• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    This layer deposition method comprises: - injecting a first reagent in the gas phase into the deposition chamber (30) by a first injection route (40); injecting a second reactant in the gas phase into the deposition chamber (30) by a second injection route (50), the second injection route (50) being distinct from the first injection route ( 40); the pressure in the deposition chamber (30) being greater than a predetermined value throughout the duration of the process; said method being characterized in that the first reagent is introduced into the deposition chamber (30) in a first pulse sequence, the second reagent is introduced into the chamber in a second pulse sequence, the first pulse sequence and the second pulse sequence being out of phase.
    公开号:FR3018825A1
    申请号:FR1452385
    申请日:2014-03-21
    公开日:2015-09-25
    发明作者:Julien Vitiello
    申请人:Altatech Semiconductor；
    IPC主号:
    专利说明:

    [0001] FIELD OF THE INVENTION The present invention relates to a method of depositing a layer in the gas phase on the surface of a substrate disposed in a deposition chamber.
    [0002] BACKGROUND OF THE INVENTION A gas phase deposition process of a layer 1 by reaction between two reactants on the surface of a substrate 2 disposed in a deposition chamber 3, illustrated in FIG. 1, and known to the State of the art comprises the following steps: a first reagent is injected in the gas phase into the deposition chamber 3 by a first injection route 4; - A second reagent is injected into the gas phase in the deposition chamber 3 by a second injection route 5, the second injection route 5 being different from the first injection route 4; - The pressure in the deposition chamber 3 is kept constant throughout the duration of the process. However, this process, commonly referred to as "Chemical Vapor Deposition" and referred to as CVD, is unsatisfactory.
    [0003] Indeed, when the first reagent and the second reagent have a high reactivity, they react with each other before reaching the surface of the substrate 2 disposed in the deposition chamber 3. These reactions, called parasitic reactions, generate a strong defectivity of the layers formed by CVD, and especially alter their properties, including electrical, optical and crystalline characteristics. On the other hand, the ability of the CVD technique to conformably cover structures present on the surface of the substrate 2 degrades as the form factor of said structures increases. Structure refers to patterns or devices present on the surface of the substrate 2. The aspect ratio is determined by the ratio between the width of a structure and its height ( or its depth if it is a hollow structure). Conforming means that the thickness of the CVD deposited layer is constant at all points on the surface of the structures exposed to the reactive gases. Thus, it is commonly recognized that the conformation of a layer formed by the CVD technique is satisfactory when the shape factor of structures present on the surface of the substrate 2 is less than 1:10. On the other hand, for higher-aspect factors, the overlap of the structures is non-uniform and / or incomplete as represented in FIG. 2. This is particularly the case in the manufacture of electromechanical microsystems (MEMS), for which the form factors can be very high, for example the filling of deep trenches (depth greater than 20 μm) and very narrow opening (less than 2 μm). An object of the invention is therefore to propose a method for forming a layer involving very reactive species, and said layer having a very low defectivity. Another object of the invention is to propose a method of forming a layer having a better conformity than conventional CVD. BRIEF DESCRIPTION OF THE INVENTION The present invention aims at remedying all or part of the aforementioned drawbacks, and relates to a process for depositing a layer in the gas phase by a reaction between two reactants on the surface of a substrate arranged in a substrate. deposition chamber, said method comprising: - injecting a first reagent in the gas phase into the deposition chamber by a first injection route; Injecting a second reactant in the gas phase into the deposition chamber by a second injection route, the second injection route being distinct from the first injection route; the pressure in the deposition chamber being greater than a predetermined value throughout the duration of the process; Said process being remarkable in that the first reagent is introduced into the deposition chamber in a first pulse sequence, the second reagent is introduced into the chamber in a second pulse sequence, the first pulse sequence and the second pulse sequence. second sequence of pulses being out of phase. By sequence of pulses is meant at least one pulse per sequence. This process is called pulsed CVD.
    [0004] Thus, it is possible to retain the advantage of a deposition rate of a layer on the surface of a substrate comparable to the technique of vapor deposition (CVD). Moreover, the conformity of the deposition of the layer is greatly improved compared to the vapor deposition technique.
    [0005] In addition, this method promotes a reaction between the first reagent and the second reagent on the surface of the substrate, thus limiting the spurious reactions, and the formation of contamination that may degrade the properties of the layer formed on the surface of the substrate. According to one embodiment, the pressure in the deposition chamber is greater than 500 mTorr, preferably greater than 1 Torr. According to one embodiment, the first reagent and the second reagent react with a reaction time shorter than the transit time of a reagent injection system on the substrate surface of the first reagent and the second reagent, the system injection of the reagents comprising the first injection route and the second injection route. According to one embodiment, the first pulse sequence is periodic, and has a first period. According to one embodiment, the second pulse sequence is periodic, and has a second period. According to one mode of implementation, the first period and the second period are equal. According to one embodiment, the overlap between the pulses of the first sequence of pulses and the second sequence of pulses is zero. According to one embodiment, the delay between two successive pulses of the first sequence of pulses is greater than the duration of the pulses of the first sequence of pulses.
    [0006] According to one embodiment, the delay between two successive pulses of the second sequence of pulses is greater than the duration of the pulses of the second sequence of pulses. BRIEF DESCRIPTION OF THE DRAWINGS Other characteristics and advantages will become apparent in the following description of the embodiments of a gas phase deposition process of a layer on the surface of a substrate according to the invention, given in FIG. As nonlimiting examples, with reference to the accompanying drawings in which: - Figure 1 shows a block diagram of deposition chamber used by a technique of the prior art; FIG. 2 shows the conformity of a layer deposited by a technique of the prior art; Fig. 3 is a depot chamber scheme used for the present invention; FIG. 4 is a block diagram of pulse sequences according to one embodiment of the invention; FIG. 5 is a block diagram of pulse sequences according to one embodiment of the invention.
    [0007] DETAILED DESCRIPTION OF EMBODIMENTS OF THE INVENTION For the various embodiments, the same references will be used for identical elements or providing the same function, for the sake of simplification of the description. The device for carrying out the invention is illustrated in FIG. 3. The substrate 20 is then placed on a substrate holder 60 in the deposition chamber 30, and comprises a free surface S on which the layer 10 can be formed by reaction. of the first reagent with the second reagent on the surface S.
    [0008] The free surface S is opposite a reagent injection system. The reagent injection system comprises a first injection route 40 and a second injection route 50 distinct from the first injection route 40. A reagent injection system that can be used in the present invention is described in US Pat. the patent application FR2930561. The first injection route 40 comprises a first plurality of channels 70 opening out of the reagent injection system (FIG. 3).
    [0009] The second injection path 50 comprises a second plurality of channels 80 opening out of the reagent injection system. The ends of the channels of the first plurality of open channels 70 and the second plurality of open channels 80 are facing the free surface S of the substrate 20.
    [0010] The channels of the first plurality of channels 70 and the second plurality of channels 80 may be evenly distributed in the reagent injection system. The regular distribution of the channels of the first plurality of channels 70 and the second plurality of channels 80 improves the uniformity of the layer 10 formed on the free surface S of the substrate 20. The reagent injection system comprises a heating system (not shown) for injecting reagents according to the first injection route 40 and the second injection route 50 in the gaseous state and at a temperature Ti.
    [0011] The substrate holder 60 also comprises a heating system (not shown) for heating the substrate 20. A gas evacuation system is disposed in the deposition chamber 30 to evacuate unreacted reagents on the free surface S of the substrate 20.
    [0012] The gas phase deposition process then comprises the injection of a first reagent in the gas phase by the first injection route 40, and the injection of a second reagent in the gas phase by the second injection route 50. We define the travel time of the first reagent and the second reagent between the reagent injection system and the free surface S of the substrate 20 as the time taken by the first and the second reagent to travel the distance between the system of injection of the reagents and the free surface S of the substrate 20. The invention seeks to place the substrate 20 under conditions such that the injection of the first reagent and the second reagent will not generate parasitic reactions likely to contaminate and degrade the properties electrical, crystalline and optical layer 10 thus formed. To do this, the invention then proposes a mode of injection of the first reagent and the second reagent adapted so that the reaction between the two reagents proceeds essentially on the free surface S of the substrate 20.
    [0013] According to one embodiment, a first reagent is injected into the deposition chamber 30 by the first injection route 40 according to a first pulse sequence and at a temperature Ti. A second reagent is injected into the deposition chamber 30 by the second injection route 50 in a second pulse sequence and at a temperature Ti. The first reagent and the second reagent are capable of reacting with one another. The kinetics of reaction between the first reagent and the second reagent increases with temperature.
    [0014] Advantageously, the heating system of the substrate holder 60 heats the substrate 20 at a temperature T2 greater than the temperature Ti. Since the reaction rate between the first reagent and the second reagent is increasing with temperature, said reaction rate will be greater on the free surface of the substrate 20.
    [0015] The first pulse sequence and the second pulse sequence are phase shifted, that is to say that there are during the deposition process successively times during which only the first reagent is injected into the deposition chamber and instants during which only the second reagent is injected into the reaction chamber.
    [0016] Optionally, there may also be times during which the two reagents are injected simultaneously and / or times during which no reagent is injected.
    [0017] Furthermore, the pressure in the deposition chamber 30 is greater than a predetermined value throughout the duration of the process unlike the techniques of deposition by atomic layer (ALD: Atomic Layer Deposition according to the terminology Anglo-Saxon).
    [0018] Indeed, ALD deposition involves the injection of only one reagent at a time, and requires a complete purge of the chamber before the other reagent is injected. In the case of the present invention, it is possible to dispense with complex pumping systems, and purge steps slowing the rates of deposition of layers on the substrates.
    [0019] By way of example, the pressure in the deposition chamber 30 is greater than 500 mTorr, preferably greater than 1 Torr. The separate management of the injection of the first reagent and the second reagent and in a mode of injection phase shifted said first and second reagents will promote the reaction of the latter on the free surface S of the substrate 20 rather than in the space between the free surface S of the substrate 20 and the injection system. Indeed, when the first reagent is injected during the duration of a pulse in the deposition chamber 30 by the first injection route 40, the first reagent is partially adsorbed on the free surface S of the substrate 20 and partly pumped by the exhaust system. Thus, the first reagent is then in a smaller amount in the space between the free surface S of the substrate 20 and the injection system. The second reagent is injected into the deposition chamber 30 in pulses out of phase with the first reagent.
    [0020] Thus, the reaction rate between the first reagent and the second reagent in the space between the free surface S of the substrate 20 and the gas injection system is reduced compared to an injection sequence of the first and second reactants in a continuous flow. The first reagent and the second reagent then preferentially react on the free surface S of the substrate 20. This mode of injection of the first reagent and the second reagent is particularly advantageous when the first reagent and the second reagent are capable of reacting for a period of time. reaction that is less than the travel time defined above. The method according to the invention thus makes it possible to reduce the rate of parasitic reactions generating particles with respect to a vapor deposition method known from the prior art. Fig. 3 gives an example of a first pulse sequence ((1) in Fig. 3), and a second pulse sequence ((2) in Fig. 3). The first pulse sequence and the second pulse sequence are represented in slot form as a function of time t, but the present invention is not limited to this embodiment. Referring to Figure 3, a reagent is injected into the deposition chamber 30 when the slot is equal to 1, the slot then corresponds to a pulse. The duration of a pulse then corresponds to the time during which a reagent is injected into the deposition chamber 30. The time separating two successive pulses of a sequence of pulses is termed delay, and corresponds to a period of time during which the reagent is not injected into the deposition chamber 30. Thus, for the first pulse sequence, we define the following terms: - the duration of a pulse of the first pulse sequence: TI1 - a delay between two successive pulses of the first sequence of pulses: D1 Equivalently, for the second sequence of pulses, we define the following terms: the duration of a pulse of the second sequence of pulses: T12 a delay between two successive pulses of the second pulse sequence: D2 It is possible to adjust the phase difference between the first pulse sequence and the second pulse sequence according to the reactivity of the first pulse sequence. first reagent and the second reagent. Indeed, the greater the reactivity between the first reagent and the second reagent, the greater the phase shift will be important. The overlap between the pulses of the first pulse sequence and the pulses of the second pulse sequence (i.e. the times during which the two reactants are injected simultaneously) will in the case of a high reactivity. between the first reagent and the second reagent then be minimized, and preferably be zero. Moreover, it may be advantageous to consider a delay D1 greater than T11, a delay D2 greater than T12. In the case of a high reactivity between the first reagent and the second reagent, this will have the effect of promoting the reaction between the first reagent and the second reagent on the free surface S of the substrate 20. Thus, according to the two conditions mentioned above, the time is allowed for each type of reagent to be adsorbed optimally on the free surface S of the substrate 20 before the arrival of the other reagent. This configuration of the process then makes it possible to minimize the spurious reactions in the space between the free surface S of the substrate 20 and the gas injection system. The first pulse sequence may be periodic, and have a first period. The second pulse sequence may also be periodic and have a second period. The first period and the second period may be equal. The duration T11 of a pulse of the first sequence of pulses can be between 0.02 s and 5 s. The delay D1 between two pulses of the first pulse sequence can be between 0.5 s and 10 s. The duration T12 of a pulse of the second sequence of pulses can be between 0.02 s and 5 s.
    [0021] The delay D2 between two pulses of the second pulse sequence can be between 0.5 s and 10 s. The pulses of the first sequence of pulses may have a duration TI1 less than the delay D1 separating two successive pulses of the first pulse sequence (FIG. 5 (1)). The pulses of the second sequence of pulses may have a duration T12 less than the delay D2 separating two successive pulses of the second pulse sequence (FIG. 4 (2)). Thus, the separate injection management of the first reagent and the second reagent, when the latter are very reactive, opens the way for the deposition of layers comprising said first and second reagents by an alternative deposition technique to ALD. . Advantageously, the deposition technique according to the invention makes it possible to obtain such layers with growth rates comparable to continuous vapor phase deposition techniques. By way of example, we present the deposition of a conductive transparent oxide layer of AZO zinc oxide type (Al doped ZnO). The precursors of choice in terms of cost and quality are usually Diethyl Zinc for the supply of Zn and TrimethylAluminium for Al intake. Unfortunately, these precursors are sensitive to any molecule of oxygen at a concentration of 5ppm. generating a white powder which blocks the growth of the film and generates on the substrate 20 a defectivity rendering the final devices inoperative. This maximum sensitivity requires the use of a low-reactivity oxygen source either by gaseous oxygen or by water vapor with conventional CVD or ALD type techniques. In the first case, it is necessary to add a plasma assistance to allow the growth of the layer on the substrate 20 but this is done to the detriment of the crystalline qualities of the layer. In the second case, the inevitable trapping of hydrogen components in the layer degrades the crystalline quality of the layer.
    [0022] The alternative to these two sources is the use of an oxygen source containing ozone. Being much more reactive than oxygen, it makes it possible to dispense with plasma assistance and therefore these disadvantages. In addition, it does not include in the hydrogen component layer with respect to the water vapor, which allows to obtain a growth of the quality layer (see performance table below). On the other hand, its high reactivity does not allow it to be used in standard CVD mode because it reacts with the precursor before the substrate 20 and turns into a powder instead of growing on the substrate 20. The ALD mode of use of the ozone allows to sequence the phases where the precursor and the ozone are in contact on the substrate 20 to avoid these problems. But it causes two difficulties compared to a continuous CVD method. This very slow growth, which makes it possible to achieve significant conformities on high-aspect ratio patterns, makes it difficult to trap the aluminum atoms that act as a dopant to form the conductive part of the layer. The resistivity properties of the layer are increased, and the transparency of the layer (especially via the extinction coefficient) is decreased. In addition, the slow growth of the zinc oxide layer will favor grains of large size for thick layers (typically greater than 20 nm) and thus limit the two properties specified above, which are the conductivity and the transparency at the White light. Conversely, the pulsed CVD method will not only make it possible to overcome the problems posed by the CVD and ALD methods for growth with ozone, but also to push the performances of the deposited film even further, particularly in terms of conductivity and transparency (see table below). This is achieved by the unique combination of pulse mode management of the reactive species, and those separately as a function of their affinities to the surface of the substrate 20. The pulse times are typically 50 to 200ms, an offset between pulses between 0 and 500ms, without purge gas. The working pressure is between 1.5 Torr and 3 Torr, preferably between 1.5 Torr and 2.3 Torr. The gas flows are between 500sccm and 3000sccm, preferably between 500sccm and 1500sccm. Specification AZO 400 ° C AZO 400 ° C A1203 400 ° C Rate of 1.24 1.2 0.33 deposition (nm / s) Resistivity 2.13 2.64 NA (mOhm.cm) Uniformity of the 8.9 4.5 NA resistivity (1s) Uniformity of 1.5% 1.5% < 2.5% thickness (1s) Transmittance> 92%> 92% 5
    权利要求:
    Claims (9)
    [0001]
    REVENDICATIONS1. A method of depositing a layer (10) in the gas phase by reacting two reactants on the surface of a substrate (20) disposed in a deposition chamber (30), said method comprising: - injecting a first a gas phase reagent in the deposition chamber (30) through a first injection path (40); injecting a second reactant in the gas phase into the deposition chamber (30) by a second injection route (50), the second injection route (50) being distinct from the first injection route ( 40); the pressure in the deposition chamber (30) being greater than a predetermined value throughout the duration of the process; said method being characterized in that the first reagent is introduced into the deposition chamber (30) in a first pulse sequence, the second reagent is introduced into the chamber in a second pulse sequence, the first pulse sequence and the second pulse sequence being out of phase.
    [0002]
    2. Method according to claim 1, wherein the pressure in the deposition chamber (30) is greater than 500 mTorr, preferably greater than 1 Torr.
    [0003]
    The method of claim 1 or 2, wherein the first reagent and the second reagent react together for a reaction time less than the time of travel of the first reagent and the second reagent between a reagent injection system and the surface of the reagent. substrate (20), the reagent injection system comprising the first (40) and the second (50) injection path.
    [0004]
    4. Method according to one of claims 1 to 3, wherein the first pulse sequence is periodic and has a first period.
    [0005]
    5. Method according to one of claims 1 to 4, wherein the second pulse sequence is periodic and has a second period.
    [0006]
    The method of claim 5 in combination with claim 4, wherein the first period and the second period are equal.
    [0007]
    7. Method according to one of claims 1 to 6, wherein the overlap between the pulses of the first pulse sequence and the pulses of the second pulse sequence is zero.
    [0008]
    8. Method according to one of claims 1 to 7, wherein the delay between two successive pulses of the first pulse sequence is greater than the duration of the pulses of the first pulse sequence.
    [0009]
    9. Method according to one of claims 1 to 8, wherein the delay between two successive pulses of the second pulse sequence is greater than the duration of the pulses of the second pulse sequence.
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    法律状态:
    2016-02-19| PLFP| Fee payment|Year of fee payment: 3 |
    2017-03-24| PLFP| Fee payment|Year of fee payment: 4 |
    2018-03-28| PLFP| Fee payment|Year of fee payment: 5 |
    2018-05-04| CA| Change of address|Effective date: 20180330 |
    2018-05-04| CD| Change of name or company name|Owner name: UNITY SEMICONDUCTOR, FR Effective date: 20180330 |
    2018-08-24| TP| Transmission of property|Owner name: KOBUS SAS, FR Effective date: 20180719 |
    2020-02-14| PLFP| Fee payment|Year of fee payment: 7 |
    2021-03-23| PLFP| Fee payment|Year of fee payment: 8 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1452385A|FR3018825B1|2014-03-21|2014-03-21|GAS PHASE DEPOSITION METHOD|FR1452385A| FR3018825B1|2014-03-21|2014-03-21|GAS PHASE DEPOSITION METHOD|
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    CN201580015091.9A| CN106170583A|2014-03-21|2015-03-19|CVD method|
    KR1020167027417A| KR20160135232A|2014-03-21|2015-03-19|Gas-phase deposition process|
    SG11201607862TA| SG11201607862TA|2014-03-21|2015-03-19|Gas-phase deposition process|
    JP2017500419A| JP2017512914A|2014-03-21|2015-03-19|Vapor deposition process|
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