WO2015184573A1 - Film isolant à constante diélectrique très faible et son procédé de fabrication - Google Patents

Film isolant à constante diélectrique très faible et son procédé de fabrication Download PDF

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Publication number
WO2015184573A1
WO2015184573A1 PCT/CN2014/000708 CN2014000708W WO2015184573A1 WO 2015184573 A1 WO2015184573 A1 WO 2015184573A1 CN 2014000708 W CN2014000708 W CN 2014000708W WO 2015184573 A1 WO2015184573 A1 WO 2015184573A1
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Prior art keywords
insulating film
dielectric constant
film
low dielectric
ultra
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PCT/CN2014/000708
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English (en)
Chinese (zh)
Inventor
丁士进
丁子君
张卫
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复旦大学
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Publication of WO2015184573A1 publication Critical patent/WO2015184573A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76837—Filling up the space between adjacent conductive structures; Gap-filling properties of dielectrics
    • 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
    • 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
    • C23C16/50—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 using electric discharges
    • C23C16/513—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 using electric discharges using plasma jets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76822—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc.
    • H01L21/76826—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc. by contacting the layer with gases, liquids or plasmas
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
    • H01L2221/10—Applying interconnections to be used for carrying current between separate components within a device
    • H01L2221/1005—Formation and after-treatment of dielectrics

Definitions

  • the present invention relates to the field of ultra-large scale integrated circuit (ULSI) interconnect technology, and more particularly to a method for fabricating a low dielectric constant insulating film between interconnect metal layers.
  • ULSI ultra-large scale integrated circuit
  • C capacitance Due to the increase in RC delay, the gain of the device speed obtained on the gate is offset by the propagation delay between the metal interconnects; see Liu Ming, Liu Yuling, Liu Bo et al. "Low-k dielectric and copper interconnect integration process [J].
  • the dielectric constant of the material is mainly related to the total polarizability of the material and the density of the material, and ultra-low dielectric is currently obtained.
  • the constant material is mainly achieved by introducing pores in the dielectric matrix (dielectric constant is approximately equal to 1), mainly because the introduction of pores can effectively reduce the density of the material itself.
  • dielectric constant is approximately equal to 1
  • the pores in the porous film material are usually added with a templating agent in the precursor, and then The templating agent is removed by a heat treatment method to obtain a porous film material.
  • a templating agent for example, Shen et al. used tetraethyl orthosilicate (TEOS) as a silicon source and hexadecanoyltrimethylammonium bromide (CTAB) as a template to prepare a porous film material by sol-gel method under acidic conditions.
  • TEOS tetraethyl orthosilicate
  • CTAB hexadecanoyltrimethylammonium bromide
  • the pore diameter is 4 nm and the dielectric constant is 2.5 (Reference J. Shen, A. Luo, LF Yao, et al. Low dielectric constant silica films with ordered nanoporous structure [J]. Materials science and Engineering, 2007, 27 (5- 8): 1145-1148).
  • the preparation method of the low dielectric constant film mentioned in the above patent "a porous ultra-low dielectric constant material film and a preparation method thereof" is spin coating
  • the film prepared by the spin coating method has many problems such as poor film formation quality and uneven thickness. Therefore, the modern large-scale integrated circuit process has basically not used the spin coating method to prepare the film, but adopts the present invention.
  • a plasma enhanced chemical vapor deposition (PECVD) method is mentioned.
  • PECVD plasma enhanced chemical vapor deposition
  • the low dielectric constant film prepared by PECVD has good uniformity and repeatability, can form a large area film, and has excellent step coverage.
  • the composition and thickness of the film are easy to control, and the range of use is wide, the equipment is simple, the production is easy, the efficiency is high, and the cost is low.
  • Reference 5 R. Navamathavan, CK Choi. Plasma enhanced chemical vapor deposition of low dielectric constant SiOC(-H) films using MTES/0 2 precursor [J], Thin Solid Films, 2007, 515(12): 5040-5044 .
  • MTES+0 2 and VTMS+0 2 were used as precursors, respectively, and films were deposited by PECVD at different temperatures, and the final annealing temperatures were 500 ° C and 450 ° C, respectively.
  • the thermal stability requirements ⁇ 420 ° C
  • the pore-forming agent was removed by heat treatment to obtain a film material with a dielectric constant of 2.05, but the mechanical properties were not satisfactory, and it was difficult to meet the requirements of the film industry for the film material.
  • the invention utilizes the novel mixed precursor of MTES and LIMO, innovatively adopts alternating PECVD insulating film and post-plasma treatment method, that is, the insulating layer deposition step and the dense layer forming step are alternately performed, and the formed film has anti-hygroscopicity. Strong, good mechanical properties, low annealing temperature, compatible with integrated processes. Disclosure of invention
  • An object of the present invention is to provide a method for preparing an ultra-low dielectric constant insulating film.
  • the insulating film prepared by the method has ideal electrical and mechanical properties and can be used in the field of extremely large-scale integrated circuit interconnection technology.
  • the present invention provides a method of preparing an ultra-low dielectric constant insulating film, the method comprising the following specific steps:
  • Step 1 Depositing a thin film by plasma enhanced chemical vapor deposition: using methyltriethoxysilane and limonene as reaction sources, and methyltriethoxysilane and limonene are introduced into the carrier gas by using helium as a carrier gas.
  • a 50-100 nm insulating layer is deposited, wherein a flow ratio of methyltriethoxysilane to limonene is 1:1 to 1:2.5, and the flow rate is in grams per minute;
  • Step 2 in-situ treatment of the surface of the insulating layer by Ar or He plasma in the above cavity for 1-5 minutes to form a dense modified layer, the function of the modified layer is to prevent water molecules from being in the entire insulating layer.
  • the lower diffusion thereby reducing the adsorption of water by the pores in the above insulating layer, and suppressing the increase of the dielectric constant caused by water absorption;
  • Step 3 repeat steps 1 and 2 above until the target thickness of the insulating film is reached, and insulation is obtained.
  • Step 4 in an inert atmosphere, the insulating film obtained in the step 3 is subjected to high temperature annealing to remove a hydrocarbon group (the hydrocarbon group includes a hydrocarbon group in the precursor and a hydrocarbon group in the limonene) Thereby, an ultra-low dielectric constant insulating film having a porous structure is formed.
  • the hydrocarbon group includes a hydrocarbon group in the precursor and a hydrocarbon group in the limonene
  • the radio frequency used in the deposition process in step 1 is 13.56 MHz
  • the initial vacuum in the reaction chamber is 0.018-0.02 Torr
  • the substrate temperature at the time of depositing the insulating layer is 100-400 ° C
  • the power is 200-600 watts
  • working pressure 2-5 Torr (1 Torr 133.322 Pa)
  • MTES flow rate into the reaction chamber is 1.0-2.0 g/min
  • LIMO flow is 1.0-3.5 g/min
  • He carrier gas flow is 500 - 5000sccm.
  • the Ar or He plasma surface treatment has a power of 300-600 watts, a treatment time of 1-5 minutes, and a gas pressure of 2-8 Torr.
  • the annealing temperature is 200-420 ° C
  • the pressure in the annealing furnace is 0.2-0.3 Torr
  • the annealing time is 2-6 hours
  • the annealing atmosphere is argon or nitrogen.
  • the room temperature rises to the annealing temperature within 5-30 minutes.
  • the present invention also provides an ultra-low dielectric constant insulating film prepared by the above method, wherein the insulating film comprises: a plurality of insulating layers; each of the insulating layers is provided with a modifying layer, and has a layer inside the insulating layer a plurality of pores; the dielectric constant of the ultra-low dielectric constant insulating film is 2.2-2.4, and the leakage current density at lMV/cm is 1 (T 9 -l (T 8 A/cm 2 ; Young's modulus is 4.2-) 17GPa, hardness 0.5-1.3GPa.
  • the ultra low dielectric constant insulating film provided by the invention is prepared by using MTES and LIMO as reaction sources respectively, and is introduced into the reaction cavity under the carrying of He carrier gas, and is deposited by plasma enhanced chemical vapor deposition to form an insulating layer, and then The surface of the insulating layer is treated in situ by argon (Ar) or helium (He) plasma to form a dense modified layer. The above process is repeated until the film of the desired thickness is reached, and finally the film is annealed at a high temperature to The hydrocarbon group is removed to form an ultra-low dielectric constant porous insulating film.
  • the film provided by the invention adopts the novel reaction sources MTES and LIMO, is simple and easy to obtain, is safe to use, and the by-products are not polluted to the environment, and the prepared dielectric constant of the film is in the range of 2.2-2.4, which satisfies the ultra-low dielectric.
  • the constant also has superior mechanical properties.
  • the film also has excellent insulation properties, and the leakage current density can be reached under an external electric field of lMV/cm. 10_ 9 -1(T 8 A/ C m 2 . Therefore, the ultra-low dielectric constant insulating film prepared by the invention can fully satisfy the requirements of the advanced integrated circuit for the electrical mechanical properties and the insulation performance of the low dielectric constant material.
  • the thin film preparation method provided by the invention innovatively adopts alternating plasma enhanced chemical vapor deposition, and the formed film has good moisture absorption resistance, good mechanical properties, and is compatible with the integrated process, and the process is simple, and the deposition rate is fast. And the film quality is good.
  • Figure la-Id is a schematic view showing the preparation process of the ultra-low dielectric constant insulating film of the present invention. The best way to implement the invention
  • the invention adopts plasma enhanced chemical vapor deposition technology to prepare an ultra-low dielectric constant insulating film, and uses helium (He) as a carrier gas to respectively drive the precursor methyltriethoxysilane (C 7 H 18 0 3 Si,
  • the MTES) and the pore former limonene (C 1() H 16 , referred to as LIMO) are introduced into the plasma enhanced chemical vapor deposition reaction chamber to form an insulating layer.
  • the RF frequency used in the plasma enhanced chemical vapor deposition process is 13.56.
  • the initial vacuum in the reaction chamber is 0.018 ⁇ 0.02 Torr
  • the substrate temperature is 100 ⁇ 400°C
  • the deposition power is 200 ⁇ 600 watts
  • the working pressure is 2 ⁇ 5 Torr
  • the He carrier gas flow is 500 ⁇ 5000sccm (standard) -state cubic centimeter per minute ).
  • the vaporization temperatures of MTES and LIMO before introduction into the reaction chamber are 50 ⁇ 60°C and 60 ⁇ 100°C respectively
  • the MTES flow rate is 1.0-2.0g g/min
  • the LIMO flow rate is 1.0-3.5g/min.
  • the ratio is 1 : 1-1: 2.5
  • a deposition thickness of 50 - 100 nm forming an insulating layer 10 as shown in FIG. 1a, the insulating layer 10 being composed of a Si-O-Si structure 11 and a hydrocarbon group 12.
  • the surface of the insulating layer is treated in situ by Ar or He plasma in the above cavity to form a dense modified layer 20 (as shown in FIG. 1b), with a power of 300-600 watts, a processing time of 1-5 minutes, and a gas pressure. It is 2-8 Torr.
  • the function of the modifying layer 20 is to seal the outer surface of the insulating layer 10 to prevent the pores formed by annealing in the insulating layer 10 from absorbing water.
  • the above two steps are respectively repeated to reach the insulating film of the target thickness, and as shown in FIG. 1c, the insulating film 30 in which the insulating layer-decorating layer is alternately disposed is formed three times.
  • the target insulating film 30 is placed in an annealing furnace, and the annealing furnace has a pressure of 0.2-0.3 Torr in Ar or N 2 atmosphere, and rises from room temperature to annealing temperature in 5-30 minutes, and is annealed at 200-420 ° C.
  • the removal of the hydrocarbon group a forms a plurality of irregular pores 13 inside the insulating layer of the insulating film (the pore 13 includes a plurality of worm-like pores and a plurality of irregular circular holes), and finally obtains an ultra-low dielectric constant having a porous structure.
  • Insulating film as shown in Figure Id.
  • the present invention uses a low-resistance silicon wafer (resistance of 0.001-0.02 ⁇ ) as a substrate, and electron beam evaporated aluminum forms a diameter of 400-420 ⁇ m on the film.
  • a circular metal electrode is used to form a capacitor, thereby obtaining a metal-insulator-semiconductor (MIS) capacitor structure.
  • the above capacitors are measured based on the capacitance-voltage characteristics at room temperature, and a reliable average capacitance value is obtained by a multi-point test, and the dielectric constant is determined in consideration of the electrode area and the film thickness.
  • the leakage characteristics of the film are obtained by measuring the current-voltage.
  • the hardness and Young's modulus of the film were obtained by a nanoindenter.
  • Example 1-6 seven different film samples (i.e., samples numbered 1-6) were prepared by varying the relative flow rates of methyltriethoxysilane and limonene.
  • Table 2 lists The electrical properties, mechanical properties and leakage current of the samples prepared under different flow ratio conditions. As the relative flow rate increases, the dielectric constant and its mechanical properties show a trend of decreasing first and then increasing. It can be seen from Table 2 that the obtained film has a minimum dielectric constant of 2.2 and a refractive index of 1.309. In terms of mechanical properties, the hardness is 0.55 GPa and the Young's modulus is 4.23 GPa, which has reached the porous low dielectric constant film mechanics reported in the literature. The general level of performance, and other samples also showed excellent mechanical properties. At the same time, the leakage current density is also small, showing good insulation performance. Therefore, it is possible to meet the requirements of the next-generation integrated circuit process for low dielectric constant thin film materials.
  • Table 2 Sample deposition rate, electrical properties, mechanical properties and leakage current

Abstract

L'invention concerne un film isolant à constante diélectrique très faible et son procédé de fabrication. Le procédé comprend : étape 1, le dépôt d'un film mince au moyen d'une technologie de dépôt chimique en phase vapeur assisté par plasma, du méthyl triéthoxysilane et du LIMO étant utilisés en tant que source de réaction et de l'hélium étant utilisé en tant que gaz porteur introduit dans une cavité de réaction de dépôt chimique en phase vapeur, le film isolant formé par dépôt ayant une épaisseur de 50 à 100 nm, et le débit du méthyl triéthoxysilane et du LIMO étant égal à 1:1 - 1:2,5; étape 2, la réalisation d'une remédiation in-situ sur la surface de la couche isolante par utilisation de plasma d'Ar pour former une couche modifiée compacte; étape 3, la répétition de l'étape 1 et de l'étape 2 afin d'obtenir le film isolant d'épaisseur cible; étape 4, le recuit du film isolant à température élevée pour former un film isolant à constante diélectrique très faible. D'autres plasmas utilisés pour améliorer le dépôt chimique en phase vapeur du film isolant et le traitement au plasma ultérieur sont utilisés de manière créative dans l'invention avec des processus simples et une bonne vitesse de dépôt, le film formé présente une bonne résistance à l'humidité et est compatible avec la technique intégrée, la qualité de formation de film est bonne, et les besoins en circuit intégré avancé en termes de propriété électrique, de propriété mécanique et de propriété d'isolation d'un matériau à faible constante diélectrique sont entièrement satisfaits.
PCT/CN2014/000708 2014-06-04 2014-07-28 Film isolant à constante diélectrique très faible et son procédé de fabrication WO2015184573A1 (fr)

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Application Number Priority Date Filing Date Title
CN201410243600.0A CN104008997A (zh) 2014-06-04 2014-06-04 一种超低介电常数绝缘薄膜及其制备方法
CN201410243600.0 2014-06-04

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US9460915B2 (en) * 2014-09-12 2016-10-04 Lam Research Corporation Systems and methods for reducing backside deposition and mitigating thickness changes at substrate edges
CN104498900A (zh) * 2014-12-23 2015-04-08 上海爱默金山药业有限公司 一种低介电常数薄膜的制备方法
CN115522180A (zh) * 2022-09-20 2022-12-27 苏州源展材料科技有限公司 一种低介电常数的硅基薄膜的制备方法及其应用

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CN1576390A (zh) * 2003-05-29 2005-02-09 气体产品与化学公司 用于低介电薄膜的机械强化添加剂
CN1651159A (zh) * 2004-01-23 2005-08-10 气体产品与化学公司 成孔材料沉积后的cvd室清洗
CN1698189A (zh) * 2003-01-13 2005-11-16 应用材料股份有限公司 改善低介电常数材料的破裂临界值及机械特性的方法
CN101575700A (zh) * 2008-05-05 2009-11-11 气体产品与化学公司 致孔剂,致孔的前体以及使用其来提供低介电常数的多孔有机硅玻璃膜的方法
CN102089405A (zh) * 2008-07-08 2011-06-08 富士胶片电子材料美国有限公司 防止环烯烃衍生物降解的添加剂

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CN1698189A (zh) * 2003-01-13 2005-11-16 应用材料股份有限公司 改善低介电常数材料的破裂临界值及机械特性的方法
CN1527366A (zh) * 2003-03-04 2004-09-08 气体产品与化学公司 通过紫外光辐射改善致密和多孔有机硅酸盐材料的机械性能
CN1576390A (zh) * 2003-05-29 2005-02-09 气体产品与化学公司 用于低介电薄膜的机械强化添加剂
CN1651159A (zh) * 2004-01-23 2005-08-10 气体产品与化学公司 成孔材料沉积后的cvd室清洗
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