CN101190780A - Device and method for stably preparing one-dimensional nanostructure material by thermal evaporation - Google Patents
Device and method for stably preparing one-dimensional nanostructure material by thermal evaporation Download PDFInfo
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- CN101190780A CN101190780A CNA2007101212784A CN200710121278A CN101190780A CN 101190780 A CN101190780 A CN 101190780A CN A2007101212784 A CNA2007101212784 A CN A2007101212784A CN 200710121278 A CN200710121278 A CN 200710121278A CN 101190780 A CN101190780 A CN 101190780A
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Abstract
The invention relates to a device and a method for stably preparing a one-dimensional nano-structure material by thermal evaporation. One end of a thermal evaporation part is provided with a carrier gas outlet, and the other end is provided with a carrier gas inlet; the thermal evaporation part is arranged in a heating furnace, one end of the thermal evaporation part, which is provided with a carrier gas inlet, is provided with a slide bar which can extend into the thermal evaporation part, the slide bar is fixedly connected with a boat for loading thermal evaporation raw materials, and a substrate for growing a one-dimensional nano structure is arranged in the thermal evaporation part positioned at the heating furnace part. After the temperature and the air pressure are stabilized at the set values, the raw materials can be transmitted to a constant temperature area of the thermal evaporation part through the slide bar, so that the raw materials are uniformly evaporated at the same temperature, and the aim of stably and uniformly preparing the one-dimensional nano structure is fulfilled. The invention overcomes the obstacle that the raw materials can not be uniformly evaporated at the same temperature when the one-dimensional nanostructure material is prepared by the conventional thermal evaporation, so that the one-dimensional nanostructure material is difficult to stably prepare, and the uniform one-dimensional nanostructure material is easier to stably prepare.
Description
Technical field
The present invention relates to a kind of apparatus and method of stably preparing one-dimensional nano structure material by heat evaporation
Background technology
One-dimensional nano structure material, comprise that nano wire, nanometer band and coaxial nano cable are the focuses of nano science and technical field research in recent years, develop several different methods at present and prepared one-dimensional nano structure material, comprised solwution method, chemical vapour deposition (CVD), template, physics thermal evaporation method.In these methods, be used widely with the physics thermal evaporation method again.Can prepare present most of one-dimensional nano structure material by this method, comprise silicon nanowires, nanometer band, numerous one-dimensional nano structure material (Advanced FunctionalMaterials such as Z.R.Dai that application prospect is arranged such as oxide nano thread and nanometer band, 13 (1), 9～24,2003; US patent 20020094450,6303015B1).But present used physics thermal evaporation method is raw material to be placed on earlier want area heated, then system is vacuumized adjusting air pressure, carries out analgesic to system again.The temperature of raw material is also in slowly rising in the process of heating, and raw material slowly start vaporizer just in the process that heats up, and evaporant can be diffused into low-temperature region with carrier gas and deposit and get off to carry out the growth of one-dimensional nano structure.In view of this, system before entering keeping warm mode, raw material start vaporizer and last till holding temperature in fact, in this process, temperature is to increase variation always, like this, the growth of one-dimensional nano structure is carried out under a kind of unsure state.Therefore, need forbid that raw material evaporated before system temperature and air pressure reach stable state.
Summary of the invention
The device that the purpose of this invention is to provide stably preparing one-dimensional nano structure material by heat evaporation.
A further object of the present invention provides the method for stably preparing one-dimensional nano structure material by heat evaporation.
The device of thermal evaporation stably preparing one-dimensional nano structure of the present invention comprises: load the boat of thermal evaporation raw material, slide bar, the substrate of growth of one-dimensional nano structure, thermal evaporation parts, heating furnace;
One end of one thermal evaporation parts has the carrier gas outlet, and the other end has carrier gas inlet;
The thermal evaporation parts place heating furnace, an end that has carrier gas inlet at the thermal evaporation parts is equipped with one, the slide bar that can stretch in the thermal evaporation parts is installed on door, slide bar fixedly connected one loads the boat of thermal evaporation raw material, and the substrate of growth of one-dimensional nano structure is arranged at the thermal evaporation parts that are arranged in the heating furnace part.
The vacuum that described carrier gas outlet is used to take out the thermal evaporation parts.
Described carrier gas inlet is used for thermotropism evaporation component logical reacting gas, carrier gas and/or protective gas.
It is that the portion of hot evaporation component is at heating furnace that described thermal evaporation parts place heating furnace.
Described thermal evaporation parts are boiler tubes, and its cross sectional shape can be circle, rectangle or ellipse; Its material can be pottery, glass, quartz or metal.The preparation of one-dimensional nano structure material is finished in the thermal evaporation parts.
For the stable purpose that reaches steady-state evaporation, the material of the boat of the raw material transmission part in apparatus of the present invention-loading thermal evaporation raw material can be pottery, quartz, glass or metal.Mainly according to the selected material that loads the boat of thermal evaporation raw material of the maximum temperature of preparation one-dimensional nano structure material; How many sizes of the boat of loading thermal evaporation raw material is according to the size of thermal evaporation parts and deciding of flat-temperature zone size and required carrying raw material.
Described slide bar material can be pottery, quartz, glass or metal.The boat that its length will guarantee to load the thermal evaporation raw material is pushed to the center, flat-temperature zone of thermal evaporation parts.Described slide bar can move by modes such as hand push, magnetic force, electric power or hydraulic pressure.
Slide bar is used under the situation of system's air pressure and temperature stabilization raw material being transported to thermal evaporation with the boat that loads the thermal evaporation raw material and reacts warm area.Slide bar can make that the maintenance system is airtight in the process that slide bar moves by seal member.Equally can by magnetic drive device, electric drive or hydraulic transmission realize that slide bar moves and system between sealing.
The boat of described loading thermal evaporation raw material can move under the drive of slide bar.The boat and the slide bar that load the thermal evaporation raw material can be one or more according to the needs of preparation one-dimensional nano structure material.
The method of stably preparing one-dimensional nano structure material by heat evaporation of the present invention, this method may further comprise the steps:
(1) substrate of the growth one-dimensional nano structure door by the thermal evaporation parts is held in place in the thermal evaporation parts in the heating furnace, the substrate of this growth of one-dimensional nano structure is according to the needs of different one-dimensional nano structure material growths, can be crystal, quartz, pottery, glass or metal, in the substrate of growth of one-dimensional nano structure, metallic catalyst or non-metal catalyst can be arranged;
(2) will prepare one-dimensional nano structure material needs the raw material of thermal evaporation to be positioned in the boat that loads the thermal evaporation raw material, closes door, the boat that loads the thermal evaporation raw material is moved to an end of the described thermal evaporation parts of step (1) by slide bar;
(3) the thermal evaporation parts are evacuated down to vacuum at the bottom of the back of the body that needs by the carrier gas outlet of the thermal evaporation parts of step (2), carrier gas inlet by the thermal evaporation parts feeds carrier gas, reacting gas and/or protective gas then, and the stable gas pressure that makes the thermal evaporation parts is under the pressure of needs;
(4) the thermal evaporation parts to step (3) are heated to required temperature and make it stable by required firing rate and program;
(5) boat that step (2) is loaded the thermal evaporation raw material moves to the flat-temperature zone (thermal evaporation warm area) of the described thermal evaporation parts of step (4) by slide bar, at this moment, raw material just under the flat-temperature zone temperature evenly the evaporation, and in the substrate of growth of one-dimensional nano structure uniform and stable growth of one-dimensional nano structural material; By the time behind the certain hour, the boat that loads the thermal evaporation raw material is pulled out the low-temperature space of flat-temperature zone to the thermal evaporation parts by slide bar, raw material just stops evaporation;
(6) the temperature speed and the program as required of the described thermal evaporation parts of step (5) reduced to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, obtain the even one-dimensional nano structure material of stable growth.
Described metallic catalyst can be gold, silver, indium, gallium, iron, tin, aluminium, copper, magnesium or zinc.
Described protective gas can be argon gas, nitrogen, helium, hydrogen, neon or the mist between them.
Described carrier gas can be argon gas, nitrogen, helium, hydrogen, neon, air or the mist between them.
Described one-dimensional nano structure material can be nano wire, heterojunction nano-wire, nanometer rods, nano-pillar, nanotube, nano whisker, nanofiber, nanometer coaxial configuration or nanometer band.
Described thermal evaporation raw material can be at gentle volatilization or the evaporated liquid raw material that is become gas by liquid of depressing of uniform temperature, also can be uniform temperature gentle depress volatilization and distillation become the solid material of gas by solid.
The present invention compares with the apparatus and method of existing physics prepared by heat evaporation one-dimensional nano structure material, the invention provides a kind of apparatus and method of stably preparing one-dimensional nano structure material.The advantage of this method is: can control the evaporation of raw material well; Raw material steady-state evaporation under a stationary temperature and pressure be can make, thereby the stable growth and the uniformity of final one-dimensional nano structure material guaranteed.This device is by further expanding, a plurality of boats are set, each boat moves by slide bar separately, as required, under needed time and temperature, shift different raw materials onto needed position, so just realize the steady-state evaporation of many raw materials, can finish the preparation or the doping of multicomponent one-dimensional nano structure material.
Description of drawings
Fig. 1. the embodiment of the invention 1,2,3 is when stablizing the preparation nano wire, and thermal evaporation part temperatures and air pressure reach stable each preceding component locations schematic diagram.
Fig. 2. the embodiment of the invention 1,2,3 is when stablizing the preparation nano wire, and thermal evaporation part temperatures and air pressure reach each the component locations schematic diagram after stablizing.
Fig. 3. adopt Shuan Zhou and two slide bars in the embodiment of the invention 4, when stablizing preparation silicon germanium heterojunction nano wire, thermal evaporation part temperatures and air pressure reach stable each preceding component locations schematic diagram.
Fig. 4. employing Shuan Zhou and two slide bars in the embodiment of the invention 4, when stablizing preparation silicon germanium heterojunction nano wire, thermal evaporation part temperatures and air pressure reach each the component locations schematic diagram after stablizing.
Fig. 5. employing Shuan Zhou and two slide bars in the embodiment of the invention 4, when stablizing preparation silicon germanium heterojunction nano wire, thermal evaporation part temperatures and air pressure reach each the component locations schematic diagram after stablizing.
Fig. 6. the silicon nanowires of embodiment 1 preparation.
Fig. 7. the zinc oxide nanowire of embodiment 2 preparations.
Fig. 8. the alumina nanowires of embodiment 3 preparations.
Reference numeral
1. load the substrate of the boat 2. slide bars 3. growth of one-dimensional nano structures of thermal evaporation raw material
4. thermal evaporation parts 5. heating furnaces
The specific embodiment
The apparatus and method of embodiment 1. stable preparation silicon nanowires stable growths
See also Fig. 1.The device of thermal evaporation stably preparing one-dimensional nano structure comprises: load the boat 1 of thermal evaporation raw material, slide bar 2, substrate 3, one ends of growth of one-dimensional nano structure have the carrier gas outlet, and the other end has thermal evaporation parts 4, one tubular heaters 5 of carrier gas inlet.
Load the boat of thermal evaporation raw material and select the high-purity alumina ceramic boat for use, the length of loading the boat of thermal evaporation raw material is 12.5 centimetres, and wide and height respectively is 1.5 centimetres.Slide bar adopts aluminium oxide bar to make, and long 110 centimetres of slide bar is fixedlyed connected between the boat of slide bar and loading thermal evaporation raw material.Silicon single crystal flake is adopted in the substrate of growth of one-dimensional nano structure, and cleans through the semiconductor cleaning of standard; 15 centimetres apart from thermal evaporation parts center of the base silicon single-chips of growth of one-dimensional nano structure also are in the downstream that carrier gas is flowed.The thermal evaporation parts are that an external diameter of pipe is that 45 millimeters, internal diameter are 42 millimeters high-purity alumina ceramic pipe, and two ends seal by sealing ring, long 140 centimetres of thermal evaporation parts.The constant temperature head of district of tubular heater is 10 centimetres;
This device is used for the stable and uniform growth of silicon nanowires.Place described position through the silicon single crystal flake substrate of cleaning by the door of thermal evaporation parts with recited above.Silicon monoxide (SiO) raw material that 2.5 grams is used for thermal evaporation places in the boat that loads the thermal evaporation raw material, closes door, the boat that loads the thermal evaporation raw material is pulled out to an end of thermal evaporation parts with slide bar.By the carrier gas outlet whole thermal evaporation parts are evacuated down to 10
-4Pa back of the body end vacuum.By the mist (argon gas: the volume ratio of hydrogen is 95: 5) of carrier gas inlet feeding protective gas argon gas and hydrogen, flow is 100sccm.With stable gas pressure at the 20000Pa of needs pressure.By the time after the stable gas pressure, the thermal evaporation parts are raised to required temperature by heating furnace program and speed as required.Adopt in the present embodiment and evenly be warming up to 1350 ℃, programming rate is 10 ℃/minute.By the time thermal evaporation parts flat-temperature zone temperature stabilization after 1350 ℃, is shifted onto the boat that is loaded with thermal evaporation raw material silicon monoxide the flat-temperature zone (shown in Figure 2) of thermal evaporation parts by slide bar.The boat that loads the thermal evaporation raw material stopped in the flat-temperature zone 2 hours.Afterwards, the boat that loads the thermal evaporation raw material is pulled out the outer end (shown in Figure 1) of getting back to the thermal evaporation parts by slide bar.Then with program and the speed cooling on demand of thermal evaporation parts.Adopt the nature cooling in the present embodiment.By the time after the temperature of whole thermal evaporation parts drops to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, can obtain the silicon nanowires of stable growth.
The apparatus and method of embodiment 2. stable preparation zinc oxide nanowire stable growths
Present embodiment adopts the device as embodiment 1 structure.
Load the boat of thermal evaporation raw material and select quartz boat for use, the length of loading the boat of thermal evaporation raw material is 10 centimetres, and wide and height respectively is 1 centimetre.Slide bar adopts quartz to make, and long 100 centimetres of slide bar is fixedlyed connected between the boat of slide bar and loading thermal evaporation raw material.Alumina ceramic plate is adopted in the substrate of growth of one-dimensional nano structure, and cleans through the semiconductor cleaning of standard; 20 centimetres at the substrate aluminium oxide ceramics pitch of fins thermal evaporation parts center of growth of one-dimensional nano structure also is in the downstream that carrier gas is flowed.The thermal evaporation parts are that an external diameter of pipe is that 40 millimeters, internal diameter are 38 millimeters quartz ampoule, and two ends seal by sealing ring, long 120 centimetres of thermal evaporation parts.The constant temperature head of district of tubular heater is 8 centimetres;
This device is used for the stable and uniform growth of zinc oxide nanowire.Place described position through the alumina ceramic plate substrate of cleaning by the door of thermal evaporation parts with recited above.Zinc oxide powder and graphite are placed on the interior raw material as thermal evaporation of the boat that loads the thermal evaporation raw material with even mixing of ratio 1.5 grams of 10: 1 (weight ratio), close door, the boat that loads the thermal evaporation raw material is pulled out to an end of thermal evaporation parts with slide bar.By the carrier gas outlet whole thermal evaporation parts are evacuated down to 10
-3Pa back of the body end vacuum.The mist that feeds argon gas and oxygen by carrier gas inlet is as carrier gas (argon gas: the volume ratio of oxygen is 98: 2), and flow is 50sccm.With stable gas pressure at the 5000Pa of needs pressure.By the time after the stable gas pressure, the thermal evaporation parts are raised to required temperature by heating furnace program and speed as required.Adopt in the present embodiment and evenly be warming up to 1100 ℃, programming rate is 10 ℃/minute.By the time thermal evaporation parts flat-temperature zone temperature stabilization after 1100 ℃, is shifted onto the boat that is loaded with the thermal evaporation raw material flat-temperature zone (shown in Figure 2) of thermal evaporation parts by slide bar.The boat that loads the thermal evaporation raw material stopped in the flat-temperature zone 1 hour.Afterwards, the boat that loads the thermal evaporation raw material is pulled out the outer end (shown in Figure 1) of getting back to the thermal evaporation parts by slide bar.Then with program and the speed cooling on demand of thermal evaporation parts.Adopt the nature cooling in the present embodiment.By the time after the temperature of whole thermal evaporation parts drops to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, can obtain the zinc oxide nanowire of stable growth.
The apparatus and method of embodiment 3. stable preparation alumina nanowires stable growths
Present embodiment adopts the device as embodiment 1 structure.
Load the boat of thermal evaporation raw material and select the high-purity alumina ceramic boat for use, the length of loading the boat of thermal evaporation raw material is 12.5 centimetres, and wide and height respectively is 1.5 centimetres.Slide bar adopts the metal stainless steel to make, and long 110 centimetres of slide bar is fixedlyed connected between the boat of slide bar and loading thermal evaporation raw material.Silicon single crystal flake is adopted in the substrate of growth of one-dimensional nano structure, and cleans through the semiconductor cleaning of standard; 10 centimetres apart from thermal evaporation parts center of the base silicon single-chips of growth of one-dimensional nano structure also are in the downstream that carrier gas is flowed.The thermal evaporation parts are that an external diameter of pipe is that 45 millimeters, internal diameter are 42 millimeters high-purity alumina ceramic pipe, and two ends seal by sealing ring, long 140 centimetres of thermal evaporation parts.The constant temperature head of district of tubular heater is 10 centimetres;
This device is used for the stable and uniform growth of alumina nanowires.Place described position through the silicon single crystal flake substrate of cleaning by the door of thermal evaporation parts with recited above.Alumina powder and aluminium powder and graphite are evenly mixed the raw material that is placed in the boat that loads the thermal evaporation raw material as thermal evaporation with ratio 1 gram of 10: 1: 5 (weight ratio), close door, the boat that loads the thermal evaporation raw material is pulled out to an end of thermal evaporation parts with slide bar.By the carrier gas outlet whole thermal evaporation parts are evacuated down to 10
-3Pa back of the body end vacuum.The mist that feeds argon gas and hydrogen by carrier gas inlet is as carrier gas (argon gas: the volume ratio of hydrogen is 95: 5), and flow is 60sccm.With stable gas pressure at the 50000Pa of needs pressure.By the time after the stable gas pressure, the thermal evaporation parts are raised to required temperature by heating furnace program and speed as required.Adopt in the present embodiment and evenly be warming up to 1150 ℃, programming rate is 10 ℃/minute.By the time thermal evaporation parts flat-temperature zone temperature stabilization after 1150 ℃, is shifted onto the boat that is loaded with the thermal evaporation raw material flat-temperature zone (shown in Figure 2) of thermal evaporation parts by slide bar.The boat that loads the thermal evaporation raw material stopped in the flat-temperature zone 90 minutes.Afterwards, the boat that loads the thermal evaporation raw material is pulled out the outer end (shown in Figure 1) of getting back to the thermal evaporation parts by slide bar.Then with program and the speed cooling on demand of thermal evaporation parts.Adopt the nature cooling in the present embodiment.By the time after the temperature of whole thermal evaporation parts drops to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, can obtain the alumina nanowires of stable growth.
The apparatus and method of embodiment 4 stable preparation silicon germanium heterojunction nano wire stable growths
See also Fig. 3, the device of thermal evaporation stably preparing one-dimensional silicon germanium heterojunction nano wire comprises: 21,2 slide bars 2 of boat that load the thermal evaporation raw material, the substrate 3 of growth of one-dimensional nano structure, one end has the carrier gas outlet, and the other end has thermal evaporation parts 4, one tubular heaters 5 of carrier gas inlet.
2 boats that load the thermal evaporation raw material are all selected the high-purity alumina ceramic boat for use, and the length of loading the boat of thermal evaporation raw material is 12.5 centimetres, and wide and height respectively is 1.5 centimetres.2 slide bars all adopt aluminium oxide bar to make, and all long 110 centimetres of slide bar, 2 slide bars are fixedlyed connected respectively with between 2 boats that load the thermal evaporation raw materials.Silicon single crystal flake is adopted in the substrate of growth of one-dimensional nano structure, and cleans through the semiconductor cleaning of standard; 15 centimetres apart from thermal evaporation parts center of the base silicon single-chips of growth of one-dimensional nano structure also are in the downstream that carrier gas is flowed.The thermal evaporation parts are that an external diameter of pipe is that 45 millimeters, internal diameter are 42 millimeters high-purity alumina ceramic pipe, and two ends seal by sealing ring, long 140 centimetres of thermal evaporation parts.The constant temperature head of district of tubular heater is 10 centimetres;
This device is used for the stable and uniform growth of silicon germanium heterojunction nano wire.Place described position through the silicon single crystal substrate of cleaning by the door of thermal evaporation parts with recited above.Silicon monoxide (SiO) raw material that 2.5 grams is used for thermal evaporation places in the boat of a loading thermal evaporation raw material, germanium monoxide (GeO) raw material that 2.5 grams is used for thermal evaporation places in another boat that loads the thermal evaporation raw material, close door, the boat of 2 loading thermal evaporation raw materials is pulled out to an end of thermal evaporation parts with slide bar.By the gas outlet whole thermal evaporation parts are evacuated down to 10
-4Pa back of the body end vacuum.By the mist (argon gas: the volume ratio of hydrogen is 95: 5) of carrier gas inlet feeding protective gas argon gas and hydrogen, flow is 100sccm.With stable gas pressure at the 20000Pa of needs pressure.By the time after the stable gas pressure, the thermal evaporation parts are raised to required temperature by heating furnace program and speed as required.Adopt in the present embodiment and evenly be warming up to 1350 ℃, programming rate is 8 ℃/minute.By the time thermal evaporation parts flat-temperature zone temperature stabilization after 1350 ℃, is shifted onto the boat that is loaded with thermal evaporation raw material silicon monoxide the flat-temperature zone (shown in Figure 4) of thermal evaporation parts by slide bar.The boat that loads thermal evaporation raw material silicon monoxide stopped in the flat-temperature zone 2 minutes.Afterwards, the boat that is loaded with thermal evaporation raw material silicon monoxide is pulled out the outer end (shown in Figure 3) of getting back to the thermal evaporation parts by slide bar.Afterwards, the boat that is loaded with thermal evaporation raw material germanium monoxide is shifted onto the flat-temperature zone (shown in Figure 5) of thermal evaporation parts by slide bar.The boat of heat-carrying evaporation raw material germanium monoxide stopped in the flat-temperature zone 2 minutes.Afterwards, the boat that will be loaded with thermal evaporation raw material germanium monoxide is again pulled out the outer end of getting back to the thermal evaporation parts by slide bar.Repeat above process, alternately shift the boat that is loaded with the boat of thermal evaporation raw material silicon monoxide and be loaded with thermal evaporation raw material germanium monoxide onto flat-temperature zone and stopped 2 minutes.Repeat 500 times.The boat of two heat-carrying evaporation raw materials is all pulled out the outer end (shown in Figure 3) of getting back to the thermal evaporation parts.Then with program and the speed cooling on demand of thermal evaporation parts.Adopt the nature cooling in the present embodiment.By the time after the temperature of whole thermal evaporation parts drops to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, can obtain the silicon germanium heterojunction nano wire of stable growth.
It must be noted that, the raw material transmission means that apparatus and method provided by the present invention are not limited to adopt among the embodiment, also adopt the raw material that other transmission means is evaporated heat-carrying in the boat of raw material under apparatus system reaches stable state, to be sent to the temperature province that needs thermal evaporation, such as, adopt magnetic force conveyer, electric power to transmit fluid-pressure transmission device etc.In a word, the present invention has comprised other method that the thermal evaporation raw material is sent to the appointment warm area.
Certainly, the present invention also comprises the transmission compound mode of other raw material, such as, as the doping of one-dimensional nano structure material preparation, can reach at thermal evaporation part temperatures and pressure and simultaneously or one in front and one in back shift one-dimensional nano structure growth raw material and doped raw material the position that needs of thermal evaporation parts onto by slide bar separately after stable by the boat of separately heat-carrying evaporation raw material.
In addition, those skilled in the art can also do other variation in spirit of the present invention, and certainly, the variation that these are done according to spirit of the present invention all should be forgiven within the present invention's scope required for protection.
Claims (10)
1. the device of a thermal evaporation stably preparing one-dimensional nano structure, this device comprises: load the boat of thermal evaporation raw material, slide bar, the substrate of growth of one-dimensional nano structure, thermal evaporation parts, heating furnace; It is characterized in that:
One end of one thermal evaporation parts has the carrier gas outlet, and the other end has carrier gas inlet;
The thermal evaporation parts place heating furnace, an end that has carrier gas inlet at the thermal evaporation parts is equipped with one, the slide bar that can stretch in the thermal evaporation parts is installed on door, slide bar fixedly connected one loads the boat of thermal evaporation raw material, and the substrate of growth of one-dimensional nano structure is arranged at the thermal evaporation parts that are arranged in the heating furnace part.
2. device according to claim 1 is characterized in that: it is that the portion of hot evaporation component is at heating furnace that described thermal evaporation parts place heating furnace.
3. device according to claim 1 and 2 is characterized in that: described thermal evaporation parts are boiler tubes, and its cross sectional shape is circle, rectangle or ellipse; The material of thermal evaporation parts is pottery, glass, quartz or metal.
4. device according to claim 1 is characterized in that: the boat of described loading thermal evaporation raw material and slide bar are one or more.
5. according to claim 1 or 4 described devices, it is characterized in that: the material of the boat of described loading thermal evaporation raw material is pottery, quartz, glass or metal; Described slide bar material is pottery, quartz, glass or metal.
6. device according to claim 1 is characterized in that: the substrate of described growth of one-dimensional nano structure is crystal, quartz, pottery, glass or metal.
7. a method of utilizing each described device stably preparing one-dimensional nano structure material by heat evaporation of claim 1～6 is characterized in that, this method may further comprise the steps:
(1) substrate of the growth one-dimensional nano structure door by the thermal evaporation parts is held in place in the thermal evaporation parts in the heating furnace;
(2) will prepare one-dimensional nano structure material needs the raw material of thermal evaporation to be positioned in the boat that loads the thermal evaporation raw material, closes door, the boat that loads the thermal evaporation raw material is moved to an end of the described thermal evaporation parts of step (1) by slide bar;
(3) the thermal evaporation parts are evacuated down to vacuum at the bottom of the back of the body that needs by the carrier gas outlet of the thermal evaporation parts of step (2), carrier gas inlet by the thermal evaporation parts feeds carrier gas, reacting gas and/or protective gas then, and the stable gas pressure that makes the thermal evaporation parts is under the pressure of needs;
(4) the thermal evaporation parts to step (3) are heated to required temperature and make it stable by required firing rate and program;
(5) boat that step (2) is loaded the thermal evaporation raw material moves to the flat-temperature zone of the described thermal evaporation parts of step (4) by slide bar, at this moment, raw material just under the flat-temperature zone temperature evenly the evaporation, and in the substrate of growth of one-dimensional nano structure stable and uniform growth of one-dimensional nano structural material; By the time behind the certain hour, the boat that loads the thermal evaporation raw material is pulled out the low-temperature space of flat-temperature zone to the thermal evaporation parts by slide bar, raw material just stops evaporation;
(6) the temperature speed and the program as required of the described thermal evaporation parts of step (5) reduced to room temperature, open the door of thermal evaporation parts, take out the substrate of growth of one-dimensional nano structure, in the substrate of growth of one-dimensional nano structure, obtain the even one-dimensional nano structure material of stable growth.
8. method according to claim 7 is characterized in that: metallic catalyst is further arranged in the substrate of growth of one-dimensional nano structure.
9. method according to claim 8 is characterized in that: described metallic catalyst is gold, silver, indium, gallium, iron, tin, aluminium, copper, magnesium or zinc.
10. method according to claim 7 is characterized in that: described one-dimensional nano structure material is nano wire, heterojunction nano-wire, nanometer rods, nano-pillar, nanotube, nano whisker, nanofiber, nanometer coaxial configuration or nanometer band.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102219180A (en) * | 2010-04-14 | 2011-10-19 | 中国科学院理化技术研究所 | Method for synthesizing one-dimensional inorganic nano cone structure material by pressure control in VLS process |
| CN106498491A (en) * | 2016-11-02 | 2017-03-15 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant of vapor phase method crystal growth raw material and its method of purification |
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| US6036774A (en) * | 1996-02-26 | 2000-03-14 | President And Fellows Of Harvard College | Method of producing metal oxide nanorods |
| CN1252311C (en) * | 2002-07-17 | 2006-04-19 | 清华大学 | Process for preparing large-area zinc oxide film with nano lines by physical gas-phase deposition |
| CN2649228Y (en) * | 2003-07-17 | 2004-10-20 | 上海交通大学 | Multi-purpose ond-dimensional nano material preparing apparatus by hight-frequency induction heating |
| JP2005336043A (en) * | 2004-05-27 | 2005-12-08 | Tomoaki Terasako | Carbon nanotube and method of manufacturing carbon fiber |
| CN1670270A (en) * | 2004-12-30 | 2005-09-21 | 湖南大学 | Nanometer material growth controllable vacuum tube type reacting equipment |
| CN1667856A (en) * | 2005-04-08 | 2005-09-14 | 中国科学院上海微系统与信息技术研究所 | High-capacity lithium ion cell anode material and process for preparing same |
| CN101007631A (en) * | 2006-01-27 | 2007-08-01 | 索尼株式会社 | Mono-layer carbon nanotube and its preparation method, and electronic element preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102219180A (en) * | 2010-04-14 | 2011-10-19 | 中国科学院理化技术研究所 | Method for synthesizing one-dimensional inorganic nano cone structure material by pressure control in VLS process |
| CN102219180B (en) * | 2010-04-14 | 2013-05-01 | 中国科学院理化技术研究所 | Method for synthesizing one-dimensional inorganic nano cone structure material by pressure control in VLS process |
| CN106498491A (en) * | 2016-11-02 | 2017-03-15 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant of vapor phase method crystal growth raw material and its method of purification |
| CN106498491B (en) * | 2016-11-02 | 2018-12-14 | 中国电子科技集团公司第四十六研究所 | A kind of purifying plant and its method of purification of vapor phase method crystal growth raw material |
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