CN104201149A - Fluorine-containing porous low-dielectric constant composite film and preparation method thereof - Google Patents
Fluorine-containing porous low-dielectric constant composite film and preparation method thereof Download PDFInfo
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- CN104201149A CN104201149A CN201410423510.XA CN201410423510A CN104201149A CN 104201149 A CN104201149 A CN 104201149A CN 201410423510 A CN201410423510 A CN 201410423510A CN 104201149 A CN104201149 A CN 104201149A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/76822—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc.
- H01L21/76828—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc. thermal treatment
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- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02203—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being porous
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
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- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/7682—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing the dielectric comprising air gaps
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- H01L23/522—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body
- H01L23/532—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body characterised by the materials
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Abstract
The invention belongs to the technical field of manufacturing of integrated circuits, and particularly relates to a fluorine-containing porous low-dielectric constant composite film and a preparation method thereof. The preparation method comprises the steps of: regarding TEOS (Tetraethyl Orthosilicate) and LIMO (Dipentene) as liquid-state source precursors, regarding C2F6 as a fluorine source, adopting a PECVD (Plasma Enhanced Chemical Vapor Deposition) process, controlling technical parameters such as a substrate temperature, a radio frequency power, a working pressure intensity in a reaction cavity, proportion of the precursors and the fluorine source in a deposition process, and depositing to obtain a fluorine-containing inorganic-organic composite film; then performing suitable thermal annealing treatment on the film to enable partial organic component to be thermally decomposed so as to obtain the fluorine-containing porous low-dielectric constant composite film. In a test at the high temperature of 100 DEG C , the dielectric constant of the film is 2.37-2.75, and the leakage current density at the field intensity of 1 MV/cm is within a range from 10 to the minus eight power to 10 to the minus nine power A/sq.cm.. In addition, the film of such type also has excellent mechanical property. The fluorine-containing porous low-dielectric constant composite film is simple in process operation, is completely compatible with a back-end interconnecting process of an existing integrated circuit, and is an ideal candidate of an interconnecting medium.
Description
Technical field
The invention belongs to ic manufacturing technology field, be specifically related to a kind of fluorine-containing porous low dielectric constant laminated film and preparation method thereof, be applied to the inter-level dielectric in copper-connection.
Background technology
Along with the development of integrated circuit technique, have high-speed, high device density, low-power consumption and cheaply chip more and more become the major product of very lagre scale integrated circuit (VLSIC).Now, the wire density in chip constantly increases, and conductor width and spacing constantly reduce, and this ghost effect that causes resistance (R) in chip backend interconnect and electric capacity (C) to produce is more and more obvious.At present, the industrial copper (Cu) that generally adopted replaces aluminium (Al) to connect up, to reduce resistance; Adopt low-k (low-
k) material replaces traditional silicon dioxide (SiO
2) the interior and interlayer dielectric as layer, to reduce parasitic capacitance.
In current scientific research and industrial production, low-
k(advanced low-k materials
k) preparation of material is mainly the technology that using plasma strengthens chemical vapor deposition (PECVD), to traditional SiO
2material carries out modification and obtains.Its concrete solution mainly contains: introduce fluorine element, introduce hydrocarbon group (CH
x), introduce hole etc.Low-the earliest
kmaterial is the silicon dioxide (F-SiO of fluorine doping
2), be used on 180 nm and 130 nm technology nodes.Mixing of fluorine element can replace SiO
2middle part oxygen element, forms the lower Si-F key of polarizability, thereby realizes the reduction of dielectric constant.Si-F key is highly stable, generally can in following process process, thermal decomposition not occur, but fluorine too high levels can cause film easily to absorb water.In addition, in PECVD process, the introducing of fluorine element is simple, without existing equipment and technique are done to larger change.
Porous membrane has also obtained research widely in recent years, and the introducing of hole can reduce the density of material, thereby reduces dielectric constant.At present, the porous low dielectric constant material of open report is mainly the SiCOH material of porous, prepares fluorine-containing porous low dielectric constant films there is not yet report for PECVD method.Therefore, the present invention is using tetraethoxysilane (TEOS) and dipentene (LIMO) as liquid source presoma, with perfluoroethane (C
2f
6) as fluorine source, adopt and the existing integrated circuit fabrication process PECVD technology of compatibility mutually, and the post-depositional heat treatment of combination film, prepare fluorine-containing porous low dielectric constant laminated film.This film also has good insulation property and mechanical property, can meet the performance requirement that integrated circuit back-end interconnects to medium.
Summary of the invention
The object of the present invention is to provide a kind of energy to meet dielectric material of interconnection requirement and preparation method thereof, i.e. fluorine-containing porous low dielectric constant laminated film and preparation method thereof.
The fluorine-containing porous low dielectric constant laminated film that the present invention proposes is as liquid source presoma, with perfluoroethane (C using tetraethoxysilane (TEOS) and dipentene (LIMO)
2f
6) as fluorine source, adopt pecvd process, obtain inorganic-organic hybrid film.Then, this film is carried out to thermal anneal process, make part organic component generation thermal decomposition, thereby obtain fluorine-containing porous low dielectric constant inorganic-organic hybrid film.
The preparation method of the fluorine-containing porous low dielectric constant laminated film that the present invention proposes, concrete steps are as follows:
(1) wafer is placed in to the reaction chamber of PECVD, then reaction cavity is vacuumized, make chamber pressure be less than 0.02 Torr; Then, by heating system, substrate is heated to 150 ~ 300 DEG C, and remains stable;
(2) in reaction cavity, pass into presoma TEOS and LIMO, both flows are 0.1 ~ 2 g/min; First adopt vaporizer to make presoma vaporization, wherein the vapourizing temperature of TEOS is 120 ~ 160 DEG C, and the vapourizing temperature of LIMO is 60 ~ 100 DEG C; Then use carrier gas (as helium) that precursor vapor is transported to reaction chamber from different gas circuits, the carrier gas flux of wherein carrying TEOS steam is 500 ~ 5000 sccm, and carrying the carrier gas flux of LIMO steam is 1000 ~ 8000 sccm;
(3) in reaction cavity, pass into C through independent pipeline
2f
6gas, flow is 10 ~ 2000 sccm;
(4) carry out plasma-reinforced chemical and deposit mutually, in deposition process, technological parameter is respectively: radio-frequency power 100 ~ 700 W; Operating pressure 1 ~ 8 Torr in reaction chamber; Upper and lower polar plate spacing 10 ~ 20 mm, obtain fluorine-containing inorganic-organic hybrid film;
In this fluorine-containing inorganic-organic hybrid film, inorganic constituents is mainly Si-O-Si structure, and organic principle is mainly CHx group; F is mainly combined with Si, is present in film with the form of Si-F key;
(5) PECVD is deposited to the inorganic-organic hybrid film obtaining and be placed in tube furnace, box type furnace or other cavitys, carry out thermal anneal process, annealing temperature is 400 ~ 600 DEG C, and annealing time is 0.5 ~ 4 hour, annealing atmosphere can be argon gas, helium or nitrogen etc., and pressure is 0.1 ~ 800 Torr.In annealing process, part organic component generation thermal decomposition is removed, and Si-F key can not decompose, and obtains thus fluorine-containing porous compound film.
Above-mentioned film is carried out to electricity and Mechanics Performance Testing, and gained performance is as follows: dielectric constant is 2.3 ~ 2.8, and the leakage current density under 1 MV/cm field intensity is 10
-7~ 10
-9a/cm
2in scope, Young's modulus is 6 ~ 9 GPa, and hardness is 0.5 ~ 1.0 GPa.
Tool of the present invention has the following advantages:
Adopt method provided by the invention, can successfully in film, introduce the hole of nanoscale, and introduce fluorine element.The film of being prepared by the method has low-k, good insulation property and excellent mechanical property.
Method provided by the invention is compatible mutually with existing integrated circuit processing technology, and prepared film can be directly as the inter-level dielectric in chip backend interconnect.Technique manipulation is easily simple, by adjusting process parameter, can effectively control the composition, chemical constitution, porosity of film etc., reaches the object of the performance such as electricity, mechanics of regulation and control low-k film.
Brief description of the drawings
Fig. 1 is different C in deposition process
2f
6the infrared spectrogram of the film that gas flow obtains after thermal anneal process.
Fig. 2 works as C in embodiment 1
2f
6the dielectric constant of film and the change curve of voltage that obtain for 300 sccm.
Fig. 3 works as C in embodiment 1
2f
6the leakage current density of film and the change curve of electric field strength that obtain for 300 sccm.
Embodiment
embodiment 1
In PECVD process, underlayer temperature is 200 DEG C, and in reaction chamber, operating pressure is 3 Torr, and deposition power is 300 W.Reaction raw materials is TEOS, LIMO and C
2f
6, wherein, the flow-rate ratio of TEOS and LIMO is that 1:1.25(flux unit is gram/minute), their vapourizing temperature is respectively 160 DEG C and 100 DEG C; After vaporization, taking helium as carrier gas, they are passed into respectively in reaction chamber, required carrier gas flux is respectively 2000 sccm and 5000 sccm; C
2f
6gas is imported in reaction chamber by independent gas piping, and its flow is 100 ~ 500sccm.The thickness of the fluorine-containing inorganic-organic hybrid film obtaining through PECVD is determined by deposition time.Then, by deposited film at nitrogen (N
2) carrying out thermal anneal process under atmosphere, air pressure is about 1 atmospheric pressure, and nitrogen flow is about 1 L/min, and annealing temperature is 450 DEG C, and annealing time is 2 h.3 kinds of different C in the present embodiment 1, are adopted
2f
6flow, is respectively 100 sccm, 300 sccm, and 500 sccm, gained film is called after sample 1, sample 2, sample 3 respectively.
embodiment 2
In PECVD process, underlayer temperature is 200 DEG C, and in reaction chamber, operating pressure is 3 Torr, and deposition power is 300 W.Reaction raw materials is TEOS and LIMO, the two flow-rate ratio is that 1:1.25(flux unit is gram/minute), they are carrier gas by helium respectively after 160 DEG C and 100 DEG C of vaporizations, are directed in reaction chamber, and required carrier gas flux is respectively 2000 sccm and 5000 sccm.Then, by deposited film at nitrogen (N
2) carrying out thermal anneal process under atmosphere, air pressure is about 1 atmospheric pressure, and nitrogen flow is about 1 L/min, and annealing temperature is 450 DEG C, and annealing time is 2 h.The film obtaining is not fluorine-containing porous membrane, as a comparison sample.
In order to obtain the electric property of above-mentioned film, the present invention is taking low-resistivity silicon chip (resistivity is as 0.001 ~ 0.005 Ω cm) as substrate, and using the aluminium of electron beam evaporation as top electrode material, wherein top electrode is the circular electrode of diameter 400 μ m.By to aluminium/low
kdielectric constant is extracted in the measurement of capacitance-voltage (C-V) curve of film/silicon substrate/aluminium (MISM) structure, and obtains average dielectric constant values by multi-point sampler.Obtain the leakage current characteristic of film by the measurement to current-voltage (I-V) curve.In order to get rid of the impact of physical absorption water on thin-film electro performance, before test, first sample is placed in to N
2/ H
2in atmosphere, under 400 DEG C of conditions, carry out the annealing in process of 30min, then at 100 DEG C, carry out electric performance test.Adopting nano-indenter test to obtain the mechanical property (Young's modulus and hardness) of film, is 600 nm left and right for the film thickness of nano-indenter test, and compression distance is film thickness 1/10.
Fig. 1 is different C
2f
6the infrared spectrogram of the film that traffic income arrives, 1140 cm
-1near have an obvious acromion, derive from the absorption of vibrations of cage modle Si-O-Si, show the existence of film mesopore.Along with C
2f
6the increase of flow, 941 cm
-1near the absorption peak strength of the Si-F of sign key increases, and shows that the incorporation of F element in film increases; Meanwhile, Si-O-Si absworption peak moves to high wave number direction, and this has also shown that mixing of more F causes the increase of Si-O bond strength.Table 1 has been listed in embodiment 1 performance of sample in sample and embodiment 2, can find out and in reaction chamber, introduce C
2f
6can reduce the k value of gained film.Work as C
2f
6flow during for 300sccm the k value of the film that obtains minimum, reach 2.37, and leakage current density is very little.In addition, this sample (sample 2 in embodiment 1) also has the Young's modulus being better than in embodiment 2, and close hardness, as shown in table 2.Fig. 2 is the dielectric constant (k) of sample 2 and the relation curve of voltage, has shown that k value is between 2.36 ~ 2.38.Fig. 3 is the leakage current density of sample 2 and the relation of extra electric field in embodiment 1, and in the time that electric field strength is 1.5MV/cm, its leakage current density is still 10
-8a/cm
2the order of magnitude.
Table 1
Table 2
| Sample | C 2F 6Flow (sccm) | Young's modulus (GPa) | Hardness (GPa) |
| Embodiment 2 | 0 | 6.65 | 0.59 |
| Embodiment 1 | 300 | 7.28 | 0.51 |
Claims (2)
1. a preparation method for fluorine-containing porous low dielectric constant laminated film, is characterized in that: using TEOS and LIMO as liquid source presoma, with C
2f
6as fluorine source, adopt pecvd process deposition, concrete steps are as follows:
(1) wafer is placed in to the reaction chamber of PECVD, reaction cavity is vacuumized, make chamber pressure be less than 0.02 Torr; Then, by heating system, substrate is heated to 150 ~ 300 DEG C, and remains stable;
(2) in reaction cavity, pass into presoma TEOS and LIMO, both flows are 0.1 ~ 2 g/min; First adopt vaporizer to make presoma vaporization, wherein the vapourizing temperature of TEOS is 120 ~ 160 DEG C, and the vapourizing temperature of LIMO is 60 ~ 100 DEG C; Then use carrier gas that precursor vapor is transported to reaction chamber from different gas circuits, the carrier gas flux of wherein carrying TEOS steam is 500 ~ 5000 sccm, and carrying the carrier gas flux of LIMO steam is 1000 ~ 8000 sccm; Wherein, TEOS is tetraethoxysilane, and LIMO is dipentene;
(3) in reaction cavity, pass into C through independent pipeline
2f
6gas, flow is 10 ~ 2000 sccm;
(4) carry out plasma-reinforced chemical and deposit mutually, in deposition process, technological parameter is respectively: radio-frequency power 100 ~ 700 W; Operating pressure 1 ~ 8 Torr in reaction chamber; Upper and lower polar plate spacing 10 ~ 20 mm, obtain fluorine-containing inorganic-organic hybrid film;
(5) PECVD is deposited to the inorganic-organic hybrid film obtaining and be placed in tube furnace, box type furnace or other cavitys, carry out thermal anneal process, annealing temperature is 400 ~ 600 DEG C, annealing time is 0.5 ~ 4 hour, annealing atmosphere is argon gas, helium or nitrogen, pressure is 0.1 ~ 800 Torr, obtains thus fluorine-containing porous low dielectric constant laminated film.
2. the fluorine-containing porous low dielectric constant laminated film being prepared by preparation method described in claim 1, wherein, inorganic constituents is mainly Si-O-Si structure, and organic principle is mainly CHx group; F is mainly combined with Si, is present in film with the form of Si-F key; Its dielectric constant is 2.3 ~ 2.8, and the leakage current density under 1 MV/cm field intensity is 10
-8~ 10
-9a/cm
2in scope, Young's modulus is 6 ~ 9 GPa, and hardness is 0.5 ~ 1.0 GPa.
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| CN101651131B (en) * | 2009-09-17 | 2011-11-02 | 复旦大学 | Low dielectric constant insulating film and preparation method thereof |
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Non-Patent Citations (1)
| Title |
|---|
| YE CHAO ET AL: "Effect of F- and CH-Doped on Dielectric Properties of SiCOH Films Deposited by Decamethylcyclopentasiloxane Electron Cyclotron Resonance Plasma", 《CHINESE PHYSICS LETTERS》 * |
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