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CN118496107B - Organic small molecule inhibitor and application method thereof in thin film deposition - Google Patents

Organic small molecule inhibitor and application method thereof in thin film deposition Download PDF

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Publication number
CN118496107B
CN118496107B CN202410962766.1A CN202410962766A CN118496107B CN 118496107 B CN118496107 B CN 118496107B CN 202410962766 A CN202410962766 A CN 202410962766A CN 118496107 B CN118496107 B CN 118496107B
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precursor
inhibitor
reaction cavity
reaction
introducing
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CN118496107A (en
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程兰云
张学奇
扈静
李建恒
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Hefei Ande Keming Semiconductor Technology Co ltd
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Hefei Ande Keming Semiconductor Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C23C16/45534—Use of auxiliary reactants other than used for contributing to the composition of the main film, e.g. catalysts, activators or scavengers
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/01—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms
    • C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C211/14—Amines containing amino groups bound to at least two aminoalkyl groups, e.g. diethylenetriamines
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
    • C07C217/02—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C217/04—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
    • C07C217/06—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one etherified hydroxy group and one amino group bound to the carbon skeleton, which is not further substituted
    • C07C217/08—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one etherified hydroxy group and one amino group bound to the carbon skeleton, which is not further substituted the oxygen atom of the etherified hydroxy group being further bound to an acyclic carbon atom
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C229/02—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C229/04—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
    • C07C229/06—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton
    • C07C229/10—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton the nitrogen atom of the amino group being further bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
    • C07C229/16—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one amino and one carboxyl group bound to the carbon skeleton the nitrogen atom of the amino group being further bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings to carbon atoms of hydrocarbon radicals substituted by amino or carboxyl groups, e.g. ethylenediamine-tetra-acetic acid, iminodiacetic acids
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    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
    • C07F5/02—Boron compounds
    • C07F5/027—Organoboranes and organoborohydrides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02—Phosphorus compounds
    • C07F9/28—Phosphorus compounds with one or more P—C bonds
    • C07F9/50—Organo-phosphines
    • C07F9/5004—Acyclic saturated phosphines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention belongs to the technical field of semiconductors, and particularly discloses an organic small molecule inhibitor. The organic small molecule inhibitor provided by the invention has a certain steric hindrance and a multifunctional group effect, so that the inhibitor can cover more active sites at the top end of a substrate through the steric hindrance effect, and the bottom active sites are not inhibited; the invention also provides an application method of the organic small molecule inhibitor in film deposition, which proves that the organic small molecule inhibitor can be favorable for uniform deposition of the film from top to bottom and obviously improves the step coverage rate.

Description

Organic small molecule inhibitor and application method thereof in thin film deposition
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to an organic small molecule inhibitor and an application method thereof in film deposition.
Background
As human society moves into the artificial intelligence era, higher demands are being made on the storage density and performance of devices, and atomic layer deposition technology (Atomic Layer Deposition, ALD) plays a vital role in the semiconductor field due to its excellent film-coating conformality and self-limiting properties. However, in high aspect ratio 3D nanostructures, such as holes or trenches, ALD deposition tends to form seams or voids during top-down gap filling, resulting in reduced device performance, electrical or thermal conductivity, and mechanical properties. The inhibitor is generally introduced in the deposition process to inhibit top deposition, and bottom deposition is not affected or is inhibited very weakly, so that the uniformity of filling the deposited film from top to bottom is enhanced, the step coverage is improved, and joints or gaps are eliminated. The existing inhibitor not only inhibits the deposition at the top of the groove, but also has a certain inhibition effect on the deposition at the bottom of the groove, so that certain non-uniformity exists in filling, and the step coverage rate improving effect is poor. For example, patent US20220119939A1 proposes small organic molecule inhibitors, such as Triethylamine (TEA), tetrahydrofuran (THF), and ethylene glycol dimethyl ether (DME), in which the inhibitor molecules are gently physically adsorbed on a high aspect ratio substrate, compete with the precursor molecules for active sites on the substrate surface, and inhibit excessive adsorption of the precursor on the top of the substrate, thereby improving step coverage, but these inhibitors often inhibit growth of thin films on the bottom of the substrate, resulting in poor effect or poor process stability, so there is still a need to find more suitable inhibitors.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide the small organic molecule inhibitor which has a certain steric hindrance and contains multiple functional groups, and compared with the prior inhibitor molecules, the inhibitor can cover more active sites at the top end of a substrate through steric hindrance effect and prevent the active sites at the bottom from being inhibited; the inhibitor contains a plurality of functional groups, so that the probability of bonding with the active site of the substrate is improved, the adsorption of a precursor on the top of the substrate is effectively reduced, the uniform deposition of a film from top to bottom is facilitated, and the step coverage rate is remarkably improved.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
An embodiment of the first aspect of the present invention provides an organic small molecule inhibitor, wherein the chemical structure of the organic small molecule inhibitor is shown as formula (i):
（Ⅰ）；
wherein M is N, P or B;
x1, X2 and X3 are integers greater than or equal to 1;
r 1、R2、R3 is any one of H, C-C10 aliphatic or cycloaliphatic substituent;
R 4、R5、R6 is present or absent;
y 1、Y2、Y3 is any one of O, N, S, -O-c=o, wherein:
When Y 1、Y2、Y3 is O, S, -O-c=o, or-c=o, then R 4、R5、R6 is absent;
When Y 1、Y2、Y3 is N, then R 4、R5、R6 is all present;
when Y 1 is N and Y 2、Y3 is O, S, -O-c=o or-c=o, then R 4 is present and R 5、R6 is absent;
When Y 2 is N and Y 1、Y3 is O, S, -O-c=o or-c=o, then R 5 is present and R 4、R6 is absent;
When Y 3 is N and Y 1、Y2 is O, S, -O-c=o or-c=o, then R 6 is present and R 4、R5 is absent;
When Y 1、Y2 is N and Y 3 is O, S, -O-c=o or-c=o, then R 4、R5 is present and R 6 is absent;
When Y 1、Y3 is N and Y 2 is O, S, -O-c=o or-c=o, then R 4、R6 is present and R 5 is absent;
When Y 2、Y3 is N and Y 1 is O, S, -O-c=o or-c=o, then R 5、R6 is present and R 4 is absent;
And, when R 4、R5、R6 is present, R 4、R5、R6 is each independently any one of H, C C10 aliphatic or cycloaliphatic substituents.
Further, the C1-C10 aliphatic or cycloaliphatic substituent is any one of alkyl, cycloalkyl, alkenyl, cycloalkenyl, alkynyl and cycloalkynyl.
Further, each of X1, X2 and X3 is an integer of 1 to 10, preferably an integer of 1 to 5.
Preferably, each of X1, X2 and X3 is an integer of 1 to 3.
In one embodiment, the M is N and the enumerated inhibitors include, but are not limited to:
Preferably, when M is N, Y 1、Y2、Y3 is O, S, -O-c=o, or-c=o.
In a preferred embodiment, when M is B, inhibitors that may be cited include, but are not limited to:
in a preferred embodiment, when M is P, inhibitors that may be cited include, but are not limited to:
Preferably, R 1 and R 4 are not simultaneously H, R 2 and R 5 are not simultaneously H, and R 3 and R 6 are not simultaneously H.
Preferably, R 1、R2、R3、R4、R5、R6 is not simultaneously H.
Further, the R 1、R2、R3、R4、R5、R6 is independently selected from C1-C10 alkyl substituents, preferably C1-C4 alkyl substituents.
In a second aspect, the invention provides a method for applying an organic small molecule inhibitor to film deposition, comprising the following steps: the inhibitor is attached to the substrate, then the precursor is introduced, and deposition is performed on the substrate.
Further, the substrate is a high aspect ratio substrate, and the aspect ratio is more than or equal to 20, preferably more than or equal to 40.
In one embodiment, the aspect ratio of the substrate is 40.
Further, the width of the opening of the high aspect ratio substrate is less than or equal to 50nm.
Further, the width of the opening of the high aspect ratio substrate is less than or equal to 30nm.
Further, the specific process of attaching the inhibitor to the substrate is: the inhibitor is heated to gas and then flows into the deposition reaction chamber through a pipeline, the heating temperature of the inhibitor is more than 30 ℃, and the heating temperature of the pipeline is more than 50 ℃.
Further, the inhibitor is attached to the substrate, and then inert gas is introduced into the reaction chamber to purge the excess inhibitor.
Further, the precursor includes, but is not limited to, at least one of a silicon-based, titanium-based, vanadium-based, tungsten-based, aluminum-based, iron-based, ruthenium-based precursor; the silicon is meant to be a silicon precursor, a germanium precursor, and a tin precursor; the titanium is a titanium precursor, a zirconium precursor and a hafnium precursor; the vanadium is a vanadium precursor, a niobium precursor, and a tantalum precursor; the tungsten system means a molybdenum precursor and a tungsten precursor; the iron system means an iron precursor, a cobalt precursor and a nickel precursor; the aluminum is boron precursor, aluminum precursor, gallium precursor, indium precursor.
Further, alternative silicon precursors include, but are not limited to, at least one of tetra (dimethylamino) silane, tetra (diethylamino) silane, diisopropylaminosilane, bis (t-butylamino) silane, bis (diethylamino) silane, bis (diisopropylamino) silane, tris (diisopropylamino) silane, dichlorosilane, silane, disilane, tetraethylorthosilicate; the germanium precursor includes, but is not limited to, at least one of tetra (dimethylamino) germanium, N' -diisopropyltert-pentylidene germanium, germane, dichlorogermane, trichlorogermane; tin precursors include, but are not limited to, at least one of tin tetrachloride, tetramethyltin, tetra (dimethylamino) tin.
Further, alternative titanium precursors include, but are not limited to, at least one of tris (dimethylamino) (cyclopentadienyl) titanium, tetrakis (dimethylamino) titanium, tris (dimethylamino) (methylcyclopentadienyl) titanium, titanium tetrachloride, tetrakis (ethoxy) titanium, tetrakis (isobutoxy) titanium, tris (methoxy) (cyclopentadienyl) titanium, trimethoxy (pentamethylcyclopentadienyl) titanium; zirconium precursors include, but are not limited to, at least one of tris (dimethylamino) (cyclopentadienyl) zirconium, tris (dimethylamino) (methylcyclopentadienyl) zirconium, tetrakis (dimethylamino) zirconium, tetrakis (diethylamino) zirconium, tetrakis (methylethylamino) zirconium, tris (methylethylamino) (cyclopentadienyl) zirconium; hafnium precursors include, but are not limited to, at least one of tris (dimethylamino) (cyclopentadienyl) hafnium, tris (dimethylamino) (methylcyclopentadienyl) hafnium, tris (diethylamino) (ethylcyclopentadienyl) hafnium, tetrakis (dimethylamino) hafnium, tetrakis (methylamino) hafnium.
Further, the optional vanadium precursor includes, but is not limited to, at least one of vanadium tetrachloride, vanadium tetra (dimethylamino) tetrakis (dimethylamino) vanadium, vanadium tetra (diethylamino) tetrakis (methylethylamino) vanadium, (tris- (2, 4-pentanedionate) vanadium, bis (cyclopentadienyl) vanadium (II), cyclopentadienyl vanadium tetra-carbonyl, the niobium precursor includes, but is not limited to, at least one of (tertiary Ding Yaan yl) tris (diethylamino) niobium, (tertiary Ding Yaan yl) bis (dimethylamino) (cyclopentadienyl) niobium, and the tantalum precursor includes, but is not limited to, at least one of penta (diethylamino) tantalum, penta (methylethylamino) tantalum, and (tertiary Ding Yaan yl) tris (diethylamino) tantalum.
Further, alternative molybdenum precursors include, but are not limited to, at least one of molybdenum hexacarbonyl, molybdenum dichloride, molybdenum pentachloride, molybdenum hexafluoride, bis (tertiary Ding Yaan yl) bis (dimethylamino) molybdenum; tungsten precursors include, but are not limited to, at least one of bis (tertiary Ding Yaan yl) bis (dimethylamino) tungsten, tungsten hexafluoride, bis (tertiary Ding Yaan yl) bis (diethylamino) tungsten, bis (tertiary Ding Yaan yl) bis (methylamino) tungsten.
Further, alternative iron precursors include, but are not limited to, at least one of bis (cyclopentadienyl) iron, pentacarbonyl iron; cobalt precursors include, but are not limited to, at least one of (3, 3-dimethyl-1-butyne) hexacarbonyl cobalt, octacarbonyl cobalt, bis (N, N' -di-isopropyl acetamido) cobalt; the nickel precursor includes, but is not limited to, at least one of nickel acetylacetonate, bis (cyclopentadienyl) nickel, bis (dimethylamino-2-methyl-2-butoxy) nickel.
Further, alternative ruthenium precursors include, but are not limited to, at least one of bis (cyclopentadienyl) ruthenium, bis (ethylcyclopentadienyl) ruthenium, tris (2, 6-tetramethyl-3, 5-heptanedionate) ruthenium.
Further, optional boron precursors include, but are not limited to, at least one of borane, diborane, trimethylboron; aluminum precursors include, but are not limited to, at least one of trimethylaluminum, triethylaluminum, dimethylethylaminoalane, trimethylaminoalane, N-methylpyrrolidine, triisobutylaluminum, dimethylaluminum hydride; gallium precursors include, but are not limited to, at least one of gallium chloride, trimethylgallium, tris (dimethylamino) gallium; the indium precursor includes, but is not limited to, at least one of trimethylindium, cyclopentadienyl indium.
Further, the type of thin film deposited includes any one or more of an oxide film, a nitride film, an oxynitride film, a metal film, or a group thereof.
In one embodiment, the method of using the small organic molecule inhibitor in thin film deposition comprises the steps of:
S1: placing a high aspect ratio substrate into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 100-450 ℃, and vacuumizing the reaction cavity to 0-30Pa;
s2: the inhibitor is arranged in a source bottle, the source bottle is communicated with a reaction cavity through a first pipeline, the source bottle is heated to be more than 30 ℃, the first pipeline is heated to be more than 50 ℃, inert gas is used as carrier gas, and the inhibitor is introduced into the reaction cavity in a pulse mode;
s3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity for 2-60s;
s4: introducing the precursor into the reaction cavity
Filling a precursor into a precursor source bottle, communicating the precursor source bottle with a reaction cavity through a second pipeline, heating the precursor source bottle and the second pipeline, and introducing the precursor into the reaction cavity in a pulse form by using inert gas as carrier gas;
S5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 2-60s;
S6: introducing reaction gas into the reaction cavity to generate a corresponding film;
S7: introducing inert gas into the reaction cavity for purging excessive reaction gas and reaction byproducts for 2-60s;
s8: repeating the steps S2-S7 until the thin film is deposited to a preset thickness.
Further, the heating temperature of the source bottle in the step S2 is 30-100 ℃, and the heating temperature of the first pipeline is 50-150 ℃.
Further, the heating temperature of the precursor source bottle in the step S4 is 30-150 ℃, preferably 30-120 ℃; the heating temperature of the second pipeline is 50-180 ℃, preferably 50-160 ℃.
In a preferred embodiment, the precursor is any one or more of diisopropylaminosilane, bis (t-butylamino) silane, tris (dimethylamino) cyclopentadienyl hafnium, tris (dimethylamino) cyclopentadienyl zirconium, tetrakis (methylethylamino) hafnium, tetrakis (methylethylamino) zirconium, trimethoxy (pentamethylcyclopentadienyl) titanium, (t-Ding Yaan yl) bis (dimethylamino) (cyclopentadienyl) niobium, (t-Ding Yaan yl) tris (diethylamino) niobium, mixed in any ratio.
Further, the reactant gases include, but are not limited to, any of O 3、O2、H2O、H2O2、O2 plasma, formic acid, acetic anhydride, NH 3、NF3 plasma, NO 2, organic amines, hydrogen.
Further, the inert gases in steps S2, S3, S4, S5, S7 are any one of N 2, ar, he, kr.
Further, the preset thickness of the film is 2-20nm.
Compared with the prior art, the invention has the beneficial effects that:
1. The invention provides an organic small molecule inhibitor which has a certain steric hindrance and a multifunctional group effect, and compared with the prior inhibitor molecule, the inhibitor can cover more active sites at the top end of a substrate through the steric hindrance effect and prevent the active sites at the bottom from being inhibited; the inhibitor contains a plurality of functional groups, so that the probability of bonding with the active site of the substrate is improved, the adsorption of a precursor on the top of the substrate is effectively reduced, the uniform deposition of a film from top to bottom is facilitated, and the step coverage rate is remarkably improved.
2. In the structural formula of the organic small molecule inhibitor, X1, X2 and X3 are integers more than or equal to 1 and can be unequal, so that at least one-CH 2 -on a chain connected with a central atom is limited, the steric hindrance of the structure is regulated, and the inhibiting effect can be better exerted.
3. The organic small molecule inhibitor provided by the invention has the advantages that the central atom M can be N, P or B, Y 1、Y2、Y3 is any one of O, N, S, -O-C=O and-C=O, and the central atom M, Y 1、Y2、Y3 of the structure can have an affinity effect with a deposition matrix, so that the adhesion of the inhibitor on the matrix is ensured.
4. The affinity function and the proper steric hindrance function expressed by the structure are combined to play a role, so that the organic small molecule inhibitor provided by the invention fully plays a role, and in film deposition, the precursor deposition at the top end of a groove is inhibited, the precursor deposition at the bottom of the groove is not influenced as little as possible, the film is promoted to be uniformly deposited from top to bottom, and the groove filling of a matrix is further ensured.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a TEM image and EDS image of a deposited film provided in example 1 of the present invention; in FIG. 1, (a) is a slit image of the top deposited film of example 1, scale 100nm; (b) For the slit image of the bottom deposited film of example 1, the scale is 100nm; (c) Elemental distribution of Hf in the film (EDS plot), scale 200nm; (d) For a cross-sectional image of the top deposited film of example 1, the scale is 20nm; (e) For a cross-sectional image of the bottom deposited film of example 1, the scale is 20nm.
FIG. 2 is a TEM image and EDS image of a deposited film provided by example 2 of the present invention; in FIG. 2, (a) is a slit image of the top deposited film of example 2, scale 100nm; (b) For the slit image of the bottom deposited film of example 2, the scale is 100nm; (c) Elemental distribution of Hf in the film (EDS plot), scale 200nm; (d) A cross-sectional image of the top deposited film of example 2, scale 20nm; (e) For a cross-sectional image of the bottom deposited film of example 2, the scale is 20nm.
FIG. 3 is a TEM image and EDS image of a deposited film provided by comparative example 1 of the present invention; in FIG. 3, (a) is a slit image of the top deposited film of comparative example 1, scale 100nm; (b) Longitudinal cut image of the bottom deposited film of comparative example 1, scale 100nm; (c) Elemental distribution of Hf in the film (EDS plot), scale 200nm; (d) For a cross-sectional image of the top deposited film of comparative example 1, the scale is 50nm; (e) For a cross-sectional image of the bottom deposited film of comparative example 1, the scale is 50nm.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
An embodiment of the first aspect of the present invention provides an organic small molecule inhibitor, which is characterized in that the chemical structure of the organic small molecule inhibitor is shown in formula (i):
（Ⅰ）；
wherein M is N, P or B;
X1, X2 and X3 are integers greater than or equal to 1, and X1, X2 and X3 can be the same or different;
R 1、R2、R3 is any one of H, C-C10 aliphatic or cycloaliphatic substituent, and R 1、R2、R3 can be the same or different;
R 4、R5、R6 is present or absent;
Y 1、Y2、Y3 is any one of O, N, S, -O-c=o, and Y 1、Y2、Y3 may be the same or different;
Wherein, for the presence or absence of R 4、R5、R6, the specific analysis is the following:
Case 1: when Y 1、Y2、Y3 is O, S, -O-c=o, or-c=o, then none of R 4、R5、R6 is present;
case 2: when Y 1、Y2、Y3 is N, then R 4、R5、R6 is all present;
Case 3: when Y 1 is N and Y 2、Y3 is O, S, -O-c=o or-c=o, then R 4 is present and none of R 5、R6 is present;
Case 4: when Y 2 is N and Y 1、Y3 is O, S, -O-c=o or-c=o, then R 5 is present and none of R 4、R6 is present;
case 5: when Y 3 is N and Y 1、Y2 is O, S, -O-c=o or-c=o, then R 6 is present and none of R 4、R5 is present;
case 6: when Y 1、Y2 is N and Y 3 is O, S, -O-c=o or-c=o, then R 4、R5 is present and R 6 is absent;
Case 7: when Y 1、Y3 is N and Y 2 is O, S, -O-c=o or-c=o, then R 4、R6 is present and R 5 is absent;
Case 8: when Y 2、Y3 is N and Y 1 is O, S, -O-c=o or-c=o, then R 5、R6 is present and R 4 is absent;
And, when R 4、R5、R6 is present, R 4、R5、R6 are each independently any one of H, C1-C10 aliphatic or cycloaliphatic substituents; wherein the C1-C10 aliphatic or cycloaliphatic substituent is any one of alkyl, cycloalkyl, alkenyl, cycloalkenyl, alkynyl and cycloalkynyl.
Embodiments of the second aspect of the present invention provide a method for applying an organic small molecule inhibitor in thin film deposition, the method comprising the steps of:
S1: placing a high aspect ratio substrate into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 100-450 ℃, and vacuumizing the reaction cavity to 0-30Pa;
S2: placing the inhibitor in a first stainless steel source bottle, communicating the first stainless steel source bottle with the reaction cavity through a first pipeline, setting the heating temperature of the first stainless steel source bottle to be 30-100 ℃, setting the heating temperature of the first pipeline to be 50-150 ℃, and introducing the inhibitor into the reaction cavity in a pulse form by using inert gas as carrier gas;
s3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity for 2-60s;
s4: introducing the precursor into the reaction cavity
Filling a precursor into a second stainless steel source bottle, communicating the second stainless steel source bottle with the reaction cavity through a second pipeline, heating the second stainless steel source bottle to 30-150 ℃, heating the second pipeline to 50-180 ℃, and introducing the precursor into the reaction cavity in a pulse form by using inert gas as carrier gas;
In the step S4, the precursor is a silicon-based precursor and/or a metal-based precursor; specifically, the precursor is any one or more of Diisopropylaminosilane (DIPAS), bis (tertiary butylamino) silane (BTBAS), tris (dimethylamino) cyclopentadienyl hafnium ([ CpHf (NMe 2)3 ]), tris (dimethylamino) cyclopentadienyl zirconium ([ CpZr (NMe 2)3 ])), tetrakis (methylethylamino) hafnium (TEMAHf), tetrakis (methylethylamino) zirconium (TEMAZr), trimethoxy (pentamethylcyclopentadienyl) titanium ([ cp×ti (OMe) 3 ], abbreviated to Star-Ti), (tertiary Ding Yaan yl) bis (dimethylamino) (cyclopentadienyl) niobium ([ CpNb (tBuN) (NMe 2)2 ])), (tertiary Ding Yaan yl) tris (diethylamino) niobium (TBTDEN) according to any proportion;
S5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 2-60s;
S6: introducing reaction gas into the reaction cavity to generate a corresponding film;
S7: introducing inert gas into the reaction cavity for purging excessive reaction gas and reaction byproducts for 2-60s;
in the steps S2, S3, S4, S5 and S7, the inert gas is any one of N 2, ar, he and Kr;
s8: repeating the steps S2-S7 until the film is deposited to a preset thickness, wherein the preset thickness is 2-20nm.
The following examples are given as examples, and the raw materials in the following examples are all commercially available unless otherwise specified.
Example 1
The embodiment provides an organic small molecule inhibitor, which is tris [2- (dimethylamino) ethyl ] amine, and has the following chemical structure:
。
The embodiment also provides an application method of the small organic molecule inhibitor in film deposition, which specifically comprises the following steps:
S1: placing a substrate with an aspect ratio of 40 (the opening width is 20 nm) into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 350 ℃, and vacuumizing the reaction cavity to 15Pa;
s2: placing an inhibitor, namely tris [2- (dimethylamino) ethyl ] amine, in a first stainless steel source bottle, communicating the first stainless steel source bottle with a reaction cavity through a first pipeline, setting the heating temperature of the first stainless steel source bottle to be 45 ℃, pulsing for 0.5s, setting the heating temperature of the first pipeline to be 100 ℃, using inert gas as carrier gas, and introducing the inhibitor into the reaction cavity in a pulse mode;
S3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity, wherein the purging time is 15s;
s4: introducing a precursor, namely tris (dimethylamino) cyclopentadienyl hafnium CpHf (NMe 2)3), into a reaction cavity, wherein the precursor is filled into a second stainless steel source bottle, the second stainless steel source bottle is communicated with the reaction cavity through a second pipeline, the heating temperature of the second stainless steel source bottle is 80 ℃, the pulse 2s is carried out, the heating temperature of the second pipeline is 150 ℃, inert gas is used as carrier gas, and the precursor is introduced into the reaction cavity in a pulse mode;
s5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 20s;
s6: introducing reaction gas into the reaction cavity, wherein the reaction gas adopts O 3 to generate a hafnium oxide film;
S7: introducing inert gas into the reaction cavity for purging excessive oxygen sources and reaction byproducts for 15s;
in the steps S2, S3, S4, S5 and S7, the inert gas is Ar;
S8: steps S2-S7 to 100cyc (i.e. steps S2-S7 are sequentially cycled 100 times) are repeated until the film is deposited to a predetermined thickness of about 6 nm.
Example 2
The embodiment provides an organic small molecule inhibitor which is 1-methoxy-N, N' -bis (methoxymethyl) methylamine, and has the following chemical structure:
。
The embodiment also provides an application method of the small organic molecule inhibitor in film deposition, which specifically comprises the following steps:
S1: placing a substrate with an aspect ratio of 40 (the opening width is 20 nm) into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 350 ℃, and vacuumizing the reaction cavity to 15Pa;
S2: placing an inhibitor, namely 1-methoxy-N, N' -bis (methoxymethyl) methylamine, in a first stainless steel source bottle, communicating the first stainless steel source bottle with a reaction cavity through a first pipeline, setting the heating temperature of the first stainless steel source bottle to be 35 ℃, pulsing for 0.2s, heating the first pipeline to be 100 ℃, using inert gas as carrier gas, and introducing the inhibitor into the reaction cavity in a pulse mode;
S3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity, wherein the purging time is 15s;
s4: introducing a precursor, namely tris (dimethylamino) cyclopentadienyl hafnium CpHf (NMe 2)3), into a reaction cavity, wherein the precursor is filled into a second stainless steel source bottle, the second stainless steel source bottle is communicated with the reaction cavity through a second pipeline, the heating temperature of the second stainless steel source bottle is 80 ℃, the pulse 2s is carried out, the heating temperature of the second pipeline is 150 ℃, inert gas is used as carrier gas, and the precursor is introduced into the reaction cavity in a pulse mode;
s5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 20s;
s6: introducing reaction gas into the reaction cavity, wherein the reaction gas adopts O 3 to generate a hafnium oxide film;
S7: introducing inert gas into the reaction cavity for purging excessive oxygen sources and reaction byproducts for 15s;
in the steps S2, S3, S4, S5 and S7, the inert gas is Ar;
S8: steps S2-S7 to 100cyc (i.e. steps S2-S7 are sequentially cycled 100 times) are repeated until the film is deposited to a predetermined thickness of about 6 nm.
Example 3
The embodiment provides an organic small molecule inhibitor which is bis (diethylaminomethyl) methoxymethyl amine and has the following chemical structure:
。
The embodiment also provides an application method of the small organic molecule inhibitor in film deposition, which specifically comprises the following steps:
s1: placing a substrate with an aspect ratio of 40 (the opening width is 20 nm) into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 300 ℃, and vacuumizing the reaction cavity to 15Pa;
S2: the inhibitor is arranged in a stainless steel source bottle I, the stainless steel source bottle I is communicated with a reaction cavity through a pipeline I, the heating temperature of the stainless steel source bottle I is set to be 45 ℃, the heating temperature of the pipeline I is set to be 130 ℃ in a pulse mode, inert gas is used as carrier gas, and the inhibitor is introduced into the reaction cavity in a pulse mode;
S3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity, wherein the purging time is 15s;
S4: filling a precursor, namely tris (dimethylamino) cyclopentadienyl zirconium CpZr (NMe 2)3), into a second stainless steel source bottle, wherein the second stainless steel source bottle is communicated with the reaction cavity through a pipeline II, the heating temperature of the second stainless steel source bottle is 90 ℃, the pulse 1s, the heating temperature of the pipeline II is 150 ℃, inert gas is used as carrier gas, and the precursor is filled into the reaction cavity in a pulse mode;
s5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 20s;
S6: introducing reaction gas into the reaction cavity, wherein the reaction gas adopts O 3 to generate a zirconia film;
S7: introducing inert gas into the reaction cavity for purging excessive oxygen sources and reaction byproducts for 15s;
in the steps S2, S3, S4, S5 and S7, the inert gas is Ar;
S8: steps S2-S7 to 100cyc (i.e. steps S2-S7 are sequentially cycled 100 times) are repeated until the film is deposited to a predetermined thickness of about 6 nm.
Example 4
The embodiment provides an organic small molecule inhibitor, which is bis (ethoxyethyl) (diethylamino) ethylamine, and has the following chemical structure:
。
The embodiment also provides an application method of the small organic molecule inhibitor in film deposition, which specifically comprises the following steps:
s1: placing a substrate with an aspect ratio of 40 (the opening width is 20 nm) into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 300 ℃, and vacuumizing the reaction cavity to 15Pa;
s2: the inhibitor is arranged in a stainless steel source bottle I, the stainless steel source bottle I is communicated with a reaction cavity through a pipeline I, the heating temperature of the stainless steel source bottle I is set to be 50 ℃, the heating temperature of the pipeline I is set to be 130 ℃ in a pulse mode, inert gas is used as carrier gas, and the inhibitor is introduced into the reaction cavity in a pulse mode;
S3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity, wherein the purging time is 15s;
S4: filling a precursor, namely tris (dimethylamino) cyclopentadienyl zirconium CpZr (NMe 2)3), into a second stainless steel source bottle, wherein the second stainless steel source bottle is communicated with the reaction cavity through a pipeline II, the heating temperature of the second stainless steel source bottle is 90 ℃, the pulse 1s, the heating temperature of the pipeline II is 150 ℃, inert gas is used as carrier gas, and the precursor is filled into the reaction cavity in a pulse mode;
s5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 20s;
S6: introducing reaction gas into the reaction cavity, wherein the reaction gas adopts O 3 to generate a zirconia film;
S7: introducing inert gas into the reaction cavity for purging excessive oxygen sources and reaction byproducts, wherein the purging time is 15S;
in the steps S2, S3, S4, S5 and S7, the inert gas is Ar;
S8: steps S2-S7 to 100cyc (i.e. steps S2-S7 are sequentially cycled 100 times) are repeated until the film is deposited to a predetermined thickness of about 6 nm.
Comparative example 1
No inhibitor was used in this comparative example.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed with reference to the application method of the small organic molecule inhibitor in thin film deposition provided in example 1, and compared with example 1, no inhibitor is added in this comparative example, and the rest of the operation process and operation method are the same as in example 1.
Comparative example 2
No inhibitor was used in this comparative example.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed with reference to the application method of the small organic molecule inhibitor in thin film deposition provided in example 3, and compared with example 3, no inhibitor is added in this comparative example, and the rest of the operation process and operation method are the same as in example 3.
Comparative example 3
The inhibitor used in this comparative example was triethylamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed by referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 1, and compared with example 1, the inhibitor in this comparative example is replaced by triethylamine with tris [2- (dimethylamino) ethyl ] amine, and the rest of the operation procedures and operation methods are the same as in example 1.
Comparative example 4
The inhibitor used in this comparative example was methoxyamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed by referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 1, compared with example 1, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine to methoxyamine, and the rest of the operation procedures and operation methods are the same as in example 1.
Comparative example 5
The inhibitor used in this comparative example was N-ethyl-N- (methoxymethyl) ethylamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed by referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 1, and compared with example 1, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine with N-ethyl-N- (methoxymethyl) ethylamine, and the rest of the operation procedures and the operation methods are the same as in example 1.
Comparative example 6
The inhibitor used in this comparative example was bis (2-methoxyethyl) amine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed by referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 1, and compared with example 1, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine for bis (2-methoxyethyl) amine, and the rest of the operation procedures and operation methods are the same as in example 1.
Comparative example 7
The inhibitor used in this comparative example was N, N-bis (methoxymethyl) ethylamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 3, and compared with example 3, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine with N, N-bis (methoxymethyl) ethylamine, and the rest of the operation procedures and operation methods are the same as in example 3.
Comparative example 8
The inhibitor used in this comparative example was bis [2- (dimethylamino) ethyl ] ethylamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed by referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 3, and compared with example 3, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine to bis [2- (dimethylamino) ethyl ] ethylamine, and the rest of the operation procedures and operation methods are the same as in example 3.
Comparative example 9
The inhibitor used in this comparative example was [2- (dimethylamino) ethyl ] diethylamine.
The application method of the inhibitor in thin film deposition provided in this comparative example is performed referring to the application method of the small organic molecule inhibitor in thin film deposition provided in example 3, and compared with example 3, the inhibitor in this comparative example is replaced by tris [2- (dimethylamino) ethyl ] amine to [2- (dimethylamino) ethyl ] diethylamine, and the rest of the operation procedures and operation methods are the same as in example 3.
Experimental example
The film thicknesses in examples 1 to 4 and comparative examples 1 to 9 were measured, and step coverage, and growth rate per cycle (GPC) were calculated, and the experimental data obtained are shown in Table 1 below.
Referring to fig. 1-3, the experimental examples also provide TEM images and EDS images of the films of example 1, example 2 and comparative example 1, respectively, as shown in fig. 1, fig. 2 and fig. 3, from which it can be seen that in example 1-2, the film deposition from top to bottom is better due to the small organic molecule inhibitor, tris [2- (dimethylamino) ethyl ] amine and 1-methoxy-N, N' -bis (methoxymethyl) methylamine, respectively, whereas in comparative example 1, the film deposition is non-uniform due to the absence of the inhibitor.
TABLE 1
As can be seen from the data in table 1, in examples 1 to 4, the use of the small organic molecule inhibitors having multiple tentacles in thin film deposition significantly improved step coverage compared to comparative examples 1 to 9.
The invention provides an organic small molecule inhibitor which has a certain steric hindrance and a multifunctional group effect, and compared with the prior inhibitor molecule, the inhibitor can cover more active sites at the top end of a substrate through the steric hindrance effect and prevent the active sites at the bottom from being inhibited; the inhibitor contains a plurality of functional groups, so that the probability of bonding with the active site of the substrate is improved, the adsorption of a precursor on the top of the substrate is effectively reduced, the uniform deposition of a film from top to bottom is facilitated, and the step coverage rate is remarkably improved.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.

Claims (4)

1. The organic small molecule inhibitor is characterized in that the chemical structural formula of the organic small molecule inhibitor is shown as a formula (III) or (IV):
（Ⅲ）；
（IV）。
2. a method of using the small organic molecule inhibitor of claim 1 in thin film deposition, comprising the steps of: attaching an inhibitor to a substrate, then introducing a precursor, and depositing on the substrate;
Wherein the substrate is a high aspect ratio substrate;
The specific process of attaching the inhibitor to the substrate is: the inhibitor is heated to gas and then flows into the deposition reaction chamber through the pipeline, and the heating temperature of the inhibitor is more than 30 ℃.
3. The method of using a small organic molecule inhibitor according to claim 2 for thin film deposition, comprising the steps of:
S1: placing a high aspect ratio substrate into an atomic layer deposition device, wherein the heating temperature in a reaction cavity of the atomic layer deposition device is 100-450 ℃, and vacuumizing the reaction cavity to 0-30Pa;
s2: the inhibitor is arranged in a source bottle, the source bottle is communicated with a reaction cavity through a first pipeline, the source bottle is heated to be more than 30 ℃, the first pipeline is heated to be more than 50 ℃, inert gas is used as carrier gas, and the inhibitor is introduced into the reaction cavity in a pulse mode;
s3: introducing inert gas into the reaction cavity for purging excessive inhibitor in the reaction cavity for 2-60s;
s4: introducing the precursor into the reaction cavity
Filling a precursor into a precursor source bottle, communicating the precursor source bottle with a reaction cavity through a second pipeline, heating the precursor source bottle and the second pipeline, and introducing the precursor into the reaction cavity in a pulse form by using inert gas as carrier gas;
S5: introducing inert gas into the reaction cavity for purging excessive precursor and reaction byproducts for 2-60s;
S6: introducing reaction gas into the reaction cavity to generate a corresponding film;
S7: introducing inert gas into the reaction cavity for purging excessive reaction gas and reaction byproducts for 2-60s;
s8: repeating the steps S2-S7 until the thin film is deposited to a preset thickness.
4. The method of claim 2, wherein the precursor comprises at least one of a silicon-based, titanium-based, vanadium-based, tungsten-based, aluminum-based, iron-based, ruthenium-based precursor; the silicon is meant to be a silicon precursor, a germanium precursor, and a tin precursor; the titanium is a titanium precursor, a zirconium precursor and a hafnium precursor; the vanadium is a vanadium precursor, a niobium precursor, and a tantalum precursor; the tungsten system means a molybdenum precursor and a tungsten precursor; the iron system means an iron precursor, a cobalt precursor and a nickel precursor; the aluminum is boron precursor, aluminum precursor, gallium precursor, indium precursor.
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