduction chamber body, adjusting laser power by external laser light source
400W is simultaneously directed at target；
(5), laser evaporation: by laser power increase to target fusing power: magnesium, aluminium, calcium, zinc 500-1500W, iron, cobalt,
Nickel 1500-2500W, molybdenum, niobium, tantalum 2500-3500W, by the control to laser power, come change the evaporation efficiency η of anode=
The range of P/P0, η change between 0.1-0.8 according to different metals, range: magnesium, aluminium, calcium, zinc 0.6-0.8, iron, cobalt, nickel
0.4-0.6, molybdenum, niobium, tantalum 0.1-0.4；
(6), powder is formed: by controlling the flow of cooling water or placing liquid nitrogen cooling tube in cavity, to change cavity
The operative temperature of middle temperature gradient, laser and target material surface is 5000K, and the temperature of cavity wall is 300K, and temperature gradient is
110000-14000K/m, partial size 30-60nm；
(7), metal nano powder is collected: being consumed and is completed to any one anode target material, closes the cavity and correspond to laser
Light source collects the metal nano powder taken out in the cavity；
(8), it changes target: the cavity that powder taking-up is completed being cleared up, is put into before being put into the cavity
The identical monometallic of target material composition or metallic compound target are anode, close the cavity hatch door, open the vacuum valve of the cavity
Door is evacuated to vacuum degree not higher than 10 to the cavity-4Pa closes the vacuum valve of the cavity, opens the intake valve of the cavity
Door, is passed through working gas according to the attribute of target: when target is metallic compound, being passed through working gas hydrogen；Target is Dan Jin
When category, it is passed through working gas hydrogen and reaction gas；
(9), continuous production: repeating the processing step of above-mentioned (4)-(8), realizes continuous production.
Embodiment 4
Each step of the body continuous producing method of laser evaporation Multicarity metal compound nano described in the present embodiment
It is in the same manner as in Example 1, difference are as follows:
Reaction gas is hydrogen sulfide gas, and what is obtained is nano metal sulfide powder.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. laser evaporation Multicarity metal compound nano body continuous producing method, it is characterised in that: the following steps are included:
(1), it places target: the monometallic or gold of identical component or heterogeneity is installed on the target fixator of each individual cavity
Belong to compound target, sealing installation GaAs glass at the cavity inner wall upper opening of the top of target, and to GaAs glass into
Row cooling；
(2), it vacuumizes: closing the hatch door of each individual cavity, open the vacuum valve of each individual cavity, all cavitys are taken out true
Sky to vacuum degree is not higher than 10-4Pa closes the vacuum valve of each individual cavity；
(3), it is filled with working gas: opening the air intake valve of each individual cavity, be passed through working gas according to the attribute of target: target
When for metallic compound, it is passed through working gas hydrogen；When target is monometallic, it is passed through working gas hydrogen and reaction gas；
(4), laser is imported: by external laser light source by adjusting laser power and alignment targets in GaAs glass introduction chamber body
Material；
(5), laser evaporation: laser power is increased into target fusing power, by the control to laser power, to change anode
Evaporation efficiency；
(6), form powder: the temperature gradient in control cavity is 7000-14000K/m, forms the nano-powder of different-grain diameter；
(7), metal nano powder is collected: it consumes and completes to any one anode target material, close the cavity and correspond to laser light source,
Collect the metal nano powder taken out in the cavity；
(8), it changes target: the cavity that powder taking-up is completed being cleared up, the target being put into before with the cavity is put into
The identical monometallic of ingredient or metallic compound target are anode, close the cavity hatch door, open the vacuum valve of the cavity, right
The cavity is evacuated to vacuum degree not higher than 10-4Pa closes the vacuum valve of the cavity, opens the air intake valve of the cavity, presses
Working gas is passed through according to the attribute of target: when target is metallic compound, being passed through working gas hydrogen；When target is monometallic,
It is passed through working gas hydrogen and reaction gas；
(9), continuous production: repeating the processing step of above-mentioned (4)-(8), realizes continuous production.
2. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: GaAs thickness of glass is 3-5mm in the step (1).
3. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: it is 0.1 atmospheric pressure that hydrogen gas pressure is passed through in the step (3) or step (8), and reaction gas air pressure is 0.2-0.3 atmosphere
Pressure.
4. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: the reaction gas being passed through in the step (3) or step (8) is oxygen, nitrogen, ammonia, alkanes gas or stink damp
Body.
5. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: it is 300-400W that laser power is adjusted in the step (4).
6. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: target fusing power is 500-3000W in the step (5), and evaporation efficiency range changes between 0.1-0.8.
7. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: the partial size of step (6) nano-powder is 30-120nm.
8. laser evaporation Multicarity metal compound nano body continuous producing method according to claim 1, feature
Be: the method for the temperature gradient in the step (6) in control cavity is: by controlling the flow of cooling water or in cavity
Liquid nitrogen cooling tube is placed, to control cavity medium temperature degree gradient.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6254005A (en) * | 1985-09-02 | 1987-03-09 | Hitachi Ltd | Production of hyperfine particles |
| CN104213076A (en) * | 2014-08-27 | 2014-12-17 | 慕恩慈沃迪 | Method and equipment for preparing superhard DLC coating by PVD and HIPIMS |
-
2019
- 2019-01-25 CN CN201910074759.7A patent/CN109809366A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6254005A (en) * | 1985-09-02 | 1987-03-09 | Hitachi Ltd | Production of hyperfine particles |
| CN104213076A (en) * | 2014-08-27 | 2014-12-17 | 慕恩慈沃迪 | Method and equipment for preparing superhard DLC coating by PVD and HIPIMS |
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Application publication date: 20190528 |