CN102554254B - Metal In (indium) filled MgO (magnesium oxide) nanotube, manufacturing method for same and application thereof - Google Patents
Metal In (indium) filled MgO (magnesium oxide) nanotube, manufacturing method for same and application thereof Download PDFInfo
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- CN102554254B CN102554254B CN 201110363603 CN201110363603A CN102554254B CN 102554254 B CN102554254 B CN 102554254B CN 201110363603 CN201110363603 CN 201110363603 CN 201110363603 A CN201110363603 A CN 201110363603A CN 102554254 B CN102554254 B CN 102554254B
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Abstract
The invention relates to a metal In (indium) filled MgO (magnesium oxide) nanotube temperature control device, which is mainly formed by pressing a large number of metal In filled MgO nanotubes. When the temperature is higher than 150 DEG C, the resistance of the device is abruptly reduced to the minimum, and the current of the device is detected, so that the temperature can be controlled. Manufacture of the device includes preparation of the metal In filled MgO nanotubes and tabletting of the metal In filled MgO nanotubes. The device can be used for controlling the temperature of a component made of magnetic materials such as NdFeB (neodymium iron boron) and the like, and prolonging the service life of the component.
Description
Technical field
The invention belongs to the nanotube preparation field, be specifically related to that a kind of metal In is filled the manufacture method of MgO nanotube and as the application of temperature control device.
Background technology
As everyone knows, measurement and control of temperature is one of the element task in fields such as research and production, and temperature sensor is widely used in various industries.Application comprises power supply, switch, UPS, transformer station, power distribution cabinet, lathe, boiler, pipeline, cable, liquid, gas, warehouse, greenhouse, dam, body of wall, fire-alarm, biochip and computer microprocessor environment such as (CPU).The key position of these temperature sensors-temperature perception and observing and controlling core will diminish or the microminiaturization of observing and controlling regional environment is necessary to diminish at present at electronic devices and components.Such as; the device made of NdFeB alloys for example; the Curie temperature of NdFeB is 320 ℃; if temperature is higher than Curie temperature; even temperature has descended, its magnetic also may disappear, and influences the service life of device; if add the circuit protection of a temperature switch, then can prolong the service life of device greatly.Also have CPU to dwindle half in per 1.5 years, move more and more sooner, hear rate constantly increases on the unit sizes.For carrying out temperature control and the overtemperature protection of chip film micro area, improve CPU operation stability and security, need micro temperature sensor.
Metal In is filled MgO nanotube temperature control device and is had the remarkable advantage that volume is little, heat absorption is fast, response is fast, can improve stability and the security of micro element work, and its manufacture craft is simple, is convenient to large-scale production.
Therefore, find a kind of metal In to fill optimal design and the preparation method of MgO nanotube temperature control device, reduce metal In and fill the volume of MgO nanotube temperature control device, improve the response speed that metal In is filled MgO nanotube temperature control device, this is very important.
Summary of the invention
Technical problem to be solved by this invention is: at the problem that prior art exists, provide a kind of metal In that satisfies application requirements to fill design and the manufacture method thereof of MgO nanotube temperature control device.
The present invention solves its technical problem and adopts following technical scheme:
(1) takes by weighing In by a certain percentage respectively
2O
3Powder and Mg powder evenly mix.
(2) mixed-powder is put into into graphite crucible, again it is put into vertical rf induction furnace, and be evacuated to 10
-3Pa;
(3) charge into carrier gas in induction furnace, carrier gas is that purity is 99.999% N
2, ventilation air velocity in induction furnace upper end is 400～600cm
3, lower end ventilation air velocity is 100～300cm
3And to set heating-up temperature be 1400 ℃, heat,
(4) after heating a period of time, close vertical rf induction furnace and stop carrier gas and pour, treat to take out graphite crucible after temperature is down to room temperature in the stove, namely obtain metal In and fill the MgO nanotube powder;
Metal In provided by the invention is filled MgO nanotube temperature control device, it is mainly filled the compacting of MgO nanotube by a large amount of In and forms, and when temperature was 150 ℃, the electric current in this device will reach minimum of a value, by the detection electric current, thereby reach temperature controlled purpose.
High-conductivity transparent metal single-wall nano-carbon tube film provided by the invention is made by the one-step method based on chemical vapour deposition (CVD), and its step comprises preparation and the compressing tablet of a large amount of metal In filling MgO nanotubes.
The present invention compared with prior art has following main advantage: manufacture craft is simple, cost is low and suitable large-scale application etc.The device of NdFeB alloys being made with metal In filling MgO nanotube temperature control device carries out temperature control, can protection device be within the operating temperature range, improves the service life of device.
Description of drawings
Fig. 1 .In fills the growth course simple diagram of MgO nano tube structure.
Fig. 2. preparation In fills the simple diagram of the used rf induction furnace of MgO nanotube sample.
Fig. 3. be the transmission electron microscope figure that adopts the metal In filling MgO nanotube of chemical vapor deposited one-step technology preparation.
Fig. 4. (a) under the different temperatures, In fills the current-voltage curve of MgO nanotube compressing tablet.(b) In fills the resistance of MgO nanotube compressing tablet and the relation of temperature.
The specific embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
A kind of by the low-cost method of making metal In filling MgO nanotube of one-step technology, adopt with In
2O
3The chemical vapor deposition method of powder and Mg powder.It is mainly prepared by vertical rf induction furnace.The schematic diagram of rf induction furnace is made up of major parts such as radio-frequency power supply, vacuum system, aerating system, heating system and circulations as shown in Figure 2.The outermost layer of system is used for forming current vortex round the copper coil of heating, comes heated sample with this.Because the electrical and thermal conductivity performance of graphite is fine, can guarantee in ten minutes time, makes the temperature of reaction zone reach 1400 ℃.Therefore, the heating element heater in the quartzy tube chamber mainly is made up of graphite cover, graphite felt, graphite chimney and graphite crucible etc., and this is the core of the thermal treatment zone.Medicine is put into graphite crucible by different proportionings.Quartzy tube chamber an air inlet respectively arranged up and down, can feed reacting gas or protective gas from both direction up and down, a gas outlet is arranged below, be used for getting rid of tail gas.Its concrete steps comprise:
(1) takes by weighing In respectively according to 1: 3 ratio of mol ratio
2O
3Powder and Mg powder are put into after mixing in the graphite crucible; In
2O
3The mixed proportion of powder and Mg powder can specifically be selected according to actual needs, and 1: the ratio of (1～5) can be used as preferably.
(2) graphite crucible is put into the center of vertical rf induction furnace, then vacuumized, reach 10 until vacuum
-3Pa the time stop.
(3) in system, charge into high-purity N
2(99.999%) as carrier gas, upper end ventilation air velocity is 500sccm, and lower end ventilation air velocity is 200sccm, and setting heating-up temperature is 1400 ℃, heating a period of time.Heating-up temperature and air velocity those skilled in the art can specifically select according to actual conditions, all be suitable such as 1200 ℃～1600 ℃ scopes, the upper end air velocity can be controlled at 400～600sccm, and lower end ventilation air velocity can be controlled at 100～300sccm.
(4) stop heating after, close source of the gas and vertical rf induction furnace, wait in the stove temperature to be down to room temperature, the taking-up graphite crucible obtains metal In filling MgO nanotube powder thus.
In addition, utilize the nanotube powder preparation temperature control device of method for preparing also to comprise the step of described metal In filling MgO nanotube being carried out compressing tablet:
(1) earlier a large amount of metal In being filled the MgO nanotube powder packs in the groove of tablet press machine.
(2) then that powder compaction is in blocks, obtain diameter and be about 1.3cm, thickness is about the metal In of 1.8mm and fills MgO nanotube disk.
At last, this metal In is filled MgO nanotube disk carry out electrical performance testing, simultaneously, change the environment temperature of disk, can obtain one group of current-voltage data under the different temperatures.Analysis to data draws: when environment temperature during less than 150 ℃, the resistance value of disk constantly increases with the increase of temperature.When temperature during greater than 150 ℃, the resistance value of this device reduces suddenly, and this fusing point main and metal In is closely related.Temperature is during greater than 150 ℃, and indium metal is dissolved the nanotube that makes in the disk and partly interconnected, and causes the metallicity of disk to strengthen, and resistance value must reduce, and realizing the purpose of switch resistance device, by detecting electric current, thereby reaches temperature controlled purpose.Figure (4) has confirmed that fully metal In fills the MgO nanotube as the application of temperature control device (straight line is corresponding respectively from top to bottom: 300 ℃, 260 ℃, 170 ℃, 160 ℃, 150 ℃, 110 ℃, 50 ℃, 20 ℃).
Claims (8)
1. the preparation method of a metal In filling MgO nanotube comprises the steps:
(1) takes by weighing In by a certain percentage respectively
2O
3Powder and Mg powder mix;
(2) above mixture is put into graphite crucible, again this graphite crucible is put in the vertical rf induction furnace, and vacuumized;
(3) in described vertical rf induction furnace, charge into carrier gas, and to set heating-up temperature be 1200～1400 ℃, heat;
(4) behind the heating certain hour, close vertical rf induction furnace, stop ventilation, treat to take out graphite crucible after temperature is down to room temperature in the stove, can obtain metal In and fill the MgO nanotube powder.
2. In in the method according to claim 1, described step (1)
2O
3The mol ratio of powder and Mg powder is 1:(1～5).
3. method according to claim 1 is characterized in that, in the described step (3), when charging into carrier gas, ventilation air velocity in induction furnace upper end is 400～600sccm, and lower end ventilation air velocity is 100～300sccm.
4. according to the described method of one of claim 1-3, it is characterized in that described carrier gas is that purity is 99.999% N
2
5. according to the described method of one of claim 1-3, it is characterized in that in the described step (2), being evacuated to vacuum is 10
-3Pa.
6. one kind according to the prepared nanotube powder of the method for one of claim 1-4.
7. the preparation method of a temperature control device comprises the nanotube powder compacting step in blocks that claim 6 is prepared.
8. the temperature control device of a method according to claim 7 preparation.
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|---|---|---|---|
| CN 201110363603 CN102554254B (en) | 2011-11-16 | 2011-11-16 | Metal In (indium) filled MgO (magnesium oxide) nanotube, manufacturing method for same and application thereof |
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|---|---|---|---|
| CN 201110363603 CN102554254B (en) | 2011-11-16 | 2011-11-16 | Metal In (indium) filled MgO (magnesium oxide) nanotube, manufacturing method for same and application thereof |
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| CN102554254B true CN102554254B (en) | 2013-07-10 |
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| CN104866660B (en) * | 2015-05-14 | 2017-11-10 | 西北师范大学 | A kind of method of prediction MgO nanoclusters surface gaseous deposit transition metal Au, Pt CO absorption Molecular Adsorption property |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792510A (en) * | 2005-12-23 | 2006-06-28 | 上海大学 | Method for forming nano crystal neodymium iron boron binding magnet |
| CN1805156A (en) * | 2006-01-13 | 2006-07-19 | 清华大学 | Photoelectric sensor based on one-dimensional semiconductor nano structure and manufacturing method thereof |
| CN101191794A (en) * | 2007-08-27 | 2008-06-04 | 中国科学院理化技术研究所 | Fluorescence chemical biosensor with one-dimensional nanostructure, and preparation method and application thereof |
| CN101348891A (en) * | 2008-08-29 | 2009-01-21 | 株洲硬质合金集团有限公司 | Tantalum powder controlled passivation magnesium processing deoxidization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4879128B2 (en) * | 2007-09-21 | 2012-02-22 | Ｔｄｋ株式会社 | Magnet manufacturing method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792510A (en) * | 2005-12-23 | 2006-06-28 | 上海大学 | Method for forming nano crystal neodymium iron boron binding magnet |
| CN1805156A (en) * | 2006-01-13 | 2006-07-19 | 清华大学 | Photoelectric sensor based on one-dimensional semiconductor nano structure and manufacturing method thereof |
| CN101191794A (en) * | 2007-08-27 | 2008-06-04 | 中国科学院理化技术研究所 | Fluorescence chemical biosensor with one-dimensional nanostructure, and preparation method and application thereof |
| CN101348891A (en) * | 2008-08-29 | 2009-01-21 | 株洲硬质合金集团有限公司 | Tantalum powder controlled passivation magnesium processing deoxidization method |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2009-74150A 2009.04.09 |
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