CN103205723A - Preparation device and method of nanometer superfine powder - Google Patents
Preparation device and method of nanometer superfine powder Download PDFInfo
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- CN103205723A CN103205723A CN2013101141356A CN201310114135A CN103205723A CN 103205723 A CN103205723 A CN 103205723A CN 2013101141356 A CN2013101141356 A CN 2013101141356A CN 201310114135 A CN201310114135 A CN 201310114135A CN 103205723 A CN103205723 A CN 103205723A
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Abstract
The invention relates to a preparation device and a preparation method of nanometer superfine powder by utilizing the magnetron sputtering technology, and belongs to the preparation technology and application field of nanometer materials. The method comprises the following steps of: by using a magnetron sputtering source and taking a disc solid material as a sputtered target material, leading a proper amount of inert gas or mixed atmosphere formed by the inert gas and an active reaction gas to serve as a sputtering medium; performing collision, condensation and the like on the material excited in the sputtering manner; and finally depositing the obtained material on a substrate, thereby forming the nanometer superfine powder. The method provided by the invention has the advantages of being simple in preparation process, regular in nanometer powder appearance, controllable in particle diameter, high in yield and high in purity. The prepared nanometer superfine powder can be applied to the fields of biological pharmacy, micro mechanical systems, semiconductor industry and the like.
Description
Technical field
The invention belongs to nano material preparation technology and Application Areas, particularly a kind of preparation facilities of nano ultrafine powders and method.
Background technology
Nano ultrafine powders refers to that size of particles reaches the small solids aggregate of 1 ~ 100nm, the researchdevelopment of its preparation and application is very fast, nano ultrafine powders has been applied to fields such as material, electronics, information, Aeronautics and Astronautics, medicine, military project, production, can be used for the preparation of novel high-capacity magneticsubstance, effective catalyst, magnetic fluid, absorbing material, high active combustion agent.The preparation method who has occurred various nano ultrafine powderses at present, the most frequently used method have thermal decomposition method, laser chemistry vapor phase process, explosion method, chemical reduction method etc. in condensation of gas method, arc process energising heating vaporization, the stove.
Chinese patent 02234819.0 relates to the two cold continuous processings of a kind of usefulness and prepares metal nano powder, and this invention is to adopt the metal base continuous feed, the striking of many negative electrodes tunable high-frequency, thus make the melting of metal evaporation realize the preparation of nano ultrafine powders.The preparation facilities of the nano ultrafine powders of this patent design comprises that powder generates major partss such as chamber, blast pipe, backwind tube, push-pull valve, rotational automatic decanter type collecting bin, tr, use this equipment and prepare the bar-shaped metal that the required raw material of nano ultrafine powders is certain size, can realize continuous production, be applicable to the preparation of ferrous metal, non-ferrous metal and alloy nano powder.Chinese patent 00261101.5 relates to a kind of equipment with arc process production metal nano powder, and this equipment adopts the striking of lifting electrode, makes the melting of metal evaporation in the crucible, thereby realizes producing the purpose of nano metal ultrafine powder.The equipment that this patent relates to comprises major equipments such as evaporator room, air-return duct, push-pull valve, water cooler, collecting bin, tr, adopt this equipment to produce the nano metal ultrafine powder, its raw metal geometrical shape is unrestricted, pure metal clout also can be reused, and is applicable to the preparation of metal nano powders such as iron, cobalt, nickel, chromium, manganese.Chinese patent 200610162054.3 relates to the method that a kind of applying electronic disintegrating method prepares the non-ferrous metal nano-powder.Its key step is with non-ferrous metal wire high electric current of conducting under the environment of rare gas element, makes its thawing division and forms high-quality metal nano level powder granule.The principle of this method is to utilize the infinitely-great ultimate principle of short-circuit current, in the encloses container that is full of the rare gas element helium, with the non-ferrous metal wire of several diameter lmm ~ l0mm, enters encloses container fast with certain speed.Non-ferrous metal filament material two ends import the voltage of 80V ~ 600V, utilize the effect that discharges and recharges of electrical condenser, go out the high electric current of 100A ~ 5000A in abrupt release, make non-ferrous metal wire instant melting and explosion under extreme event of overload.Under the dual function of rare gas element helium and non-ferrous metal physical property, the molten metal fluid can form the very smooth spherical particles in surface in moment.The preparation method of the described various nano ultrafine powderses of above-mentioned patent, characteristics are respectively arranged, but have certain shortcoming, mainly show as complex structure, inconvenient, the operational difficulty of maintenance, production efficiency is low, energy consumption is big, nano powder purity is low, size distribution is wide etc.
For realize that nano ultrafine powders preparation technology is simple, nano ultrafine powders pattern rule, particle diameter are controlled, high yield and high purity, the invention provides a kind of preparation facilities and method of novel nano ultrafine powders.The present invention is being target by sputter material, but the scale preparation nano ultrafine powders identical with the target composition, and finally be applied to fields such as bio-pharmaceuticals, micro mechanical system, semi-conductor industry.
Summary of the invention
The preparation technology who the purpose of this invention is to provide a kind of nano ultrafine powders, preparation facilities and the method for the nano ultrafine powders of realization mass-producing, high purity, even particle size distribution.
The preparation facilities of the nano ultrafine powders that the present invention proposes, comprise sputter cathode 1, sputter anode 2, sputter baffle plate 3, deposition substrate 4, cold-trap 5, substrate stationary platen 6, target 7, controlled sputtering source 8, power supply 9 and reaction chamber 10, wherein: described substrate stationary platen 6 is positioned at reaction chamber 10 internal upper parts, deposition substrate 4 is fixed in substrate stationary platen 6 belows, reaction chamber 10 top drillings, cold-trap 5 feeds from the perforate position, target 7 is positioned at controlled sputtering source 8 tops, and target 7 connects sputter cathode 1 and sputter anode 2 respectively, and power supply 9 connects sputter cathode 1 and sputter anode 2; Be provided with sputter baffle plate 3 between target 7 and the deposition substrate 4, reaction chamber 10 1 sides are inlet mouth, and opposite side is the air outlet.
Among the present invention, described controlled sputtering source 8 adopts direct current (DC) or radio frequency (RF) controlled sputtering source.
Among the present invention, described cold-trap is connected with liquid nitrogen cooling system.
The preparation method of the nano ultrafine powders that the present invention proposes, be excitaton source with direct current (DC)/radio frequency (RF) controlled sputtering source, with discoid be target by sputter material, under the mixed atmosphere of rare gas element or rare gas element and active reaction gas, obtain the relevant nanometer ultrafine powder behind the sputtering target material; Concrete steps are as follows:
(1) will be made high 3 ~ 5mm by sputter material, diameter is the target of 55 ~ 60mm; The distance of regulating between target and the deposition substrate is 40 ~ 80mm;
(2) reaction chamber is evacuated to 5 * 10
-6~ 6 * 10
-6Pa, charge into rare gas element or or the mixed gas of rare gas element and active reaction gas;
(3) this device is connected with cooling water system, connects power supply, regulate power parameter, the build-up of luminance sputtering target material;
(4) cold-trap is connected with liquid nitrogen cooling system, the temperature of deposition substrate is dropped to-150 ℃ ~-100 ℃; (providing scope)
(5) open target top sputter baffle plate, target begins sputter to deposition substrate;
(6) treat that nanometer powder deposits fully after, collect powder through passivation technology.
Among the present invention, the rare gas element described in the step (2) is argon gas or helium etc.
Among the present invention, described active reaction gas is one or more in oxygen, nitrogen, ammonia, methane or the ethane etc.
Among the present invention, in the mixed gas that described rare gas element and reactive gas are formed, rare gas element accounts for 50% to 70% of mixed gas volume.
The present invention is by the selection (as the selection of differential responses atmosphere) of different process; can prepare nano ultrafine powderses such as pure metal, metal nitride, metallic carbide, pottery; the preparation process simple controllable; can realize mass-producing and automatization, the purity height of gained nano ultrafine powders, even particle size distribution.
Description of drawings
Fig. 1 is the device that magnetron sputtering prepares nano ultrafine powders.
Fig. 2 is the TEM figure of embodiment 1 gained powder.
Fig. 3 is the TEM figure of embodiment 2 gained powders.Number in the figure: 1-sputter cathode, 2-sputter anode, 3-sputter baffle plate, 4-deposition substrate, 5-cold-trap, 6-substrate stationary platen, 7-target, 8-controlled sputtering source, 9-power supply, 10-reaction chamber.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for explanation the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1:
As shown in Figure 1, the device that magnetron sputtering prepares nano ultrafine powders comprises sputter cathode 1, sputter anode 2, sputter baffle plate 3, deposition substrate 4, cold-trap 5, substrate stationary platen 6, target 7, controlled sputtering source 8, power supply 9 and reaction chamber 10, described device is taked the sputter mode of upwards sputter, substrate 4 be positioned over target 7 directly over; In addition, substrate 4 directly links to each other with the bottom of cold-trap 5, and the liquid nitrogen in the cold-trap can cool off substrate 4 by heat transfer process, and its temperature is down to-150 ℃ ~-100 ℃; This device is equipped with rotary machine pump and high-vacuum molecular pump, and the final vacuum in the reaction chamber can reach 6.67X10-6Pa; Baffle plate 3 is between target 7 and substrate 4, and when formal sputtering, baffle plate 3 is in opened condition; This device power supply 9 is configuring direct current (DC) type and radio frequency (RF) type power supply simultaneously, and links to each other with controlled sputtering source 8, and different targets 7 can switch to the power supply of respective type.Choosing purity and be 99.9% metal titanium is target 7, and it is positioned over the negative electrode 1 in magnetically controlled DC sputtering source as shown in Figure 1, and the adjusting target-substrate distance is 50mm; Reaction chamber 10 is evacuated to 5 * 10
-6Pa charges into the rare gas element argon gas then; Regulate the flow of argon gas, make the pressure in the vacuum chamber reach 50Pa; The cooling circulating water system of opening device is connected dc sputtering power, and the adjusting power is 300W, and build-up of luminance also begins sputtering target material 7; Inject liquid nitrogen to cold-trap 5, cooling deposition substrate 4; Open baffle plate 3, target begins to collect the powder (see figure 2) to substrate 4 sputters and finally in substrate bottom deposition through passivation technology, and powder is of a size of 50 to 100nm.
Embodiment
2:
Choosing purity and be 99.9% TiO2 is target, and with its negative electrode 1 that is positioned over radio frequency (RF) controlled sputtering source as shown in Figure 1, the adjusting target-substrate distance is 40mm; Reaction chamber 10 is evacuated to 6 * 10
-6Pa charges into the rare gas element argon gas then; Regulate the flow of argon gas, make the pressure in the vacuum chamber reach 60Pa; The cooling circulating water system of opening device is connected the radio-frequency sputtering power supply, and the adjusting power is 500W, and build-up of luminance also begins sputtering target material 7; Inject liquid nitrogen to cold-trap 5, cooling deposition substrate 4; Open baffle plate 3, target 7 beginnings also finally deposit in the substrate bottom to the substrate sputter, thereby obtain TiO
2Nano ceramics ultrafine powder (see figure 3), powder are of a size of 40 to 70nm.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (7)
1. the preparation facilities of a nano ultrafine powders, comprise sputter cathode (1), sputter anode (2), sputter baffle plate (3), deposition substrate (4), cold-trap (5), substrate stationary platen (6), target (7), controlled sputtering source (8), power supply (9) and reaction chamber (10), it is characterized in that: described substrate stationary platen (6) is positioned at reaction chamber (10) internal upper part, deposition substrate (4) is fixed in substrate stationary platen (6) below, reaction chamber (1) 0 top drilling, cold-trap (5) feeds from the perforate position, target (7) is positioned at controlled sputtering source (8) top, and target (7) connects sputter cathode (1) and sputter anode (2) respectively, and power supply (9) connects sputter cathode (1) and sputter anode (2); Be provided with sputter baffle plate (3) between target (7) and the deposition substrate (4), reaction chamber (10) one sides are inlet mouth, and opposite side is the air outlet.
2. preparation facilities according to claim 1 is characterized in that described controlled sputtering source (8) adopts direct current or rf magnetron sputtering source.
3. preparation facilities according to claim 1 is characterized in that described cold-trap is connected with liquid nitrogen cooling system.
4. the using method of the preparation facilities of a nano ultrafine powders as claimed in claim 1 is characterized in that concrete steps are as follows:
(1) will be made high 3 ~ 5mm by sputter material, diameter is the target of 55 ~ 60mm; The distance of regulating between target and the deposition substrate is 40 ~ 80mm;
(2) reaction chamber is evacuated to 5 * 10
-6~ 6 * 10
-6Pa, charge into rare gas element or or the mixed gas of rare gas element and active reaction gas;
(3) this device is connected with cooling water system, connects power supply, regulate power parameter, the build-up of luminance sputtering target material;
(4) cold-trap is connected with liquid nitrogen cooling system, the temperature of deposition substrate is dropped to-150 ℃ ~-100 ℃;
(5) open target top sputter baffle plate, target begins sputter to deposition substrate;
(6) treat that nanometer powder deposits fully after, collect powder through passivation technology.
5. method according to claim 4 is characterized in that the rare gas element described in the step (2) is argon gas or helium.
6. method according to claim 4 is characterized in that described active reaction gas is one or more in oxygen, nitrogen, ammonia, methane or the ethane.
7. method according to claim 4 is characterized in that rare gas element accounts for 50% to 70% of mixed gas volume in the mixed gas of described rare gas element and reactive gas composition.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105452521A (en) * | 2013-08-06 | 2016-03-30 | 株式会社神户制钢所 | Film forming device |
| CN106079001A (en) * | 2016-06-20 | 2016-11-09 | 浙江旺林生物科技有限公司 | A kind of nano bamboo powdered carbon production technology |
| CN106558263A (en) * | 2016-11-01 | 2017-04-05 | 同济大学 | A kind of room temperature multistable balanced microcomputer tool system and its implementation |
| CN107620035A (en) * | 2017-08-11 | 2018-01-23 | 中北大学 | A kind of method and device for preparing TiBCN powder |
| 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 |
| CN110480025A (en) * | 2019-09-06 | 2019-11-22 | 陕西师范大学 | A kind of high-density nanomaterial gas-phase production |
| DE102020119279A1 (en) | 2020-07-22 | 2022-01-27 | Leibniz-Institut für Oberflächenmodifizierung e.V. | Method and device for nanoparticle synthesis |
| CN114797711A (en) * | 2022-04-15 | 2022-07-29 | 成都金创立科技有限责任公司 | Dual-functional complete pulverizing system and method |
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| CN1105288A (en) * | 1994-08-29 | 1995-07-19 | 青岛化工学院 | Process for preparing Nanometre Cu-Zn alloy catalyst |
| CN102492930A (en) * | 2011-12-28 | 2012-06-13 | 东北大学 | Equipment and method for preparing single or shell-core structure nanoparticle and film thereof |
| WO2012117171A1 (en) * | 2011-03-01 | 2012-09-07 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Device for producing nanoparticles at high efficiency, use of said device and method of depositing nanoparticles |
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Patent Citations (3)
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| CN1105288A (en) * | 1994-08-29 | 1995-07-19 | 青岛化工学院 | Process for preparing Nanometre Cu-Zn alloy catalyst |
| WO2012117171A1 (en) * | 2011-03-01 | 2012-09-07 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Device for producing nanoparticles at high efficiency, use of said device and method of depositing nanoparticles |
| CN102492930A (en) * | 2011-12-28 | 2012-06-13 | 东北大学 | Equipment and method for preparing single or shell-core structure nanoparticle and film thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105452521A (en) * | 2013-08-06 | 2016-03-30 | 株式会社神户制钢所 | Film forming device |
| CN106079001A (en) * | 2016-06-20 | 2016-11-09 | 浙江旺林生物科技有限公司 | A kind of nano bamboo powdered carbon production technology |
| CN106558263A (en) * | 2016-11-01 | 2017-04-05 | 同济大学 | A kind of room temperature multistable balanced microcomputer tool system and its implementation |
| CN106558263B (en) * | 2016-11-01 | 2019-01-25 | 同济大学 | A kind of room temperature multistable balanced microcomputer tool system and its implementation |
| CN107620035A (en) * | 2017-08-11 | 2018-01-23 | 中北大学 | A kind of method and device for preparing TiBCN powder |
| CN107620035B (en) * | 2017-08-11 | 2019-10-18 | 中北大学 | A kind of method and device preparing TiBCN powder |
| 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 |
| CN110480025A (en) * | 2019-09-06 | 2019-11-22 | 陕西师范大学 | A kind of high-density nanomaterial gas-phase production |
| CN110480025B (en) * | 2019-09-06 | 2020-12-08 | 陕西师范大学 | Gas phase preparation method of high-density nano material |
| DE102020119279A1 (en) | 2020-07-22 | 2022-01-27 | Leibniz-Institut für Oberflächenmodifizierung e.V. | Method and device for nanoparticle synthesis |
| CN114797711A (en) * | 2022-04-15 | 2022-07-29 | 成都金创立科技有限责任公司 | Dual-functional complete pulverizing system and method |
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Application publication date: 20130717 |