CN1316309A - Process for preparing nm material by dual-glow discharge of hollow cathodes - Google Patents
Process for preparing nm material by dual-glow discharge of hollow cathodes Download PDFInfo
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- CN1316309A CN1316309A CN 01108400 CN01108400A CN1316309A CN 1316309 A CN1316309 A CN 1316309A CN 01108400 CN01108400 CN 01108400 CN 01108400 A CN01108400 A CN 01108400A CN 1316309 A CN1316309 A CN 1316309A
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Abstract
A process for preparing nm material features that the hollow cathode effect in dual-layer glow ion discharge technique and the sputter action generated by point discharge are used to sputter out the nm material in atom, ion, or particle mode.
Description
Preparing nm material by dual-glow discharge of hollow cathodes method of the present invention belongs to the category of nano material manufacturing technology.Concrete is a kind of hollow cathode effect and point discharge phenomenon that utilizes in the double-deck glow discharge, the process program of preparation nano-grade size powder mass.
Now existing preparation of nanomaterials mainly is: sol method, thermal evaporation and ball milled.Sol method is to be used for preparing various glass and crystalline material, is to utilize alkoxide to prepare organic precursors such as oxide compound, and hydrolysis deposits and makes then.But alkoxide or colloidal sol are wanted quantitative reaction, must be through a large amount of tests repeatedly, and prepare multi-component pottery certain difficulty is arranged.Thermal evaporation is in an airtight container, with the evaporation boat, carries out thermal evaporation, cools off then and collects the particulate that these are evaporated chilling.Its main drawback is the restriction that the thermal evaporation material is subjected to crucible material, and crucible material has pollution to obtaining nano material.Ball milled is in an airtight container, many hard steel balls or coating the ball of carbide, and rotation in container, vibration or fierce shaking make by the mill material and refine to nano-grade size.But it is limited in reaching relatively firmly on the material of embrittlement, and a major issue of the consideration that requires, and is the pollution problem of nano material at surface and interface.
Its purpose of preparing nm material by dual-glow discharge of hollow cathodes method of the present invention is, for solving the existing problem and shortage of above-mentioned preparation nano material method, thereby a kind of hollow cathode effect and point discharge phenomenon that utilizes in the double-deck glow discharge disclosed, the technical scheme of preparation nano material.
Preparing nm material by dual-glow discharge of hollow cathodes method of the present invention is characterized in that, it is a kind of sputter effect that hollow cathode effect and point discharge phenomenon produced that utilizes in the double-deck glow discharge technology, material with the desire preparation, form with atom, ion, particle sputters out, thereby obtains the method for nanometer particle material.Its specific embodiment is: the hollow supply negative electrode that at first can provide the solid matter of desiring nano materials to make; The collection negative electrode that can collect the nano-grade size particulate matter with refrigerating function; And the device that quick cooling function is provided between two negative electrodes, to insert in the vacuum vessel, the shell of vacuum vessel is as public anode and ground connection.Between two negative electrodes and public anode, two cover power supplys are set, its operating voltage of supplying with negative electrode is between 800～1500V, the collection negative electrode operating voltage of collecting particulate is between 100～500V, its final vacuum is lower than 1.33Pa, charge into gas during work, as nitrogen, argon gas or reactant gases ammonia, hydrocarbon gas etc., operating air pressure is at 13.3～1333Pa, at anode with supply with negative electrode and at anode with collect between the negative electrode and produce glow discharge, in ion bombardment, under the effect of cathode sputtering, the nano material of desire preparation is with atom, the form of ion and particle is sputtered out, cooled off fast and be deposited on by the quenching apparatus space that is provided with and collected on the negative electrode, thereby obtained the particulate of nano-grade size.
Equipment characteristic of the present invention is:
1. in having a container of vacuum chamber, be provided with two negative electrodes, cathode supplied with in a title that provides desire to prepare material, and negative electrode collected in another title of collecting nano material.Wherein collect negative electrode and have the chilling function.It is public that anode connects the vacuum vessel shell, and ground connection.
2. quick refrigerative device is set between two negative electrodes, and this device is hollow but has doubleshell that inside can feed the circulating cooling liquid body.Its objective is to produce a low temperature space so that by its particulate by quick cooling.
3. provide material the supply negative electrode its be shaped as hollow, can the side of being barrel-shaped, the garden be barrel-shaped or organize the hollow shape that parallel flat is formed more, in hollow supply negative electrode, can insert plate, bar, rod, etc. the material of shape, it distributes each other at a certain distance, and this distance range is generally at 5～30mm.
4. hollow quickly cooling device that is provided with between two negative electrodes and the used refrigerant of collector with chilling function can be recirculated water, gas or other quick heat-eliminating medium (as liquid nitrogen or the like).
5. be provided with two cover power supplys between two negative electrodes and public anode, voltage is adjustable continuously at 0～1500V.Its power supply natures can be direct current, interchange, pulse.
6. operating air pressure is supplied with the negative electrode operating voltage between 800～1500V in 13.3～1333Pa scope, collects the negative electrode operating voltage between 100～500V.
7. the working gas of present method is a rare gas element, as argon gas, also can be nitrogen or reactant gases such as ammonia, hydrocarbon gas etc.
Technical characterstic of the present invention is:
1. utilize hollow cathode effect in the double-deck glow discharge technology and point discharge phenomenon to increase the sputter effect, surface mass that material the is provided form with atom, ion, particle is sputtered, to obtain more nanometer particle.
2. these nano level particles by quick cooling, reach the fine particle of nano-grade size by the quenching apparatus district time.
3. these fine particles are deposited on the collector surface to the collector migration by electric field action.
4. the present invention can prepare metal nano material.
Process characteristic of the present invention is:
1. the voltage of supplying with negative electrode is between 800～1500V, and the voltage of collecting negative electrode exists
Between 100～500V
2. operating air pressure is between 13.3～1333Pa.
Purposes of the present invention and advantage
The purposes of preparing nm material by dual-glow discharge of hollow cathodes method of the present invention is to utilize the form of various solid materials with atom, ion or particle cluster sputtered out, and these particulates are cooled off rapidly, to form the nano metal and the ceramic particle of very tiny various materials.
The major advantage of preparing nm material by dual-glow discharge of hollow cathodes method of the present invention is:
1. supplying with extremely can be various metals and the alloy thereof that metallurgy method is manufactured, thereby can form single element and alloy nano-material.Also can be the single element of various different ratioss or the supply negative electrode that powdered alloy is made of powder metallurgy process, to form multielement or alloy nano-material.
2. so long as conducting material all can be used to make to supply with negative electrode, sputtered out through ion bombardment and be prepared into nano material.
3. owing to be to form nano material, so more tiny than the particle size of general method formation with the form sputter of atomicity magnitude.
4. supply with extremely fully and can make, so the nano material of preparation does not have pollution problem, high purity with a kind of material.
5. not polluting, do not have any discharge, is a kind of environment-protective process technology.
Description of drawings of the present invention
Accompanying drawing is the rough schematic of preparing nm material by dual-glow discharge of hollow cathodes method.On behalf of desire, symbol 1 prepare the supply negative electrode of nano material among the figure, and symbol 2 representatives receive the collection negative electrode of supplying with the nanoparticle that negative electrode provided, and symbol 3 is represented the shell of vacuum vessel, and symbol 4 is represented the refrigerating unit that has the chilling function between two negative electrodes.
As the method for preparing nm material by dual-glow discharge of hollow cathodes, accompanying drawings this
As the method for preparing nm material by dual-glow discharge of hollow cathodes, accompanying drawings the present invention finishes like this:
As accompanying drawing, the nano material molybdenum of desire preparation is made supply source as a negative electrode 1, be called the supply negative electrode.With receiving the particulate collecting utmost point that supply source provided as another negative electrode 2, be called the collection negative electrode, anode be public and with vacuum vessel 3 ground connection simultaneously.Between two negative electrodes, add a cover quenching apparatus 4, between negative electrode 1,2 and public anode, adopt the adjustable direct supply of two cover 0～1500V.In above-mentioned negative electrode 1, the synthetic metal molybdenum material of wanting is barrel-shaped, arranging 20 millimeters of diameter 4 millimeters long and the molybdenum filament of arranging in barrel-shaped circumferential direction inside by 5～20 millimeters spacing, when vacuum vessel is extracted into 1.33Pa, charge into certain rare gas element Jie top argon gas, to operating air pressure 30Pa, and add voltage this moment between these two negative electrodes and public anode, make the voltage of supplying with the utmost point at 1000V, the voltage of collector is at 200V, produce glow discharge in the container, supply with utmost point negative electrode 1 inside and will produce hollow cathode effect and point discharge phenomenon, the point discharge phenomenon of this hollow cathode effect and material inside, to the ionization level in the negative electrode bucket be improved greatly, ion bombardment energy increases, sputtering raste increases, the more synthetic particles of material of wanting is sputtered out, these particulates are under effect of electric field, move to alive collector, in the process of motion, when being provided with quenching apparatus and being connected with the quench zone of cooled with liquid nitrogen liquid, these particulates are cooled and are collected on the collector pole plate with speed of cooling faster, thereby obtain metal molybdenum nano material particulate.
Claims (6)
1. preparing nm material by dual-glow discharge of hollow cathodes method of the present invention, it is a kind of sputter effect that hollow cathode effect and point discharge phenomenon produced that utilizes in the double-deck glow discharge technology, nano material with the desire preparation, with atom, ion, the form of particle sputters out, thereby obtain the method for nanometer particle material, its specific embodiment is: the solid matter of desiring nano materials at first can be provided, as hollow supply negative electrode, the utmost point that can collect the nano-grade size particulate matter and have a refrigerating function is as collecting negative electrode, and between two negative electrodes, having quick refrigerative device inserts in the vacuum vessel, its container is as public anode and ground connection, between two negative electrodes and public anode, two cover power supplys are set, the operating voltage of wherein supplying with negative electrode is between 800～1500V, the collection negative electrode operating voltage of collecting particulate is between 100～500V, final vacuum is lower than 1.33Pa, charge into rare gas element during work, as nitrogen, argon gas or reactant gases ammonia, hydrocarbon gas etc., operating air pressure is at 13.3～1333Pa, produce glow discharge in the vacuum vessel in this processing range, in ion bombardment, under the effect of cathode sputtering, the material of desire preparation is with atom, ion, the form of particle is sputtered out, cooled off fast and be deposited on and collected on the negative electrode by the quenching apparatus space is set, thereby obtained the particulate of nano-grade size.
2. the method for preparing nm material by dual-glow discharge of hollow cathodes according to claim 1, it is characterized in that: can provide desire nano materials the formed supply negative electrode of solid matter its be shaped as hollow, can be square also can be garden shape, also can adopt many row's parallel flats, can arrange also that therebetween silk, plate, bar, band etc. desire the synthetic material, be that the distance of 5～30mm is arranged in the hollow supply negative electrode by mutual spacing.
3. the method for preparing nm material by dual-glow discharge of hollow cathodes according to claim 1 is characterized in that: the collection negative electrode of collecting the nanometer particle that is sputtered itself has the chilling function, and heat-eliminating medium can adopt water, liquid nitrogen or other refrigerating fulid.
4. the method for preparing nm material by dual-glow discharge of hollow cathodes according to claim 1 is characterized in that: add quenching apparatus supplying with negative electrode and collect between the negative electrode, the heat-eliminating medium of employing can water, liquid nitrogen or other cooling fluid.
5. the method for preparing nm material by dual-glow discharge of hollow cathodes according to claim 1, it is characterized in that: be added in the cover of two between two negative electrodes and public anode power supply, its voltage is adjustable at 0～1500V, and its power supply natures can be direct current, interchange, pulse.
6. the method for preparing nm material by dual-glow discharge of hollow cathodes according to claim 1, it is characterized in that: the rare gas element of feeding or reactant gases can be: argon gas, nitrogen or ammonia, hydrocarbon gas.
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| CNB011084006A CN1140367C (en) | 2001-03-16 | 2001-03-16 | Process for preparing nm material by dual-glow discharge of hollow cathodes |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101469407B (en) * | 2007-12-28 | 2011-06-08 | 北京有色金属研究总院 | Sputtering equipment with close packing tip anode |
| CN103128303A (en) * | 2013-02-28 | 2013-06-05 | 北京科技大学 | Method for preparing nanogold by vapor deposition process |
| CN104846343A (en) * | 2015-05-27 | 2015-08-19 | 杨小天 | Sputtering glow discharge generation method and device |
| CN105951048A (en) * | 2016-06-30 | 2016-09-21 | 南京航空航天大学 | Ta2N nanocrystalline coating with biological activity and preparing method of Ta2N nanocrystalline coating |
| CN106006758A (en) * | 2016-05-20 | 2016-10-12 | 西北师范大学 | Method for preparing nanometer Fe3O4 by virtue of waste iron wires |
| CN106048548A (en) * | 2016-06-16 | 2016-10-26 | 南京航空航天大学 | Preparation method of biological active nanocrystal beta-Ta coating |
| CN107699858A (en) * | 2017-10-18 | 2018-02-16 | 苏州贝龙光电科技有限公司 | A kind of nanometer photoelectronic material preparation method |
| CN109187496A (en) * | 2018-10-16 | 2019-01-11 | 四川大学 | A kind of Atomic Emission Spectral Analysis device based on electric heating evaporation and point discharge |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100457337C (en) * | 2006-04-28 | 2009-02-04 | 上海大学 | Method of preparing conductive metal nanometer powder by consumbale-cathode DC electric arc method |
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2001
- 2001-03-16 CN CNB011084006A patent/CN1140367C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101469407B (en) * | 2007-12-28 | 2011-06-08 | 北京有色金属研究总院 | Sputtering equipment with close packing tip anode |
| CN103128303A (en) * | 2013-02-28 | 2013-06-05 | 北京科技大学 | Method for preparing nanogold by vapor deposition process |
| CN104846343A (en) * | 2015-05-27 | 2015-08-19 | 杨小天 | Sputtering glow discharge generation method and device |
| CN106006758A (en) * | 2016-05-20 | 2016-10-12 | 西北师范大学 | Method for preparing nanometer Fe3O4 by virtue of waste iron wires |
| CN106006758B (en) * | 2016-05-20 | 2017-07-18 | 西北师范大学 | One kind prepares nanometer Fe using waste iron wire3O4Method |
| CN106048548A (en) * | 2016-06-16 | 2016-10-26 | 南京航空航天大学 | Preparation method of biological active nanocrystal beta-Ta coating |
| CN105951048A (en) * | 2016-06-30 | 2016-09-21 | 南京航空航天大学 | Ta2N nanocrystalline coating with biological activity and preparing method of Ta2N nanocrystalline coating |
| CN107699858A (en) * | 2017-10-18 | 2018-02-16 | 苏州贝龙光电科技有限公司 | A kind of nanometer photoelectronic material preparation method |
| CN109187496A (en) * | 2018-10-16 | 2019-01-11 | 四川大学 | A kind of Atomic Emission Spectral Analysis device based on electric heating evaporation and point discharge |
| CN109187496B (en) * | 2018-10-16 | 2024-02-06 | 四川大学 | Atomic emission spectrum analysis device based on electrothermal evaporation and tip discharge |
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|---|---|
| CN1140367C (en) | 2004-03-03 |
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