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US20180019165A1 - CVD Mo DEPOSITION BY USING MoOCl4 - Google Patents

CVD Mo DEPOSITION BY USING MoOCl4 Download PDF

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Publication number
US20180019165A1
US20180019165A1 US15/649,248 US201715649248A US2018019165A1 US 20180019165 A1 US20180019165 A1 US 20180019165A1 US 201715649248 A US201715649248 A US 201715649248A US 2018019165 A1 US2018019165 A1 US 2018019165A1
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Prior art keywords
molybdenum
substrate
moocl
vapor
containing material
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US15/649,248
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English (en)
Inventor
Thomas H. Baum
Philip S.H. Chen
Robert Wright
Bryan Hendrix
Shuang Meng
Richard Assion
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Entegris Inc
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Entegris Inc
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Priority to US15/649,248 priority Critical patent/US20180019165A1/en
Publication of US20180019165A1 publication Critical patent/US20180019165A1/en
Priority to US15/963,656 priority patent/US11107675B2/en
Abandoned legal-status Critical Current

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    • 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
    • H01L21/76838—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 conductors
    • H01L21/76841—Barrier, adhesion or liner layers
    • H01L21/76871—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
    • H01L21/76876—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers for deposition from the gas phase, e.g. CVD
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    • 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
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    • 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
    • C23C16/04—Coating on selected surface areas, e.g. using masks
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    • 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
    • C23C16/06—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 deposition of metallic material
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    • 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
    • C23C16/06—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 deposition of metallic material
    • C23C16/08—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 deposition of metallic material from metal halides
    • C23C16/14—Deposition of only one other metal element
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    • 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
    • C23C16/45523—Pulsed gas flow or change of composition over time
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    • 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
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
    • 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
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
    • H01L21/28568—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table the conductive layers comprising transition metals
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    • 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
    • H01L21/76838—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 conductors
    • H01L21/76841—Barrier, adhesion or liner layers
    • H01L21/76843—Barrier, adhesion or liner layers formed in openings in a dielectric
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • 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
    • H01L21/76838—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 conductors
    • H01L21/76841—Barrier, adhesion or liner layers
    • H01L21/7685—Barrier, adhesion or liner layers the layer covering a conductive structure
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    • H10B—ELECTRONIC MEMORY DEVICES
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    • H10B—ELECTRONIC MEMORY DEVICES
    • H10B41/00—Electrically erasable-and-programmable ROM [EEPROM] devices comprising floating gates
    • H10B41/30—Electrically erasable-and-programmable ROM [EEPROM] devices comprising floating gates characterised by the memory core region
    • H10B41/35—Electrically erasable-and-programmable ROM [EEPROM] devices comprising floating gates characterised by the memory core region with a cell select transistor, e.g. NAND
    • H10P14/412—
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    • H10W20/0425—
    • H10W20/4441—

Definitions

  • the present disclosure relates to vapor deposition of molybdenum-containing material.
  • the present disclosure relates to the use of molybdenum oxytetrachloride (MoOCl 4 ) as a precursor for such deposition.
  • MoOCl 4 molybdenum oxytetrachloride
  • molybdenum is increasingly utilized in the manufacture of semiconductor devices, including use in diffusion barriers, electrodes, photomasks, power electronics substrates, low-resistivity gates, and interconnects.
  • Molybdenum pentachloride is most commonly used as a molybdenum source for chemical vapour deposition of molybdenum-containing material.
  • Molybdenum pentachloride is most commonly used as a molybdenum source for chemical vapour deposition of molybdenum-containing material.
  • the present disclosure relates to vapor deposition of molybdenum-containing material, and more specifically to the use of molybdenum oxytetrachloride (MoOCl 4 ) as a source reagent for such vapor deposition, as well as to processes and devices employing molybdenum oxytetrachloride (MoOCl 4 ) as a source reagent.
  • MoOCl 4 molybdenum oxytetrachloride
  • the disclosure relates to a method of forming a molybdenum-containing material on a substrate, comprising contacting the substrate with molybdenum oxytetrachloride (MoOCl 4 ) vapor under vapor deposition conditions, to deposit the molybdenum-containing material on the substrate.
  • MoOCl 4 molybdenum oxytetrachloride
  • the disclosure relates to a method of forming a molybdenum-containing material on a substrate, comprising contacting the substrate with diborane under contacting conditions establishing nucleation surface on the substrate, and depositing molybdenum on the nucleation surface by a vapor deposition process utilizing molybdenum oxytetrachloride (MoOCl 4 ) precursor, to produce the molybdenum-containing material on the substrate.
  • MoOCl 4 molybdenum oxytetrachloride
  • FIG. 1 is a graph of the thermogravimetric analysis (TGA) of molybdenum oxytetrachloride.
  • FIG. 2 is a schematic cross-sectional elevation view of a semiconductor device structure comprising molybdenum-containing material deposited in accordance with an embodiment of the present disclosure.
  • FIG. 3 shows a molybdenum oxytetrachloride (MoOCl 4 )/hydrogen (H 2 ) deposition curve illustrating results from Example 1.
  • FIG. 4 is a graph of resistivity, as a function of thickness, for deposition of molybdenum by a MoOCl 4 /H 2 process in accordance with Example 1.
  • FIG. 5 and FIG. 6 are scanning electron micrograph (SEM) images of a deposited molybdenum film formed in accordance with Example 2.
  • FIG. 7 is a graph of molybdenum thickness as a function of deposition time for deposition of molybdenum by a MoOCl 4 /H 2 process in accordance with Example 3.
  • FIG. 8 is a graph of film resistivity as a function of molybdenum thickness for molybdenum deposition conducted by a MoOCl 4 /H 2 process in accordance with Example 4.
  • FIG. 9 is a graph comparing deposition rate as a function of run number, for molybdenum deposition in accordance with Example 5.
  • FIG. 10 is a graph comparing film resistivity of deposited molybdenum films as a function of molybdenum film thickness in accordance with Example 6.
  • FIG. 11 is a graph of molybdenum film thickness, as a function of diborane soak time illustrating results from Example 7.
  • FIGS. 12 and 13 are SEM micrographs of film depositions formed in Example 8.
  • FIGS. 14 and 15 are SEM images of deposited films in vias formed in Example 9.
  • FIG. 16 is a graph of molybdenum thickness and resistivity as a function of diborane soak time for a deposition process in accordance with Example 10.
  • FIG. 17 is a graph of molybdenum thickness and resistivity as a function of MoOCl 4 /H 2 exposure time, for a deposition process in accordance with Example 11.
  • FIG. 18 is an SEM image of a molybdenum film deposited in accordance with Example 12.
  • FIG. 19 is an SEM cross-section image of a molybdenum film deposited in accordance with Example 12.
  • FIG. 20 is a graph of molybdenum thickness and resistivity as a function of stage temperature, showing a reaction rate limited regime for the MoOCl 4 /H 2 process without diborane nucleation, according to Example 13.
  • FIG. 21 is a graph of molybdenum thickness and resistivity as a function of stage temperature, showing a reaction rate limited regime for the MoOCl 4 /H 2 process with diborane nucleation, according to Example 13.
  • FIGS. 23 and 24 show step coverage on a via structure by a nucleation and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, as conducted in Example 15.
  • FIGS. 25, 26, and 27 show respective via structures deposited with molybdenum in accordance with Example 16.
  • FIGS. 28, 29, and 30 show respective via structures deposited with molybdenum in accordance with Example 17.
  • FIGS. 31, 32, and 33 show respective via structures deposited with molybdenum in accordance with Example 18.
  • FIGS. 34, 35, and 36 are SEM images of a via structure deposited with molybdenum in accordance with Example 19.
  • FIGS. 37 and 38 are SEM images of a via structure deposited with molybdenum in accordance with Example 20.
  • FIGS. 39 and 40 are SEM images of a via structure deposited with molybdenum in accordance with Example 21.
  • the present disclosure relates to vapor deposition of molybdenum, and to use of molybdenum oxytetrachloride (MoOCl 4 ) for such deposition, e.g., in the manufacture of semiconductor devices in which molybdenum films of superior conformality and performance properties are desired.
  • MoOCl 4 molybdenum oxytetrachloride
  • molybdenum oxytetrachloride MoOCl 4
  • vapor deposition processes such as chemical vapor deposition to provide low resistivity, high deposition rate films of a highly conformal character.
  • the disclosure relates in one aspect to a method of forming a molybdenum-containing material on a substrate, comprising contacting the substrate with molybdenum oxytetrachloride (MoOCl 4 ) vapor under vapor deposition conditions, to deposit the molybdenum-containing material on the substrate.
  • MoOCl 4 molybdenum oxytetrachloride
  • molybdenum oxytetrachloride MoOCl 4
  • MoOCl 4 molybdenum oxytetrachloride
  • deposition of molybdenum oxytetrachloride MoOCl 4
  • MoCl 5 molybdenum pentachloride
  • the molybdenum-containing material can have low resistivity and oxygen content.
  • the method comprises establishing a nucleation surface on the substrate and said contacting of the substrate with molybdenum oxytetrachloride (MoOCl 4 ) vapor comprises contacting the nucleation surface of the substrate with molybdenum oxytetrachloride (MoOCl 4 ) vapor to deposit the molybdenum-containing material on the substrate.
  • MoOCl 4 molybdenum oxytetrachloride
  • a nucleation surface may advantageously facilitate deposition of low resistivity molybdenum-containing material on the substrate at lower temperatures.
  • Establishing the nucleation surface on the substrate may suitably comprise contacting the substrate with diborane vapor and optionally separately with molybdenum oxytetrachloride (MoOCl 4 ) vapor.
  • establishing the nucleation surface may comprise a plurality of cycles of contacting the substrate with diborane vapor and separately with molybdenum oxytetrachloride (MoOCl 4 ) vapor.
  • contact of the titanium nitride layer with diborane vapor is conducted at temperature in a range of from 300° C. to 450° C.
  • the vapor deposition conditions may be pulsed. It has been found that this can improve step coverage of the deposition.
  • the “pulse” and “purge” time of pulsed deposition may each independently be in the range of from 1 to 20 seconds.
  • the vapor conditions are selected such that the deposited molybdenum-containing material has a resistivity of at most 20 ⁇ cm, optionally at most 15 ⁇ cm.
  • the molybdenum-containing material may be deposited at a (stage) temperature in the range of from 400° C. to 750° C., or in the range of from 400° C. to 600° C., or in the range of from 400° C. to 575° C.
  • the molybdenum-containing material may be deposited at a (stage) temperature in the range of from 450° C. to 750° C., or in the range of from 450° C. to 600° C., or in the range of from 450° C. to 575° C.
  • the molybdenum-containing material may be deposited at a (stage) temperature in the range of from 500° C. to 750° C., or in the range of from 500° C. to 600° C., or in the range of from 500° C. to 575° C.
  • the vapor deposition conditions comprise an inert atmosphere, save for the optional presence of a reducing agent such as hydrogen.
  • a reducing agent such as hydrogen.
  • the molybdenum oxytetrachloride (MoOCl 4 ) vapor may be deposited in the substantial absence of other metal vapors.
  • the method may comprise volatilizing molybdenum oxytetrachloride (MoOCl 4 ) to form the molybdenum oxytetrachloride (MoOCl 4 ) vapor for the vapor deposition operation.
  • the vapor deposition conditions may be of any suitable type, and may for example comprise a reducing ambient so that the molybdenum-containing material comprises elemental molybdenum material.
  • the molybdenum-containing material may comprise, or alternatively consist, or consist essentially of, elemental molybdenum, or molybdenum oxide, or other molybdenum-containing material.
  • the substrate utilized in the method of the disclosure may be of any suitable type, and may for example comprise a semiconductor device substrate, e.g., a silicon substrate, a silicon dioxide substrate, or other silicon-based substrate.
  • the substrate may comprise one or more of TiN, Mo, MoC, B, SiO 2 , W, and WCN.
  • the substrate may be processed or fabricated to include a barrier layer thereon, e.g. titanium nitride, for subsequently deposited material.
  • a barrier layer e.g. titanium nitride
  • the substrate may comprise a nucleation layer on a titanium nitride layer, with the molybdenum-containing material being deposited on the nucleation layer in the appertaining process flow sequence.
  • Such a nucleation layer or surface may for example be formed by pulsed CVD or ALD or other vapor deposition technique, and the formation of such a nucleation layer may be carried out by contacting of the titanium nitride layer with diborane vapor and separately with molybdenum oxytetrachloride (MoOCl 4 ) vapor.
  • the respective diborane vapor and molybdenum oxytetrachloride (MoOCl 4 ) contacting steps may be carried out alternatingly and repetitively for as many cycles as are desired to form the nucleation layer of desired thickness.
  • the process conditions for such nucleation layer formation may comprise any suitable desired temperature, pressure, flow rate, and other process conditions.
  • the contact of the titanium nitride layer with diborane vapor is conducted at temperature in a range of from 300° C. to 450° C. In various embodiments, the contact of the titanium nitride layer with molybdenum oxytetrachloride (MoOCl 4 ) vapor is conducted at temperature in a range of from 400° C. to 575° C., or another range as defined hereinabove for (MoOCl 4 ) vapor deposition.
  • MoOCl 4 molybdenum oxytetrachloride
  • the molybdenum-containing material can be deposited on the nucleation layer, to form a bulk deposit of elemental molybdenum or molybdenum oxide or other molybdenum-containing compound or composition.
  • the molybdenum-containing material is deposited on the nucleation layer or surface at temperature in a range of from 400° C. to 575° C. or another range as defined hereinabove for (MoOCl 4 ) vapor deposition.
  • the process may be carried out, so that the vapor deposition conditions produce deposition of elemental molybdenum as the molybdenum-containing material on the nucleation layer of the substrate.
  • the vapor deposition conditions may be of any suitable character, and may for example comprise presence of hydrogen or other reducing gas, to form a bulk layer of elemental molybdenum on the nucleation layer.
  • the broad method of forming a molybdenum-containing material on a substrate in accordance with the present disclosure may comprise vapor deposition conditions comprising presence of hydrogen or other reducing gas.
  • the molybdenum-containing material may be deposited on the barrier layer or nucleation layer or surface in the presence or absence of hydrogen.
  • the barrier layer may be constituted by titanium nitride, and the titanium nitride layer may be contacted with molybdenum oxytetrachloride (MoOCl 4 ) vapor in the presence of hydrogen.
  • the method of the present disclosure may be carried out in numerous alternative ways, and under a wide variety of process conditions.
  • the method of the disclosure may for example be carried out in a process for making a semiconductor device on the substrate.
  • the semiconductor device may be of any suitable type, and may for example comprise a DRAM device, 3-D NAND device, or other device or device precursor structure.
  • the substrate may comprise a via in which the molybdenum-containing material is deposited.
  • the via may for example have an aspect ratio of depth to lateral dimension that is in a range of from 20:1 to 30:1.
  • the process chemistry for depositing molybdenum-containing material in accordance with the present disclosure may include deposition of elemental molybdenum, Mo(0), by the reaction MoOCl4+3H2 ⁇ Mo+4 HCl+H2O.
  • a nucleation layer or surface formed as described hereinabove by successive contacting of the substrate with diborane and MoOCl 4 to form the nucleation layer may involve the formation reaction of 2MoOCl 4 +B 2 H 6 ⁇ 2Mo+2BOCl+6HCl.
  • the molybdenum-containing material deposited in accordance with the method of the present disclosure may be characterized by any appropriate evaluation metrics and parameters, such as deposition rate of the molybdenum-containing material, film resistivity of the deposited molybdenum-containing material, film morphology of the deposited molybdenum-containing material, film stress of the deposited molybdenum-containing material, step coverage of the material, and the process window or process envelope of appropriate process conditions. Any appropriate evaluation metrics and parameters may be employed, to characterize the deposited material and correlate same to specific process conditions, to enable mass production of corresponding semiconductor products.
  • the disclosure relates to a method of forming a molybdenum-containing material on a substrate, comprising contacting the substrate with diborane under contacting conditions establishing nucleation surface on the substrate, and depositing molybdenum on the nucleation surface by a vapor deposition process utilizing molybdenum oxytetrachloride (MoOCl 4 ) precursor, to produce the molybdenum-containing material on the substrate.
  • MoOCl 4 molybdenum oxytetrachloride
  • Such method may be carried out in any suitable manner as variously described herein.
  • such method may be conducted with a vapor deposition process comprising chemical vapor deposition, e.g., pulsed chemical vapor deposition.
  • the method may be carried out so that the resulting molybdenum-containing material is composed essentially of elemental molybdenum, and in various embodiments the molybdenum may be deposited on the nucleation surface in the presence of hydrogen or other suitable reducing gas.
  • the method may be carried out in the manufacture of a semiconductor product, such as a DRAM device, or a 3-D NAND device.
  • step coverage e.g., step coverage of from 90 to 110%.
  • FIG. 1 there is shown a graph of the thermogravimetric analysis (TGA) of molybdenum oxytetrachloride, plotted as weight percent as a function of temperature, in degrees Centigrade, showing the characteristics of the thermal behavior of molybdenum oxytetrachloride.
  • TGA thermogravimetric analysis
  • MoOCl 4 molybdenum oxytetrachloride
  • MoCl 5 molybdenum pentachloride
  • a semiconductor device structure comprising molybdenum-containing material deposited in accordance with an embodiment of the present disclosure includes a base layer of silicon dioxide (SiO 2 ), overlying which is a barrier layer of titanium nitride (TiN), over which a nucleation layer has been formed by contact of the substrate with molybdenum oxytetrachloride (MoOCl 4 ) and diborane, with a layer of elemental molybdenum (Mo) as an upper layer deposited on the nucleation layer from molybdenum oxytetrachloride (MoOCl 4 ) in the presence of hydrogen (H 2 ).
  • SiO 2 silicon dioxide
  • TiN titanium nitride
  • MoOCl 4 molybdenum oxytetrachloride
  • diborane a layer of elemental molybdenum (Mo) as an upper layer deposited on the nucleation layer from molybdenum oxytetrachloride (MoOC
  • the FIG. 2 semiconductor device may be fabricated by the following sequence of process steps on the substrate comprising the titanium nitride barrier layer on the silicon dioxide base layer.
  • Step 1 contacting the barrier layer (TiN layer) of the substrate with a pulse of diborane (B 2 H 6 ), for example at temperature in a range of from 300 to 450° C.;
  • Step 2 pumping/purging the deposition chamber
  • Step 3 contacting the barrier layer (TiN layer) of the substrate with a pulse of molybdenum pentachloride (MoCl 5 ) or molybdenum oxytetrachloride (MoOCl 4 ) vapor, in the presence of hydrogen (H2) or argon (Ar), for example at temperature on the order of 500° C.;
  • MoCl 5 molybdenum pentachloride
  • MoOCl 4 molybdenum oxytetrachloride
  • H2 hydrogen
  • Ar argon
  • Step 4 pumping/purging the deposition chamber
  • Step 5 repeating Steps 1-4 (optional) to form a nucleation layer of desired characteristics
  • Step 6 depositing bulk molybdenum on the nucleation layer, by contact of the substrate with molybdenum oxytetrachloride (MoOCl 4 ) vapor, in the presence of hydrogen (H 2 ), for example at temperature on the order of 500° C.
  • MoOCl 4 molybdenum oxytetrachloride
  • Steps 1 to 5 are optional and may be left out if no nucleation layer is required.
  • a chemical vapor deposition (CVD) molybdenum deposition with molybdenum oxytetrachloride (MoOCl 4 )/hydrogen (H 2 ) was carried out utilizing the following process conditions: a 700° C. stage on which substrate was maintained; a 70° C. ampoule from which the molybdenum oxytetrachloride (MoOCl 4 ) precursor was dispensed for the vapor deposition operation; 60 torr pressure in the vapor deposition operation; 50 standard cubic centimeter per minute (sccm) argon carrier gas flow, and 2000 standard cubic feet per minute (sccm) of hydrogen (H 2 ).
  • CVD chemical vapor deposition
  • results of the deposition are shown in FIG. 3 and FIG. 4 .
  • the data showed that the chemical vapor deposition (CVD) molybdenum oxytetrachloride (MoOCl 4 )/hydrogen (H 2 ) deposition process at 700° C. exhibited high deposition rate on the order of about 110 ⁇ /minute with the ampoule set at temperature of 70° C.
  • CVD chemical vapor deposition
  • MoOCl 4 molybdenum oxytetrachloride
  • H 2 hydrogen
  • FIG. 5 and FIG. 6 show a uniformly deposited molybdenum film with relatively large grain size.
  • FIG. 7 is a graph of molybdenum thickness, in ⁇ ngströms, as a function of deposition time, in seconds, for deposition of molybdenum by MoOCl 4 /H 2 process, ampoule temperature of 70° C., pressure of 60 torr, argon carrier gas flow rate of 50 sccm, and hydrogen gas flow rate of 2000 sccm, as carried out in respective runs at temperature of 550° C. (bottom curve), 600° C. (second curve from bottom at 600° C.), 650° C. (third curve from bottom at 600° C.), and 700° C. (top curve at 600° C.).
  • the chemical vapor deposition of molybdenum by MoOCl 4 /H 2 process, without a nucleation layer, showed temperature cut off at 550° C. Deposition rates are similar from 600° C. to 700° C. (stage temperatures).
  • FIG. 8 is a graph of film resistivity, in ⁇ cm, as a function of molybdenum thickness, in ⁇ ngströms, for molybdenum deposition conducted by MoOCl 4 /H 2 process at conditions of 70° C. ampoule temperature, 60 torr pressure, 50 sccm argon carrier gas flow rate, and 2000 sccm hydrogen gas flow rate, in which the process was conducted in separate runs at temperature of 600° C. (top curve), 650° C. (middle curve) and 700° C. (bottom curve).
  • the data show that the processes conducted at 600° C. and 650° C. showed slightly higher resistivity compared to the 700° C. process.
  • the film resistivity drops to approximately 11 ⁇ cm for a molybdenum film thickness in the order of 500 ⁇ .
  • FIG. 9 is a graph of deposition rate, in ⁇ ngströms/minute, as a function of run number, for molybdenum deposition using molybdenum oxytetrachloride (MoOCl 4 ) as the molybdenum precursor ( ⁇ ), and for molybdenum deposition using sublimed molybdenum pentachloride (MoCl5) as the molybdenum precursor ( ⁇ ).
  • MoOCl 4 molybdenum oxytetrachloride
  • MoCl5 sublimed molybdenum pentachloride
  • FIG. 10 is a graph of film resistivity of deposited molybdenum films, in ⁇ cm, as a function of molybdenum film thickness, in ⁇ ngströms, for a CVD deposition process conducted at 700° C., for molybdenum film deposited using unpurified MoCl 5 precursor ( ⁇ ), molybdenum film deposited using sublimed MoCl 5 precursor ( ⁇ ), and molybdenum film deposited using molybdenum oxytetrachloride (MoOCl 4 ) precursor ( ⁇ ).
  • the results show that MoOCl 4 precursor produced molybdenum films with higher resistivity values compared to films formed using unpurified MoCl 5 precursor and sublimed MoCl 5 precursor.
  • FIG. 11 is a graph of molybdenum film thickness, in ⁇ ngströms, as a function of diborane soak time, in seconds, for diborane exposure at 400° C., and 500° C. bulk molybdenum deposition using molybdenum oxytetrachloride (MoOCl 4 ) precursor ( ⁇ ), and for diborane exposure at 300° C., and 500° C. bulk molybdenum deposition using molybdenum oxytetrachloride (MoOCl 4 ) precursor ( ⁇ ).
  • MoOCl 4 molybdenum oxytetrachloride
  • FIGS. 12 and 13 are SEM micrographs of film depositions formed using 500° C. diborane nucleation, and 500° C. bulk molybdenum deposition using molybdenum oxytetrachloride (MoOCl 4 ) precursor in the presence of hydrogen.
  • FIGS. 14 and 15 are SEM images of deposited films in vias, showing step coverage for a 3 cycle nucleation and molybdenum bulk deposition with MoOCl 4 /H 2 .
  • the SEM images show that the MoOCl 4 /B2H 6 nucleation process (3 cycles) exhibited good step coverage on the via structure.
  • the associated process chemistry includes the following reactions: MoOCl 4 +3 H 2 ⁇ Mo+4 HCl+H 2 O; and 2 MoOCl 4 +B 2 H 6 ⁇ 2 Mo+2 BCl 3 +2 HCl+2H 2 O.
  • X-ray reflectivity (XRR) measurements on a representative molybdenum film formed in accordance with the present disclosure showed ⁇ 13.4 nm molybdenum with a density of approximately 8.33 g/cm 3 on a 147 ⁇ x-ray fluorescence (XRF) spectrometry-measured film.
  • XRR X-ray reflectivity
  • the data show that with 60 seconds or longer diborane pre-soak, molybdenum deposition is enabled at 550° C. stage temperature. As shown, film resistivity increases at longer diborane soak time periods.
  • pressure 60 torr
  • argon carrier gas flow rate 50 sccm
  • hydrogen gas flow rate 2000 sccm.
  • FIG. 18 is an SEM image of a molybdenum film deposited at 550° C.
  • the X RF thickness of the film was 1693.6 ⁇ , and the resistivity was determined as 21.6 ⁇ cm.
  • the SEM images showed approximately 40-70 nm grain size for molybdenum deposited at 550° C. with 90 seconds diborane pre-soak.
  • the cross-section SEM image shows approximately 7.7 nm boron layer underneath the deposited molybdenum.
  • the data show that with diborane nucleation, molybdenum deposition cutoff temperature is reduced to 500° C. with rapid deposition rate drop off between 500°
  • the data show that deposition rates for the CVD process without diborane nucleation drop-off rapidly below 600° C. with cutoff temperature at approximately 560° C.
  • the data show that the extracted activation energy for the MoOCl 4 /H 2 reaction is approximately 233 kJ/mole for the bulk molybdenum process deposition without nucleation, and approximately 251 kJ/mole for the bulk molybdenum deposition process with diborane nucleation.
  • the images show that the 520° C. MoOCl 4 /H 2 process with one cycle of diborane nucleation showed approximately 50% step coverage (
  • FIGS. 25, 26, and 27 show respective via structures deposited with molybdenum by diborane nucleation (soak) and 520° C.
  • FIGS. 28, 29, and 30 show respective via structures deposited with molybdenum by diborane nucleation (soak) and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, at bulk deposition temperature of 510° C., 520° C., and 530° C., respectively.
  • stage temperature 300° C.
  • argon carrier gas flow rate 250 sccm
  • hydrogen gas flow rate 0 sccm
  • FIGS. 31, 32, and 33 show respective via structures deposited with molybdenum by diborane nucleation (soak) and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, at diborane dose (soak) times of 45 seconds ( FIG. 31 ), 60 seconds ( FIG. 32 ), and 75 seconds ( FIG. 33 ), respectively.
  • the images show a boron layer clearly visible underneath the deposited molybdenum for the 60 second and 75 seconds diborane soak conditions.
  • FIGS. 34, 35, and 36 are SEM images of a via structure deposited with molybdenum by diborane nucleation (soak) and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, involving a pulsed CVD process conducted at 60 torr for 120 cycles, wherein FIG. 34 shows the via having an upper portion with a molybdenum film thickness of 510 ⁇ and a lower portion with a molybdenum film thickness of 375 ⁇ , FIG. 35 shows the via at an intermediate portion thereof with a molybdenum film thickness of 480 ⁇ , and FIG.
  • FIGS. 37 and 38 are SEM images of a via structure deposited with molybdenum by diborane nucleation (soak) and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, involving a pulsed CVD process conducted at 40 torr for 120 cycles, wherein FIG. 37 shows the via having an upper portion having a molybdenum film thickness of 320 ⁇ , and intermediate portion with a molybdenum film thickness of 520 ⁇ , and a lower portion with a molybdenum film thickness of 460 ⁇ , and FIG.
  • FIGS. 39 and 40 are SEM images of a via structure deposited with molybdenum by diborane nucleation (soak) and CVD bulk molybdenum deposition MoOCl 4 /H 2 process, involving a pulsed CVD process conducted at 40 torr for 240 cycles, wherein FIG. 39 shows the via having an intermediate portion with a molybdenum film thickness of 720 ⁇ , and a lower portion with a molybdenum film thickness of 460 ⁇ , and FIG.
  • the etch rate was not impacted by exposure to air.
  • the etch rate of thick boron film on a Mo substrate was much higher than on boron film on TiN substrate. This may be due to surface roughness of the thick boron films.
  • resistivity did not vary with thickness where the substrate was PVD Mo. As noted from previous results, resistivity was very dependent on stage temperature of TiN substrates without a boron nucleation layer.
  • CVD molybdenum films deposited using MoOCl 4 precursor showed good film resistivity of less than 15 ⁇ cm at thickness of 400 ⁇ , and SIMS analyses showed oxygen concentration in the bulk molybdenum film to be well below 1 atomic percent for films deposited using MoOCl 4 precursor.
  • the CVD MoOCl 4 /H 2 process exhibited deposition temperature cut off at approximate 560° C. without diborane nucleation, and cut off at approximately 500° C. with diborane nucleation.
  • Activation energy extracted from Arrhenius plot is approximately 223 kJ/mole for the process without nucleation, and approximately 251 kJ/mole for the process with diborane nucleation.
  • the CVD MoOCl 4 /H 2 process with diborane nucleation exhibited excellent step coverage on via structures, and the pulsed CVD process was demonstrated to achieve and even exceed 100% step coverage at film thickness of 500 ⁇ .

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