CN2030322U - Heat degassing and room-temperature gassing experiment measuring set-up - Google Patents
Heat degassing and room-temperature gassing experiment measuring set-up Download PDFInfo
- Publication number
- CN2030322U CN2030322U CN 88208696 CN88208696U CN2030322U CN 2030322 U CN2030322 U CN 2030322U CN 88208696 CN88208696 CN 88208696 CN 88208696 U CN88208696 U CN 88208696U CN 2030322 U CN2030322 U CN 2030322U
- Authority
- CN
- China
- Prior art keywords
- sample
- spiral arm
- vacuum chamber
- experiment
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000002474 experimental method Methods 0.000 title claims abstract description 26
- 238000007872 degassing Methods 0.000 title description 2
- 238000012360 testing method Methods 0.000 claims abstract description 11
- 230000005540 biological transmission Effects 0.000 claims abstract description 8
- 230000005484 gravity Effects 0.000 claims description 3
- 238000005452 bending Methods 0.000 claims 1
- 238000003795 desorption Methods 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 5
- 238000005211 surface analysis Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 100
- 238000012546 transfer Methods 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 230000007246 mechanism Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 101100366060 Caenorhabditis elegans snap-29 gene Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001073 sample cooling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Thermal desorption and room temperature outlet experimental provision, belong to measurement, testing field. Its sample transmission lever spiral arm is
Shape, sample are suspended on spiral arm, and two pieces of clasp pieces are placed on sample two sides on spiral arm, and limitation sample is moved forward and backward; Sample support is the approximate U shape structure of lying; Sample and sample support point contact, directly contact with pyrometer fire-end; The apparatus structure is simple, and survey, temperature control are accurate, and thermal radiation loss is few, and background influence is very few, can once complete the tests of thermal desorption and room temperature outlet two experiments in an experiment. It can be used for the fields such as surface analysis technique material science.
Description
The utility model belongs to measurement, field tests, is a kind of experimental provision.
Thermal desorption and normal temperature are given vent to anger and tested is the most direct and widely used method of research material vacuum performance.This experiment generally must be equipped with the sample transmission mechanism, finish on the vacuum system of survey, temperature regulating device and monitoring record device (as mass spectrum and vacuum gauge) etc., sample transmission that is equipped with in the vacuum system and survey, temperature regulating device play decisive role to the success or not of experiment and the order of accuarcy of test result.
Existing thermal desorption and normal temperature are given vent to anger, and measurement mechanism commonly used has two kinds in the experimental technique: a kind of is that its sample support is a base type, referring to accompanying drawing 1: one of form that is installed on the base type sample support in the main vacuum chamber places on the metal plate (being substrate) (2) for sheet sample (1), under dull and stereotyped heat filament (3) is set, thermal radiation by filament heats metal plate, metal plate reaches sample with heat, and sample is heated up; Two of form is: sample places one section pipeline that communicates with vacuum system, is vacuum in the pipeline, and the outside is an atmosphere.In the pipeline outside pipeline is heated the heat heating that sample is transmitted by tube wall in the pipeline during heating.In the base type sample support of above-mentioned two kinds of forms, temperature probe (as thermopair (4)) all is fixed in the substrate (metal plate or tube wall), directly do not contact with sample, only be similar to the actual temperature that replaces sample during thermometric with base reservoir temperature, and during this structure program temperature control, thermal inertia is big, is difficult to accurately control in temperature-rise period sample temperature.Simultaneously, the substrate sheet size of this base type sample support is often identical or greater than sample size, sample warming room ground connection relies on the thermal radiation of heat filament under the substrate, because sample and substrate heat up simultaneously, and filament transmits heat to the wall thermal radiation, all can cause the particle in substrate and wall and sample surfaces and the body to deviate from simultaneously, influence the order of accuarcy of test result.
Another kind of measurement mechanism commonly used is: sample is made thread (being only applicable to conducting sample), and the silk two ends add electrode, and the thermopair generic point is welded on the silk.Thread sample is heated during energising, and electrode and thermopair also are heated simultaneously, because the discharge quantity of electrode and thermopair can be comparable with the sample air output, thereby causes test result also inaccurate.
Task of the present utility model is to avoid the deficiency of above-mentioned prior art, proposes a kind of survey, temperature control and result measurement mechanism comparatively accurately.
The purpose of this utility model can reach by following measure:
Adopt two-dimentional sample transfer device, some contact sample holder and thermocouple direct contact type survey, temperature regulating device etc. are realized simple and direct quick sample presentation sampling, accurate measuring and controlling temp, and same sample is once finished the test that normal temperature is given vent to anger and thermal desorption is tested in experiment.
The utility model is described in further detail below in conjunction with accompanying drawing.
Accompanying drawing 2 is for adopting experimental system theory diagram of the present utility model.Two-dimentional sample is housed in the pre-vacuum chamber (17) transmits bar (14), it links to each other with main vacuum chamber (16) by shutdown valve (13), main vacuum chamber (16) is connected to mass spectrometer (11) and vacuum gauge (12), in sample support (8) and direct contact type thermometric, the temperature regulating device mainly be made up of filament (7), thermopair (9) etc. are housed.(6) are that program temperature controller (10) is a cryo pump among the figure, and (15) are the molecular pump unit.
Pre-vacuum chamber (17) is exposed to atmosphere, and cylindric sample is delivered to and hung on sample transmission masthead end in this pre-vacuum chamber, and pre-vacuum chamber is evacuated to 10
-6Torr is opened the shutdown valve (13) between pre-vacuum chamber and the main vacuum chamber, and sample transmits bar the sample straight line is sent into main vacuum chamber (16), and this moment, main vacuum chamber's pressure was 10
-9Torr, sample transmit bar Rotate 180 °, and sample is placed on the sample support (8), and straight line withdraws from sample and transmits bar again, closes shutdown valve.This process only needs to plant somewhat.At this moment sample is by action of gravity, contact with four pad points of sample support (8), and well contact with the warm galvanic couple of the observing and controlling that flexure strip is housed, heat filament also is positioned evenly over tubular sample center, so far sample presentation is just accused and is finished, and can do that normal temperature is given vent to anger and experiment such as thermal desorption.
Measurement mechanism of the present utility model is mainly partly formed by two, and a part of is the eccentric transmission mechanism of sample two dimension (straight line and rotatablely move), and another partly is a sample holder.The close fit of two parts can be finished experimentations such as sample presentation sampling and observing and controlling temperature.
Accompanying drawing 3(a) be the eccentric transfer device of sample two dimension,
Shape spiral arm (18) by connecting link (21) with can do straight line with the rotation two dimensional motion sample transfer bar end (22) link to each other, connecting link (21) two ends have the concentric circle holes two ends and are connected with spiral arm (18) transition fit with sample transfer bar end (1) respectively, and be fixed along the connecting link warp-wise with screw (23), sample (19) is suspended on the spiral arm (18), and two pieces are placed on the spiral arm clasp piece (20) restriction sample (19) with spiral arm (18) transition loose fit because various vibrations moving forward and backward on spiral arm (18).When sample transfer bar end (22) rotate, spiral arm (18) serves as axle rotation synchronously with the axle of sample transfer bar end (22), the tubular sample that is suspended on the spiral arm (18) is then done the translation rotation, as accompanying drawing 4(a), the arrow direction indication is sense of rotation (the axle center decentraction of sample axle center and sample transfer bar, be eccentric structure) the sample transfer bar straight ahead or when retreating, spiral arm (18) is being with the sample advanced in unison or is being retreated, accompanying drawing 4(b).
Accompanying drawing 3(b) for being fixed in the structural drawing of the sample holder in the main vacuum chamber, filament (7) extension line receiving electrode.Sample support (8) is the approximate U-shaped one-piece construction of a lying, two parallel bars of this structure are the level of state, connect with one section reclinate bow between two bars, bar material therefor specification is decided on the temperature required and example weight of experiment, the fusing point of material should be higher than the maximum temperature of experiment, and material is indeformable substantially during with maximum temperature is as the criterion.Respectively be with at least two friction tight high temperature resistant pads (28) that slide on support two parallel bars, its thickness should approach (as about 0.5mm) to reduce heat conduction as far as possible.Distance between two pads of every limit is adjusted, to adapt to the sample of all lengths.Distance between two parallel bars should be less than the sample external diameter, and when guaranteeing that as far as possible sample is placed on the support, filament is in the sample center.Filament is in the position at sample center also can be realized with the relative position of support (8) by regulating filament (7).One end points of metal clips (24) is welded in the center of filament length direction on the support, the other end is welded on the becket (25) that trip bolt (26) are housed, thermocouple insulation diplopore ceramic pipe (27) passes from becket (25), thermopair is arranged in ceramic pipe, regulate the upper-lower position of ceramic pipe in becket, when sample is placed on the support, thermocouple hot junction and sample can be good contact till.Screw trip bolt (26) ceramic pipe and thermocouple and promptly be fixed, and sample is when being pressed in the thermocouple hot junction, metal clips is painstaking, and is promptly flexible on gravity direction.
Sample is pushed into main vacuum chamber in the experiment, and as accompanying drawing 5, heat filament (7) is in the interior bottom of tubular sample (19), and makes it uniform on the sample length direction, to guarantee even heating.
The rotation sample transfer bar, sample at first contacts two in four support pad (28) in rotation process, sample surfaces contacts the thermocouple hot junction again, contact two other support pad at last, at this moment sample transfer bar has turned over about 180 ° angle, and breaks away from sample, as accompanying drawing 6, straight line is withdrawn from sample transfer bar to pre-vacuum chamber, closes the shutdown valve between main vacuum chamber and the pre-vacuum chamber, promptly finishes the sample presentation process.Carry out the inverse process of sample presentation process during sampling fully, can fast sample be taken out, so that do next experiment.
The desired sample of the utility model is generally cylindric.
The inventor once be equipped with thermal desorption of the present utility model and normal temperature give vent to anger the experimental system experiment of having done that a large amount of thermal desorptions such as polycrystalline copper, polycrystalline nickel, stainless steel, aluminium alloy are given vent to anger and normal temperature is given vent to anger, all obtain good result.Experiment with polycrystalline copper is that example is described further below.
The polycrystalline copper sample is processed into φ 28 * 25 * 1mm
3Cylinder, carry out surperficial mechanical polishing, sample in the experimental system pre-vacuum chamber is transmitted the bar rotation, make spiral arm be in the extreme higher position, sample is hung thereon, regulate two snap rings on the spiral arm, to limit sample seesawing on spiral arm, as accompanying drawing 3, pre-vacuum chamber reaches 1.0 * 10 after vacuumizing 6 minutes
-6The torr vacuum is opened shutdown valve, and straight-forward push is transmitted bar, and it is 10 that sample is pushed the base vacuum degree
-10The main vacuum chamber of torr, the position of sample and filament is regulated in front and back, make filament be in middle position on the sample length direction, 180 ° of angles of bar are transmitted in rotation then, copper sample falls within on the sample holder, contact with four pads (distance on every bar between two pads be tuned to sample length about 1/3) and thermocouple hot junction, four pads are in about 1/3 position about sample respectively, and the thermocouple hot junction is in the sample bottom center.Straight line recession sample transmits bar, closes shutdown valve, and sample presentation is promptly accused and finished.
The linear temperature increase thermal desorption experiment that polycrystalline copper mechanical buffing that the inventor did is handled, 12 ℃/minute of heating rates are heated to 420 ℃, unbaked thermal desorption spectrogram such as the accompanying drawing 7 of giving vent to anger that heat up.After treating the sample cooling, carry out the inverse process of sample presentation, sample is withdrawn from pre-vacuum chamber rapidly, close shutdown valve, the thermal desorption experiment pre-vacuum chamber of then doing the instantaneous exposure atmosphere of copper sample exposes atmosphere 2 minutes, and promptly copper sample was by instantaneous exposure atmosphere 2 minutes, pre-vacuum chamber vacuumizes, repeat the experimentation of above-mentioned experiment, make the thermal desorption spectrogram that obtains after the polycrystalline copper sample exposes atmosphere, as accompanying drawing 8.The thermal desorption spec-troscopy (TDS) comparison of this spectrogram and last experiment can obtain more information, (the pure surface adsorption characteristic that extends influence as No oxided film and body), and this experiment only has the sampling sent fast and accurately on the utility model experimental provision of observing and controlling temperature (having guaranteed good reproducibility), just is being achieved.
Compared with the prior art the utility model has the following advantages:
1. the structure of the utility model sample transfer device is simple than mechanical arm commonly used or multidimensional mechanism etc., cost is low, easily processing, than the vacuum device expose big pneumatic transmission, sampling method is easy, quick, have advantages such as not destroying the sample primary characteristic, be particularly useful for the research of original material intensification thermal desorption.
2. the more existing base type support of sample holder of the present utility model simply is easy to do, and to the sample homogeneous heating, surveys, temperature control is accurate, and thermal radiation loss is few, and the background influence is very little.
The utility model removes and can be used for normal temperature give vent to anger experiment and thermal desorption experiment, is implemented in outside the test of once finishing above-mentioned two experiments in the experiment, also can serve the not easy-operating experimental provision of other staff, proper its sample feeding mechanism.
The utility model is applicable to surface analysis technique, research, test in material such as vacuum, absorption and the chemical field.
Claims (2)
1, a kind of experiment test device, mainly form, it is characterized in that by two dimensional motion sample transmission bar (14), main vacuum chamber (16), pre-vacuum chamber (17), mass spectrometer (11), vacuum gauge (12), sample support (8), filament (7), thermopair parts such as (9):
1. the spiral arm (18) of sample transmission bar is
Shape, the snap ring that restricted sample of cover moves on it;
2. sample is by gravity direct contact heat galvanic couple hot junction;
3. sample support two respectively is with at least two pads (28) on parallel, contacts with pad point when sample is placed;
4. the bow with one section bending connects between sample support two parallel bars.
2,, it is characterized in that between pad (28) and the parallel bar on the sample support that for the slip wringing fit is connected, the distance between the pad of the every side of parallel bar is adjustable according to the said experiment test device of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88208696 CN2030322U (en) | 1988-07-25 | 1988-07-25 | Heat degassing and room-temperature gassing experiment measuring set-up |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88208696 CN2030322U (en) | 1988-07-25 | 1988-07-25 | Heat degassing and room-temperature gassing experiment measuring set-up |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2030322U true CN2030322U (en) | 1989-01-04 |
Family
ID=4842462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88208696 Withdrawn CN2030322U (en) | 1988-07-25 | 1988-07-25 | Heat degassing and room-temperature gassing experiment measuring set-up |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2030322U (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532192A (en) * | 2014-12-19 | 2015-04-22 | 深圳市华星光电技术有限公司 | Evaporation device |
| CN104596879A (en) * | 2015-01-18 | 2015-05-06 | 北京工业大学 | Temperature-controllable vacuum desorption performance testing system |
| CN109342699A (en) * | 2018-12-20 | 2019-02-15 | 麦加涂料(南通)有限公司 | A kind of condensation water test device and the test method using the condensation water test device |
| CN111299312A (en) * | 2020-02-26 | 2020-06-19 | 苏州市环境科学研究所 | In-situ resistance thermal desorption simulation device |
-
1988
- 1988-07-25 CN CN 88208696 patent/CN2030322U/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532192A (en) * | 2014-12-19 | 2015-04-22 | 深圳市华星光电技术有限公司 | Evaporation device |
| CN104596879A (en) * | 2015-01-18 | 2015-05-06 | 北京工业大学 | Temperature-controllable vacuum desorption performance testing system |
| CN109342699A (en) * | 2018-12-20 | 2019-02-15 | 麦加涂料(南通)有限公司 | A kind of condensation water test device and the test method using the condensation water test device |
| CN111299312A (en) * | 2020-02-26 | 2020-06-19 | 苏州市环境科学研究所 | In-situ resistance thermal desorption simulation device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101482527B (en) | Integrated measurement device and method for heat pipe performance | |
| CN107228877B (en) | Flat heat pipe heat transfer performance testing device with adjustable inclination angle | |
| CN109613051B (en) | Device and method for measuring Seebeck coefficient of material by using contrast method | |
| CN110895287A (en) | Vacuum interconnected surface analysis device and use method thereof | |
| CN2030322U (en) | Heat degassing and room-temperature gassing experiment measuring set-up | |
| US20070121700A1 (en) | Performance testing apparatus for heat pipes | |
| CN116337929A (en) | Experimental device and method for testing heat transfer limit of non-uniform-power high-temperature heat pipe | |
| CN109406574A (en) | A kind of flat-plate heat pipe test device and system | |
| US3881359A (en) | Hot atmosphere particulate sampler | |
| CN111337535A (en) | Heat pipe heat transfer performance testing device and testing method thereof | |
| Niksa et al. | Captive sample reactor for kinetic studies of coal pyrolysis and hydropyrolysis on short time scales | |
| US3737762A (en) | Apparatus and method for measuring the seebeck coefficient and resistivity of materials | |
| CN212364156U (en) | Adjustable thermal conductivity coefficient testing arrangement | |
| US7553072B2 (en) | Performance testing apparatus for heat pipes | |
| Meyer et al. | Energy exchange between cold gas molecules and a hot graphite surface | |
| CN110262587A (en) | Intelligent controllable temperature formula Hopkinson pressure bar test low temperature loading device and temperature control method | |
| CN115436727A (en) | Thermoelectric device performance testing device | |
| CN102243116B (en) | Method and device for quickly detecting thermoelectric properties of polycrystalline diamond (PCD) blade | |
| CN209327255U (en) | A kind of flat-plate heat pipe test device and system | |
| CN209027283U (en) | A kind of tube furnace for nano material growth | |
| CN218601203U (en) | Thermal desorption disposal contaminated soil heat conductivity coefficient test system | |
| CN107653443B (en) | Double alkali photocathodes plating membrane module and control method in a kind of extremely high vacuum system | |
| CN217786967U (en) | Constant temperature and constant pressure interface thermal resistance testing device | |
| CN111595901A (en) | Device and method for measuring heat conductivity coefficient of refractory material | |
| Beebe et al. | Calorimetric Heats of Adsorption of Nitrogen, Carbon Monoxide, and Argon on Graphon at-70° |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |