CN104280280A - Device for preparing unimolecular sample by microleakage sample injection method - Google Patents
Device for preparing unimolecular sample by microleakage sample injection method Download PDFInfo
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- CN104280280A CN104280280A CN201410582243.0A CN201410582243A CN104280280A CN 104280280 A CN104280280 A CN 104280280A CN 201410582243 A CN201410582243 A CN 201410582243A CN 104280280 A CN104280280 A CN 104280280A
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- microleakage
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Abstract
The invention relates to the technical field of unimolecular sample preparation. A device for preparing a unimolecular sample by a microleakage sample injection method mainly comprises a heater, a sample container, a microleakage valve, a capillary, a substrate, a vacuum cavity and a vacuometer, wherein the heater, the sample container, the microleakage valve, the vacuum cavity and the vacuometer are connected in sequence; the substrate is positioned in the vacuum cavity. The device is characterized in that the inlet end of the microleakage valve is connected with the opening end of the sample container; the outlet end of the microleakage valve is connected with the capillary; the capillary extends into the vacuum cavity. According to the device for preparing the unimolecular sample by the microleakage sample injection method, the microleakage valve is used for feeding molecules in a solid powder state; during baking in the vacuum cavity, the microleakage valve is closed, so that a sample cannot enter the vacuum cavity; the device is suitable for preparing the unimolecular sample in an ultrahigh vacuum environment, the molecules of the sample are not damaged, and the ultrahigh vacuum environment cannot be affected.
Description
Technical field
The present invention relates to unimolecule sample preparation technology field, particularly a kind ofly have employed powder micro-leakage principle and a kind of micro-leakage sampling system that can adapt to prepare unimolecule sample in ultra-high vacuum environment prepares the device of unimolecule sample.
Background technology
Prepare unimolecule sample for the thermal evaporation method in ultra-high vacuum environment should require: one is do not destroy sample molecule, and two is easier control evaporation rate.Unimolecule sample preparation in current ultra-high vacuum environment uses the method for thermal evaporation to be sublimate on substrate by powder art sample usually, general thermal evaporation sources makes the sample of solid state distil by resistance wire or high-energy electron beam heating crucible, some portions under heat is uneven, for some macromolecular sample, its structure may be destroyed, cause the generation of molecular fragment, reduce the quality of obtained sample; For the sample that some sublimation temperature is lower, when vacuum cavity toasts (about 200 degrees Celsius), likely sample molecule in evaporation source is evaporated, pollutes vacuum chamber; Because resistance wire or high-energy electron beam heating crucible opening are about 5-10 square millimeter, therefore easily evaporate suddenly a large amount of molecule, also easily pollute vacuum cavity.The device that described a kind of micro-leakage sampling system prepares unimolecule sample can address this problem.
Summary of the invention
In order to solve the problem, a kind of micro-leakage sampling system of the present invention device of preparing unimolecule sample by microleak valve (microleak valve is former be equipment) for minimum gas molecule being passed into ultrahigh vacuum cavity for passing into the molecule of solid powder art state, during vacuum cavity baking, close described microleak valve, sample would not enter vacuum chamber, can not pollute.Can adapt in ultra-high vacuum environment, prepare unimolecule sample, not destroy sample molecule, can not ultra-high vacuum environment be affected.
The technical solution adopted in the present invention is:
Described a kind of micro-leakage sampling system prepares the device of unimolecule sample primarily of well heater, sampling receptacle, microleak valve, kapillary, substrate, vacuum chamber, vacuum meter composition, described well heater, described sampling receptacle, described microleak valve, described vacuum chamber, described vacuum meter connect successively, described substrate is arranged in described vacuum chamber, described microleak valve entrance point connects the openend of described sampling receptacle, described microleak valve endpiece connects described kapillary, and described kapillary stretches in described vacuum chamber.
The invention has the beneficial effects as follows:
Described microleak valve is used for passing into the molecule of pressed powder state by the device that described a kind of micro-leakage sampling system prepares unimolecule sample, when vacuum cavity toasts, close described microleak valve sample and would not enter vacuum chamber, can adapt in ultra-high vacuum environment, prepare unimolecule sample and do not destroy sample molecule, can not ultra-high vacuum environment be affected again.
Accompanying drawing explanation
Further illustrate below in conjunction with figure of the present invention:
Fig. 1 is schematic diagram of the present invention.
In figure, 1. well heater, 2. sampling receptacle, 3. microleak valve, 4. kapillary, 5. substrate, 6. vacuum chamber, 7. vacuum meter.
Embodiment
If Fig. 1 is schematic diagram of the present invention, primarily of well heater (1), sampling receptacle (2), microleak valve (3), kapillary (4), substrate (5), vacuum chamber (6), vacuum meter (7) forms, described well heater (1), described sampling receptacle (2), described microleak valve (3), described vacuum chamber (6), described vacuum meter (7) connects successively, described substrate (5) is arranged in described vacuum chamber (6), described microleak valve (3) entrance point connects the openend of described sampling receptacle (2), described microleak valve (3) endpiece connects described kapillary (4), described kapillary (4) stretches in described vacuum chamber (6).
During work, sample powder be placed in described sampling receptacle (2) and be connected to described microleak valve (3), open described microleak valve (3) to maximal value, described vacuum chamber (6) is vacuumized to (now sampling receptacle is communicated with vacuum chamber, also the state of vacuumizing is in), after vacuum is higher than certain value, close described microleak valve (3), described vacuum chamber (6) is toasted, baking terminates rear preparation when preparing sample, heated to described sampling receptacle (2) by described well heater (1), according to the registration of described vacuum meter (7), open described microleak valve (3) slowly, until described vacuum meter (7) shows certain special value.
Because sample can move to close to described kapillary (4) outlet very, therefore compared to ordinary hot evaporation source, the temperature of heating can control lower, sample can be deposited on described substrate (5) with monomolecular form again while ensureing not destroy sample molecule.
Claims (1)
1. a micro-leakage sampling system prepares the device of unimolecule sample, primarily of well heater (1), sampling receptacle (2), microleak valve (3), kapillary (4), substrate (5), vacuum chamber (6), vacuum meter (7) forms, described well heater (1), described sampling receptacle (2), described microleak valve (3), described vacuum chamber (6), described vacuum meter (7) connects successively, described substrate (5) is arranged in described vacuum chamber (6), it is characterized in that: described microleak valve (3) entrance point connects the openend of described sampling receptacle (2), described microleak valve (3) endpiece connects described kapillary (4), described kapillary (4) stretches in described vacuum chamber (6).
Priority Applications (1)
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CN201410582243.0A CN104280280B (en) | 2014-10-13 | 2014-10-13 | A kind of micro-sample method that leaks into prepares the device of unimolecule sample |
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CN201410582243.0A CN104280280B (en) | 2014-10-13 | 2014-10-13 | A kind of micro-sample method that leaks into prepares the device of unimolecule sample |
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CN104280280A true CN104280280A (en) | 2015-01-14 |
CN104280280B CN104280280B (en) | 2016-12-07 |
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CN102735522A (en) * | 2011-04-12 | 2012-10-17 | 金华职业技术学院 | Apparatus for preparing single-molecule sample by supersonic wave |
CN103323303A (en) * | 2013-05-22 | 2013-09-25 | 长沙开元仪器股份有限公司 | Combined sample preparation system |
CN103439164A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院新疆生态与地理研究所 | Quick plant or soil water vacuum-extraction method based on microwave heating |
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2014
- 2014-10-13 CN CN201410582243.0A patent/CN104280280B/en not_active Expired - Fee Related
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CN86104853A (en) * | 1986-07-01 | 1987-02-11 | 刘幸生 | Automatic vacuum activator for activated water |
US5013006A (en) * | 1989-07-24 | 1991-05-07 | Cosmo Instruments Co., Ltd. | Micro-leakage regulating valve |
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CN1479031A (en) * | 2003-07-08 | 2004-03-03 | 中国科学院武汉物理与数学研究所 | Filtering type temperature controlled helium gas microleak valve |
WO2005033650A2 (en) * | 2003-09-17 | 2005-04-14 | Carl Zeiss Nts Gmbh | Method for preparing a sample for electron microscope examination and a sample carrier and transport holder used therefor |
CN101445955A (en) * | 2007-11-28 | 2009-06-03 | 中国科学院半导体研究所 | Device for space-modulating atomic layer chemical vapour deposition epitaxial growth and method thereof |
CN102687023A (en) * | 2009-11-13 | 2012-09-19 | 文塔纳医疗系统公司 | Thin film processing apparatuses for adjustable volume accommodation |
CN101717479A (en) * | 2009-11-24 | 2010-06-02 | 武汉理工大学 | Amphiphilic gradient copolymer |
CN102735522A (en) * | 2011-04-12 | 2012-10-17 | 金华职业技术学院 | Apparatus for preparing single-molecule sample by supersonic wave |
CN103323303A (en) * | 2013-05-22 | 2013-09-25 | 长沙开元仪器股份有限公司 | Combined sample preparation system |
CN103439164A (en) * | 2013-09-05 | 2013-12-11 | 中国科学院新疆生态与地理研究所 | Quick plant or soil water vacuum-extraction method based on microwave heating |
CN204128873U (en) * | 2014-10-13 | 2015-01-28 | 赵烨梁 | A kind of micro-leakage sampling system prepares the device of unimolecule sample |
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