• 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:
    The invention relates to a method for manufacturing a layer (103) containing quantum boxes, said layer comprising first regions (103a) in which the quantum boxes are active and second regions (103b) in which the quantum boxes are inactive the method comprising: a) depositing on a support (101) a first layer (103) of a matrix containing quantum boxes; b) depositing on the first layer (103) a second layer (105) of photoresist; c) insolating the second layer (105) through a mask (107) delimiting the first (103a) and second (103b) regions and then developing the resin of the second layer (105) to remove the resin from the second layer ( 105) opposite the second regions (103b) while keeping it opposite the first regions (103a); and d) removing the resin from the second layer (105) facing the first regions (103a) without removing the first layer (103).
    公开号:FR3043838A1
    申请号:FR1561047
    申请日:2015-11-17
    公开日:2017-05-19
    发明作者:Audrey Sanchot；Bernard Aventurier
    申请人:Commissariat a lEnergie Atomique CEA；Commissariat a lEnergie Atomique et aux Energies Alternatives CEA；
    IPC主号:
    专利说明:

    METHOD FOR MANUFACTURING LAYER CONTAINING BOXES
    QUANTUM
    Field
    The present application relates to a method of manufacturing a layer containing quantum boxes, this layer having first regions in which the quantum boxes are active, and second regions in which the quantum boxes are inactive.
    Presentation of the prior art
    A quantum dot (quantum dot) is a three-dimensional semiconducting nanoparticle of crystalline structure, with quantum confinement properties in the three dimensions of space. The quantum boxes have physical properties, including magnetic properties, electrical properties, and optical properties, which vary according to their dimensions and according to the materials constituting them. The dimensions of a quantum box are typically between 1 and 100 nm.
    Quantum boxes have the particular property of being photoluminescent, that is to say that, when they are illuminated by a light source, they absorb photons coming from the light source, then re-emit light in response to this photoexcitation. While the absorption wavelength band, i.e. the wavelength band of illumination in which a quantum dot absorbs photons, may be relatively broad, the length band of emission waves, that is to say the wavelength band in which the quantum dot retransmits light, is generally very narrow, for example half-way width less than 50 nm. In addition, the central wavelength of the emission band can be adjusted finely, in particular by playing on the dimensions of the quantum dot. One of the applications of quantum dots in the field of optics is color conversion. In particular, it has been proposed to produce a luminous display screen comprising a plurality of light-emitting diodes adapted to emit light of a first color, for example blue light, this set of diodes being coated with a layer comprising quantum boxes for converting into one or more other colors, for example red light in certain regions of the screen and green light in other regions of the screen, the light emitted by the light-emitting diodes.
    The realization of such a screen, however, poses practical difficulties, particularly related to the properties that must present the quantum dot layer, and in particular its thickness and its concentration in quantum boxes, to be able to absorb all or almost all of the light emitted by the light-emitting diodes in the areas of the screen in which it is desired to convert this light. Another difficulty is that it must be possible to define with a resolution adapted to the size of the pixels or emitting areas of the screen the different emission regions of the quantum dot layer. summary
    Thus, an embodiment provides a method for manufacturing a layer containing quantum boxes, this layer comprising first regions in which the quantum boxes are active, and second regions in which the quantum boxes are inactive, this method comprising the following steps: a) depositing on a support a first layer of a matrix in which quantum boxes are incorporated; b) depositing on the first layer a second layer of photoresist; c) insolating the second layer through a mask delimiting, in plan view, the first and second regions, then developing the resin of the second layer so as to remove the resin from the second layer opposite the second regions, and to preserve the resin of the second layer opposite the first regions; and d) removing the resin from the second layer facing the first regions without removing the matrix of the first layer opposite the first regions.
    According to one embodiment, the matrix of the first layer is a photosensitive resin.
    According to one embodiment, the photosensitive resin of the first layer is chosen from one of the families of the set comprising the family of positive photosensitive resins and the family of negative photosensitive resins, and in which the photosensitive resin of the second layer is selected from the other family of said set.
    According to one embodiment, the matrix of the first layer is a negative photosensitive resin and the resin of the second layer is a positive photosensitive resin.
    According to one embodiment, the matrix of the first layer is an SU8-type photosensitive resin, and the resin of the second layer is a TELR-type resin.
    According to one embodiment, the method does not include a step of insolation of the matrix of the first layer before the deposition of the second layer.
    According to one embodiment, the step of developing the resin of the second layer comprises dipping the second layer in a solution based on TMAH.
    According to one embodiment, the quantum boxes incorporated in the matrix of the first layer are quantum boxes of CdSe / ZnS type.
    According to one embodiment, during step d), the resin of the second layer is removed by oxygen plasma etching.
    According to one embodiment, the method further comprises, after step d), a step of etching an upper surface portion of the first layer.
    According to one embodiment, the step of etching an upper surface portion of the first layer is carried out by plasma etching with oxygen and sulfur hexafluoride.
    According to one embodiment, the steps a), b), c) and d) are repeated a second time to form, on the first layer, a third layer containing quantum boxes, this third layer comprising first regions in which the quantum boxes are active, and second regions in which the quantum boxes are inactive.
    According to one embodiment, the first regions of the third layer are arranged facing second regions of the first layer, and second regions of the third layer are arranged opposite first regions of the first layer.
    Another embodiment provides a device comprising a light source and, facing the light source, a layer containing quantum boxes made by a method of the aforementioned type.
    Another embodiment provides a device comprising a light source and, facing the light source, a stack of a first layer containing quantum boxes and a second layer containing quantum boxes, produced by a method of the invention. aforementioned type.
    Brief description of the drawings
    These features and their advantages, as well as others, will be set forth in detail in the following description of particular embodiments in a nonlimiting manner in connection with the accompanying drawings in which: FIGS. 1A, 1B, 1C, and 1D are sectional views schematically illustrating steps of an example of an embodiment of a method of manufacturing a layer containing quantum boxes, this layer having first regions in which the quantum boxes are active, and second regions in which the quantum boxes are inactive; and Figure 2 is a sectional view schematically illustrating an alternative embodiment of the method described in connection with Figures IA to 1D.
    detailed description
    The same elements have been designated with the same references in the various figures and, moreover, the various figures are not drawn to scale. In the description which follows, when reference is made to positional qualifiers such as the terms "above", "below", "upper", "lower", etc., reference is made to the orientation of the figures. it being understood that, in practice, the described structures may be oriented differently. Unless otherwise specified, the expressions "substantially", "almost", "about" and "of the order of" mean within 10%, preferably within 5%.
    FIG. 1A illustrates a deposition step, on the upper face of a support substrate 101, for example a silicon substrate, of a layer 103 comprising a matrix of a transparent photosensitive resin in which quantum boxes are incorporated. In this example, the photosensitive resin of the layer 103 belongs to the family of negative photosensitive resins, that is to say the resins for which the parts exposed to light radiation during a step of insolation of the resin become insoluble in a developer applied to the resin at a later stage of development, and for which the non-exposed parts of the light are soluble in the developer. The photosensitive resin of the layer 103 is, for example, a resin based on polyepoxides, for example a resin chosen from the family of negative resins of the SU8 type, that is to say whose elementary molecule comprises eight polyepoxide groups. By way of example, the photosensitive resin of the layer 103 is a resin of the type designated under the trade name SU8 1020PI by the company GERSELTEC ENGINEERING SOLUTIONS.
    The quantum boxes mixed with the resin of the layer 103 are, for example, quantum dots based on cadmium selenide (CdSe), for example quantum boxes with a core-shell structure of CdSe / ZnS type. Alternatively, the quantum boxes of the layer 103 are quantum boxes with core-shell structure of the InP / ZnS type or of the CdS / ZnS type or of the CdSe / ZnSe or PbS / CdS type type. By way of example, the incorporation of the quantum boxes into the photosensitive resin may comprise a step of mixing the quantum boxes initially in the form of a powder in a solvent, for example chloroform. The solution thus obtained can then be mixed with the resin. By way of example, the quantum boxes may be mixed in the solvent at a concentration of between 1 and 100 mg / ml, and then the solution obtained may be mixed with the resin, for example in a ratio of about 2 to 1 by volume (2 volumes of solution for 1 volume of resin).
    Prior to the deposition of the layer 103, the upper surface of the support substrate 101 may be prepared, for example by means of an oxygen plasma, in order to improve the adhesion and / or the uniformity of the layer 103. .
    The resin layer 103 may be spread on the upper surface of the substrate 101, for example by spin coating ("spin coating" in English). Annealing the structure, for example at a temperature between 80 and 150 ° C for a period of between 30 and 120 seconds, can then be performed to harden the resin layer 103 to enhance its mechanical strength. By way of example, the thickness of the layer 103 is between 0.5 and 50 μm, for example of the order of 0.9 μm. By way of illustrative example, the calculations carried out by the inventors have shown that a thickness of the order of 1 μm makes it possible to absorb 99% of the blue light emitted by a light-emitting diode with gallium nitride for a filling ratio. in volume of the layer 103 of the order of 50%.
    FIG. 1B illustrates a deposition step, on the upper face of the layer 103, of a photoresist layer 105. In this example, the photosensitive resin of the layer 105 belongs to the family of positive photosensitive resins, it is that is to say the resins for which the parts exposed to light radiation during a step of insolation of the resin become soluble in a developer applied to the resin at a later stage of development, and for which the non exposed to light radiation are insoluble in the developer. By way of example, the photosensitive resin of the layer 105 is a resin of the type designated under the trade name TELR by the company TOK EUROPE. Unlike the layer 103, the resin layer 105 does not contain quantum boxes. It will furthermore be noted that there is no provision for insolation of the layer 103, that is to say exposure of the layer 103 to a light radiation capable of modifying its structure, between the step of forming the layer 103 and the step of depositing the layer 105.
    The resin layer 105 may be spread on the upper surface of the substrate 101, for example by centrifugal coating. Annealing the structure, for example at a temperature between 80 and 150 ° C for a period of between 30 and 120 seconds, can then be performed to harden the resin layer 105 to enhance its mechanical strength.
    Figure 1B further illustrates a step subsequent to the deposition of the resin layer 105, during which the layer 105 is insolated through a mask 107 disposed above its upper surface. The mask 107 covers first regions 105a of the layer 105 and has openings facing second regions 105b of the layer 105. During the exposure step, the upper surface of the assembly is exposed to a light radiation 109 adapted to modify the chemical structure of the resin of the layer 105 in the regions of the layer 105 exposed to this radiation. The radiation applied to irradiate the resin of the layer 105 is for example a violet or ultraviolet radiation, for example a radiation with a wavelength of between 350 and 450 nm.
    After the insolation step, the mask 107 is removed, and a stabilization annealing of the structure, for example at a temperature between 80 and 150 ° C for a period of between 30 and 120 seconds, can be achieved.
    FIG. 1C illustrates a step of developing the resin layer 105, subsequent to the insolation step described in relation with FIG. 1B. During this step, the assembly formed by the substrate 101 and the layers 103 and 105 is immersed in a developer bath adapted to reveal in the resin layer 105 the pattern exposed through the mask 107 during the step of sunstroke. The developer bath comprises, for example, a solution based on tetramethylammonium hydroxide (TMAH), for example a solution designated by the trade name TMAH238 by the company MICROCHEMICALS. During this step, the regions 105b of the resin layer 105 previously exposed during the insolation step are removed by dissolution in the developer. Thus, at the end of the development step, only the regions 105a masked during the insolation step remain from layer 105. For example, during the development stage, the structure is soaked in the developer bath for 30 to 120 seconds until net patterns in the layer 105, then rinsed with water and dried.
    Surprisingly, the inventors have found that at the end of the development step of FIG. 1C, the quantum boxes contained in the regions 103b of the layer 103 above which the resin of the layer 105 is entirely removed. during the development stage, are inactive, whereas the quantum boxes contained in the regions 103a of the layer 103 above which the resin of the layer 105 is not removed during the development stage, have remained active. The term "inactive" is understood here to mean that the quantum boxes contained in the regions 103b of the layer 103 have lost their photoluminescent properties, and that the regions 103b of the layer 103 are now substantially transparent for visible light, that is to say to say that they transmit without significant modifications, in particular of color, the light which they receive. In addition, "active" is understood here to mean that the quantum boxes contained in the regions 103a of the layer 103 have retained their initial photoluminescent properties.
    FIG. 1D illustrates a step after the step of developing FIG. 1C, in which the remaining regions 105a are removed from the resin layer 105, without first removing and without simultaneously removing the regions 103b from the layer 103. In other words, the removal of the remaining regions 105a from the resin layer 105 is a selective shrinkage from the resin of the layer 103. By way of example, the removal of the regions 105a from the resin layer 105 is produced by dry etching using an oxygen plasma.
    The measurements carried out show that after the removal of the regions 105a of the layer 105, the quantum boxes contained in the regions 103a of the layer 103 are still active, and the quantum boxes contained in the regions 103b of the layer 103 are still inactive.
    Thus, the proposed method makes it possible to obtain a layer 103 of substantially constant thickness containing quantum boxes, this layer comprising first regions 103a in which the quantum boxes are active, and second regions 103b in which the quantum boxes are inactive.
    After the step of removing the regions 105a from the layer 105, an additional step of physically etching an upper surface portion of the layer 103, for example using an oxygen plasma and sulfur hexafluoride (SFg), can be implemented. This additional etching step makes it possible to accentuate the contrast of the photoluminescent pattern defined in the layer 103.
    In a subsequent step, the layer 103 in which the photo-luminescent pattern is formed may, for example, be attached to a lighting device, for example an array of light-emitting diodes, and then the support substrate 101 may be removed. . Alternatively, the support substrate 101 may be of a transparent material, for example glass, in which case the assembly comprising the support substrate 101 and the layer 103 may be arranged facing the lighting device. Alternatively, the support substrate 101 may be directly a semiconductor substrate in which light-emitting diodes have previously been formed, the layer 103 then being formed directly above the light-emitting diodes.
    An advantage of the proposed method lies in the fact that the color conversion layer 103 obtained has a constant or quasi-constant thickness, which gives it a relatively high robustness, and makes it easier to assemble with a possible additional optical element .
    Another advantage of the proposed method lies in the fact that the quantum dot layer 103, by its morphology and its stability, is compatible with standard microelectronic transfer, bonding and alignment techniques.
    Another advantage of the proposed method is related to the fact that the incorporation of the quantum dots in a resin layer makes it possible to obtain a relatively thick layer 103, which is particularly suitable for color conversion applications in screens. bright display.
    Another advantage of the proposed method is that the photoluminescent patterns can be defined in the layer 103 with a relatively high resolution. By way of illustrative example, the proposed method makes it possible to define in the layer 103 photoluminescent pads having lateral dimensions of the order of 1 to 10 μm and a spacing of the order of 1 to 10 μm, which is compatible with with the realization of a light display screen based on light-emitting diodes.
    Figure 2 is a sectional view schematically illustrating an alternative embodiment of the method described in connection with Figures IA to 1D.
    In the example of FIG. 2, the method described with reference to FIGS. 1A to 1D is repeated a second time so as to form, on the upper surface of the layer 103, a layer of resin 103 'in which are incorporated quantum boxes, this layer having regions 103a 'in which the quantum boxes are active, and regions 103b' in which the quantum boxes are inactive. By way of example, the active quantum boxes of the layer 103 are adapted to convert the light of an excitation light source into a light of a first color, for example in red light, and the active quantum boxes of the layer 103 'are adapted to convert the light of the excitation light source into a light of a second color different from the first color, for example green light. The quantum boxes of the layer 103 'are for example of the same nature as the quantum boxes of the layer 103, but of different dimensions.
    The active regions 103a 'of the layer 103' are for example arranged opposite inactive regions 103b of the layer 103. Although this is not visible in FIG. 2, inactive regions 103b 'of the layer 103' can be arranged. opposite inactive regions 103b of the layer 103, so as to transmit without significant color change the light emitted by the light source.
    Particular embodiments have been described. Various variations and modifications will be apparent to those skilled in the art. In particular, the described embodiments are not limited to the particular examples of dimensions and materials mentioned above.
    In addition, although an example of a method in which the matrix of the layer 103 is a negative photoresist and the resin of the layer 105 is a positive photoresist, the two types of resin may be the matrix of the layer 103 may be chosen from the family of positive photosensitive resins, the resin of the layer 105 then being chosen from the family of negative photosensitive resins.
    More generally, the matrix of the layer 103 may be of a material other than a photosensitive resin, for example a non-photosensitive resin, silicone, or any other suitable polymer material.
    In addition, the embodiments described are not limited to the above-mentioned particular example of application to color conversion in a bright display screen. More generally, the proposed method for delimiting active zones and inactive zones in a layer of a matrix incorporating quantum boxes may be used in other areas.
    权利要求:
    Claims (15)
    [1" id="c-fr-0001]
    A method of manufacturing a layer (103) containing quantum boxes, said layer having first regions (103a) in which the quantum boxes are active, and second regions (103b) in which the quantum boxes are inactive, and method comprising the following steps: a) depositing on a support (101) a first layer (103) of a matrix in which quantum boxes are incorporated; b) depositing on the first layer (103) a second layer (105) of photoresist; c) exposing the second layer (105) through a mask (107) delimiting, in plan view, the first (103a) and second (103b) regions, and then developing the resin of the second layer (105) so as to removing the resin from the second layer (105) facing the second regions (103b), and keeping the resin of the second layer (105) facing the first regions (103a); and d) removing the resin from the second layer (105) facing the first regions (103a) without removing the matrix of the first layer (103) facing the first regions (103a).
    [2" id="c-fr-0002]
    The method of claim 1, wherein the matrix of the first layer (103) is a photosensitive resin.
    [3" id="c-fr-0003]
    The method of claim 2, wherein the photosensitive resin of the first layer (103) is selected from one of the families of the set comprising the family of positive photosensitive resins and the family of negative photosensitive resins, and wherein the photosensitive resin of the second layer (105) is selected from the other family of said set.
    [4" id="c-fr-0004]
    The method of any one of claims 1 to 3, wherein the matrix of the first layer (103) is a negative photoresist and wherein the resin of the second layer (105) is a positive photoresist.
    [5" id="c-fr-0005]
    The method according to any one of claims 1 to 4, wherein the matrix of the first layer (103) is an SU8-type photosensitive resin, and wherein the resin of the second layer (105) is a resin of the type TELR.
    [6" id="c-fr-0006]
    6. Method according to any one of claims 1 to 5, having no step of insolation of the matrix of the first layer (103) before the deposition of the second layer (105).
    [7" id="c-fr-0007]
    The method of any one of claims 1 to 6, wherein the step of developing the resin of the second layer (105) comprises dipping the second layer (105) in a TMAH-based solution.
    [8" id="c-fr-0008]
    The method of any one of claims 1 to 7, wherein the quantum boxes embedded in the matrix of the first layer (103) are CdSe / ZnS quantum boxes.
    [9" id="c-fr-0009]
    The method of any one of claims 1 to 8, wherein in step d), the resin of the second layer (105) is removed by plasma etching with oxygen.
    [10" id="c-fr-0010]
    10. A method according to any one of claims 1 to 9, further comprising, after step d), a step of etching an upper surface portion of the first layer (103).
    [11" id="c-fr-0011]
    11. The method of claim 9, wherein said step of etching an upper surface portion of the first layer (103) is performed by plasma etching with oxygen and sulfur hexafluoride.
    [12" id="c-fr-0012]
    The method according to any one of claims 1 to 11, wherein steps a), b), c) and d) are repeated a second time to form, on the first layer (103), a third layer (103). ') containing quantum boxes, this third layer having first regions (103a') in which the quantum boxes are active, and second regions (103b ') in which the quantum boxes are inactive.
    [13" id="c-fr-0013]
    The method according to claim 12, wherein the first regions (103a ') of the third layer (103') are arranged facing second regions (103b) of the first layer (103), and in which second regions (103b) of 103b ') of the third layer (103') are arranged facing first regions (103a) of the first layer (103).
    [14" id="c-fr-0014]
    14. A device comprising a light source and, facing the light source, a layer (103) containing quantum boxes produced by a method according to any one of claims 1 to 12.
    [15" id="c-fr-0015]
    15. A device comprising a light source and, facing the light source, a stack of a first layer (103) containing quantum boxes and a second layer (103 ') containing quantum boxes, made by a process according to claim 12 or 13.
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1561047A|FR3043838B1|2015-11-17|2015-11-17|PROCESS FOR PRODUCING A LAYER CONTAINING QUANTUM BOXES|
    FR1561047|2015-11-17|FR1561047A| FR3043838B1|2015-11-17|2015-11-17|PROCESS FOR PRODUCING A LAYER CONTAINING QUANTUM BOXES|
    EP16197403.5A| EP3171415B1|2015-11-17|2016-11-04|Method for producing a layer containing quantum dots|
    US15/350,174| US10232404B2|2015-11-17|2016-11-14|Method of manufacturing a layer containing quantum dots|
    KR1020160151784A| KR20170057843A|2015-11-17|2016-11-15|Method of manufacturing a layer containing quantum dots|
    JP2016222429A| JP2017097348A|2015-11-17|2016-11-15|Method for manufacturing layer containing quantum dots|
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