CN103210479A - Process for lowering adhesion layer thickness and improving damage resistance for thin ultra low-k dielectric film - Google Patents

Process for lowering adhesion layer thickness and improving damage resistance for thin ultra low-k dielectric film Download PDF

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CN103210479A
CN103210479A CN2011800538803A CN201180053880A CN103210479A CN 103210479 A CN103210479 A CN 103210479A CN 2011800538803 A CN2011800538803 A CN 2011800538803A CN 201180053880 A CN201180053880 A CN 201180053880A CN 103210479 A CN103210479 A CN 103210479A
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transition zone
pore
gas
foaming agent
flow velocity
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M·查布拉
K·S·伊姆
A·T·迪莫斯
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Applied Materials Inc
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Abstract

An improved method for depositing an ultra low dielectric constant film stack is provided. Embodiments of the invention minimize k (dielectric constant) impact from initial stages of depositing the ultra low dielectric constant film stack by reducing a thickness of an oxide adhesion layer in the ultra low dielectric film stack, thereby lowering the thickness non-uniformity of the film stack to less than 2%. The improved process deposits the oxide adhesion layer and the bulk layer in the ultra low dielectric film stack at lower deposition rate and lower plasma density in combination with higher total flow rate, resulting in better packing/ordering of the co-deposited species during film deposition which causes higher mechanical strength and lower porosity.

Description

In order to the adhesion layer thickness that reduces ultralow k dielectric film and the technology that improves anti-destructive
Background of invention
Background technology
The initial introduction since the semiconductor device before many decades, the geometry of this type of device dwindles dimensionally significantly.Afterwards, integrated circuit is followed the rule (being commonly referred to Moore's Law) that size every two years reduces by half substantially, and the number of devices that described rule is represented to be contained on the chip every two years can double.Manufacturing works now produce routinely have 65nm with in addition be the device of 45nm characteristic size, and the factory in future will produce the device with littler geometry soon.
In copper dual-damascene interconnection process technology, owing to must dwindle between the capacitive couplings between the adjacent wires further dwindling the device size on the integrated circuit, so the lasting reduction of device geometries need have the film than low-k (k) value.A kind of method of acquisition ultralow dielectric (k＜2.5) that is used for is for making the mixed film of silicon matrix and organic pore-foaming agent, described mixed film is to be got with the compound deposition that comprises determination system of thermal unstable material or volatile groups (pore-foaming agent) by the admixture of gas that includes organic silicon compound, and then the film that will deposit carries out reprocessing with UV curing or heat treatment, by the determination system of thermal unstable material or the volatile groups that remove pore-foaming agent in the described film that has deposited, thereby produce pore of nanometer in these films, described method has reduced the dielectric constant of these films.
Known nano-pore (nanoporous) film for the tackness of following stopping/laying less than silica.Can obtain the improvement of tackness by the deposition oxide adhesion layer, described oxide adhesion layer can promote tackness at the interface.In order further to improve tackness, suggestion can stick together and main low k thin film deposition steps between use and have the gradient layer that increases carbon content gradually.Yet, the uncontrolled transfer that silicon and pore-foaming agent flow in this gradient layer can cause unexpected gas-phase reaction (owing to the various variations of RF power, pressure and flow velocity etc.), thereby causes swarm of particles and/or form the carbon projection in film or at interface at film.
In addition, known as the above-mentioned ultralow dielectric film of developing presents than the worse engineering properties of expectation, for example, bad mechanical strength (modulus approximates 4GPa), described bad mechanical strength make described film suffer damage easily during follow-up semiconductor processes step.And, constitute the major part of described dielectric film storehouse owing to the oxide adhesion layer that is used at present making ultralow dielectric film and following stopping/laying have preferable tackness, and described oxide adhesion layer has higher dielectric constant (k is about 3.5) and very high thickness heterogeneity usually, therefore can't be as reducing total dielectric constant and the thickness heterogeneity of the dielectric film storehouse that produces as the expection.
Therefore, need a kind of technology of making ultra-low dielectric constant material, described ultra-low dielectric constant material have improvement mechanical strength, reduction the thickness heterogeneity and make the k (dielectric constant) of the initial period of auto-deposition ultra-low dielectric constant material to increase to minimize, and can not work the mischief for the controllability of low applied thickness.
Technical field
The embodiment of the invention relates generally to the manufacturing of integrated circuit.More specifically, these embodiment relate to the technology for the low dielectric constant films of deposition integrated circuit.
Summary of the invention
The embodiment of the invention provides a kind of method substantially, is used for depositing the ultralow dielectric film with brand-new technological parameter.In one embodiment, described method comprises: admixture of gas is flowed in the treatment chamber, with by radio frequency (RF) power is applied to described treatment chamber, and depositing initial layers (oxide skin(coating)) at substrate, described admixture of gas comprises the flow velocity of one or more organosilicon compound flow rate and one or more pore-foaming agent compounds; Improve described one or more organosilicon compound flow rate, up to the final flow rate that reaches described one or more organo-silicon compound, in order to deposit first transition zone at described initial layers; And when described one or more organo-silicon compound flow with final flow rate, improve the flow velocity of described one or more pore-foaming agent compounds, up to the final flow rate that reaches described one or more pore-foaming agent compounds, in order to deposit second transition zone at described first transition zone, wherein to the low RF power of about 500W, carrying out described deposition between about 350W, and the ratio of described RF power and overall flow rate is to about 0.3W/sccm between about 0.1W/sccm.In execution mode, various processing parameters and predecessor will be discussed further.
In another embodiment, described method comprises the substrate that carrying pad/barrier layer is provided; With between about 1000
Figure BDA00003159748200031
To about 3500 Deposition rate, deposited carbon-containing oxide adhesion layer on described pad/barrier layer, described deposition comprises: admixture of gas is flowed in the treatment chamber, with by will about 300W under 13.56MHz being applied to described treatment chamber to radio frequency (RF) power level of about 600W, and depositing initial layers at substrate, described admixture of gas comprises the flow velocity of one or more organosilicon compound flow rate and one or more pore-foaming agent compounds; Improve described one or more organosilicon compound flow rate, up to the final flow rate that reaches described one or more organo-silicon compound, in order to deposit first transition zone at described initial layers; And improve the flow velocity of described one or more pore-foaming agent compounds, up to the final flow rate that reaches described one or more pore-foaming agent compounds, described one or more organo-silicon compound flow with final flow rate simultaneously, in order to deposit second transition zone at described first transition zone; At the low k film of described adhesion layer deposition; And solidify the low k film that has deposited, in order in the low k film that has deposited, to form nano-pore.In execution mode, various processing parameters and predecessor will be discussed further.
Description of drawings
More specific description of the present invention, above simplified summary can be understood by some embodiment that narrate in reference to the accompanying drawings, therefore detail knowledge above-mentioned feature of the present invention more.Yet, should be noted that accompanying drawing only illustrates exemplary embodiments of the present invention, and therefore should not be regarded as limitation of the scope of the invention, because other equivalent embodiment of tolerable of the present invention.
Figure 1A is the viewgraph of cross-section according to the formed dielectric film storehouse of the embodiment of the invention.
Figure 1B is the amplification cross-sectional view of the part of the film storehouse shown in Figure 1A.
Fig. 2 is process chart, and described process chart explanation is according to the method for the ultralow k nano-porous thin film of the deposition of embodiment of the invention storehouse.
Fig. 3 is the cross-sectional view of exemplary process chamber, and described treatment chamber can be used for implementing the embodiment of the invention.
Fig. 4 is by the depth distribution of sims analysis explanation concentration of element in organosilicate dielectric film storehouse.
Embodiment
The invention provides a kind of method that deposits low dielectric constant films.Described low dielectric constant films comprises silicon, oxygen, hydrogen and carbon.Proved that the embodiment of the invention can reduce adhesion layer by the thickness that reduces adhesion layer significantly for k (dielectric constant) influence of ultralow dielectric film storehouse.By adhesion layer thickness being reduced to approximately or being less than
Figure BDA00003159748200043
Figure BDA00003159748200041
Also can with ultralow dielectric film storehouse (less than
Figure BDA00003159748200042
) the thickness heterogeneity be reduced to less than 2%.As will be discussed, deposit the oxide adhesion layer of improvement with lower deposition rate and lower plasma density and higher overall flow rate, thereby during thin film deposition, produce the preferable encapsulation/ordering of codeposition material, this causes higher mechanical strength and lower porosity.The adhesion layer of improvement provides high energy of attachment, makes ultralow dielectric film and following stopping/laying have preferable tackness.The low dielectric film that produces has the hole of nano-scale and bore hole size distribution more closely.Described low dielectric constant films has about 3.0 or lower dielectric constant, and preferable is about 2.5 or lower.Described low dielectric constant films can have at least about 6.5GPa or higher modulus of elasticity.
Figure 1A schematically illustrates the viewgraph of cross-section according to the formed dielectric film storehouse 100 of the embodiment of the invention.Although not in this expression, but can consider that dielectric film storehouse 100 of the present invention can be used as the metal intermetallic dielectric layer in the dual-damascene structure, described dual-damascene structure comprises to replace or metal intermetallic dielectric layer (not shown) and one or more etch stop layer (not shown) of one or more nano-pores that desired sequence was deposited usually, and described etch stop layer is silica, silicon nitride, silicon oxynitride or armorphous hydrogenated silicon carbide.Then, antireflecting coating (not shown) and the groove photomask (not shown) that comprises photoresist layer are deposited on respectively on the thin layer that has deposited, and with habitual photoetching technique in the mode of development metallization structure with antireflecting coating and groove optical mask patternization, described metallization structure is filled with required metal (for example, copper).Can repeat described dual damascene and form technology, in order to deposit the interconnect levels of requirement.Can benefit from exemplary dual-damascene structure of the present invention and further in licensing to the U.S. Patent number 7,547,643 of common transfer of Francimar Schmitt etc. on June 16th, 2009, describe, incorporate among the present invention by reference in full.
Substantially, dielectric film storehouse 100 shown in Figure 1A comprises the substrate 102 of carrying pad/barrier layer 104, and described pad/barrier layer 104 is as follow-up adhesion layer 106 and following substrate surface 103 and be formed on separator between the metal wire 108 on the substrate surface 103.To hang down k layer 110 and be deposited on the adhesion layer 106, described low k layer 110 bound the layer 112 bind.Come the method for this type of dielectric film storehouse 100 of cutline deposition according to various embodiments of the present invention with reference to Fig. 2 and Figure 1B.
The illustrative processes that is used for the organic silicate layer of deposition
Fig. 2 is technological process Figure 200, and described technological process Figure 200 illustrates the method for deposit dielectric film storehouse 100 according to an embodiment of the invention.Substantially, typical porous dielectric films need deposit one or more organo-silicon compound and one or more unsaturated non-silicon compounds simultaneously, described organo-silicon compound become the silicon main chain, described one or more unsaturated non-silicon compounds have the thermally labile group, and described unsaturated non-silicon compound is as the pore-foaming agent of sacrificing.In step 202, the substrate 102 of carrying pad/barrier layer 104 is placed on the substrate support in the treatment chamber, described treatment chamber can be carried out plasma enhanced chemical vapor deposition (PECVD) technology.Can be by pecvd process, by plasma-deposited described pad/barrier layer 104, described plasma includes organic silane compound, ammonia, oxygen and inert substance.According to the method that is known in the art, described depositing operation can comprise capacitance coupling plasma or inductance and capacitance coupling plasma in treatment chamber.Can use inert gas (for example, helium, argon gas and nitrogen) to produce plasma.Usually in the PECVD deposition, use and assist plasma generation such as the inert gas of helium.
In step 204, with admixture of gas by gas distribution plate (for example, spray head) introduce in the treatment chamber, described admixture of gas has the component that comprises one or more organo-silicon compound, one or more pore-foaming agent compounds and one or more oxidizing gases.Before starting RF power, the initial gas component of oxygen and/or helium can be introduced in the treatment chamber, to stablize the environment of subsequent deposition.
In one embodiment, so that () flow velocity for example, between about 350 milligrams/minute to about 2500 milligrams/minute is introduced one or more organo-silicon compound in chambers between about 200 milligrams/minute to about 5000 milligrams/minute; With between about 100sccm to about 1000sccm(for example, between about 125sccm about 550sccm extremely) flow velocity, in one or more oxidizing gases introducing chambers; And with the flow velocity between about 50 milligrams/minute to about 5000 milligrams/minute (for example, between about 150 gram/minute to about 1500 gram/minute), one or more pore-foaming agent compounds are introduced in chambers.For the plasma treatment environment is provided in chamber, radio frequency (RF) power is applied to electrode, for example, spray head.The RF power that is fit to can be extremely in the about 2000W scope power of (for example, about 300W extremely about 600W) of about 10W under the frequency of about 13.56MHz.Under the situation that RF power exists, described admixture of gas reacts in chamber, comprises the initial layers 106a of oxide skin(coating) in order to deposition, and described oxide skin(coating) is adhered to following pad/barrier layer 104 securely.
Described admixture of gas alternative comprises one or more carrier gas.Usually, one or more carrier gas are introduced in the treatment chamber with one or more organo-silicon compound and one or more pore-foaming agent compounds.Spendable examples of carrier gases comprises the combination of helium, argon gas, carbon dioxide and aforementioned gas.In using the embodiment of helium as carrier gas, with between about 1500sccm to about 8000sccm(for example, between about 3500sccm about 5500sccm extremely) flow velocity, helium is introduced in the chamber with one or more organo-silicon compound.With between about 300sccm to about 1800sccm(for example, between about 700sccm about 1250sccm extremely) flow velocity, in helium and one or more pore-foaming agent compounds introducing chamber.
Initial layers 106a comprises silicon oxide layer substantially.As described below, initial layers 106a and the first transition zone 106b and second transition zone 106c(Figure 1B) constitute adhesion layer 106, the pad/barrier layer 104 below described adhesion layer 106 promotes and the tack between the follow-up low k layer 110.In one embodiment, the initial layers deposition can be carried out between about 0.5 second to about 10 seconds time range, as long as described deposition cycle is the adhesion that is long enough to guarantee whole film.In an example, initial layers deposits sustainable about 1 second.Initial layers 106a can be deposited into approximately
Figure BDA00003159748200061
To about
Figure BDA00003159748200062
Thickness in the scope is preferably approximately
Figure BDA00003159748200063
To about
Figure BDA00003159748200064
Should be taken into account, can adjust the description various cycles in the present invention according to the demand of specific embodiment.For example, when describing time range in certain embodiments and be about 0.5 second to about 10 seconds, sustainable 0 second of described start cycle.Represent that after air-flow was introduced chamber, will begin in a minute changed the flow velocity of air-flow 0 second start cycle.Therefore, should be taken into account the embodiment with start cycle.
Before the low k layer 110 of deposition, to carry out independent transfer step and be formed in the film to avoid any unwanted swarm of particles, described swarm of particles is the unexpected gas-phase reaction that flows owing to silicon and pore-foaming agent in the generation of gas distribution plate place.Also observe and enter in the chamber stably that liquid shifts the generation that can reduce the carbon projection significantly.Can be by under required raising speed, the transfer of two liquid precursor (that is, organo-silicon compound and pore-foaming agent compound) is separated these problems that solves.In the very first time of independent transfer step section 206, or simply be expressed as step 206, with between about 100 the milli Grams Per Seconds to about 5000 the milli Grams Per Seconds (for example, between about 800 the milli Grams Per Seconds to about 1200 the milli Grams Per Seconds) raising speed (for example, about 1000 milli Grams Per Seconds), improve one or more organosilicon compound flow rate gradually, under situation about existing at RF power, at the initial layers 106a deposition first transition zone 106b, up to reaching predetermined organic silicon compound gas mixture (see also Figure 1B, Figure 1B is that the part of the film storehouse shown in Figure 1A is amplified cross-sectional view).In the embodiment that uses the helium carrier gas, the flow velocity of one or more organo-silicon compound and helium can be reduced between about 2500sccm to the scope of about 4000sccm.In one embodiment, first transition zone deposition can be carried out about 0.5 second to about 10 seconds time range.In an example, the first transition zone sedimentation time can be about 1 second.The first transition zone 106b can be deposited into approximately
Figure BDA00003159748200071
To about
Figure BDA00003159748200072
(for example, approximately
Figure BDA00003159748200073
To about
Figure BDA00003159748200077
) scope in a thickness.
In second time period 208 of described transfer step, or simply be expressed as step 208, keep predetermined organic silicon compound gas mixture constant in, with between about 100 the milli Grams Per Seconds to about 5000 the milli Grams Per Seconds (for example, between about 200 the milli Grams Per Seconds to about 350 the milli Grams Per Seconds) raising speed (for example, about 300 milli Grams Per Seconds), improve the flow velocity of one or more pore-foaming agent compounds gradually in order to deposit the second transition zone 106c (Figure 1B) at the first transition zone 106b, up to reaching predetermined final admixture of gas.In the embodiment that uses the helium carrier gas, the flow velocity of one or more pore-foaming agent compounds and helium can be increased to the scope to about 2000sccm between about 800sccm.In one embodiment, second transition zone deposition can be carried out between about 1 second to about 180 seconds time range.In an example, the second transition zone sedimentation time can be about 3 seconds.The second transition zone 106c can be deposited into approximately
Figure BDA00003159748200075
To about
Figure BDA00003159748200076
Thickness, preferably about
Figure BDA00003159748200081
To about
Figure BDA00003159748200082
Between the depositional stage of initial layers 106a and the first transition zone 106b and the second transition zone 106c, preferably produce thin part 106 depositions of film storehouse (106a, 106b and 106c), as shown in the figure.The described thin part 106 of film storehouse provides tack preferable between ultralow dielectric film and the following stopping/laying as adhesion layer.In most embodiment, the thickness of described part can reduce makes an appointment with half, for example, is less than about 200 dusts.Can be by the duration section of relative weak point and/or the deposition that low deposition rate realizes the thin part 106 of film storehouse (106a, 106b and 106c).In one embodiment, the deposition rate of the thin part of film storehouse between about 1000 dusts/minute to about 3500 dusts/minute, for example, about 2500 dusts/minute.When the thin part 106 of film storehouse (106a, 106b and 106c) constitutes when having thickness less than the ultralow k nano-porous thin film storehouse (106a, 106b, 106c and 110) of 2000 dusts most of, can be by the thickness of the thin part that reduces described film storehouse, and the thickness heterogeneity of dielectric film storehouse 100 is reduced to less than 2%.The most important thing is that the thickness of the thin part 106 of film storehouse (106a, 106b and 106c) reduces the k influence that can make to whole nano-porous thin film storehouse and minimizes.
In step 210, after reaching final admixture of gas component, form the plasma of final admixture of gas, the organosilicate dielectric layer that contains pore-foaming agent with deposition (namely, low k layer 110), described final admixture of gas comprises the flow velocity of one or more organosilicon compound flow rate and one or more pore-foaming agent compounds.In one embodiment, low k layer deposition can be carried out between about 15 seconds to about 180 seconds time range.In an example, final layer sedimentation time can be about 130 seconds.Can be deposited into approximately hanging down k layer 110 To about
Figure BDA00003159748200084
Scope in thickness, till RF power stops.Without wanting to be limited by theory, believe by the raising speed of separating organo-silicon compound and pore-foaming agent compound, can obtain technology more stable and that can make, thereby produce the organosilicate dielectric layer with obvious less defect problem (for example, carbon projection).
Perhaps, can be with the step 208 of the deposition second transition zone 106c and step 210 merging of the final pore-foaming agent silicon oxide layer of deposition.In this type of embodiment, can improve the flow velocity of pore-foaming agent compound continuously, flow at the predetermined organic silicon compound gas mixture of pore-foaming agent silica depositional stage chien shih simultaneously.Step 208 can be carried out between about 1 second to about 180 seconds time range with the merging of step 210.In this way, final pore-foaming agent silicon oxide layer can have the gradient concentration of pore-foaming agent, and the pore-foaming agent concentration in described silicon oxide layer increases along with the deposition of pore-foaming agent silicon oxide layer.Described gradient layer can be deposited into approximately To about
Figure BDA00003159748200092
Thickness, preferably, approximately
Figure BDA00003159748200093
To about Till RF power stops.
During above-mentioned technology, usually substrate is maintained under the temperature of about 100 ℃ to about 400 ℃ (for example, between about 200 ℃ to about 350 ℃).Chamber pressure can be between about 1 holder (Torr) between about 20Torr, for example, between about 9Torr, and the spacing between substrate support and the chamber spray head can be between about 200mil extremely between about 1500mil between about 7Torr, for example, between about 280mil between about 450mil.For the substrate of 300mm, can use between about 100W to the RF power level between about 600W.To the frequency (for example, about 13.56MHz) of about 300MHz, providing described RF power between about 0.01MHz.Can under hybrid frequency (for example, in the high-frequency of about 13.56MHz and the low frequency of about 350kHz), provide RF power.Capable of circulation or pulsed RF power, reducing the heating of substrate, and promote in deposit film than macroporosity.According to application, described RF power also can be continuous or discrete.
In certain embodiments, use than low plasma density and higher overall flow rate.In order to obtain than low plasma density, can use between about 300W to about 600W(for example, between about 350W about 500W extremely) the RF power level.Using between about 350W to the situation of the RF power level of about 500W, preferably about 0.1W/sccm is to RF power/overall flow rate of about 0.3W/sccm.Perhaps, preferred about 0.2W/cm 3To about 0.5W/cm 3RF power/cumulative volume stream.Term " overall flow rate " or " cumulative volume stream " are intended to represent as discussed previously between depositional stage as used in this, introduce the admixture of gas for the treatment of chamber and mobile/volume of selectable carrier gas.This case inventor has found to use than low plasma density and higher overall flow rate, during thin film deposition, can allow the codeposition material than compact package, thereby produce higher mechanical strength, less bore hole size (less than
Figure BDA00003159748200095
) and cell size distribution of sizes more closely.By improving the anti-infringement of film to the subsequent device manufacturing process, significantly improve the mechanical integrity of film.
In any one embodiment as herein described, deposited the organosilicate dielectric layer that contains pore-foaming agent by the processing admixture of gas that includes organic silicon compound and pore-foaming agent.Described organic silicic acid salt deposit can be used as dielectric layer.Can use described dielectric layer in the different levels place in dual-damascene structure or suitable device.For example, described dielectric layer can be used as preceding metal dielectric layer, metal intermetallic dielectric layer or gate dielectric.The organic silicic acid salt deposit that deposits of identity basis various embodiment of the present invention can provide and be lower than 3.0 low-k, for example, and about 2.5.
Can use various processing admixture of gas to deposit the organosilicate dielectric layer, the limiting examples of this type of admixture of gas below will be provided.Substantially, admixture of gas comprises one or more organo-silicon compound (for example, first and second organo-silicon compound), one or more pore-foaming agent compounds, carrier gas and oxidizing gas.Comprise that (many other admixture of gas of) additional component for example, aliphatic hydrocarbon are not so should be considered as said components restriction such as hydrocarbon because consider.
As used herein term " organo-silicon compound " is intended to represent the silicon-containing compound that comprises carbon atom in organic group.Described organo-silicon compound can comprise the combination of one or more cyclic organosilicon compounds, one or more aliphat organo-silicon compound or aforesaid compound.Some exemplary organo-silicon compound comprise: methyldiethoxysilane (mDEOS), tetramethyl-ring tetrasiloxane (TMCTS), octamethylcy-clotetrasiloxane (OMCTS), trimethyl silane (TMS), the pentamethyl D5, hexamethyl cyclotrisiloxane, the dimethyl disiloxane, 2,6-dioxy base-4,8-dimethylene tetrasilane, tetramethyl disiloxane, HMDO (HMDS), two (silylation dimethylene) disiloxane of 1,3-, two (1-methyl disiloxanyl) methane, two (1-methyl disiloxanyl) propane, hexa methoxy disiloxane (HMDOS), dimethyldimethoxysil,ne (DMDMOS) and dimethoxymethylvinylchlane (DMMVS), the perhaps derivative of aforesaid compound.(flow velocity in) the scope for example, between about 350 milligrams/minute to about 2500 milligrams/minute can be introduced described one or more organo-silicon compound in treatment chamber with about 200 milligrams/minute to about 5000 milligrams/minute.
As used herein term " pore-foaming agent compound " is intended to represent the compound that comprises the thermally labile group.Described thermally labile group can be cyclic group, for example, and the unsaturated cyclic organic group.As used herein term " cyclic group " is intended to represent circulus.Described circulus can comprise few to three atoms.For example, these atoms can comprise the combination of carbon, nitrogen, oxygen, fluorine and aforementioned atom.Described cyclic group can comprise one or more singly-bounds, two key, triple bond and aforesaid any combination.For example, cyclic group can comprise the combination of one or more aromatic series, aromatic radical, phenyl, cyclohexane, cyclohexadiene, cycloheptadiene and aforementioned group.Described cyclic group also can be dicyclo or three rings.In one embodiment, the functional group bonding of described cyclic group and straight or branched.The functional group of described straight or branched preferably comprises alkyl or vinyl alkyl group, and has the carbon atom between 1 to 20.The functional group of described straight or branched also can comprise the oxygen atom in for example ketone, ether and the ester.Pore-foaming agent can comprise the ring-type hydrocarbon.Some spendable exemplary pore-foaming agents comprise: bicycloheptadiene (BCHD, two ring (2.2.1) heptan-2, the 5-diene), 1-methyl-4 (1-Methylethyl)-1,3-cyclohexadiene (ATP or α-terpinene), vinyl cyclohexane (VCH), phenylacetate, butadiene, isoprene, cyclohexadiene, bicyclo-heptadiene, 1-methyl-4-(1-Methylethyl) benzene (cumene), 3-corner of the eyes alkene, fenchone, citrene, cyclopentene oxide, vinyl-1,4-dioxin base ether, vinyl furyl ether, vinyl-1, the 4-dioxane, the vinyl furans, methylfuroate, formic acid furans ester, acetic acid furans ester, furfural, difuryl ketone, difuryl ether, furfuryl ether, furans and 1,4-dioxane, and the fluorocarbons derivative of aforesaid compound.(flow velocity in) the scope for example, between about 150 milligrams/minute to about 1500 milligrams/minute is introduced described one or more pore-foaming agent compounds in treatment chamber with about 50 milligrams/minute to about 5000 milligrams/minute.
As previously mentioned, described admixture of gas alternative comprises one or more carrier gas.Usually, one or more carrier gas are introduced in the described treatment chamber with one or more organo-silicon compound and one or more pore-foaming agent compounds.Spendable examples of carrier gases comprises: the combination of helium, argon gas, carbon dioxide and aforementioned gas.Partly according to the size of chamber interior, can be less than about 20, the flow velocity of 000sccm is introduced one or more carrier gas in treatment chamber.Flow rate of carrier gas is preferably at about 500sccm to the scope of about 5000sccm.In some technologies, before introducing reactive processing gas, will insert in the treatment chamber such as the inert gas of helium or argon gas, with the indoor pressure of stable cavity.
Admixture of gas also comprises one or more oxidizing gases.The oxidizing gas that is fit to comprises: oxygen (O 2), ozone (O 3), nitrous oxide (N 2O), carbon monoxide (CO), carbon dioxide (CO 2) with the combination of aforementioned gas.Partly according to the size of chamber interior, the flow velocity of described oxidizing gas can be about 100sccm to about 3, in the scope of 000sccm.Usually, the flow velocity of oxidizing gas is extremely about 1 for about 100sccm, in the scope of 000sccm, for example, about 450sccm.Enter before the deposition chambers and/or as in chamber, RF power is applied to when handling gas, in the microwave chamber, can produce oxygen or the dissociating of oxygenatedchemicals.
Aftertreatment technology
After the deposition low dielectric constant films, described film is carried out reprocessing.Can use thermal annealing separately or so that ultraviolet ray (UV) radiation is auxiliary film be carried out reprocessing, removing organic unstable material, and in final material, produce the hole down and go into thing.In one embodiment, with the UV curing process low dielectric constant films is carried out reprocessing.Can in same treatment chamber or system, original position carry out the UV reprocessing, for example, be transferred to another chamber by a chamber, and do not destroy vacuum state.Spendable exemplary UV post-treatment condition comprises: between chamber pressure and the substrate support temperature between about 350 ℃ to about 500 ℃ between of about 1Torr between about 10Torr.UV ray radiation source can be away from the about 100mil of substrate surface between about 1400mil.Selectively, during ultraviolet curing process, can introduce processing gas.The processing gas that is fit to comprises: oxygen (O 2), nitrogen (N 2), hydrogen (H 2), helium (He), argon gas (Ar), steam (H 2O), the combination of carbon monoxide, carbon dioxide, hydrocarbon gas, fluorocarbon gas and fluorinated hydrocarbon gas or aforementioned gas.
Can provide UV radiation by any UV source, for example, mercury microwave arc lamp, pulsed xenon flashing light or high efficiency UV light emitting diode matrix.Ultraviolet radiation can comprise a ultraviolet range, and comprises one or more synchronous mode wavelength.Suitable ultraviolet wavelength comprises between about 1nm between about 400nm, and can further comprise up to about 600 or the choosing wavelength of 780nm.In addition or alternatively, can or under the modulation between a plurality of expectation wavelength, apply described ultraviolet radiation in multi-wavelength, the radiation of adjustable wavelength and the radiation of adjustable power, and described ultraviolet radiation can be radiated or be applied by the ultra-violet lamp array by single UV lamp.The example that is fit to ultra-violet lamp comprises: the Zeridex that xenon is filled TMUltra-violet lamp, Ushio Excimer ultra-violet lamp, DSS ultra-violet lamp or mercury-arc lamp.The low dielectric constant films that has deposited is exposed to described ultraviolet radiation reaches between about 10 seconds to about 600 seconds, for example, between about 60 seconds to about 600 seconds.The wavelength of UV radiation can be between for example, and about 170nm is to about 400nm.The further details of spendable UV chamber and treatment conditions on May 9th, 2005 submit to and the common U.S. Patent Application Serial Number of transferring the possession of 11/124,908 in describe, described application is incorporated herein by reference.NanoCure from Applied Materials TMChamber is an example that can be used for the commercially available chamber of UV reprocessing.
In another embodiment, utilizing heat or plasma to strengthen annealing process comes low dielectric constant films is carried out reprocessing.Between about 200 ℃ to about 400 ℃ temperature, can be in chamber film being annealed reaches about 2 seconds to about 1 hour, preferably is about 30 minutes.To about 10, the speed of 000sccm is introduced non-reactive gas with about 100sccm, and described non-reactive gas for example is the mixing of helium, hydrogen, nitrogen or aforementioned gas.Chamber pressure is maintained between about 1Torr between about 10Torr.RF power during the annealing under the frequency of about 13.56MHz for about 200W to about 1,000W, and the substrate spacing that is fit to is between about 300mil extremely between about 800mil.Make described low dielectric constant films annealing at least some organic groups in the film that volatilized to about 400 ℃ substrate temperature at about 200 ℃ behind the described low dielectric constant films of deposition, thereby in film, forming hole.
In another embodiment, come low dielectric constant films is carried out reprocessing with electron beam treatment.Spendable exemplary electron beam condition comprises: the chamber temp between about 200 ℃ to about 600 ℃, for example, about 350 ℃ to about 400 ℃.Electron beam energy can be about 0.5keV to about 30keV.Exposing dosage to the open air can be between about 1 μ C/cm 2To about 400 μ C/cm 2Chamber pressure can be between about 1mTorr to about 100mTorr.Gaseous environment in the chamber can be any of following gas: any combination of the mixing of nitrogen, oxygen, hydrogen, argon gas, hydrogen and nitrogen, ammonia, xenon or aforementioned gas.Electron beam current can be between about 0.15mA to about 50mA.Electron beam treatment can be carried out and reach about 1 minute to about 15 minutes.Spendable exemplary electron beam chamber is EBk TMElectron beam chamber, described EBk TMElectron beam chamber can be available from the Applied Materials that is positioned at the Santa Clara city, yet can use any electron beam equipment.
The electronic beam curing process improving is the mechanical strength of deposit film network, and also reduces the k value.The electron beam that is excited changes the chemical bonding in the molecular network of deposit film, and the molecular radical from described thin film removing at least a portion, for example, from the ring-type organic component of one or more oxygen-free hydrocarbons, described oxygen-free hydrocarbon comprises a ring and one or two carbon-to-carbon double bond in described ring.Removing of molecular radical can produce hole or hole in described film, thereby reduces the k value.
Exemplary hardware
Fig. 3 shows the cross-sectional view of chemical vapor deposition (CVD) chamber 300, and described chamber 300 is used for the silicon oxide layer of deposit carbon-doped.Described figure is based at present by Applied Materials's manufacturing
Figure BDA00003159748200141
The feature of chamber.
Figure BDA00003159748200142
Chamber (200mm or 300mm) has the processing region of two isolation, and described processing region can be used for silica and other material of deposit carbon-doped.Have the chamber in two isolation processing zones at U.S. Patent number 5,855, describe in 681, described patent is incorporated herein by reference.
Deposition chambers 300 has chamber body 302, and described chamber body 302 defines the processing region 318,320 of separation.Each processing region 318,320 has pedestal 328, and described pedestal 328 is used at chamber 300 supporting substrates (not shown).Pedestal 328 comprises heating element (not icon) usually.Preferably, by trunk 326 pedestal 328 is arranged in each processing region 318,320 movably, described trunk 326 extends through the bottom of chamber body 302, and described trunk 326 is connected with drive system 303 in the bottom of chamber body 302.With inside movably lift pin (not shown) preferably be provided in the pedestal 328, in order to mesh the low surface of substrate.Can mesh described lift pin by elevating mechanism (not shown), in order to before handling, receiving substrate, or after deposition, promote substrate, to transfer to the next stop.
Each processing region 318,320 is air inclusion allocation component 308 preferably also, and described gas distribution assembly 308 arranges and passes Pit cover 304, in order to provide gas tangentially in the processing region 318,320.The gas distribution assembly 308 of each processing region comprises the gas access passage 340 that passes branch pipe 348 usually, and described branch pipe 348 distributes branch pipe 319 to pass baffler 346 by gas and then passes spray head 342 and come supply gas.Spray head 342 comprises a plurality of nozzles (not shown), during handling, by these nozzle injecting gas mixtures.RF (radio frequency) supply 325 provides bias to spray head 342, generates in order to help the plasma between spray head and pedestal 328.Performed depositing operation can be non-plasma technology or the plasma-enhanced process on the substrate pedestal 328 of cooling in deposition chambers 300.In plasma process, usually by the RF energy that is applied to spray head 342 from RF power provider 325 (with the pedestal 328 of ground connection), at the plasma of adjacent substrate place formation through control.Perhaps, under different frequency, RF power provider 325 can be provided to pedestal 328 or provide to different parts.
Can use high-frequency RF (HFRF) power and low frequency RF (LFRF) power (for example, double frequency RF), constant RF, pulsed RF or any known or still undiscovered plasma generation technique produce plasma.RF power provider 325 can be supplied between about 5MHz to the single-frequency RF between about 300MHz.In addition, RF power provider 325 also can be supplied between about 300Hz to about 1, the low frequency RF between the 000kHz, and the frequency of mixing with supply, and strengthen the decomposition of the reactive materials of introducing the processing gas in the treatment chamber.The described RF power of capable of circulation or pulse, reducing the heating of substrate, and promote in the deposit film than macroporosity.Suitable RF power can be about 10W power of (for example, at about 200W extremely in the scope of about 600W) to about 5000W scope.Suitable LFRF power can be about 0W power of (for example, at about 0W extremely in the scope of about 200W) to about 5000W scope.
The function of the various parts of system controller 334 controls is for example controlled RF power provider 325, drive system 303, elevating mechanism, gas distribution branch pipe 319 and other chamber that is associated and/or processing capacity.System controller 334 is carried out the system controlling software that is stored in the memory 338, and in preferred embodiment, described memory 338 is hard disk, and can comprise simulation and digital input/output board, interface board and stepper motor control board.Usually use optics and/or magnetic sensor to move and confirm the position of removable mechanical component.
Above-mentioned CVD system narration mainly is for reaching illustrative purposes, also can adopting other plasma process chamber to implement these embodiment of the present invention.
Example
The embodiment of the invention is showed the deposition of ultralow k nano-porous thin film, and described ultralow k nano-porous thin film has the trickle pore through disperseing.In aforesaid any one embodiment, following technological parameter and scope are conducive to main and/or adhesion layer depositing operation usually:
Parameter Scope
Heating-up temperature (℃) 200 to 350
Sedimentation time (second) 15 to 360
Pressure (Torr) 7 to 9
Spacing (mil) 280 to 450
HF?RF(Watt) 300 to 600
MDEOS (milligram) 200 to 2500
BCHD (milligram) 200 to 1600
Oxygen (sccm) 125 to 500
MDEOS helium flow rate of carrier gas (sccm) 500 to 5000
MBCHD helium flow rate of carrier gas (sccm) 500 to 1250
During the deposition adhesion layer, in various transfers, the raising speed of one or more organo-silicon compound and one or more pore-foaming agent compounds is usually respectively between between 800 milli Grams Per Second to the 1200 milli Grams Per Seconds and between 200 milli Grams Per Second to 350 milli Grams Per Seconds.Preferably, during various transfer step, only change in organo-silicon compound and the pore-foaming agent compound one flow, to avoid in film, producing any defective, as previously mentioned.
In an aforementioned specific embodiment relevant with Figure 1A and 1B, will contain the organosilicate dielectric layer deposition of pore-foaming agent on substrate.Use
Figure BDA00003159748200161
PECVD chamber in the system (that is, the CVD chamber) deposits described film, and is described
Figure BDA00003159748200162
System can be available from the Applied Materials that is positioned at the Santa Clara city.Between depositional stage, chamber pressure is maintained the pressure of about 6.5Torr, and substrate is maintained about 270 ℃ temperature.Substrate is placed on the substrate support that is arranged in the treatment chamber.Substrate is placed on the place apart from chamber spray head 450mil.
To handle admixture of gas and introduce in the chamber, and stablized flow velocity before starting RF power, the initial gas component of described processing gas is the oxygen of 300sccm and the helium of 3800sccm.Subsequently, RF power level that will about 600W under the 13.56MHz frequency is applied to spray head, to form the admixture of gas plasma, in order to the cvd silicon oxide initial layers, described admixture of gas comprises methyldiethoxysilane (mDEOS), and with about 600 milligrams flow velocity admixture of gas is introduced in the chamber.After starting about 1 second of RF power, with the raising speed of about 1000 milli Grams Per Seconds the flow velocity of mDEOS is increased to 2200 milligrams and reach about 1 second.In addition, helium mobile is reduced to about 3000sccm.
After reaching and keeping about 2200 milligrams/minute final mDEOS flow velocity, reach about 3 seconds in the mobile introducing chamber of raising speed with BCHD with about 400 milli Grams Per Seconds, to reach about 1300 milligrams pore-foaming agent deposition rate.Final admixture of gas component also comprises the helium of 3000sccm and the oxygen of 225sccm.After the expectation thickness that reaches the organosilicate dielectric layer that contains pore-foaming agent, stop RF power, to stop further deposition.After stopping RF power, open chamber throttle valve, extract out from chamber to allow handling admixture of gas.The independent transfer of liquid precursor entered the defective that can reduce in the chamber in the film.Carry out secondary ion mass spectroscopy (SIMS) and analyze the depth distribution of concentration of element in the dielectric film storehouse, as shown in Figure 4.The depth distribution of carbon is presented at carbon phase shift more smooth-going in these films, thereby the technology of hint usage example can not produce the carbon projection in film.
Should be taken into account the various variations that to implement above-mentioned example.For example, can use other organosilan predecessor, pore-foaming agent predecessor, oxidizing gas and inert gas.In addition, can adopt different flow velocitys and/or raising speed.According to application, when the each several part of deposit film (for example, initial layers 106a and/or transition zone 106b, 106c) time, can adjust the flow velocity of various predecessors, to change carbon content, make that the start-up portion of deposit film has low carbon content, and therefore be similar to oxide, part in succession has higher carbon content simultaneously, is similar to oxycarbide thereby become.
Proved that the embodiment of the invention can significantly reduce the oxide adhesion layer by the thickness that reduces adhesion layer to the k influence of ultralow dielectric film storehouse, described adhesion layer utilizes brand-new technological parameter to deposit.By adhesion layer thickness is reduced to approximately or less than
Figure BDA00003159748200187
Figure BDA00003159748200181
Also can with ultralow dielectric film storehouse (less than
Figure BDA00003159748200182
) the thickness heterogeneity be reduced to less than 2%.With about
Figure BDA00003159748200186
Deposit the oxide adhesion layer of improvement than low deposition rate and lower plasma density and higher overall flow rate (RF power/overall flow rate between about 0.1W/sccm between about 0.3W/sccm), thereby produce the preferable encapsulation/ordering of codeposition material during thin film deposition, described preferable encapsulation/ordering causes the higher mechanical strength of about 6.9Gpa.The adhesion layer of improvement provides enough good energy of attachment (about 4.5J/m2), makes between ultralow dielectric film and following stopping/laying to have preferable tack.The ultralow k nano-porous thin film that produces has between about To about
Figure BDA00003159748200185
Smaller aperture due and the closely bore hole size with porosity of about 15% to about 25% distribute.
Although above stated specification relates to these embodiment of the present invention, can carry out of the present invention other with further embodiment, and do not depart from base region of the present invention, and decide scope of the present invention by appended claim.

Claims (15)

1. the method for a treatment substrate, described substrate is arranged in the treatment chamber, and described method comprises:
Admixture of gas is flowed in the described treatment chamber, with by radio frequency (RF) power is applied to described treatment chamber, and initial layers is deposited on the described substrate, described admixture of gas comprises the flow velocity of one or more organosilicon compound flow rate and one or more pore-foaming agent compounds;
Improve the described flow velocity of described one or more organo-silicon compound, up to the final flow rate that reaches described one or more organo-silicon compound, in order to deposit first transition zone at described initial layers; And
Improve the described flow velocity of described one or more pore-foaming agent compounds, up to the final flow rate that reaches described one or more pore-foaming agent compounds, described one or more organo-silicon compound flow with described final flow rate simultaneously, in order to deposit second transition zone at described first transition zone, wherein the ratio of described RF power and overall flow rate be between about 0.1W/sccm to about 0.3W/sccm, carry out the described deposition of described initial layers, described first transition zone and second transition zone.
2. the method for claim 1 was carried out in the described time cycle that is deposited between about 0.5 second to about 5 seconds of wherein said initial layers.
3. the method for claim 1, the described deposition of wherein said first transition zone and second transition zone are respectively between carrying out between about 1 second to about 5 seconds and in the time cycle between about 1 second to about 10 seconds.
4. the method for claim 1, wherein described one or more organo-silicon compound being introduced in the described chamber to about 700 milligrams flow velocity between about 200 milligrams, and with between about 200 milligrams extremely about 1600 milligrams flow velocity described one or more pore-foaming agent compounds are introduced in the described chamber.
5. the method for claim 1, wherein with between
Figure FDA00003159748100013
To about
Figure FDA00003159748100014
Between deposition rate and between the low RF power of about 350W between about 500W, carry out the described deposition of described initial layers, described first transition zone and described second transition zone.
6. the method for claim 1, wherein with the raising speed between the extremely about 1500 milli Grams Per Seconds of about 600 milli Grams Per Seconds, improve the described flow velocity of described one or more organo-silicon compound, and with the raising speed between the extremely about 600 milli Grams Per Seconds of about 200 milli Grams Per Seconds, improve the described flow velocity of described one or more pore-foaming agent compounds.
7. the method for claim 1, wherein said admixture of gas further comprises one or more oxidizing gases and inert gas, described one or more oxidizing gases are selected from the group that is made up of following: ozone, oxygen, carbon dioxide, carbon monoxide, water, nitrous oxide, 2, the described inert gas of the combination of 3-diacetyl and aforementioned gas is selected from the group that is made up of helium, argon gas or nitrogen.
8. the method for claim 1, wherein said one or more organo-silicon compound are selected from the group that is made up of following: methyldiethoxysilane (mDEOS), tetramethyl-ring tetrasiloxane (TMCTS), octamethylcy-clotetrasiloxane (OMCTS), trimethyl silane (TMS), the pentamethyl D5, hexamethyl cyclotrisiloxane, the dimethyl disiloxane, 2,6-dioxy base-4,8-dimethylene tetrasilane, tetramethyl disiloxane, HMDO (HMDS), two (silylation dimethylene) disiloxane of 1,3-, two (1-methyl disiloxanyl) methane, two (1-methyl disiloxanyl) propane, hexa methoxy disiloxane (HMDOS), dimethyldimethoxysil,ne (DMDMOS), dimethoxymethylvinylchlane (DMMVS), and the derivative of aforesaid compound.
9. the method for claim 1, wherein said one or more pore-foaming agent compounds are selected from the group that is made up of following: bicycloheptadiene (BCHD; Two ring (2.2.1) heptan-2, the 5-diene), 1-methyl-4 (1-Methylethyl)-1,3-cyclohexadiene (ATP or α-terpinene), vinyl cyclohexane (VCH), phenylacetate, butadiene, isoprene, cyclohexadiene, bicyclo-heptadiene, 1-methyl-4-(1-Methylethyl) benzene (cumene), 3-corner of the eyes alkene, fenchone, citrene, cyclopentene oxide, vinyl-1,4-dioxin base ether, vinyl furyl ether, vinyl-1, the 4-dioxane, the vinyl furans, methylfuroate, formic acid furans ester, acetic acid furans ester, furfural, difuryl ketone, difuryl ether, furfuryl ether, furans, 1,4-dioxane, and the fluorocarbons derivative of aforesaid compound.
10. the method for a treatment substrate, described substrate is arranged in the treatment chamber, and described method comprises:
The substrate of carrying pad/barrier layer is provided;
With between approximately
Figure FDA00003159748100023
To about
Figure FDA00003159748100024
Between deposition rate, the carbon oxide adhesion layer is deposited on described pad/barrier layer top, described deposition comprises:
Admixture of gas is flowed in the described treatment chamber, with by will about 300W under the 13.56MHz frequency being applied to described treatment chamber to radio frequency (RF) power level of about 600W, and depositing initial layers at described substrate, described admixture of gas comprises the flow velocity of one or more organosilicon compound flow rate and one or more pore-foaming agent compounds;
Improve the described flow velocity of described one or more organo-silicon compound, up to the final flow rate that reaches described one or more organo-silicon compound, in order to deposit first transition zone at described initial layers; And
Improve the described flow velocity of described one or more pore-foaming agent compounds, up to the final flow rate that reaches described one or more pore-foaming agent compounds, described one or more organo-silicon compound flow with described final flow rate simultaneously, in order to deposit second transition zone at described first transition zone;
To hang down the k thin film deposition above described adhesion layer; And
Solidify the described low k film that has deposited, in order in described film, to form nano-pore.
11. method as claimed in claim 10, wherein said initial layers described is deposited on carry out described first transition zone in time cycle in about 0.5 second to about 5 seconds scope described and is deposited in time cycle in about 1 second to about 5 seconds scope and carries out, and described second transition zone described is deposited in time cycle in about 1 second to about 10 seconds scope and carries out.
12. method as claimed in claim 11, wherein described one or more organo-silicon compound being introduced in the described chamber to about 700 milligrams flow velocity between about 200 milligrams, and with between about 200 milligrams extremely about 1600 milligrams flow velocity described one or more pore-foaming agent compounds are introduced in the described chamber.
13. method as claimed in claim 10 wherein deposits described initial layers, described first transition zone and described second transition zone, to provide approximately
Figure FDA00003159748100031
To about Scope in gross thickness.
14. method as claimed in claim 10, wherein with the raising speed between the extremely about 1500 milli Grams Per Seconds of about 600 milli Grams Per Seconds, improve the described flow velocity of described one or more organo-silicon compound, and with the raising speed between the extremely about 600 milli Grams Per Seconds of about 200 milli Grams Per Seconds, improve the described flow velocity of described one or more pore-foaming agent compounds.
15. method as claimed in claim 10, wherein the ratio of described RF power and overall flow rate be between about 0.1W/sccm between about 0.3W/sccm, carry out the described deposition of described initial layers, described first transition zone and second transition zone.
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