CN101323970A - Tubular furnace and method for changing growth substrate or source material position using the same - Google Patents
Tubular furnace and method for changing growth substrate or source material position using the same Download PDFInfo
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- CN101323970A CN101323970A CNA2008101167514A CN200810116751A CN101323970A CN 101323970 A CN101323970 A CN 101323970A CN A2008101167514 A CNA2008101167514 A CN A2008101167514A CN 200810116751 A CN200810116751 A CN 200810116751A CN 101323970 A CN101323970 A CN 101323970A
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Abstract
The invention discloses a tubular furnace and comprises following components: a furnace body; a refractory tube that has one part placed inside the furnace body and the other part exposed outside the furnace body; a sample platform that is placed inside the refractory tube; a ferromagnetic drive element that is placed inside the refractory tube, connected with the sample platform through a connecting rod and placed in the part of the refractory tube that is exposed outside the furnace body; a magnet that is arranged on an outer wall of the part of the refractory tube that is exposed outside the furnace body, moves along the axial direction of the refractory tube and drives the ferromagnetic drive element, the connecting rod and the sample platform to move under magnetic force. The tubular furnace utilizes that temperature is different in different positions inside the tubular furnace, can quickly change the positions of growth substrates or source materials so as to adjust the temperature of the growth substrates or the source materials, and can be used in heated state without affecting the air tightness of the tubular furnace, and can be used for preparing various nano wire and nano film materials. Furthermore, the tubular furnace has the advantages of simple operations, low cost, high movement precision and high speed.
Description
Technical field
The present invention relates to field of nano material preparation, particularly relate to a kind of position and method of temperature that in tube furnace, changes growth substrate or source material.
Background technology
Many nano materials can prepare by vapor growth method.The vapor phase growth ratio juris is to be gaseous state with the source material thermal conversion, deposits out in the growth substrate position under the condition of catalyzer catalyzer being arranged or do not have then, is grown to nanocrystal.The general crystal mass of the nano material that obtains in this way is good, and controllability is stronger, can obtain the extraordinary one dimension of quality, two-dimensional nano material.
Vacuum tube furnace is a vapor growth method equipment commonly used, its interior temperature distribution is heterogeneity often, usually one or several source materials being placed on the interior a certain position of pipe evaporates, atom that evaporates or elementide arrive the growth substrate position under the conveying of carrier gas, catalyzer being arranged or not having the condition deposit of catalyzer to come out, obtain product.Vacuum tube furnace has that equipment is simple, and expense is low, and is simple to operate, vacuum tightness advantages of higher, the nano material that can obtain being of high quality.
General vacuum tube furnace is in order to guarantee resistance to air loss, and the back of starting working just can't mobile growth substrate or source material, also is difficult in the temperature that change growth substrate fast or source material are carried out in the process in reaction.This makes many special constructions, is restricted such as the preparation of high temperature crystal phase structure, heterojunction structure, one dimension block structure, multi-layer film structure.
Summary of the invention
The objective of the invention is to overcome the defective of above-described vacuum tube furnace, a kind of resistance to air loss that does not influence tube furnace is provided, in under tube furnace is in running order, move forward and backward growth substrate or source material position, and then the tube furnace and the method for control growing substrate or source material temperature of living in.
For achieving the above object, on the one hand, technical scheme of the present invention provides a kind of tube furnace, comprises body of heater, also comprises: high-temperature resistant tube, comprise two portions, and a part is placed in the body of heater, and a part is exposed to outside the body of heater; Sample table is placed in described anti-this high temperature pipe, is used to place growth substrate or source material; Ferromagnetic driving element is placed in described anti-this high temperature pipe, is connected with described sample table by union lever, and described ferromagnetic driving element is positioned over described high-temperature resistant tube and is exposed to the outer part of body of heater; Magnet is arranged on the outer wall that described high-temperature resistant tube is exposed to the body of heater outside part, and described magnet moves along described high-temperature resistant tube axial direction due, drives described ferromagnetic driving element, union lever and sample table and move under the effect of magnetic force.
Wherein, described sample table and union lever are made by high temperature material.
Wherein, described high temperature material is fused quartz or aluminium sesquioxide.
Wherein, described ferromagnetic driving element is made by the material that magneticsubstance maybe can be magnetized.
Wherein, described ferromagnetic driving element is colyliform, bulk or thread.
Wherein, described magnet is permanent magnet or electro-magnet.
Wherein, described permanent magnet is a SmCo magnet.
Wherein, described SmCo magnet is cylindrical.
On the other hand, technical scheme of the present invention provides a kind of method of utilizing above-mentioned tube furnace to change the position of growth substrate or source material, may further comprise the steps: growth substrate or source material are positioned on the sample table, vacuumize the logical argon gas in back in the tube furnace repeatedly, remove furnace air, stop logical rare gas element then, and vacuumize; Heating tube furnace center feeds rare gas element, and begins to bleed to design temperature, keep-ups pressure in setup pressure value; Be incubated under described design temperature, the insulation back attracts ferromagnetic driving element with magnet, adjusts described growth substrate or the source material position at described tube furnace, changes warm area, continues insulation; Attract with magnet at last, growth substrate or source material are drawn out to high-temperature resistant tube are exposed to the outer part of body of heater, reduce to room temperature, logical rare gas element is opened tube furnace to normal pressure, takes out growth substrate or source material.
Wherein, growth substrate or source material being drawn out to after high-temperature resistant tube is exposed to part outside the body of heater, also comprise: use cooling fluid or radiator element that high-temperature resistant tube is exposed to the outer part of body of heater and lower the temperature.
Technique scheme only is an optimal technical scheme of the present invention, has following advantage: the temperature difference of utilizing different positions in the tube furnace, change the position of growth substrate or source material fast, adjust the temperature of growth substrate or source material, can under heated condition, use, not influence the resistance to air loss of tube furnace, can be used for vapor growth method and prepare diversified nano material, realize changing fast the material growth conditions, to prepare various nano wires, nano film material.And the advantage that the present invention has is simple to operate, mobile accuracy is high, speed is fast, cost is low.
Description of drawings
Fig. 1 is the structural representation of a kind of tube furnace of the embodiment of the invention.
Wherein, 1: ferromagnetic driving element; 2: union lever; 3: sample table; 4: magnet; 5: high-temperature resistant tube; 6: body of heater.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
In conjunction with Fig. 1, the tube furnace of present embodiment comprises body of heater 6, high-temperature resistant tube 5, sample table 3, ferromagnetic driving element 1, magnet 4 and union lever 2.At first, sample table 3, ferromagnetic driving element 1 and union lever 2 are placed in anti-this high temperature pipe 5, and the used high-temperature resistant tube 5 of tube furnace need have a segment length to be exposed to outside the body of heater 6.Growth substrate or source material are positioned on the high temperature material manufactured samples platform 3, and the union lever of making by high temperature material 2 links to each other with ferromagnetic driving element 1.Before the heating beginning, sample table 3, union lever 2 are put into tube furnace with ferromagnetic driving element 1, wherein ferromagnetic driving element 1 is positioned over high-temperature resistant tube 5 and is exposed to body of heater 6 part outward.Tube furnace sealing, and after beginning to enter working order, put sample well after, high temperature pipe 5 two ends seals down in working order, attract ferromagnetic driving element 1 to make its motion in high-temperature resistant tube 5 outsides by magnet 4, and drive growth substrate or source material change position.Utilize the temperature difference of different positions in the tube furnace, regulate the temperature of growth substrate or source material.Also sample or source material can be moved to high-temperature resistant tube and be exposed to the outer part of body of heater, use outer heating/cooling device, as the quick cooling of realization sample such as radiator element, cooling fluid or source material.
The material of the sample table 3 that the present invention adopts can be chosen fused quartz, Al2O3 or other high temperature materials according to Heating temperature.Its size shape must guarantee that it can put into tube furnace, and carrying growth substrate or source material that can be safe.Make the material of union lever 2 and can choose fused quartz, Al2O3 or other high temperature materials according to Heating temperature.Union lever 2 can be by mechanical connection with sample table 3, also can sintering together.Can also directly make longer sample table 3, the function of the bar 2 that is integrated and connected directly links to each other with ferromagnetic driving element 1.Total length from sample table 3 to ferromagnetic driving element 1 needs to decide on moving range, can not surpass the length of high-temperature resistant tube 5.Ferromagnetic driving element 1 need be made by the material that magneticsubstance maybe can be magnetized, and magneticsubstance is meant all kinds of magnet or the material with magnetic, and the material that can be magnetized is meant can be by the material of magnet magnetization, for example iron, iron, cobalt, nickel etc.Ferromagnetic driving element 1 can be made colyliform, bulk or thread, for example makes the iron tyre that is installed in union lever 2 one ends, if less demanding, also could be iron block or the iron wire that is fixed on union lever 2 one ends.Be used to attract the magnet 4 (magnet) of ferromagnetic driving element 1 to need to produce enough magneticstrengties driving ferromagnetic driving element 1, and certain high temperature tolerance ability is arranged, to adapt to the comparatively high temps of tube furnace port, such as SmCo magnet.The magnet of peak performance is rare earth element magnet at present, and neodymium iron boron is the most powerful magnet in rare-earth magnet.But in the environment more than 200 degrees centigrade, SmCo magnet is the most powerful magnet.In addition, if do not consider cost, or because consider other factors, magnet 4 can be electro-magnet.For the ferromagnetic driving element 1 of iron wheel type, can adopt cylinder-shaped magnet, after the outer wall rolling of high-temperature resistant tube 5 moves to desired location with drive iron tyre growth substrate or source material, can take magnet away.
High-temperature resistant tube 5 is exposed to the length decision growth substrate of body of heater 6 outside part or the moving range of source material, can use longer high-temperature resistant tube to obtain bigger moving range.In addition, high-temperature resistant tube 5 two ends can all be exposed to outside the body of heater 6, two cover sample table 3, union lever 2, ferromagnetic driving element 1 are housed simultaneously at two ends, thereby the position to growth substrate or source material control effectively all in once testing.For the situation of multiple source material, can select as required together to move, or wherein one or more source materials are positioned in the vacuum tube furnace in addition by last fixed position, only change the position of residue source material.The high temperature resistant high temperature that can bear in the tube furnace that is meant in the present embodiment, the temperature of tube furnace is usually about room temperature to 1400 degree centigrade, the material that depends on boiler tube, silica tube can arrive 1000 degrees centigrade, the Al2O3 pipe can arrive 1400 degree, that is to say the material that can bear in 1000 to 1400 degrees centigrade.
Below position and the method for temperature of utilizing above-mentioned tube furnace to carry out in tube furnace to change growth substrate or source material being elaborated, is example with preparation ZnS nanometer stick array.Quick cooling after the vapor phase growth of ZnS material.Stable crystal structure under the ZnS material at high temperature is different with stable crystal structure under the room temperature, and at high temperature oxidized easily, and general vapor phase growth process must guarantee certain vacuum tightness, and the oxygen in the stove is removed in strictness.The product that obtains after firing is difficult to fast cooling, makes that the stable crystal structure under the high temperature is difficult to obtain.Use present method, can be after the vapor phase growth of ZnS material finishes, growth substrate or source material are pulled to high-temperature resistant tube are exposed to the outer part of body of heater, add cooling fluid (water), make its quick cooling, can reach room temperature in 10 minutes, can open sealing blowing air cooling afterwards and not oxidized, thereby saved experimental period, and may for obtaining that stable crystal structure under the ZnS high temperature provides.
Preparation ZnS nanometer stick array.Long substrate of ZnS powder or source material are placed the tube furnace middle part, silicon substrate is positioned on the sample table 3 that is connected with ferromagnetic driving element 1, and put distance center 35 centimeters in the tube furnace, vacuumize repeatedly in the stove, logical argon gas is removed furnace air, stops after the logical argon gas, be evacuated to 60Pa, stop to bleed.30 minutes process furnace centers to 1020 degree centigrade, feed the argon gas of 20sccm, and begin to bleed, keep-up pressure at 500Pa, 1020 degrees centigrade of insulations 30 minutes, use magnet 4 (magnet) to attract ferromagnetic driving element 1 afterwards, adjust growth substrate or the position of source material in stove, promptly adjust the temperature of growth substrate or source material, growth substrate or source material are pushed more high-temperature zone, apart from tube furnace center 27 centimeters, be incubated 30 minutes.Use attraction at last, pull out growth substrate or source material to high-temperature resistant tube 5 and be exposed to part outside the body of heater, add water cooling, reduced to room temperature in 10 minutes, logical nitrogen is opened tube furnace to normal pressure, takes out growth substrate or source material.Can obtain about length 500 nanometers the ZnS nanometer stick array about diameter 50 nanometers.
As can be seen from the above embodiments, the embodiment of the invention is utilized the temperature difference of different positions in the tube furnace, change the position of growth substrate or source material fast, adjust the temperature of growth substrate or source material, can under heated condition, use, do not influence the resistance to air loss of tube furnace, the mobile accuracy height, speed is fast.Can be used for vapor growth method and prepare diversified nano material, realize changing fast the material growth conditions, to prepare various nano wires, nano film material.And the advantage that the present invention has is simple to operate, cost is low.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1, a kind of tube furnace comprises body of heater, it is characterized in that, also comprises:
High-temperature resistant tube comprises two portions, and a part is placed in the body of heater, and a part is exposed to outside the body of heater;
Sample table is placed in described anti-this high temperature pipe, is used to place growth substrate or source material;
Ferromagnetic driving element is placed in described anti-this high temperature pipe, is connected with described sample table by union lever, and described ferromagnetic driving element is positioned over described high-temperature resistant tube and is exposed to the outer part of body of heater;
Magnet is arranged on the outer wall that described high-temperature resistant tube is exposed to the body of heater outside part, and described magnet moves along described high-temperature resistant tube axial direction due, drives described ferromagnetic driving element, union lever and sample table and move under the effect of magnetic force.
2, tube furnace as claimed in claim 1 is characterized in that, described sample table and union lever are made by high temperature material.
3, tube furnace as claimed in claim 2 is characterized in that, described high temperature material is fused quartz or aluminium sesquioxide.
4, tube furnace as claimed in claim 1 is characterized in that, described ferromagnetic driving element is made by the material that magneticsubstance maybe can be magnetized.
5, tube furnace as claimed in claim 4 is characterized in that, described ferromagnetic driving element is colyliform, bulk or thread.
6, tube furnace as claimed in claim 1 is characterized in that, described magnet is permanent magnet or electro-magnet.
7, tube furnace as claimed in claim 6 is characterized in that, described permanent magnet is a SmCo magnet.
8, tube furnace as claimed in claim 7 is characterized in that, described SmCo magnet is cylindrical.
9, a kind of tube furnace that utilizes claim 1 changes the method for the position of growth substrate or source material, it is characterized in that, may further comprise the steps:
Growth substrate or source material are positioned on the sample table, vacuumize the logical argon gas in back in the tube furnace repeatedly, remove furnace air, stop logical rare gas element then, and vacuumize;
Heating tube furnace center feeds rare gas element, and begins to bleed to design temperature, keep-ups pressure in setup pressure value;
Be incubated under described design temperature, the insulation back attracts ferromagnetic driving element with magnet, adjusts described growth substrate or the source material position at described tube furnace, changes warm area, continues insulation;
Attract with magnet at last, growth substrate or source material are drawn out to high-temperature resistant tube are exposed to the outer part of body of heater, reduce to room temperature, logical rare gas element is opened tube furnace to normal pressure, takes out growth substrate or source material.
10, the method for the position of change growth substrate as claimed in claim 9 or source material is characterized in that, growth substrate or source material is being drawn out to after high-temperature resistant tube is exposed to part outside the body of heater, also comprises:
Using cooling fluid or radiator element that high-temperature resistant tube is exposed to the outer part of body of heater lowers the temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101167514A CN101323970A (en) | 2008-07-16 | 2008-07-16 | Tubular furnace and method for changing growth substrate or source material position using the same |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101167514A CN101323970A (en) | 2008-07-16 | 2008-07-16 | Tubular furnace and method for changing growth substrate or source material position using the same |
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| CN101323970A true CN101323970A (en) | 2008-12-17 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985774A (en) * | 2010-11-09 | 2011-03-16 | 北京大学 | Method for synthesizing single crystal nano wire array |
| CN105675796A (en) * | 2016-03-29 | 2016-06-15 | 中国科学技术大学 | Material combustion experiment device capable of simulating low-pressure environment |
| CN106091691A (en) * | 2016-05-31 | 2016-11-09 | 广东工业大学 | A kind of crucible clamp and apply its diamond heating device |
| CN108469393A (en) * | 2018-02-02 | 2018-08-31 | 中山市积目科技有限公司 | A kind of cold shock testing equipment |
| CN112831833A (en) * | 2020-12-31 | 2021-05-25 | 中核北方核燃料元件有限公司 | Material boat that can fix a position |
-
2008
- 2008-07-16 CN CNA2008101167514A patent/CN101323970A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985774A (en) * | 2010-11-09 | 2011-03-16 | 北京大学 | Method for synthesizing single crystal nano wire array |
| CN105675796A (en) * | 2016-03-29 | 2016-06-15 | 中国科学技术大学 | Material combustion experiment device capable of simulating low-pressure environment |
| CN106091691A (en) * | 2016-05-31 | 2016-11-09 | 广东工业大学 | A kind of crucible clamp and apply its diamond heating device |
| CN106091691B (en) * | 2016-05-31 | 2018-04-06 | 广东工业大学 | A kind of crucible clamp and apply its diamond heating device |
| CN108469393A (en) * | 2018-02-02 | 2018-08-31 | 中山市积目科技有限公司 | A kind of cold shock testing equipment |
| CN112831833A (en) * | 2020-12-31 | 2021-05-25 | 中核北方核燃料元件有限公司 | Material boat that can fix a position |
| CN112831833B (en) * | 2020-12-31 | 2024-04-09 | 中核北方核燃料元件有限公司 | Material boat capable of being positioned |
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Open date: 20081217 |