CN1039304A - The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating - Google Patents
The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating Download PDFInfo
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- CN1039304A CN1039304A CN 88104186 CN88104186A CN1039304A CN 1039304 A CN1039304 A CN 1039304A CN 88104186 CN88104186 CN 88104186 CN 88104186 A CN88104186 A CN 88104186A CN 1039304 A CN1039304 A CN 1039304A
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Abstract
The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating belong to field tests.It scans fast relevant specific charge number by mass spectrum and obtains reaction and the middle spectrum of the thermal desorption that dissociates, and draws by the ratio of curve in the spectrum of centre and reacts and the thermal desorption spec-troscopy (TDS) that dissociates.The adsorbable multiple gases of sample among the present invention.Except that comprising traditional thermal desorption spec-troscopy (TDS) method, the present invention also has the function of the not available research surface reaction of traditional thermal desorption method and the state that dissociates, and has developed thermal desorption spectroscopy, TDS.The present invention can be used for fields such as surface analysis, vacuum material, catalysis material, catalysis.
Description
The invention belongs to field tests, be the analysis test method of research material surface adsorption, desorption and body diffusion.
Traditional thermal desorption spec-troscopy (TDS) (being TDS) method is to study thermal desorption dynamics at present, decision heat of adsorption, surface reaction exponent number, adsorbed state number and the most frequently used technology of crystal face absorbing molecules concentration.It is the granule for absorbing (as atom, molecule etc.) with thermal excitation (heating up with certain intensification form) material surface, make it break away from material surface, or excite the particle in the body to be diffused into the surface, break away from the surface then, by instrument detecting such as mass spectrum, record, characterization of adsorption and the process that spectrogram comes research material drawn in the back.
" surface analysis technique " (Chen Jia of Tsing-Hua University and, Chen Changyan writes, the Electronic Industry Press published in 1987) a kind of thermal desorption spec-troscopy (TDS) analytical approach proposed:
Sample is delivered in the ultra high vacuum container, after cleaning (as the high temperature heating), introduce the test gas of certain pressure intensity, after going through certain hour, test specimen heats according to certain rules, makes adsorbed gas emit again, and the total pressure in instrument detecting such as the mass spectrum records vacuum chamber (or partial pressure of the corresponding specific charge number of test gas) in time or the variation of temperature relation, be thermal desorption spec-troscopy (TDS) (TDS), subsequently to the analysis and research of thermal desorption spec-troscopy (TDS) march wire shaped etc.
The normal temperature research method of giving vent to anger then is the particle that utilizes apparatus measures material surfaces such as mass spectrum to desorb in the vacuum under normal temperature, with the adsorption process on research material surface and the method for characteristic.Patent documentation SU819625 just belongs to this type of research.
Above-mentioned two kinds of methods are widely used in research fields such as vacuum material, sorbing material, catalysis, surface and the department.
But up to now, traditional thermal desorption spec-troscopy (TDS) method is only adsorbed a kind of material, study the particle (as molecule) of the single mass number of this material or the population effect of all adsorbents, the strong temperature variant rule of development test partial pressure, only study material molecule or atom characterization of adsorption, almost can't judge the normal reaction and the phenomenon of dissociating that takes place on the material surface of being studied at material surface.
The weak point of the thermal desorption spectrometry that the objective of the invention is to avoid traditional, a kind of thermal desorption spectrometry of studying the reaction and the phenomenon of dissociating is provided, makes the research material surface become possibility to adsorbent and in reaction and the situation of dissociating between the adsorbent under the material surface influence.
Purpose of the present invention can reach by following measure:
1. multiple gases absorption;
2. mass spectrometer scans (with respect to heating rate) fast to relevant specific charge number;
3. collection of illustrative plates and ratio collection of illustrative plates (RDTDS) in the middle of calculating, drawing;
Below in conjunction with accompanying drawing and with water is that example describes working condition of the present invention in detail:
Fig. 1 is an implementation system block diagram of the present invention.Implementation system of the present invention mainly is made up of sample driven rod, vacuum chamber, vacuum pump group, mass spectrometer, two-pen recorder, air supply plant, refrigerating plant, heating arrangement, vacuum gauge, programmable temperature instrument, temperature probe etc.
The specific works step is as follows:
1. survey background:
(vacuum gauge records at this moment, and pressure is 1.0 * 10 to vacuum chamber by air supply plant-9Torr) is filled with a certain amount of gas that is studied (such as H2O), make pressure rising (such as one and half magnitudes) in the vacuum chamber, after stopping to inflate a period of time, the relevant charge-mass ratio number of mass spectrum continuous sweep is (such as 1,16,17,18), simultaneously, vacuum gauge is measured pressure in vacuum tank, the pressure values that the recorder record changes is until vacuum chamber returns to the front vacuum (base vacuum degree) of inflation substantially. So just, can be at different pressure (in such as an order magnitude range 1.0 * 10-9～1.0×10
-8Torr) under, is recorded to the signal strength signal intensity of each relevant charge-mass ratio number, i.e. background values, ratio value between them is (generally to be studied gas as the ratio denominator, each relevant charge-mass ratio number (1,16,17,18) signal strength values is the ratio molecule), i.e. background ratio;
2. the sample driven rod is sent into sample in the vacuum chamber;
3. high-temperature heating sample is with clean sample surfaces;
4. refrigerating plant cools off or refrigeration sample (as to 80K);
5. according to the different requirements of research purpose, air supply plant while or priority are sent into a kind of (as H of the interior certain Langmuir number of vacuum chamber
2O) or multiple gases, make sample absorption;
The vacuum pump group to vacuum chamber take out cause certain vacuum tightness treat that it is stable (slightly higher than background pressure, as 2 * 10
-9Torr);
Mass spectrometer as far as possible fast (speed greater than 0.1 the scan period/degree) the scanning specific charge number (1,16,17,18 etc.) of being correlated with;
8. heating arrangements heats up to sample programmed control (or non-programmed control), the particle desorption of surface adsorption in the temperature-rise period;
9. the registering instrument record varies with temperature the signal intensity of each specific charge number (1,16,17,18);
10. the corresponding background of subduction is (in the step 12 * 10
-91,16,17,18 of correspondence signal intensity under the torr pressure) after, in same coordinate, makes collection of illustrative plates.Horizontal ordinate is a temperature, and ordinate is the signal intensity of each specific charge number (1,16,17,18).This spectrogram has comprised traditional thermal desorption spec-troscopy (TDS) (H
2O desorption curve), and in addition other is dissociated and the specific charge number of resultant of reaction, as the fragment that dissociates (as OH, H), also is plotted on the spectrogram simultaneously.This spectrogram is referred to as to compose in the middle of reaction and the thermal desorption that dissociates (RDTDS).
11. with the temperature is horizontal ordinate, counting ratio value with any two specific charges is that ordinate is made curve map and (generally got and charge into the denominator of test gas as ratio, dissociate or resultant of reaction etc. is the ratio molecule, as OH/H
2O and H/H
2O etc.), method is as follows:
The background ratio of getting this two specific charges number earlier is (in the step 12 * 10
-9The specific charge several 17 and 18 and 1 and 18 of torr pressure correspondence) ratio is made a horizontal straight line, it is background ratio straight line, that gets in the middle of the RDTDS this two specific charges number in the spectrogram (17 and 18, or 1 and 18) curve again likens another curve (dynamic ratio curve) to, and this spectrogram is (OH/H
2O or H/H
2O) reaction and the thermal desorption that dissociates (RDTDS) spectrum.
Relatively performance graph and background ratio straight line can analyze the situation of reacting and dissociating among the RDTDS:
Be higher than background ratio straight line as performance graph, illustrate that the ratio of the material (OH or H) that ratio molecule specific charge number (17 or 1) is corresponding increases.If this ratio molecule is dissociating product (OH or H), then the interpret sample surface produces the (H that dissociates
2O → 1/2 H
2+ OH).As this ratio molecule is a certain resultant of reaction, and then reaction has taken place on the interpret sample surface.
When being lower than its background straight line, illustrate that then the denominator specific charge counts the amount of correspondence and increase as dynamic ratio curve;
Overlap as two curves and to illustrate that then the desorption thing is the same with the background component ratio, do not dissociate or react.
Step 11 form such as can also tabulate realizes.
If only interested, then can list peak position place and background ratio table and compare and get final product the reaction and the situation of dissociating of curve peak position in the spectrum in the middle of the RDTDS.
The present invention also can be used for normal temperature and intensification is given vent to anger.Give vent to anger for material normal temperature and can use step 1,2,7,9,10,11, give vent to anger, then can use step 1,2 and 6～10 for intensification.
Be described further below in conjunction with embodiment.One of embodiments of the invention are water (H
2O) at monocrystalline alundum (Al (Al
2O
3) research of adsorbing on (0001) face, this problem is a research alundum (Al when using as catalyst support, its surface action mechanism.
At first air supply plant is to 5 * 10
-10After the vacuum chamber of torr charged into pure water vapour survey background, the sample driven rod was with monocrystalline alundum (Al (Al
2O
3(0001) after face) sample is sent into vacuum chamber, sample is warming up to 750K is incubated 5 minutes with the cleaning sample surfaces, and then by refrigerating plant sample is cooled to 80K with liquid nitrogen, and at this moment in vacuum chamber, feeding the pure water vapour of different Langmuir numbers, the vacuum pump group is evacuated to 1.0 * 10 to vacuum chamber
-9Torr, quadrupole mass spectrometer is to 17 and 18 specific charge number (OH and H
2O) scanning fast repeatedly, sweep velocity is 2.5 specific charge number/seconds, again with the sample heat temperature raising, in sample heat temperature raising process, scanning survey writes down 17,18 signal intensity, subtracts to obtain H after background is drawn
2O is from Al
2O
3(0001) composes and the RDTDS spectrogram in the middle of the RDTDS of desorption on the face.Accompanying drawing 2(a, b, c) be spectrum in the middle of the RDTDS, subordinate list is that the RDTDS spectrogram provides with tabular form.
Various H
2The ratio of background and each peak position place specific charge several 17 and 18 during the exposed amount of O
Spectrum curve has its peak position.Compared under the different exposed amounts (different Langmuir number) each peak position OH/H
2The OH/H of O ratio and its background
2O ratio has proved in 152 peak positions, and OH is directly from monocrystalline alundum (Al (Al
2O
3) surface directly deviates from, and H is described
2O has taken place to dissociate on the alundum (Al surface.
The present invention and prior art contrast have the following advantages:
To material require plasticity strong, the material that is studied can be solid, liquid, can be monocrystalline, polycrystalline, alloy, semiconductor, insulator etc.;
2. can study material all or the relevant temperature variant rule of charge-mass ratio number (particle) partly, and compare each other with background or each correlated quality number, the information that obtains reaction and dissociate judges whether the adsorption material has taken place to react and dissociate and which kind of reaction has taken place and dissociate.
The present invention also be applicable to normal temperature give vent to anger and heat up research material surface when giving vent to anger reaction and dissociate.
4. present invention includes traditional thermal desorption spectrometry, in addition, also can study material surface reaction and the phenomenon of dissociating that it can not be studied.
The present invention is applicable to the research fields such as vacuum material, sorbing material, catalysis, surface analysis.
Claims (5)
1, a kind of thermal desorption spec-troscopy (TDS) analytical approach, sample is in supervacuum chamber, after cleaning, introduce the test gas of certain pressure intensity, go through certain hour after, sample is by definite form heating, make adsorbed gas emit again, by instrument detecting such as mass spectrum, record, draw spectrogram, it is characterized in that having adopted following method:
Spectrum in the middle of the relevant specific charge number curve spectrum that a. will reduce background is plotted in and obtains in the same coordinate;
B. draw the ratio collection of illustrative plates with the ratio between curve in the middle spectrogram, promptly react and the thermal desorption spec-troscopy (TDS) that dissociates.
2, according to the said analytic approach of claim 1, it is characterized in that said in the middle of spectrum except that comprising traditional thermal desorption spec-troscopy (TDS), also comprise other relevant dissociating and the specific charge number curve of resultant of reaction.
3, according to claim 1 or 2 said analytical approachs, it is characterized in that relatively reacting and the thermal desorption spec-troscopy (TDS) that dissociates in dynamically ratio curve and background ratio curve, can judge just whether material surface reacts and dissociate.
4,, it is characterized in that sample surfaces can successively or adsorb multiple gases simultaneously according to claim 1 or 2 said analytical approachs.
5,, it is characterized in that sample surfaces can successively or adsorb multiple gases simultaneously according to the said analytical approach of claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88104186 CN1017651B (en) | 1988-07-12 | 1988-07-12 | The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88104186 CN1017651B (en) | 1988-07-12 | 1988-07-12 | The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1039304A true CN1039304A (en) | 1990-01-31 |
| CN1017651B CN1017651B (en) | 1992-07-29 |
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ID=4832910
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88104186 Expired CN1017651B (en) | 1988-07-12 | 1988-07-12 | The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating |
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| Country | Link |
|---|---|
| CN (1) | CN1017651B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561315A (en) * | 2017-09-14 | 2018-01-09 | 浙江大学 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
| CN109173576A (en) * | 2018-09-14 | 2019-01-11 | 中国工程物理研究院材料研究所 | A kind of high uniformity capillary array gas adsorbing device |
-
1988
- 1988-07-12 CN CN 88104186 patent/CN1017651B/en not_active Expired
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561315A (en) * | 2017-09-14 | 2018-01-09 | 浙江大学 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
| CN107561315B (en) * | 2017-09-14 | 2019-08-30 | 浙江大学 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
| CN109173576A (en) * | 2018-09-14 | 2019-01-11 | 中国工程物理研究院材料研究所 | A kind of high uniformity capillary array gas adsorbing device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1017651B (en) | 1992-07-29 |
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