CN1460638A - Flaky carbon nano tube, preparation method and special equipment - Google Patents
Flaky carbon nano tube, preparation method and special equipment Download PDFInfo
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Abstract
The present invention relates to a flaky carbon nano tube, its preparation method and special-purpose equipment. The described flaky carbon nano tube is characterized by that its outer diameter is 15-50 nano, inner diameter is 5-20 nano, length is 10-100 micrometers, flaky actual raised length is 100 nano, its width is 50 nano and it has 3-10 layers of coiled actual raise formed from several layers of graphite flakes. Its preparation method includes three processes of preparing intermediate layer, preparing transition metal catalyst and carbon nano tube growth, and its special-purpose equipment includes vacuum system, heating system, gas distribution system, plasma generation system and film growth system.
Description
Technical field
The present invention relates to a kind of nano material, particularly relate to a kind of carbon nano-tube material and its preparation method and isolated plant that has flaky graphite synusia projection.Belong to the monodimension nanometer material field.
Background technology:
Carbon nanotube is the carbon pipe that a kind of diameter of being made up of carbon atom is a nanometer scale, be 1991 by Iijima[Nature354,56 (1991)] in the product of arc-over, find first.The special construction of carbon nanotube has determined it to have high-tensile, high thermostability and chemical stability, high field emission performance, excellent heat conductivility and special electric property.Being expected it plays a significant role in fields such as nanoelectronics, Materials science, biology, chemistry.
The method of existing synthesizing carbon nanotubes has a lot, as arc discharge method (people such as C.Joumet, Nature, 388,756 (1997) and people such as D.S.Bethune, Nature, 363,605 (1993)), laser deposition method (people such as R.E.Smally, Science, 273,483 (1996)), gas phase synthesis method (people such as R.Andrew, Chem.Phys.Lett., 303,468,1999) and heat/plasma enhanced chemical vapor deposition method (people such as W.Z.Li, Science, 274,1701,1996 and people such as Z.F.Ren, Science, 282,1105,1998) etc.These methods generally all need the temperature of complicated experimental installation and technological process or very high work, have improved the cost of manufacture of carbon nanotube.The more important thing is, usually contain carbon granule with these method synthetic carbon nanotubes, it generally be mixed in carbon nanotube dust or the film or the irregular inner and outer wall that adheres to some carbon nanotube on, influence the purity of carbon nanotube, thereby influence the performance of carbon nanotube.Therefore, must adopt appropriate means to remove these carbon granules.Yet owing to tend to some carbon granule attached on the single-root carbon nano-tube, and carbon material has good chemical stability, therefore is difficult to effectively remove these carbon granules, obtains large batch of high-purity nano pipe.
Important application with maximum application prospect of carbon nanotube is the electronic field emission device.Electronic field emission about carbon nanotube, it is generally acknowledged that electronic field emission takes place at the tip of having only carbon nanotube, but up-to-date result of study (people such as Y.Chen, Appl.Phys.Lett.76 (17) 2000) shows that also there is contribution the side of carbon nanotube to electronic field emission.And the carbon nanotube outside surface that general method obtains is slick, and electronic field emission comes from the textural defect on surface, so the outside surface of carbon nanotube is limited to the contribution of electronic field emission.
Carbon nanotube another one important applied field is a reinforced composite.Because the carbon nano tube surface smoother, carbon is very stable, and carbon nanotube can only combine by Intermolecular Forces with body material, and bonding force is very low.Therefore the fracture of these matrix materials also generally along carbon nanotube and matrix begin at the interface take place, reduced carbon nanotube and mixed the effect of strengthening bulk material.At present, employing is hung the chemical functional group or generated nano particle by solid state reaction outside carbon nanotube increases bonding strength.These methods are not only very complicated, and effect is also bad.
Summary of the invention:
In order to overcome the shortcoming and defect in the above-mentioned prior art, reasonably control and utilize the carbon nano-particle of " being harmful to ", the invention provides a kind of control " carbon nano-particle " growthhabit and distribution on carbon nanotube, their regular carbon nanotube outside surfaces that is arranged in uniformly that make, form a kind of squamous carbon nanotube, and provided its preparation technology parameter and isolated plant.
The object of the present invention is achieved like this:
1. squamous carbon nanotube provided by the invention be purity up to more than 99%, crystallization degree height, external diameter 15～50 nanometers, internal diameter 5～20 nanometers, the carbon nanotube that length is 10～100 microns.Squamous projection on its outer wall is the graphite linings chip architecture, long 100 about nanometers, wide about 50 nanometers contain 3～10 graphite linings, from the carbon nanotube root to the top uniform distribution.That is from the root to the top, be covered with at whole carbon nanotube outer wall.
2. the invention provides a kind of method for preparing the squamous carbon nanotube, this method is divided into middle layer preparation, transition-metal catalyst and three technological processs of carbon nano tube growth:
(1) the special middle layer of preparation
Body material is chosen as tinsel, silicon chip, ceramic plate or high temp glass etc.Adopt the method for vacuum vapor deposition to prepare special intermediate layer material.The middle layer is the film of the continuous whole of thickness more than 200nm.The oxide material stoichiometric ratio departs from about 10%.A kind of method is to adopt the method for electron beam evaporation to obtain metal (Ti, Al, Cu etc.), metal oxide (TiO
x, AlO
x, ZrO
xDeng), metal nitride (TiN, AlN) film.Evaporation source is selected these material blocks for use, and purity is more than 99.9%.The vacuum tightness of sediment chamber is higher than 10
-5Pa, the rotating speed of sample are 1～5 week of per second.Vaporator rate is per second 2～5 nanometers, thickness be 200～500 receive above, to guarantee the effective isolation between matrix and the catalyst layer.Another kind method is, adopts magnetically controlled sputter method to obtain above-mentioned middle layer, and for magnetically controlled DC sputtering, source metal adopts the discoid body material of associated metal, feeds corresponding gas, as argon gas (metallic membrane), and argon gas oxygen (oxide compound), argon gas adds nitrogen or ammonia.For rf magnetron sputtering, adopt corresponding body material as target material.The basic technology parameter is consistent with preceding a kind of method, or the film-forming process of the standard of employing.The third method is to adopt Vacuum Arc magnetic filtration method, makes target with graphite rod, the preparation diamond-like carbon film.Or adopt the method for pulse plasma body chemical vapor phase growing to obtain hydrogenous diamond-like carbon film.For preceding a kind of method, vacuum tightness is higher than 10
-3Pa, arc current are 5～20 amperes, 10～20 volts of arc voltages.Filter 1.5 amperes of coil currents, sedimentation rate 2 nm/minute, thickness 50～100 nanometers.For the latter, promptly plasma pulse strengthens chemical gaseous phase depositing process, back of the body end vacuum 10
-3～10
-5During Pa, feed acetylene gas, flow is 10～50sccm, and vacustat adds 4～10 kilovolts pulsed negative bias on sample behind 1～3Pa, pulse width 5～20 microseconds, and 50～100 hertz of frequencies, the mean current of sample is 5～10 milliamperes at this moment.1～2 hour plated film time.The hydrogeneous diamond-like carbon film that obtains, very smooth, color even, thickness is about 200～500 nanometers, and surfaceness is less than 1 nanometer, and the resistance of film is greater than 200 megaohms.
(2) preparation of transition-metal catalyst
Transition metal is selected iron, nickel for use, cobalt or their alloy.The method of electron beam evaporation is selected in the preparation of film for use, and evaporation source is the iron block of purity 99.999%, and with the speed of per second 0.1 nanometer, thickness is 2～10 nanometers.The vacuum tightness of sediment chamber remains on 10
-5More than the Pa, the rotating speed of sample is 5 weeks of per second.Also can in isolated plant, prepare catalyst film in position, under the prerequisite that guarantees thickness 2～10 nanometers, adopt general processing parameter.Treating processes then is: utilize the lattice mismatch between transiting metal film and the middle layer, by heating, cause catalytic metal film and middle layer to produce stress, under the effect of stress, make catalyzing metal layer chap into nano level isolated metallic particles.Control size, the shape of nano-catalytic metallic particles by composition, thickness and the crystalline state in control catalyzing metal layer and middle layer.Sample for the ex situ processing, be that middle layer, catalyzing metal layer and heat treated are not the samples of finishing in same vacuum system, need to obtain the nano particle of pure metal with hydrogen, ammonia and other reactive gas reduced nano surface of metal particles zone of oxidation.
(3) growth of squamous nanotube
Adopt the method for low density plasma activated chemical vapour deposition, in isolated plant, selecting acetylene (99.9%) and hydrogen (99.9%) is preferred combination of gases, gas flow is respectively 150～300sccm (hydrogen), 50～100sccm (acetylene), fixed ratio is 3:1, growth temperature is 650～750 ℃, 1000 volts of radio-frequency power supply bias voltages, 250～400 volts of output voltages, 100～150 volts of matrix negative bias direct currents, plasma density be less than 0.1 microampere/square centimeter, growth time 5～30 minutes.Because middle layer, the catalytic metal nano particle selected for use are different with the parameter of gas ratio, flow and plasma body, therefore nanotube density, external diameter, length and the purity that is obtained is also inequality, is essentially identical but obtain carbon nanotube under the identical conditions.Even general still fine and close under high power SEM, external diameter 15～50 nanometers, 10～100 microns of length.Long 100 nanometers of squamous projection, wide 50 nanometers contain 3～10 graphite linings, are covered with from the root to the top at whole carbon nanotube outer wall.
3. the present invention's device of being used to prepare the squamous carbon nanotube is made up of vacuum system, heating unit, gas distributing system, plasma generating system, film growth system.According to the carbon nanotube technical process, the annexation of each several part and effect are as follows: (1) vacuum system comprises that main vacuum chamber, prechamber and vacuum obtain, detecting instrument is formed, main vacuum chamber is whole device main body and support, separate by high vacuum valve between prechamber and the main vacuum chamber, guarantee that when changing sample the vacuum of main vacuum chamber is constant.(2) well heater is a vacuum armouring electric furnace, is placed on the sample delivery frame, with sample turnover main vacuum chamber, controls the temperature of sample by the temperature of control electric furnace, is beneficial to the growth of carbon nanotube.(3) gas distributing system is made up of gas circuit and mass-flow gas meter.They are connected to each other by stainless steel tube and are connected to the main vacuum chamber top.Gaseous species when adjusting carbon nano tube growth, proportioning and dividing potential drop by the flow of controlling each road gas.(4) the low frequency plasma body generation power supply in the plasma generating system links to each other with condenser antenna in the main vacuum chamber with the vacuum connector by concentric cable, produces plasma body by the output voltage that changes power supply, the density of control plasma body.(5) film growth system.It is made up of magnetron sputtering or Vacuum Arc deposit subassembly and line related.Annex during as nanotube growth is preferably grown the catalytic metal film or/and the middle layer with it.Utilize this isolated plant hydrogen once to finish to comprise sample cleaning, pre-treatment, middle layer with the whole technological processs such as growth of deposition, Preparation of catalysts and carbon nanotube, have complete function, the characteristics of the simple relatively easy handling of device.Utilize the squamous carbon nanotube of method preparation of the present invention to have following performance:
1. the squamous carbon nanotube has very high tensile strength and low proportion, has the outside surface of unique lamellar process, can be used for the enhancing compound of all types of matrix materials.
2. the squamous carbon nanotube has very high aspect ratio, and a certain position electric field is concentrated, and obtains high strength of electric field, the projection of outside surface particularly, increase electronic launching point, improved electronic field emission density, can be used to make the negative electrode of Field Emission Display.
3. carbon nanotube has the capillary siphonage, tungsten, caesium, lead and some radioelement can be filled in the carbon nanotube.The big outer surface area that also can utilize the squamous carbon nanotube is coated on some metal (caesium, titanium, copper) or metal oxide (gallium oxide, magnesium oxide, barium oxide) or other materials on the carbon nanotube, makes the nano material with special purpose
4. carbon nanotube is as gas such as the carrier of some catalyzer, Chu Qing, methane and lithium ion etc., particularly because outside surface has flaky graphite-structure projection, makes it at storage hydrogen with store up and have special advantages aspect the lithium, can be used for fields such as chemical industry, the energy.Superiority of the present invention:
(1) utilize device of the present invention can on a cover system, finish three processes of growth of middle layer deposition, the making of catalytic metal nano particle and carbon nanotube simultaneously.The nanotube technological process of preparation is simple, and safety is easy to operate.Temperature, air-flow, air pressure and plasma density precise control, preparation process is easy to repetition.The growth area of carbon nanotube is only relevant with heater size, system bulk, can carry out the mass production carbon nanotube.
(2) utilize method of the present invention, plasma density requires low, changes the not influence of form to the squamous carbon nanotube in the certain limit.Compare with microwave plasma, hot filament plasma body, common radio-frequency plasma and ICP plasma body, the power supply architecture of plasma body is simple, and radio-frequency antenna is easy to obtain, and technology is easy to operation, and equipment manufacturing cost is also very low.Like this, greatly reducing the squamous carbon nanotube increases because of using the cost that plasma body brought.
(3) utilize carbon nanotube density height, the diameter of method and apparatus preparation of the present invention very even, purity height (more than 99%) is big with basal body binding force.The output height of carbon nanotube, the degree of graphitization height.According to the length in reaction times can controlling carbon nanotube length.The outer surface area of carbon nanotube is big, has evenly distributed flake graphite projection.
Description of drawings
Fig. 1 is the grow device synoptic diagram of squamous carbon nanotube of the present invention.
Fig. 2 be field emission scanning electron microscope take at the high-density of growing during for the middle layer, the photo of highly purified squamous carbon nano-tube film with the titanium oxide
Fig. 3 is the high power photo at the single squamous carbon nanotube of growing during for the middle layer with the titanium oxide that field emission scanning electron microscope is taken
Fig. 4 is the high resolution picture photo of the single squamous carbon nanotube of growing during for the middle layer with the titanium oxide taken of transmission electron microscope.Its tubulose feature is many wall constructions as can be seen, the graphite linings striped picture on the tube wall.There is the graphite synusia projection of curling in the carbon nanotube outside surface.Among the figure:
1. gas circuit 2. sample 3.200KHz radio-frequency power supplies 4. main vacuum chamber 5. radio-frequency antennas, 6. thin film deposition assemblies, 7. thin film deposition power supplys, 8. well heaters 9. main vacuum chamber's rough vacuum extraction valves 10. master control valves 11. mechanical pumps 12. diffusion pump 13. main vacuum chamber's fine pumping valves 14. prechamber extraction valves 15. sample delivery framves 16. prechambers 17. master/prechamber segregaion valves 18. thermopairs 19. control dampers 20. mass-flow gas meter groups
Device of the present invention mainly by vacuum system, heater, air distribution system, etc. Gas ions generation systems, film growth system form. Wherein, vacuum system is by main true Empty chamber 4, prechamber 16 and vacuum obtain, control system 9,10,11,12, 13,14,17 form. Air distribution system is by gas circuit 1, mass-flow gas meter group 20 Form with control damper 19. Heater is by sample delivery frame 16, vacuum armour Dress electric furnace 8 and thermocouple 18 form. Plasma generating system is penetrated by 200KHz Frequency power 3 and ring-type radio-frequency antenna 5 form. Coil antenna has also guaranteed the radio frequency merit Rate is exported effectively, can make again in the film-forming system to produce particle and can arrive sample position. Film growth system is made up of thin film deposition assembly 7 and thin film deposition power supply 8. According to CNT preparation technology flow process, the contact in the each several part between the unit and effect as Lower: main vacuum chamber 4 is the cavitys that made by stainless steel cylinder in the vacuum system, forevacuum Chamber 16 is coupled by isolating valve 17, and master control valve 10 is shut, and opens pre-true Empty chamber extraction valve 14 and isolating valve 17, in advance/main vacuum chamber's forvacuum. Work as vacuum Degree is shut isolating valve 17 and prechamber extraction valve 14 during less than 1Pa, opens the master Control valve 10, isolating valve 17 and and main vacuum chamber's fine pumping valve 13, simultaneously general The sample delivery frame 15 that is placed with sample advances in the main vacuum chamber 4, and opens diffusion pump 12, vacuumize. When vacuum less than 10-3During Pa, begin with electric furnace 8 heated sample, Carry out the Quality control temperature with thermocouple 18, after the arrival temperature, passed into by gas circuit 1 Reacting gas, ratio and the flow of mass flowmenter group 20 control gases, air-flow control The air pressure that valve 19 processed is controlled in the main vacuum chamber. After stable, open the 200KHz radio frequency Power supply 3 produces plasma by radio-frequency antenna 5, to metal surface reduction and growth CNT.
Embodiment
Further illustrating substantive distinguishing features of the present invention and obvious improvement, but the present invention only is confined to embodiment by no means below by embodiment.
Embodiment 1:
In the device of the carbon nano-tube of special use of the present invention, be matrix with the monocrystalline silicon piece, titanium oxide is as the middle layer, and the preparation outside diameter is 30 nanometers, and length is greater than 30 microns, and purity reaches the carbon nanotube with flaky graphite synusia projection more than 99%.
1. preparation has the substrate in titanium oxide middle layer, and in-situ deposition iron film is as catalytic metal film.Selecting the monocrystalline silicon piece of CZ type of Si (100) of three inches N type for use, clean with the silicon wafer cleaning of standard, promptly is earlier 1: 1: 5 the aqueous solution with the ratio of ammoniacal liquor, hydrogen peroxide and deionized water, heats to boiling, boils 15 minutes; Using rinsed with deionized water then 5 minutes, is that 1: 1: 6 the aqueous solution boiled rinsed with deionized water 5 minutes 15 minutes with the ratio of ebullient hydrochloric acid, hydrogen peroxide and deionized water again; At last, under the high pure nitrogen protection, oven dry.Silicon chip after cleaning is put in the ultra vacuum electron beam evaporation equipment, and purity is that 99.99% titanium oxide block is placed in the water jacketed copper crucible as evaporation source, with the speed of per second 2 nanometers, makes the thin film of titanium oxide that thickness is 200 nanometers.The vacuum tightness of sediment chamber is 10
-5Pa, the rotating speed of sample are 1 week of per second.Evaporation source changed into the copper crucible that purity is 99.999% iron block is housed, with the speed of per second 0.1 nanometer, in-situ deposition thickness is the iron film of 5 nanometers.The vacuum tightness of sediment chamber remains on 10
-5Pa, the rotating speed of sample are 5 weeks of per second.
2. prepare catalytic nanometer metallic particles, growth in situ squamous carbon nanotube.
The above-mentioned catalytic templating with titanium oxide middle layer for preparing is placed on heater surfaces, is advanced in the main vacuum chamber of device, when vacuum reaches 10
-3Behind the Pa, sample is rapidly heated, and speed is 50 ℃/min, after temperature arrives 750 ℃, be incubated 5 minutes, feed hydrogen (purity 99.99%) then in vacuum chamber, flow 180sccm lights radio-frequency plasma, the rf bias of this moment is 360 volts, the direct-current biasing of sample is 100 volts, and current density is 0.05 microampere every square centimeter, and the treatment time is 10 minutes.At this moment, the iron film has split into nano level (about 30 nanometers) particle, and the surface is fully reduced.Then, feed acetylene gas (99%) in main vacuum chamber, flow is 60sccm, and the rf bias of this moment is reduced to 300 volts, sample approaching 0.07 microampere every square centimeter of current density, the reaction times is 15 minutes.Behind the growth ending, turn off plasma electrical source, acetylene gas and hydrogen successively, be incubated after 5 minutes, turn off heater power source, cool to room temperature with the furnace.The squamous nanotube external diameter that generates is 30 nanometers (the squamous projection is not counted in), even compact, and purity all has the squamous projection on the every carbon pipe more than 99%, and the squamous projection is evenly distributed on individual tubes, consistent size, the length of carbon nanotube is above 30 microns.
Embodiment 2:
In the device of the above embodiments 1, be matrix with the monocrystalline silicon piece, hydrogeneous diamond-like carbon film is as the middle layer, and the preparation outside diameter is 50 nanometers, and length is greater than 10 microns, and purity reaches the carbon nanotube with flaky graphite synusia projection more than 99%.
1. the preparation of hydrogeneous diamond-like carbon film
The selection of monocrystalline silicon piece is identical with embodiment one with cleaning process.The silicon chip of cleaning is placed into plasma pulse strengthens in the chemical gas-phase deposition system back of the body end vacuum 10
-3During Pa, feed acetylene gas, flow is 32sccm, and vacustat adds 6 kilovolts pulsed negative bias on sample behind 1.7Pa, pulse width 10 microseconds, and 78 hertz of frequencies, the mean current of sample is 5 milliamperes at this moment.1 hour plated film time.The hydrogeneous diamond-like carbon film that obtains, very smooth, color even, thickness is about 200 nanometers, and surfaceness is less than 1 nanometer, and the resistance of film is greater than 200 megaohms.
2. prepare catalytic metal film and nano-metal particle, growth in situ squamous carbon nanotube.
Adopt with embodiment one same process and prepare catalysis iron film and nano-metal particle, growth in situ squamous carbon nanotube.The squamous nanotube external diameter that generate this moment is 50 nanometers (the squamous projection is not counted in), even compact, and purity all has the squamous projection on the every carbon pipe more than 99%, and the squamous projection is evenly distributed on individual tubes, consistent size, the length of carbon nanotube is above 20 microns.The root of squamous carbon nanotube is inserted into graphited hydrogeneous diamond-like carbon film inside.
Claims (9)
1. flaky carbon nanotube, it is characterized in that: it is the carbon nanotube that a kind of outer wall length has the squamous projection, its external diameter 15～50 nanometers, internal diameter 5～20 nanometers, 10～100 microns of length; Squamous projection length 100 nanometers, wide 50 nanometers, the graphite synusia by 3～10 constitutes, and is covered with from the root to the top at whole carbon nanotube outer wall.
2. by the described squamous carbon nanotube of claim 1, the purity that it is characterized in that carbon nanotube is many wall constructions up to more than 99%, and there is the projection of the multilayer graphite synusia of curling in outside surface.
3. the preparation method of a squamous carbon nanotube is characterized in that comprising the preparation in middle layer, transition-metal catalyst preparation and three technological processs of made of carbon nanotubes:
Substrate material when (1) middle layer prepares is tinsel, silicon chip, ceramic plate or high temp glass, adopt the method for vacuum vapor deposition, the thickness in middle layer is more than 200 nanometers, and the surface evenly, smooth, compact structure, oxide material should depart from its stoichiometric ratio;
(2) transition-metal catalyst is selected iron, cobalt, nickel or their alloy, preferably selects electron beam evaporation iron film, and thickness is about 5 nanometers; During heating,, make transition metal films be broken into nano level particle because transition metal films, the especially lattice mismatch in iron film and middle layer produce stress;
(3) growth of squamous carbon nanotube is to finish under extremely low plasma density; Select hydrogen: the acetylene ratio is 3: 1, and temperature is 650～750 ℃, and the radio frequency output voltage is 250～400 volts, and the matrix negative bias is 100～150 volts, and the plasma density of this moment is lower than 0.1 μ A/cm
2, growth time is 5～30 minutes.
4. by the described method for preparing the squamous carbon nanotube of claim 3, it is characterized in that the preparation in described middle layer selects for use vacuum gas phase process deposition method to be:
(1) adopts methods such as electron beam evaporation, magnetron sputtering, preferably prepare the oxide compound TiO of non-stoichiometric
x, AlO
x, ZrO
x, or films such as nitride TiN, AlN, its stoichiometric ratio departs from about 10%;
(2) adopt Vacuum Arc magnetic filtration method to prepare diamond-like carbon film as the middle layer, vacuum tightness is higher than 10
-3Pa, arc current are 5～20 amperes, and 10～20 volts of arc voltages are filtered 1.5 amperes of coil currents, sedimentation rate 2 nm/minute, thickness 50～100 nanometers; Utilize plasma pulse to strengthen chemical gaseous phase depositing process, back of the body end vacuum 10
-3～10
-5During Pa, feed acetylene gas, flow is 10～50sccm, and vacustat adds 4～10 kilovolts pulsed negative bias on sample behind 1～3Pa, pulse width 5～20 microseconds, and 50～100 hertz of frequencies, the mean current of sample is 5～10 milliamperes at this moment.1～2 hour plated film time; The hydrogeneous diamond-like carbon film that obtains, thickness is about 200～500 nanometers, and surfaceness is less than 1 nanometer, and the resistance of film is greater than 200 megaohms.
5. by the described method for preparing the squamous carbon nanotube of claim 3, it is characterized in that selecting for use purity is 99.97% acetylene and hydrogen, their flow is respectively 150～300sccm and 50～100sccm, plasma body select capacitive coupling for use, frequency is 300KHz, and operating voltage is 1000 volts.
6. isolated plant for preparing the squamous carbon nanotube is characterized in that:
(1) whole device is made of vacuum system, heating unit, gas distributing system, plasma producing apparatus and film growth system;
(2) described vacuum system comprises that main vacuum chamber, prechamber and vacuum obtain, detecting instrument, is separated by high vacuum valve between prechamber and the main vacuum chamber;
(3) described heating unit is made up of with armouring electric furnace and thermopair sample delivery frame, vacuum, and the armouring electric furnace is placed on the sample delivery frame, with sample turnover main vacuum chamber, controls the temperature of sample by the temperature of control electric furnace;
(4) described gas distributing system is made up of gas circuit and gas mass flow spare, and they are connected to each other by stainless steel tube and link to each other with the main vacuum chamber top, the kind of gas when controlling the Flow-rate adjustment nanotube growth of each gas circuit, proportioning and dividing potential drop;
(5) described plasma generating system is made up of ring-type radio-frequency antenna, low frequency radio frequency power supply and concentric cable, and the low frequency radio frequency electric current links to each other with condenser antenna in the main vacuum chamber by concentric cable and vacuum plug-in unit;
(6) described film growth system is made up of thin film deposition assembly and thin film deposition power supply.
7. by the described isolated plant of claim 6, it is characterized in that main vacuum chamber is the cavity that is made by stainless steel cylinder.
8. by the described isolated plant of claim 6, it is characterized in that described film growth system thin film deposition assembly or be magnetron sputtering or Vacuum Arc deposition.
9. by the described isolated plant of claim 6, it is characterized in that the plasma generating system radio-frequency power supply is 200KHz.
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| CN102534544A (en) * | 2010-12-14 | 2012-07-04 | 财团法人工业技术研究院 | Carbon nanotube composite material and its preparation method |
| US9248281B2 (en) | 2011-10-28 | 2016-02-02 | Tsinghua University | Pacemakers and pacemaker leads |
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| CN103266306B (en) * | 2013-05-22 | 2015-11-18 | 宜昌后皇真空科技有限公司 | A kind of PVD technology prepares the method for Graphene or ultrathin carbon films |
| CN103266306A (en) * | 2013-05-22 | 2013-08-28 | 宜昌后皇真空科技有限公司 | Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique |
| CN104073767B (en) * | 2014-06-20 | 2016-08-17 | 钢铁研究总院 | A kind of uniform, preparation method of high-compactness nano-particular film and device |
| CN104073767A (en) * | 2014-06-20 | 2014-10-01 | 钢铁研究总院 | Preparation method and device of uniform and high-density nanoparticle film |
| US9708189B2 (en) | 2014-07-25 | 2017-07-18 | Tsinghua University | Carbon fiber film |
| TWI608994B (en) * | 2014-07-25 | 2017-12-21 | 鴻海精密工業股份有限公司 | Carbon fiber film |
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| CN105070619A (en) * | 2015-07-17 | 2015-11-18 | 兰州空间技术物理研究所 | Preparation method for carbon nanotube array cathode on Fe-based metal alloy substrate |
| CN105070619B (en) * | 2015-07-17 | 2017-05-03 | 兰州空间技术物理研究所 | Preparation method for carbon nanotube array cathode on Fe-based metal alloy substrate |
| CN110747437A (en) * | 2019-12-06 | 2020-02-04 | 北京师范大学 | Magnetic filtering pipeline |
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