CN101091893A - Vacuum tube furnace for preparing Nano material - Google Patents
Vacuum tube furnace for preparing Nano material Download PDFInfo
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- CN101091893A CN101091893A CN 200710017880 CN200710017880A CN101091893A CN 101091893 A CN101091893 A CN 101091893A CN 200710017880 CN200710017880 CN 200710017880 CN 200710017880 A CN200710017880 A CN 200710017880A CN 101091893 A CN101091893 A CN 101091893A
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- vacuum chamber
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Abstract
The invention publishes a vacuum pipe heater for producing nano-materials. It includes the seal vacuum chamber (2), which is inside of the furnace body (1). The substrate (7) establishes at the bottom of the seal vacuum chamber (2). Its characteristic is: the vacuum chamber (2) connects with a source material evaporator (16) which can control and adjust the source material evaporation speed. The source material evaporator (16) connects with the end of the seal vacuum chamber (2) in vertical. The invention uses the control source constituent technology, which can realize accuracy control, gradient doping and substrate operation. The whole system use computer to control, therefore it has high automaticity, high control precision, accurate data. The equipment also has simple character, compact structure, simple operation, low working cost, high production efficiency, saving energy and so on.
Description
Technical field
The present invention relates to a kind of equipment for preparing nano material, particularly a kind of vacuum tube furnace for preparing nano material.
Background technology
Nano wire, nano thin-film can be synthetic by several different methods, and wherein vapor growth method is topmost method.The principle of vapor phase growth is that source material is converted into gaseous state by processes such as distillation, evaporation, decomposition, makes it become supersaturated vapour then under suitable condition, grows crystal through condensation-crystallization.Sheng Chang crystal purity height in this way, integrality is good.Because fluid phase (gas phase) molecular density of crystal growth is very low, the specific volume of gas phase and solid phase differs greatly, make that the speed of grown crystal is all more much lower than the speed from melt or growth from solution from gas phase, so this method mainly is to be used for growing whisker and thickness greatly about the films of several microns to the hundreds of micron, promptly usually said vapor phase epitaxy technique at present.This be most important in the present vapor phase method also be a field with the fastest developing speed.
In physical vaporous deposition, thermal evaporation is the most frequently used growing method.Way commonly used is, utilize vacuum tube furnace, single source material, or evaporate a certain position that the source material that mixes is placed in the vacuum drying oven, material atom that evaporates or atomic group family are under the conveying of carrier gas, under certain metallic catalyst effect,, form one-dimensional nano line through the vapour deposition process of self-organization according to VLS (vapor-liquid-solid) mechanism.Thermal evaporation is one of physical vaporous deposition (PVD), thermal evaporation has advantages such as equipment is simple, easy and simple to handle, cost of use is low, also has higher deposition velocity, higher relatively vacuum, and cause thus than characteristics such as high-crystal qualities, so evaporation has been subjected to largely paying attention to.But this method also has its tangible limitation.As, above-mentioned single source evaporation technique can be applied to element, or the compound that evenly distils, perhaps those more approaching materials of the steaming pressure ratio of component.And the vapour pressure that can not be applied to component has the very evaporation of those compounds of big difference, because than the constituent element that is easier to volatilize before another constituent element of any considerable amount is transported to, just almost can all evaporate, in this case, finally can make the deposited film layering, or gradient appears on composition, and promptly enabling to reach stable state, its composition also can have very big difference with initial feed.Therefore, present thermal evaporation tube furnace technology can not effectively address this problem, want this compounds is adopted vacuum evaporation technique, present method is: adopt continuous dosing flash evaporation technology, the compound crystal growth of big-difference has certain effect although this technology is pressed with very for the steam that overcomes component element, but effect is still unsatisfactory, still can not more accurately control the composition of growth material.
Molecular beam epitaxy (MBE) is a kind of epitaxy technology that grows up on the basis of vacuum evaporation.It mainly comprises: the ultravacuum system; Molecular beam, specimen holder and sample transmission system; QMS; The detection system on monocrystal thin films surface.Major advantage is: growth temperature is low, has very low growth rate; Growth conditions can accurately be controlled, and in the molecular beam epitaxy device, is equipped with the molecular beam evaporation source, and the component of film and doping content can be adjusted rapidly with the variation of evaporation source.But the shortcoming of molecular beam epitaxy technique is: the equipment complexity, cost an arm and a leg, and will consume a large amount of liquid nitrogen during use, and rate of crystalline growth is very slow.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of vacuum tube furnace for preparing nano material is provided, and this vacuum tube furnace can be controlled the evaporation rate of each source material respectively, finally improves the Composition Control precision of tube furnace growth material.
For solving the problems of the technologies described above, the present invention is achieved in that it comprises the vacuum chamber (2) of sealing, described vacuum chamber (2) is arranged in the body of heater (1), the interior airflow downstream of vacuum chamber (2) place is provided with substrate (7), it is characterized in that: this vacuum chamber (2) is connected with at least one the source material evaporimeter (16) that can control and regulate the source material evaporation rate, and described source material evaporimeter (16) is connected the end of vacuum chamber (2) perpendicular to airflow direction.
Described source material evaporimeter (16) comprises end cap (20), lead (21), sleeve (22), encapsulant (25), evaporation cover (26), heating wire (27); One end of described sleeve (22) inserts in the described evaporation cover (26), the other end of sleeve (22) connects end cap (20), lead (21) passes end cap (20) and links to each other with the interior heating wire (27) of sleeve (22) and evaporation cover (26), is provided with circular open (28) on described evaporation cover (26).
Described source material evaporimeter (16) is connected with vacuum chamber (2) by sealing termination (3).
For in crystal growth, substrate is carried out former bit manipulation, the other end of described vacuum chamber (2) is provided with magnetic push rod (5).
Described magnetic links to each other with push rod (5) with vacuum chamber (2) magnetic by sealing termination (3) with push rod (5).
Described vacuum chamber (2) is connected with carrier gas system (11,12) along an end of airflow direction by sealing termination (3).
Described sealing termination (3) is connected with cooling water system (10).
Be provided with O RunddichtringO (9) between described sealing termination (3) and the vacuum chamber (2).
Described vacuum chamber (2) is provided with thermocouple (17).
The invention has the beneficial effects as follows:
The present invention is equipped with the source material evaporimeter on tube furnace, control the evaporation rate of each source material respectively, finally improves the Composition Control precision of tube furnace growth material; On tube furnace, set up the magnetic force push rod, in crystal growth, can carry out former bit manipulation substrate.The present invention adopts control source component flux technique, can realize the functions such as former bit manipulation of accurate control, grade doping and the substrate of component; Total system is by computer control, so the accuracy of automaticity height, control accuracy height, data is strong; This equipment has also that equipment is simple, compact conformation, easy and simple to handle, cost of use is low etc., production efficiency height, energy savings advantage.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the structural representation of source material evaporimeter 16 of the present invention.
The specific embodiment
As shown in Figure 1, the whole nano material growth course of the present invention is carried out in vacuum chamber, in order to control the evaporation rate of each source material respectively, the final Composition Control precision that improves the tube furnace growth material is provided with the source material evaporimeter 16 that at least one could control and regulate the source material evaporation rate at vacuum chamber 2 one ends.Described vacuum chamber 2 is arranged in the body of heater 1, is provided with calandria 8 in body of heater 1, and described body of heater 1 is connected with body of heater heating power supply 15, and described vacuum chamber 2 is provided with thermocouple 17, is used to measure temperature in the stove.Owing to produce very high temperature during the source material evaporation, be connected with cooling water system 10 in described sealing termination 3.The airflow downstream place is provided with substrate 7 in vacuum chamber 2, is used to receive the nano material of growth; The two ends of vacuum chamber 2 are provided with O RunddichtringO 9 by 3 sealings of sealing termination between sealing termination 3 and the vacuum chamber 2, and vacuum chamber 2 also is connected with the vacuum system 6 that is used to bleed.For the source material that makes evaporation is transported on the substrate 7, described vacuum chamber 2 is connected with carrier gas system 11,12; For in crystal growth, substrate is carried out former bit manipulation, the other end of described vacuum chamber 2 is provided with magnetic push rod 5.
As shown in Figure 2, described source material evaporimeter 16 comprises end cap 20, lead 21, sleeve 22, encapsulant 25, evaporation cover 26, heating wire 27; One end of described sleeve 22 inserts in the described evaporation cover 26, and the other end of sleeve 22 connects end cap 20, and lead 21 passes end cap 20 and links to each other with the heating wire 27 that sleeve 22 and evaporation are overlapped in 26, is provided with circular open 28 at described evaporation cover 26.Nut 18 seal washers 19 are fixed on source material evaporimeter 16 on the sealing termination 3 and with vacuum chamber 2 with nut 24, seal washer 23 and link to each other.
Embodiment 1: growth ZnCdO nano wire
Growth course is as follows:
Whole nanometer village material growth course is carried out in vacuum chamber (quartz ampoule), before the material growth of nanometer village, earlier source material Zn, Cd metal dust is placed on respectively in the source material evaporimeter 16, and substrate 7 is placed on airflow downstream place in the quartz ampoule.Start cooling water system 10, vacuum system 6, make the middle vacuum of vacuum chamber (quartz ampoule) be not less than 5 * 10
-3Pa.According to the thermograde of setting, start body of heater 1 heating power supply 15, the temperature at substrate 7 places is reached～500 ℃, and meet technological requirement, if be not suitable for, can use the position of 5 pairs of substrates 7 of magnetic force push rod to adjust.According to technology, open source material evaporimeter power supply 14, control and regulate the evaporation rate of each constituent element respectively, component source is entered in the vacuum chamber 2 (quartz ampoule) according to certain flow, each source material heating-up temperature is controlled at respectively in the temperature range of fusing point+50 ℃, the temperature that is Zn (fusing point is 419 ℃) is about 469 ℃, and the temperature of Cd (fusing point is 321 ℃) is 371 ℃.Open carrier gas system 11 output carrier gas 1, carrier gas 1 is a high-purity argon gas, and purity is 99.9%, and (sccm is cm with 5～10sccm in carrier gas 1
3/ min) flow enters in the quartz ampoule, arrives under the conveying of carrier gas 1 above the substrate.Open carrier gas system 12, output carrier gas 2 (reacting gas, as high-purity oxygen, purity is 99.99%) enters in the vacuum chamber 2 (quartz ampoule) its flow with 2～5sccm, and the ZnCdO nano wire is in the silicon substrate crystallization under carrier gas 2 effects.Behind the growth ending, powered-down is opened vacuum chamber, takes out sample and can observe and test sample.
The present invention can grow as required ZnO and various zno-based compound semiconductor nano material are as semiconductor nano materials such as ZnO, ZnS, ZnMnO and ZnMgO.
The growth of the nano material of the present invention's growth and prior art growth has the following advantages:
1. composition precision height;
2. the crystal mass height of nano material, defective is few;
Embodiment 2: growth ZnMgO nano wire
Growth ZnMgO nano wire is similar substantially to the growth course of growth ZnCdO nano wire, and the present embodiment evaporating temperature is that the temperature of Zn (fusing point is 419 ℃) is about 469 ℃, and the temperature of Mg (fusing point is: 649 ℃) is 699 ℃.
Claims (9)
1, a kind of vacuum tube furnace for preparing nano material, it comprises the vacuum chamber (2) of sealing, described vacuum chamber (2) is arranged in the body of heater (1), described vacuum chamber (2) is provided with the carrier gas (11) that is used for delivery source material steam and is used for carrier gas (12) with the source material vapor reaction, the interior airflow downstream of vacuum chamber (2) place is provided with substrate (7), it is characterized in that: this vacuum chamber (2) is connected with at least one the source material evaporimeter (16) that can control and regulate the source material evaporation rate, and described source material evaporimeter (16) is connected the end of vacuum chamber (2) perpendicular to airflow direction.
2, the vacuum tube furnace of preparation nano material according to claim 1 is characterized in that: described source material evaporimeter (16) comprises end cap (20), lead (21), sleeve (22), encapsulant (25), evaporation cover (26), heating wire (27); One end of described sleeve (22) inserts in the described evaporation cover (26), the other end of sleeve (22) connects end cap (20), lead (21) passes end cap (20) and links to each other with the interior heating wire (27) of sleeve (22) and evaporation cover (26), is provided with circular open (28) on described evaporation cover (26).
3, the vacuum tube furnace of preparation nano material according to claim 1 and 2 is characterized in that: described source material evaporimeter (16) is connected with vacuum chamber (2) by sealing termination (3).
4, the vacuum tube furnace of preparation nano material according to claim 1 is characterized in that: described vacuum chamber (2) is provided with magnetic push rod (5).
5, the vacuum tube furnace of preparation nano material according to claim 4 is characterized in that: described magnetic links to each other with push rod (5) with vacuum chamber (2) magnetic by sealing termination (3) with push rod (5).
6, the vacuum tube furnace of preparation nano material according to claim 1 is characterized in that: described vacuum chamber (2) is connected with carrier gas system (11,12) along an end of airflow direction by sealing termination (3).
7, according to the vacuum tube furnace of claim 3 or 5 or 6 described preparation nano materials, it is characterized in that: described sealing termination (3) is connected with cooling water system (10).
8, the vacuum tube furnace of preparation nano material according to claim 7 is characterized in that: be provided with O RunddichtringO (9) between described sealing termination (3) and the vacuum chamber (2).
9, the vacuum tube furnace of preparation nano material according to claim 1 is characterized in that: described vacuum chamber (2) is provided with thermocouple (17).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100178803A CN101091893B (en) | 2007-05-18 | 2007-05-18 | Vacuum tube furnace for preparing nano material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100178803A CN101091893B (en) | 2007-05-18 | 2007-05-18 | Vacuum tube furnace for preparing nano material |
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| Publication Number | Publication Date |
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| CN101091893A true CN101091893A (en) | 2007-12-26 |
| CN101091893B CN101091893B (en) | 2010-12-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2007100178803A Expired - Fee Related CN101091893B (en) | 2007-05-18 | 2007-05-18 | Vacuum tube furnace for preparing nano material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268736A (en) * | 2011-07-06 | 2011-12-07 | 西安建筑科技大学 | Method for preparing silicon carbide nanowire array through gas phase interlayer diffusion reaction process |
| CN105908254A (en) * | 2016-06-12 | 2016-08-31 | 中国科学院上海技术物理研究所 | Casing pipe type cavity structure for preparing semiconductor material |
| CN109423696A (en) * | 2017-08-24 | 2019-03-05 | 北京大学深圳研究生院 | A kind of grower of multilayer organic single-crystal structure |
-
2007
- 2007-05-18 CN CN2007100178803A patent/CN101091893B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268736A (en) * | 2011-07-06 | 2011-12-07 | 西安建筑科技大学 | Method for preparing silicon carbide nanowire array through gas phase interlayer diffusion reaction process |
| CN102268736B (en) * | 2011-07-06 | 2013-05-08 | 西安建筑科技大学 | Method for preparing silicon carbide nanowire array through gas phase interlayer diffusion reaction process |
| CN105908254A (en) * | 2016-06-12 | 2016-08-31 | 中国科学院上海技术物理研究所 | Casing pipe type cavity structure for preparing semiconductor material |
| CN105908254B (en) * | 2016-06-12 | 2018-07-06 | 中国科学院上海技术物理研究所 | A kind of bushing type cavity body structure for being used to prepare semi-conducting material |
| CN109423696A (en) * | 2017-08-24 | 2019-03-05 | 北京大学深圳研究生院 | A kind of grower of multilayer organic single-crystal structure |
| CN109423696B (en) * | 2017-08-24 | 2021-07-23 | 北京大学深圳研究生院 | Growing device of multilayer organic single crystal structure |
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| Publication number | Publication date |
|---|---|
| CN101091893B (en) | 2010-12-08 |
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Granted publication date: 20101208 Termination date: 20110518 |