FR2822166A1 - Control of a reactor for vapor phase chemical deposition using the reactor pressure variations to control the opening of the precursor liquid injector - Google Patents
Control of a reactor for vapor phase chemical deposition using the reactor pressure variations to control the opening of the precursor liquid injector Download PDFInfo
- Publication number
- FR2822166A1 FR2822166A1 FR0103582A FR0103582A FR2822166A1 FR 2822166 A1 FR2822166 A1 FR 2822166A1 FR 0103582 A FR0103582 A FR 0103582A FR 0103582 A FR0103582 A FR 0103582A FR 2822166 A1 FR2822166 A1 FR 2822166A1
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- France
- Prior art keywords
- control
- reactor
- injector
- pressure
- variations
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45557—Pulsed pressure or control pressure
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
Abstract
Description
<Desc/Clms Page number 1> <Desc / Clms Page number 1>
1-1 PROCÉDÉ DE CONTRÔLE D'UN RÉACTEUR DE DEPOT CHIMIQUE EN PHASE VAPEUR À INJECTION DE GOUTTES DE PRÉCURSEURS LIQUIDES
La présente invention concerne un procédé de contrôle de la génération de la phase gazeuse dans un réacteur de dépôt chimique en phase vapeur à injection de gouttes de précurseurs liquides. 1-1 METHOD FOR CONTROLLING A CHEMICAL VAPOR DEPOSIT REACTOR WITH LIQUID PRECURSOR DROP INJECTION
The present invention relates to a process for controlling the generation of the gas phase in a chemical vapor deposition reactor with injection of drops of liquid precursors.
La présente invention s'applique plus particulièrement à un réacteur du type décrit dans le brevet français 2707671. The present invention applies more particularly to a reactor of the type described in French patent 2707671.
Un tel réacteur est représenté très schématiquement en figure 1. Un ou plusieurs injecteurs 1 sont alimentés par un liquide 2 à pression constante. Chaque injecteur est commandé en fréquence et en durée d'ouverture par un microprocesseur 3 pour envoyer une gouttelette calibrée dans une enceinte 4 de dépôt chimique en phase vapeur, pour développer une couche sur un substrat 5. Such a reactor is shown very diagrammatically in FIG. 1. One or more injectors 1 are supplied with a liquid 2 at constant pressure. Each injector is controlled in frequency and in opening time by a microprocessor 3 to send a calibrated droplet into an enclosure 4 of chemical vapor deposition, to develop a layer on a substrate 5.
Ainsi, quand la pression et la viscosité du liquide 2 sont déterminées, on envoie dans l'enceinte 4 à chaque ouverture de l'injecteur 1 une gouttelette bien calibrée. Thus, when the pressure and viscosity of the liquid 2 are determined, a well-calibrated droplet is sent to the enclosure 4 at each opening of the injector 1.
Ce procédé a donné de bons résultats. Toutefois, on s'aperçoit que, dans certains cas, les paramètres d'injection peuvent dériver au cours d'une phase de dépôt sur le substrat 5. This process has given good results. However, it can be seen that, in certain cases, the injection parameters can drift during a deposition phase on the substrate 5.
Cette dérive peut résulter de variations de température du liquide source 2 qui entraînent des variations de viscosité, ou This drift can result from variations in temperature of the source liquid 2 which cause variations in viscosity, or
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de variations de la pression appliquée au liquide source 2 qui résultent par exemple de la présence de bulles d'air dans les tuyauteries de l'injecteur. variations in the pressure applied to the source liquid 2 which result, for example, from the presence of air bubbles in the injector pipes.
Pour éviter ces inconvénients, on a prévu dans l'art antérieur divers moyens pour fixer avec précision la pression en amont de l'injecteur et pour stabiliser autant que faire se peut la température de la source et des canalisations. Toutefois, les inventeurs ont constaté que toutes les causes possibles de dérive des caractéristiques de l'injecteur ne peuvent pas être contrôlées en amont (par exemple la présence de bulles d'air dans l'injecteur, une obstruction partielle ou une obstruction mécanique de l'injecteur, une variation de viscosité du liquide...). To avoid these drawbacks, various means have been provided in the prior art for precisely fixing the pressure upstream of the injector and for stabilizing as much as possible the temperature of the source and of the pipes. However, the inventors have found that all the possible causes of drift in the characteristics of the injector cannot be checked upstream (for example the presence of air bubbles in the injector, a partial obstruction or a mechanical obstruction of the injector, a change in viscosity of the liquid ...).
Un objet de la présente invention est de prévoir un procédé de contrôle simple et précis de la quantité de liquide effectivement injectée dans un réacteur de dépôt chimique en phase vapeur à injection périodique de gouttelettes d'un liquide. An object of the present invention is to provide a simple and precise method for controlling the quantity of liquid actually injected into a chemical vapor deposition reactor with periodic injection of droplets of a liquid.
Pour atteindre cet objet, la présente invention prévoit un procédé de contrôle d'un réacteur de dépôt chimique en phase vapeur dans lequel on injecte périodiquement et de façon contrôlée des gouttes de précurseurs liquides, consistant à mesurer les variations de pression dans le réacteur, et asservir la commande d'ouverture d'un injecteur pour obtenir une variation de pression constante. To achieve this object, the present invention provides a method for controlling a chemical vapor deposition reactor into which drops of liquid precursors are injected periodically and in a controlled manner, consisting in measuring the variations in pressure in the reactor, and control the opening command of an injector to obtain a constant pressure variation.
Selon un mode de réalisation de la présente invention, lesdites variations de pression sont des variations d'amplitude. According to an embodiment of the present invention, said pressure variations are amplitude variations.
Selon un mode de réalisation de la présente invention, lesdites variations de pression correspondent à l'intégrale des variations sur au moins une partie de la durée entre deux injections. According to an embodiment of the present invention, said pressure variations correspond to the integral of the variations over at least part of the duration between two injections.
Selon un mode de réalisation de la présente invention, l'asservissement de la commande est un asservissement en fréquence. According to an embodiment of the present invention, the control of the control is a frequency control.
Selon un mode de réalisation de la présente invention, l'asservissement de la commande est un asservissement de durée d'ouverture. According to an embodiment of the present invention, the control of the command is a control of the opening time.
<Desc/Clms Page number 3> <Desc / Clms Page number 3>
Selon un mode de réalisation de la présente invention, il est en outre prévu de mesurer l'intégrale de la pression entre deux injections et à interrompre le fonctionnement de l'injecteur quand la sommation des valeurs intégrales a atteint une valeur déterminée. According to an embodiment of the present invention, it is further provided to measure the integral of the pressure between two injections and to interrupt the operation of the injector when the summation of the integral values has reached a determined value.
Ces objets, caractéristiques et avantages, ainsi que d'autres de la présente invention seront exposés en détail dans la description suivante de modes de réalisation particuliers faite à titre non-limitatif en relation avec les figures jointes parmi lesquelles : la figure 1 représente un réacteur de dépôt chimique en phase vapeur auquel s'applique la présente invention ; et la figure 2 représente l'allure de la pression P dans un réacteur à injection de gouttes de précurseurs liquides en fonction du temps t. These objects, characteristics and advantages, as well as others of the present invention will be explained in detail in the following description of particular embodiments given without limitation in relation to the attached figures, among which: FIG. 1 represents a reactor chemical vapor deposition to which the present invention applies; and FIG. 2 represents the shape of the pressure P in a reactor for injecting drops of liquid precursors as a function of time t.
La présente invention prévoit d'adjoindre à un réacteur 4 à injection de gouttes de précurseurs liquides un capteur de pression 10. L'invention se base sur la constatation faite par les inventeurs que les fluctuations de pression dans le réacteur résultant de l'injection séquentielle de gouttes de précurseurs liquides constituent une image fidèle de la croissance du dépôt sur le substrat 5. The present invention provides for adding a pressure sensor 10 to a reactor 4 for injecting drops of liquid precursors. The invention is based on the observation made by the inventors that the pressure fluctuations in the reactor resulting from the sequential injection drops of liquid precursors constitute a faithful image of the growth of the deposit on the substrate 5.
La présente invention utilise la mesure de ces variations de pression pour stabiliser le débit de liquide injecté. The present invention uses the measurement of these pressure variations to stabilize the flow rate of injected liquid.
Ainsi le signal de pression dans le réacteur 4 est envoyé au microprocesseur 3 où il est traité et utilisé pour asservir le fonctionnement de l'injecteur 1. Thus the pressure signal in the reactor 4 is sent to the microprocessor 3 where it is processed and used to control the operation of the injector 1.
Selon l'invention, l'asservissement est réalisé de façon à stabiliser l'amplitude ou l'aire A (ou une partie de cette aire) de la partie oscillante du signal de pression (voir figure 2). Les paramètres d'injection (durée d'ouverture et/ou fréquence) sont corrigés à chaque injection ou sur plusieurs injections pour maintenir constante l'amplitude de la variation du signal entre son minimum et son maximum (AP en figure 2), ou pour maintenir constante l'aire (ou une partie de l'aire, ou leur According to the invention, the control is carried out so as to stabilize the amplitude or the area A (or part of this area) of the oscillating part of the pressure signal (see FIG. 2). The injection parameters (opening time and / or frequency) are corrected with each injection or over several injections to keep the amplitude of the signal variation constant between its minimum and its maximum (AP in Figure 2), or for keep the area constant (or part of the area, or their
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moyenne sur plusieurs injections) sous la courbe (aire A hachurée en figure 2). average over several injections) below the curve (area A hatched in Figure 2).
La somme de toutes les aires ou parties d'aire délimitées par la courbe de pression sur la durée d'une phase de dépôt est une fonction directe de la masse de liquide injecté. The sum of all the areas or parts of area delimited by the pressure curve over the duration of a deposition phase is a direct function of the mass of liquid injected.
Ceci permet en outre d'arrêter l'injection pour divers cycles de dépôt lorsque les mêmes quantités actives ont été injectées. La reproductibilité des épaisseurs déposées est ainsi fixée avec une grande précision. This also makes it possible to stop the injection for various deposition cycles when the same active quantities have been injected. The reproducibility of the deposited thicknesses is thus fixed with great precision.
La présente invention s'applique au cas où plusieurs injecteurs sont utilisés. On veille alors à ce que les périodes d'injection des divers injecteurs soient décalées les unes par rapport aux autres et on considère les variations de pression sur la période qui sépare le début de l'injection par un injecteur donné du début de l'injection par un autre injecteur. The present invention applies to the case where several injectors are used. Care is then taken that the injection periods of the various injectors are offset from one another and the pressure variations over the period between the start of injection by a given injector and the start of injection are considered. by another injector.
La présente invention est susceptible de diverses modifications et variantes qui apparaîtront à l'homme de l'art. The present invention is susceptible to various modifications and variants which will appear to those skilled in the art.
Notamment, d'autres paramètres fluctuant dans le réacteur pourront être choisis comme indicateurs de la masse déposée sur un substrat dans le réacteur et pourront être mesurés et utilisés pour asservir le fonctionnement de l'injecteur.In particular, other parameters fluctuating in the reactor can be chosen as indicators of the mass deposited on a substrate in the reactor and can be measured and used to control the operation of the injector.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0103582A FR2822166B1 (en) | 2001-03-16 | 2001-03-16 | METHOD FOR CONTROLLING A CHEMICAL VAPOR DEPOSIT REACTOR WITH LIQUID PRECURSOR DROP INJECTION |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0103582A FR2822166B1 (en) | 2001-03-16 | 2001-03-16 | METHOD FOR CONTROLLING A CHEMICAL VAPOR DEPOSIT REACTOR WITH LIQUID PRECURSOR DROP INJECTION |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| FR2822166A1 true FR2822166A1 (en) | 2002-09-20 |
| FR2822166B1 FR2822166B1 (en) | 2004-01-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR0103582A Expired - Fee Related FR2822166B1 (en) | 2001-03-16 | 2001-03-16 | METHOD FOR CONTROLLING A CHEMICAL VAPOR DEPOSIT REACTOR WITH LIQUID PRECURSOR DROP INJECTION |
Country Status (1)
| Country | Link |
|---|---|
| FR (1) | FR2822166B1 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5451260A (en) * | 1994-04-15 | 1995-09-19 | Cornell Research Foundation, Inc. | Method and apparatus for CVD using liquid delivery system with an ultrasonic nozzle |
| JPH10135195A (en) * | 1996-10-30 | 1998-05-22 | Hitachi Ltd | Manufacture of semiconductor, semiconductor wafer, semiconductor element, and semiconductor manufacturing apparatus |
-
2001
- 2001-03-16 FR FR0103582A patent/FR2822166B1/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5451260A (en) * | 1994-04-15 | 1995-09-19 | Cornell Research Foundation, Inc. | Method and apparatus for CVD using liquid delivery system with an ultrasonic nozzle |
| JPH10135195A (en) * | 1996-10-30 | 1998-05-22 | Hitachi Ltd | Manufacture of semiconductor, semiconductor wafer, semiconductor element, and semiconductor manufacturing apparatus |
Non-Patent Citations (1)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 1998, no. 10 31 August 1998 (1998-08-31) * |
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| Publication number | Publication date |
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| FR2822166B1 (en) | 2004-01-02 |
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