WO2004077027A1 - Procede pour determiner les repartitions de tailles de particules d'un ensemble de particules polydisperse - Google Patents
Procede pour determiner les repartitions de tailles de particules d'un ensemble de particules polydisperse Download PDFInfo
- Publication number
- WO2004077027A1 WO2004077027A1 PCT/EP2004/001749 EP2004001749W WO2004077027A1 WO 2004077027 A1 WO2004077027 A1 WO 2004077027A1 EP 2004001749 W EP2004001749 W EP 2004001749W WO 2004077027 A1 WO2004077027 A1 WO 2004077027A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particle
- particles
- signal
- time
- distribution
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 64
- 238000009826 distribution Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 6
- 238000012512 characterization method Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000002485 combustion reaction Methods 0.000 claims abstract description 4
- 230000006978 adaptation Effects 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- 238000004886 process control Methods 0.000 claims abstract 2
- 230000005855 radiation Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012821 model calculation Methods 0.000 claims description 3
- 230000002123 temporal effect Effects 0.000 claims description 3
- 230000005284 excitation Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 abstract description 3
- 238000005315 distribution function Methods 0.000 abstract description 2
- 238000011156 evaluation Methods 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 230000001934 delay Effects 0.000 abstract 2
- 239000002912 waste gas Substances 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/18—Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
Definitions
- the thermal signal thus contains the information about the specific surface and thus about the particle size and in principle about its distribution.
- the problem of reconstructing the size distribution is underdetermined because different distributions can cause similar waveforms and thus does not allow a clear analytical solution. This necessitates the development of approximations based on the nature and scope of the assumptions about the distribution and the mathematical approach can differ and thus also require a different amount of computational effort, which determines the application as an online method.
- the simple procedure described in this invention is based on the evaluation of the complete time profile of the radiation signal or several parts thereof during the cooling to determine higher moments of a particle size distribution.
- the proposed method makes use of the fact that the weighting of the signal contributions of individual particle size classes changes during cooling. Smaller particles provide faster signal drops and thus provide a time-decreasing contribution to the total signal of the particle collective.
- TIRE-II Time-Resolved Laser-Induced Incandescence
- TIRE-II time-Resolved Laser-Induced Incandescence
- the thermal radiation of particles is analyzed after irradiation with a high-energy laser pulse. This irradiation of the examination volume leads to a strong heating up to the partial evaporation of particles.
- the process can be described by a power balance, the model calculation of the temporal temperature and Waveforms allowed.
- the method described exploits the fact that the total signal of a polydispersed particle collective does not fall purely exponentially, but the signal decay time changes with time after the exciting laser pulse, it increases (FIG. 1).
- the procedure according to the invention is that the theoretical signal of a particle collective is obtained directly by summation of the (monodisperse) LH signals which are weighted with a predetermined particle size distribution and which are available from model calculations.
- the average particle size, the distribution width and the ambient temperature are input parameters.
- the mean particle diameter d p med and the distribution width ⁇ are determined unambiguously and optionally online
- Example in Fig. 1 result from Fig. 2 for the particle diameter 11.5 nm and for the standard deviation of the distribution 0.42.
- the method according to the invention which makes it possible to determine characteristics of primary particle size distributions online, must be clearly differentiated from previous attempts to reconstruct particle size distributions.
- These previous approaches are based on the example LII usually on a nonlinear adjustment of the entire signal.
- a response signal for a specific particle size distribution is generated from the model description of the LH process (for example in H. Bockhorn, B. Jungyak, T. Lehre and R. Suntz, VDI reports 1629, 435 (2001)).
- the LII signal of a monodisperse particle collective is first calculated, which, taking into account a particle size distribution p (r) through integration weighted with p (r) over all particle radii, yields the desired response signal.
- the searched parameters are then replaced by a nonlinear fit from the experimental ones time-resolved Lll signal curves determined.
- different parameters are adjusted by least-squares minimization. This adaptation is relatively computationally intensive and must be performed individually for each experimental curve, ie it is not possible to resort to a library, which is currently the case. an online determination does not allow.
- model signal is not required in analytical form, but as a library, only the functions
- the method described in this invention can be used in various fields of application in the analysis of particle blends to characterize the particle size distribution in terms of the moments of distribution, e.g. in the analysis of soot emission from engine or other technical combustion processes or for the analysis and / or control of particle synthesis processes or for product characterization within or after the production process of particles.
Landscapes
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
L'invention concerne un procédé pour déterminer des répartitions de tailles de particules d'un ensemble de particules à partir de la mesure à résolution temporelle du rayonnement thermique de particules chauffées temporairement. Afin de permettre la caractérisation étendue d'un ensemble de particules, il est nécessaire de déterminer, de préférence en ligne, des répartitions granulométriques de particules et, en particulier, de particules primaires. Ledit procédé repose sur le fait que la pondération des contributions de catégories de tailles de particules individuelles au signal de rayonnement thermique varie pendant le refroidissement des particules chauffées en raison de la conduction thermique. Les particules de taille inférieure fournissent des retombées de signal plus rapides et apportent ainsi une contribution décroissante dans le temps au signal de somme de l'ensemble de particules. Ainsi, le signal de somme d'un ensemble de particules polydispersé ne retombe pas d'une façon simplement exponentielle, mais le temps de descente du signal varie dans le temps et augmente. L'évaluation en ligne du signal à résolution temporelle par l'adaptation mathématique dans deux ou plusieurs plages temporelles pendant le refroidissement fournit des temps de descente de signal caractéristiques pour les différentes plages temporelles. Les moments supérieurs de la répartition granulométrique peuvent être ainsi clairement déterminés par certaines suppositions sur la fonction de répartition. Ladite invention concerne également le contrôle ou l'analyse en ligne de processus de synthèse de particules lors de la caractérisation de produits ou lors de l'analyse de gaz d'échappement issus de processus de combustion techniques de moteurs ou autres.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP04713523A EP1604186A1 (fr) | 2003-02-28 | 2004-02-23 | Procede pour determiner les repartitions de tailles de particules d'un ensemble de particules polydisperse |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2003108741 DE10308741A1 (de) | 2003-02-28 | 2003-02-28 | Verfahren zur Bestimmung der Verteilungen von Partikelgrößen eines polydispersen Partikelensembles |
| DE10308741.9 | 2003-02-28 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2004077027A1 true WO2004077027A1 (fr) | 2004-09-10 |
Family
ID=32863971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2004/001749 WO2004077027A1 (fr) | 2003-02-28 | 2004-02-23 | Procede pour determiner les repartitions de tailles de particules d'un ensemble de particules polydisperse |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP1604186A1 (fr) |
| DE (1) | DE10308741A1 (fr) |
| WO (1) | WO2004077027A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896436A (zh) * | 2020-08-11 | 2020-11-06 | 哈尔滨工业大学 | 碳黑团聚体一次粒径分布和热适应系数同时测量方法及装置 |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2953598B1 (fr) | 2009-12-08 | 2012-03-23 | Rhodia Operations | Procede et dispositif de caracterisation de materiaux solides, ainsi que procede et installation de determination d'une caracterisque thermodynamique de molecules sondes |
| FR2953599B1 (fr) * | 2009-12-08 | 2013-08-30 | Rhodia Operations | Procede et installation de caracterisation de surface de materiaux solides |
| CN103439229B (zh) * | 2013-08-06 | 2016-01-20 | 西安交通大学 | 一种基于数字视频的快速铁谱分析方法 |
| CN104865168A (zh) * | 2014-02-26 | 2015-08-26 | 南京理工大学 | 船用铁谱仪及其测量与分析方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0959329A2 (fr) * | 1998-05-22 | 1999-11-24 | National Research Council Of Canada | Mesure de l' intensité absolue pendant l' incandescence induite par laser |
| US6496258B1 (en) * | 1999-02-05 | 2002-12-17 | Esytec Energie-Und Systemtechnik Gmbh | Device and method for simultaneous in-situ determination of particle size and mass concentration of fluid-borne particles |
| WO2004010123A1 (fr) * | 2002-07-19 | 2004-01-29 | Columbian Chemicals Company | Echantillonage de noirs de carbone pour la mesure d'une surface particulaire au moyen d'une incandescence induite par laser et commande associee d'un processus a reacteur |
-
2003
- 2003-02-28 DE DE2003108741 patent/DE10308741A1/de not_active Withdrawn
-
2004
- 2004-02-23 WO PCT/EP2004/001749 patent/WO2004077027A1/fr active Application Filing
- 2004-02-23 EP EP04713523A patent/EP1604186A1/fr not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0959329A2 (fr) * | 1998-05-22 | 1999-11-24 | National Research Council Of Canada | Mesure de l' intensité absolue pendant l' incandescence induite par laser |
| US6496258B1 (en) * | 1999-02-05 | 2002-12-17 | Esytec Energie-Und Systemtechnik Gmbh | Device and method for simultaneous in-situ determination of particle size and mass concentration of fluid-borne particles |
| WO2004010123A1 (fr) * | 2002-07-19 | 2004-01-29 | Columbian Chemicals Company | Echantillonage de noirs de carbone pour la mesure d'une surface particulaire au moyen d'une incandescence induite par laser et commande associee d'un processus a reacteur |
Non-Patent Citations (3)
| Title |
|---|
| BOCKHORN H ET AL: "PROGRESS IN CHARACTERIZATION OF SOOT FORMATION BY OPTICAL METHODS", PHYSICAL CHEMISTRY CHEMICAL PHYSICS, ROYAL SOCIETY OF CHEMISTRY, CAMBRIDGE, GB, vol. 4, no. 15, 1 August 2002 (2002-08-01), pages 3780 - 3793, XP001184402, ISSN: 1463-9076 * |
| FILIPOVV ET AL: "IN_SITU CHARACTERIZATION OF ULTRAFINE PARTICLES BY LASER INDUCED INCANDESCENCE: SIZING AND PARTICLE STRUCTURE DETERMINATION", JOURNAL OF AEROSOL SCIENCE, vol. 30, no. 1, 1 January 1999 (1999-01-01), pages 71 - 87, XP002279196 * |
| LEIPERTZ A; DANKERS S: "CHARACTERIZATION OF NANO-PARTICLES USING LASER-INDUCED INCANDESCENCE", PARTICLE AND PARTICLE SYSTEMS CHARACTERIZATION, WILEY-VCH VERLAG GMBH & CO, WEINHEIM, vol. 20, April 2003 (2003-04-01), pages 81 - 93, XP009030424 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896436A (zh) * | 2020-08-11 | 2020-11-06 | 哈尔滨工业大学 | 碳黑团聚体一次粒径分布和热适应系数同时测量方法及装置 |
| CN111896436B (zh) * | 2020-08-11 | 2023-08-01 | 哈尔滨工业大学 | 碳黑团聚体一次粒径分布和热适应系数同时测量方法及装置 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1604186A1 (fr) | 2005-12-14 |
| DE10308741A1 (de) | 2004-09-16 |
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