CN104008997A - Ultra-low dielectric constant insulating film and manufacturing method thereof - Google Patents
Ultra-low dielectric constant insulating film and manufacturing method thereof Download PDFInfo
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- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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Abstract
The invention discloses an ultra-low dielectric constant insulating film and a manufacturing method thereof. The method comprises the steps that first, a film is deposited by a technology that plasma enhances chemical vapor deposition, wherein MTES and LIMO are used as reaction sources, helium is used as carrier gas to be led into a chemical vapor deposition reaction cavity, a 50-100 nm insulating layer is formed through deposition, and the flow ratio of the NTES and the LIMO is equal to 1:1 - 1:2.5; second, Ar plasma is used for conducting in-situ remediation on the surface of the insulating layer to form a compact modified layer; third, the first step and the second step are executed again to obtain the insulating film of the target thickness; fourth, the insulating film is subjected to high temperature annealing to form the ultra-low dielectric constant insulating film. According to the ultra-low dielectric constant insulating film and the manufacturing method thereof, the method that alternative plasma is used for enhancing the chemical vapor deposition insulating film and a post-plasma processing method are creatively used, the process is simple, the deposition speed is high, the formed film has good moisture resistance and is compatible with an integrated technique, the film forming quality is good, and the demands for the electrical property, the mechanical property and the insulating property of low dielectric constant materials of an integrated circuit can be fully met.
Description
Technical field
The invention belongs to very lagre scale integrated circuit (VLSIC) (ULSI) field of interconnect technologies, be specially for filling the preparation method of the low dielectric constant insulating film between interconnecting metal layer.
Background technology
Along with device size is constantly reduced to deep-submicron, just require to adopt multilayer interconnect structure, so that the time delay producing due to dead resistance (R) and electric capacity (C) minimizes.Due to the increase of RC time delay, the gain of the device speed obtaining on grid is offset by the propagation delay between metal interconnecting wires; Referring to Liu Ming, Liu Yuling, Liu Bo etc. " low k dielectric and copper-connection integrated technique " .[J]. < < micro-nano electronic technology > >, 2006,10 (6): 464-469.In order to reduce the RC constant in ULSI circuit, need interconnection material to there is the low electric capacity between low-resistivity and rete.As everyone knows,
, wherein
be dielectric constant, A is area, and d is dielectric film layer thickness, dielectric long number
equal k and ε
0product, ε
0for the dielectric constant of vacuum, k is relative dielectric constant.Consider low electric capacity situation, by increase dielectric layer thickness (causing that gap-fill is more difficult) or reduce conductor thickness and area (causing resistance to increase) to reduce parasitic capacitance be more difficult.So this just requires material to have lower dielectric constant, produces thus the demand to advanced low-k materials.
Very lagre scale integrated circuit (VLSIC) development, requiring to adopt the lower material of dielectric constant is the dielectric film of k<2.6, yet the dielectric constant of material is main and the total polarizability of material and the density dependent of material, obtain at present ultra-low dielectric constant material and mainly by introduce hole (dielectric constant approximates 1) in dielectric matrix, realize, this is main because introduce the density that hole can effectively reduce material itself.According to document both domestic and external (as, the research [J] of the In search of low-k dielectrics. low-k dielectric constants such as Miller R.D. Miller R.D.. < < Science science > >, 1999, 286(5439): 421-423) and Chinese patent (Ding Shijin etc., " a kind of porous ultra-low dielectric constant material film and preparation method thereof ", publication number CN 101789418 A) report, hole in porous film material normally adds template in presoma, by heat treatment method, remove template again, thereby acquisition porous film material.The method for example, the people such as Shen be take tetraethoxysilane (TEOS) as silicon source, softex kw (CTAB) is template, under acid condition, adopt sol-gel method to prepare porous film material, aperture is 4nm, dielectric constant is 2.5(list of references J. Shen, A. Luo, L. F. Yao, et al. Low dielectric constant silica films with ordered nanoporous structure [J]. Materials science and Engineering, 2007,27 (5-8): 1145-1148).But the preparation method of the low dielectric constant films of mentioning in above-mentioned patent " a kind of porous ultra-low dielectric constant material film and preparation method thereof " is spin coating (spin-coating) film forming, film prepared by spin coating method exists quality of forming film poor more, the first-class problem of uneven thickness, therefore modern lsi technology has not adopted spin coating method to prepare film substantially, but plasma enhanced chemical vapor deposition (plasma enhanced chemical vapor deposition, the PECVD) method that adopts the present invention to mention.The spin coating method of comparing, utilizes PECVD technology to prepare low dielectric constant films and has uniformity and reproducible, can large area film forming, and Step Coverage is good.In addition, thin film composition and thickness are easy to control, and the scope of application is wide, and device simple, is easy to industrialization, and efficiency is high and cost is low.
Since people's reported first PECVD technology such as calendar year 2001 Grill have been prepared low-k porous film material, there is successively in the world relevant bibliographical information, as shown in table 1:
Table 1. PECVD method is prepared low-k porous film material
List of references 5:R. Navamathavan, C. K. Choi. Plasma enhanced chemical vapor deposition of low dielectric constant SiOC (H) films using MTES/O
2precursor [J], Thin Solid Films, 2007,515 (12): 5040-5044.
List of references 6:Grill Alfred. Plasma enhanced chemical vapor deposited SiCOH dielectrics:from low-k to extreme low-k interconnect materials [J], Journal of Applied Physics, 2003,93 (3): 1785-1790.
List of references 7:S.-K. Kwak, K.-H. Jeong, S.-W. Rhee et al., Nanocomposite Low-k SiCOH Films by Direct PECVD Using Vinyltrimethylsilane [J]. Journal of the Electrochemical Society, 2004,151 (2): F11-F16.
As shown in table 1, in document 5 and 7, report adopts respectively MTES+O
2and VTMS+O
2for presoma, under different temperatures, utilize PECVD deposition techniques film, final annealing temperature is respectively 500 ℃ and 450 ℃, yet so high annealing temperature condition can not meet the thermal stability requirement (≤420 ℃) of common integrated circuit postchannel process to advanced low-k materials.Document 6 adopt heat treatment methods to remove pore formers to obtain dielectric constant be 2.05 thin-film material, but mechanical property is undesirable, is difficult to meet the requirement of technique bound pair thin-film material.Utilization of the present invention has the MTES of novelty and the mixing presoma of LIMO, the method that adopts innovatively alternative P ECVD insulation film and post plasma to process, soon insulating layer deposition step and compacted zone formation step hocket, it is strong that the film forming has resistance to water soak, mechanical property is good, Thin-film anneal temperature is low, with the integrated technique advantage such as compatible mutually.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of ultralow dielectric insulation film, the insulation film of preparing by the method has desirable electric property and mechanical property, can be used for great scale integrated circuit field of interconnect technologies.
In order to achieve the above object, the invention provides a kind of preparation method of ultralow dielectric insulation film, the method comprises following concrete steps:
Step 1, utilize plasma enhanced chemical vapor deposition deposition techniques film: take methyl triethoxysilane and citrene as reaction source, and methyl triethoxysilane and citrene all be take helium and are directed in chemical vapour deposition reaction chamber as carrier gas, deposition forms the insulating barrier of 50-100nm, wherein, flow-rate ratio=1:1 ~ the 1:2.5 of methyl triethoxysilane and citrene, this flow is in gram/minute;
Step 2, in above-mentioned cavity, adopt Ar or He plasma to carry out in-situ treatment 1-5 minute to surface of insulating layer, form fine and close decorative layer, the effect of this decorative layer is to stop hydrone diffusion from top to bottom in whole insulating barrier, thereby reduced the absorption of above-mentioned insulating barrier mesopore to water, contained that water suction causes the rising of dielectric constant;
Step 3, repeats above-mentioned steps 1 and 2, until reach the target thickness of insulation film, obtains insulation film;
Step 4, in inert atmosphere, the insulation film that step 3 is obtained carries out high annealing, removes hydrocarbon group wherein (this hydrocarbon group comprise hydrocarbon group in precursor and the hydrocarbon group in citrene), thereby forms a kind of ultralow dielectric insulation film with loose structure.
Above-mentioned method, wherein, the rf frequency that depositing operation in step 1 is used is 13.56MHz, in reaction cavity, initial vacuum is 0.018-0.02 holder, and underlayer temperature during depositing insulating layer is 100-400 ℃, and power is 200-600 watt, operating pressure is 2-5 holder (1 holder=133.322Pa), importing MTES flow in reaction chamber is 1.0-2.0 gram/minute, and LIMO flow is 1.0-3.5 gram/minute, and He carrier gas flux is 500-5000sccm.
Above-mentioned method, wherein, in step 2, when Ar or He plasma surface treatment, power is 300-600 watt, and the processing time is 1-5 minute, and air pressure is 2-8 holder.
Above-mentioned method, wherein, in step 4, annealing temperature is 200-420 ℃, and the pressure in annealing furnace is 0.2-0.3 holder, and annealing time is 2-6 hour, and annealing atmosphere is argon gas or nitrogen.Preferably, in above-mentioned annealing process, by room temperature, rise to described annealing temperature in 5-30 minute.
Above-mentioned method, wherein, described methyl triethoxysilane and the citrene vapourizing temperature before importing reaction cavity is respectively 50-60 ℃ and 60-100 ℃.
The present invention also provides a kind of ultralow dielectric insulation film that adopts above-mentioned method to prepare, and wherein, this insulation film comprises: some layer insulatings; On this every layer insulating, be provided with decorative layer, in insulating barrier inside, there are some holes; This ultralow dielectric insulation film dielectric constant is 2.2-2.4, and the leakage current density when 1MV/cm is 10
-9-10
-8a/cm
2; Young's modulus is 4.2-17GPa, and hardness is 0.5-1.3GPa.
The preparation method of ultralow dielectric insulation film provided by the invention is that to take respectively MTES and LIMO be reaction source, importing reaction cavity under the carrying of He carrier gas, using plasma strengthens chemical vapour deposition technique deposition and forms insulating barrier, then adopt argon gas (Ar) or helium (He) plasma to carry out in-situ treatment to aforementioned dielectric layer surface, form fine and close decorative layer, repeat said process until reach the film of required thickness, finally this film is placed under high temperature and is annealed, to remove hydrocarbon group, thereby form ultralow dielectric porous insulation film.
Film provided by the present invention adopts reaction source MTES and the LIMO with novelty, simple and easy to get, use safety, accessory substance environmentally safe, the thin-film dielectric constant of preparation, within the scope of 2.2-2.4, also has more excellent mechanical characteristic when meeting ultralow dielectric.In addition, film also has good insulation property, and under the external electric field of 1MV/cm, leakage current density can reach 10
-9-10
-8a/cm
2.Therefore, the prepared ultralow dielectric insulation film of the present invention can fully meet the requirement of Advanced Integrated Circuits to the electric property of advanced low-k materials, mechanical property and insulation property.
In addition, method for manufacturing thin film provided by the invention adopts alternately plasma enhanced chemical vapor deposition innovatively, and the film of formation has good resistance to water soak, mechanical property is better, and compatible mutually with integrated technique, not only technique is simple, deposition rate is fast, and quality of forming film is good.
Accompanying drawing explanation
Fig. 1 a-1d is the preparation process schematic diagram of ultralow dielectric insulation film of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail.In the drawings, for convenience of description, zoomed in or out the size in different layers and region, shown in size do not represent actual size, do not reflect the proportionate relationship of size yet.
Using plasma of the present invention strengthens chemical vapour deposition technique and prepares ultralow dielectric insulation film, and the helium (He) of take is carrier gas, respectively by presoma methyl triethoxysilane (C
7h
18o
3si, is called for short MTES) and pore former citrene (C
10h
16abbreviation LIMO) bring deposition in plasma enhanced chemical vapor deposition reaction cavity into and form insulating barrier, the rf frequency that plasma enhanced chemical vapor deposition technique is used is 13.56MHz, in reaction cavity, initial vacuum is 0.018 ~ 0.02 holder, underlayer temperature is 100 ~ 400 ℃, deposition power is 200 ~ 600 watts, and operating pressure is 2 ~ 5 holders, and He carrier gas flux is 500 ~ 5000sccm(standard-state cubic centimeter per minute).MTES and the LIMO vapourizing temperature before importing reaction cavity is respectively 50 ~ 60 ℃ and 60 ~ 100 ℃, MTES flow is 1.0-2.0g gram/minute, LIMO flow is 1.0-3.5 gram/minute, ratio is 1:1-1:2.5, deposit thickness is 50-100nm, form insulating barrier 10 as shown in Figure 1a, this insulating barrier 10 consists of Si-O-Si structure 11 and hydrocarbon group 12.
In above-mentioned cavity, adopt Ar or He plasma to carry out in-situ treatment to form fine and close decorative layer 20(as shown in Figure 1 b to surface of insulating layer), power is 300-600 watt, and the processing time is 1-5 minute, and air pressure is 2-8 holder.The effect of this decorative layer 20 is the outer surfaces that seal insulating barrier 10, prevents the hole water suction that the interior annealing of insulating barrier 10 forms.
Thereby repeat respectively the insulation film that above-mentioned two steps reach target thickness, as shown in Fig. 1 c, formed the insulation film 30 that 3 minor insulation layer-decorative layers are arranged alternately.
Above-mentioned target insulation film 30 is placed in to annealing furnace, Ar or N
2under atmosphere, annealing furnace pressure is 0.2-0.3 holder, in 5-30 minute, by room temperature, rise to annealing temperature, 2-6 hour anneals under 200-420 ℃ of condition, remove hydrocarbon group, some these holes 13 of irregular hole 13(of the inner formation of insulating barrier at insulation film comprise some vermiforms hole and some irregular circular holes), the final ultralow dielectric insulation film with loose structure that obtains, as shown in Figure 1 d.
Film performance is measured: in order to measure the electric property of above-mentioned film, it is substrate that low resistance silicon chip (resistivity is 0.001-0.02 Ω cm) is take in the present invention, the aluminium of electron beam evaporation of take forms circular metal electrode that diameter is 400-420 micron to form capacitor on film, thereby obtains metal-insulator semiconductor (being called for short MIS) capacitance structure.At room temperature above-mentioned capacitor is measured electric capacity based on capacitance-voltage characteristics, and obtains reliable average electrical capacitance by multi-point sampler, considers that the area of electrode and film thickness determine dielectric constant simultaneously.In addition by the measurement to current-voltage, obtain, the leakage current characteristic of film.By nano-hardness tester, obtain hardness and the Young's modulus of film.
In embodiment 1-6, by changing the relative discharge of methyl triethoxysilane and citrene, 7 kinds of different film samples (that is, being numbered the sample of 1-6) have been prepared, table 2 has been listed at different flow than the electric property of the sample of preparing under condition, mechanical property and leakage current.Along with relative discharge increases gradually, dielectric constant and mechanical property thereof all show the trend that first reduces rear increase.As can be seen from Table 2, the lowest dielectric constant of gained film is 2.2, refractive index is 1.309, mechanical property aspect, hardness is 0.55GPa, Young's modulus is 4.23GPa, reaches the general level of the porous low dielectric constant films mechanical property of bibliographical information, and other samples have also shown good mechanical property in addition.Leakage current density is also less simultaneously, shows good insulation property.Therefore, can meet the requirement of integrated circuit technology of future generation to low dielectric constant material film.
Deposition rate, electric property, mechanical property and the leakage current of subordinate list 2. samples
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Those skilled in the art, read after foregoing, for multiple modification of the present invention with to substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (7)
1. a preparation method for ultralow dielectric insulation film, is characterized in that, the method comprises following concrete steps:
Step 1, utilize plasma enhanced chemical vapor deposition deposition techniques film: take methyl triethoxysilane (MTES) and citrene (LIMO) is reaction source, and methyl triethoxysilane and citrene all be take helium and are formed insulating barrier as carrier gas is directed in chemical vapour deposition reaction chamber, thickness is 50-100nm, wherein, the flow-rate ratio of methyl triethoxysilane and citrene is 1:1 ~ 1:2.5, and this flow is in gram/minute;
Step 2 adopts Ar or He plasma to carry out in-situ treatment to form fine and close decorative layer to surface of insulating layer in above-mentioned cavity, and plasma treatment time is 1-5 minute;
Step 3, repeats above-mentioned steps 1 and 2, until reach the target thickness of insulation film, obtains insulation film;
Step 4, in inert atmosphere, the insulation film that step 3 is obtained carries out high annealing, removes hydrocarbon group wherein, thereby forms a kind of ultralow dielectric insulation film with loose structure.
2. the method for claim 1, it is characterized in that, the rf frequency that depositing operation in step 1 is used is 13.56MHz, in reaction cavity, initial vacuum is 0.018-0.02 holder, and underlayer temperature during depositing insulating layer is 100-400 ℃, and power is 200-600 watt, operating pressure is 2-5 holder, importing MTES flow in reaction chamber is 1.0-2.0 gram/minute, and LIMO flow is 1.0-3.5 gram/minute, and He carrier gas flux is 500-5000sccm.
3. the method for claim 1, is characterized in that, in step 2, when Ar or He plasma surface treatment, power is 300-600 watt, and the processing time is 1-5 minute, and air pressure is 2-8 holder.
4. the method for claim 1, is characterized in that, in step 4, annealing process is: annealing temperature is 200-420 ℃, and the pressure in annealing furnace is 0.2-0.3 holder, and annealing time is 2-6 hour, and annealing atmosphere is argon gas or nitrogen.
5. method as claimed in claim 4, is characterized in that, in above-mentioned annealing process, rises to described annealing temperature in 5-30 minute by room temperature.
6. the method for claim 1, is characterized in that, described methyl triethoxysilane and the citrene vapourizing temperature before importing reaction cavity is respectively 50-60 ℃ and 60-100 ℃.
7. a ultralow dielectric insulation film that adopts method claimed in claim 1 to prepare, is characterized in that, this insulation film comprises: some layer insulatings (10); On this every layer insulating (10), be provided with decorative layer (20), in insulating barrier (10) inside, there are some holes (13); This ultralow dielectric insulation film dielectric constant is 2.2-2.4, and the leakage current density when 1MV/cm is 10
-9-10
-8a/cm
2; Young's modulus is 4.2-17GPa, and hardness is 0.5-1.3GPa.
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|---|---|---|---|
| CN201410243600.0A CN104008997A (en) | 2014-06-04 | 2014-06-04 | Ultra-low dielectric constant insulating film and manufacturing method thereof |
| PCT/CN2014/000708 WO2015184573A1 (en) | 2014-06-04 | 2014-07-28 | Ultra-low dielectric constant insulating film and method for manufacturing same |
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| CN104498900A (en) * | 2014-12-23 | 2015-04-08 | 上海爱默金山药业有限公司 | Preparation method of low-dielectric-constant thin film |
| TWI675124B (en) * | 2014-09-12 | 2019-10-21 | 美商蘭姆研究公司 | Systems and methods for reducing backside deposition and mitigating thickness changes at substrate edges |
| CN115522180A (en) * | 2022-09-20 | 2022-12-27 | 苏州源展材料科技有限公司 | Preparation method and application of silicon-based thin film with low dielectric constant |
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|---|---|---|---|---|
| TWI675124B (en) * | 2014-09-12 | 2019-10-21 | 美商蘭姆研究公司 | Systems and methods for reducing backside deposition and mitigating thickness changes at substrate edges |
| TWI682062B (en) * | 2014-09-12 | 2020-01-11 | 美商蘭姆研究公司 | Systems and methods for reducing backside deposition and mitigating thickness changes at substrate edges |
| CN104498900A (en) * | 2014-12-23 | 2015-04-08 | 上海爱默金山药业有限公司 | Preparation method of low-dielectric-constant thin film |
| CN115522180A (en) * | 2022-09-20 | 2022-12-27 | 苏州源展材料科技有限公司 | Preparation method and application of silicon-based thin film with low dielectric constant |
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