CN103646913A - Method for improving moisture-absorption-resistance performance of ultra-low-dielectric-constant porous SiCOH film - Google Patents

Method for improving moisture-absorption-resistance performance of ultra-low-dielectric-constant porous SiCOH film Download PDF

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CN103646913A
CN103646913A CN201310565850.1A CN201310565850A CN103646913A CN 103646913 A CN103646913 A CN 103646913A CN 201310565850 A CN201310565850 A CN 201310565850A CN 103646913 A CN103646913 A CN 103646913A
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film
low
ultra
sicoh
moisture absorption
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丁士进
蒋涛
张卫
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Fudan University
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Fudan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—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.
    • H01L21/76825—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc. by exposing the layer to particle radiation, e.g. ion implantation, irradiation with UV light or electrons etc.

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Abstract

The invention discloses a method for improving moisture-absorption-resistance performance of an ultra-low-dielectric-constant porous SiCOH film. In the method, at an environment temperature, the ultra-low-dielectric-constant porous SiCOH film with a k value of 1.6 to 2.0 is placed under ultraviolet light so as to be irradiated so that the moisture-absorption-resistance performance is improved, wherein the wavelength range of the ultraviolet light is 200 to 400 nm, the temperature environment is 50 to 100 DEG C and the irradiation time is 2 to 10 hours. Through the processing, the moisture-absorption-resistance performance of the film can be improved obviously without affecting other properties of the film and at a normal temperature, when the film is placed statically for more than 12 hours in an environment with humidity of 80%, the k value only rises by 1-5%. The method is not only capable of improving the hydrophobic performance of the film, but also capable of improving the mechanical performance (Young modulus and hardness) and electricity leakage performance of the film; and the method is simple in operation process, great in controllability and low in cost. The SiCOH film obtained through the method has a low enough dielectric constant (k (2.0)) and meets properties required by an integrated-circuit interconnection process and the method is compatible well with an interconnection process under a 22nm feature size.

Description

A kind of method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property
Technical field
The invention belongs to integrated circuit interconnection media processes field under 22nm characteristic size condition, be specifically related to a kind of method of improving ultra-low dielectric constant material porous SiCOH ultra-low-k film anti-moisture absorption property.
Background technology
Development along with very lagre scale integrated circuit (VLSIC) (ULSI), device feature size constantly dwindles, interconnection resistance-electric capacity (RC) late effect has seriously limited the raising of device performance, in order to reduce RC, postpones, and need to adopt low-k (k) material to replace traditional Si O 2as connected medium material, SiCOH material, because it is easy to preparation and has lower dielectric constant, has become the optimal selection of the following technology node connected medium of 90nm at present.Yet, along with constantly reducing of characteristic size, need in material, introduce hole further to reduce dielectric constant, can bring thus the problem of many material property reliabilities, such as anti-moisture-absorption characteristics, mechanical characteristic, thermal stability etc.When ULSI characteristic size enters 22nm when following, advanced low-k materials properties is had higher requirement.Wherein, anti-moisture absorption property has directly affected the practical application of advanced low-k materials.Nowadays all can there is a certain amount of hydrophilic Si-OH key at surf zone in the standby porous SiCOH ultra-low-k film material of majority system, exposes and can absorb rapidly moisture in a humid environment; On the other hand, due to the introducing of a large amount of holes, moisture is easy to be penetrated in material and goes, and causes the increase of moisture to thin film physics adsorption capacity, causes k value to increase considerably.Therefore,, not changing on the basis of original dielectric property and other performances, the anti-moisture absorption property of film is improved and just seems extremely important.
Summary of the invention
In view of above technical problem, the object of the invention is to propose a kind of method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, and the film after the method is processed can demonstrate excellent anti-moisture absorption property.
In order to achieve the above object, the invention provides a kind of method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, the ultralow dielectric porous SiCOH ultra-low-k film that the method is is 1.6-2.0 by k value, at ambient temperature, be placed under ultraviolet light and irradiate, to improve the anti-moisture absorption property of film, wherein, ultraviolet wavelength scope is 200-400nm, and ambient temperature is 50-100 ℃, and irradiation time is 2-10 hour.By ultraviolet irradiation, process, the anti-moisture absorption property of film significantly improves, the above k value of the standing 12h 1-5% that only rises in the environment that is 80% in humidity under normal temperature.
The above-mentioned method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, wherein, described irradiation time is 2-10 hour.
The above-mentioned method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, wherein, described ultralow dielectric porous SiCOH ultra-low-k film has the structure of Al-SiCOH-Si-Al, this structure is that the upper surface at silicon substrate is provided with SiCOH thin layer, at the lower surface of silicon substrate and thin layer upper surface deposit Al electrode respectively.
The above-mentioned method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, wherein, the preparation method of described ultralow dielectric porous SiCOH ultra-low-k film comprises:
Step 1, for presoma, take block copolymer P123 as pore former with 1,2-bis-(triethoxy is silica-based) ethane, take watery hydrochloric acid as catalyst, and adds ethanol as solvent, is placed in the oil bath continuous stirring 1-5 hour of 40-80 ℃, obtains transparent film forming liquid; The mol ratio of above-mentioned each component is: 1,2-bis-(triethoxy is silica-based) ethane: P 123: H 2o: HCl: EtOH=(3-10): (0.02-0.15): (100-300): (0.09-0.5): (70-250);
Step 2, by above-mentioned film forming drop to clean silicon chip, spin-coating film;
Step 3, is first placed in baking oven ageing 20-100h under 40-100 ℃ of condition by above-mentioned gained film, is then placed in annealing furnace, passes into nitrogen, slowly rises to 350 ℃-600 ℃, and keep 1h by room temperature, is finally slowly down to room temperature;
Step 4, the method for employing electron beam evaporation, at the film upper surface of step 3 gained and the Al electrode of the above thickness of substrate lower surface difference deposit one deck 500nm, forms the structure of Al-SiCOH-Si-Al.
The above-mentioned method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, wherein, described spin-coating film process is divided into three phases: the first stage, with the rotating speed rotation 5-15s of 500-800 rpm; Second stage, with the rotating speed rotation 20-45s of 1500-3000 rpm; Phase III, with the rotating speed rotation 5-15s of 800-1500 rpm.
The present invention has the following advantages:
(1) method proposed by the invention, can effectively improve the anti-moisture absorption property of porous SiCOH ultra-low-k film, and does not affect other performances of film, such as stability, dielectric constant etc.;
(2) the resulting ultralow dielectric SiCOH of the method film that the present invention proposes, there is enough low dielectric constant (k<2.0) and meet the desired performance of integrated circuit interconnection technique (thermal stability, leakage current characteristic and mechanical property), thus can be well with 22nm characteristic size under interconnection process compatible mutually;
(3) method proposed by the invention, not only can improve the hydrophobic performance of film, can also improve mechanical property (Young's modulus and hardness) and the electric leakage performance of film;
(4) procedure proposed by the invention is simple, easy to operate, controllability is good, cost is low.
Accompanying drawing explanation
Fig. 1 is the hygroscopic sample structure schematic diagram of ultralow dielectric porous SiCOH ultra-low-k film that the present invention studies.
Fig. 2 is that before ultraviolet is processed, the dielectric constant values before and after film sample moisture absorption changes.
Fig. 3 is the variation of film moisture absorption front and back leak current characteristics before ultraviolet is processed.
Fig. 4 is that the dielectric constant values before and after ultraviolet of the present invention is processed rear film moisture absorption changes.
Fig. 5 processes the variation of rear film moisture absorption front and back leak current characteristics through ultraviolet of the present invention.
Embodiment
The preparation method of ultralow dielectric porous SiCOH ultra-low-k film of the present invention comprises:
Step 1, for presoma, take block copolymer P123 as pore former with 1,2-bis-(triethoxy is silica-based) ethane, take watery hydrochloric acid as catalyst, and adds ethanol as solvent, is placed in the oil bath continuous stirring 1-5 hour of 40-80 ℃, obtains transparent film forming liquid; The mol ratio of above-mentioned each component is: 1,2-bis-(triethoxy is silica-based) ethane: P 123: H 2o: HCl: EtOH=(3-10): (0.02-0.15): (100-300): (0.09-0.5): (70-250);
Step 2, by above-mentioned film forming drop to clean silicon chip, spin-coating film;
Step 3, is first placed in baking oven ageing 20-100h under 40-100 ℃ of condition by above-mentioned gained film, is then placed in annealing furnace, passes into nitrogen, slowly rises to 350 ℃-600 ℃, and keep 1h by room temperature, is finally slowly down to room temperature;
Step 4, the method for employing electron beam evaporation, at the film upper surface of step 3 gained and the Al electrode of the above thickness of substrate lower surface difference deposit one deck 500nm, forms the structure of Al-SiCOH-Si-Al.
Below in conjunction with embodiment and accompanying drawing, method of the present invention is described further.
Embodiment 1
Be to adopt a proposed by the invention embodiment who improves ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property below, concrete steps are as follows:
(1) p type single crystal silicon (100) of getting a low-resistance is as substrate, and the column criterion of going forward side by side RCA technique is cleaned, and with HF, removes the oxide layer of silicon chip surface;
(2) by presoma (EtO) 3si-CH 2-CH 2-Si (OEt) 3(producer source is Gelest.inc), pore former P 123(producer source is IGMA-Aldrich), hydrochloric acid, second alcohol and water mix, and the oil bath that then said mixture is placed in to 60 ℃ is stirred 2 hours, obtains sol solution.In said mixture, the mol ratio of material is: (EtO) 3si-CH 2-CH 2-Si (OEt) 3: P 123: HCl:H 2o:EtOH=0.5:0.8 * 10 -2: 1.8 * 10 -2: 20:13.9;
(3) above-mentioned sol solution is at room temperature spun on the silicon chip through standard RCA cleaning.Wherein, in order to obtain evenly smooth film, rotary course is divided into three control stages: with the rotating speed rotation 10s of 800 rpm; Rotating speed rotation 30s with 2500 rpm; Rotating speed rotation 10s with 1000 rpm;
(4) first above-mentioned gained film is placed in to baking oven ageing 65h under 60 ℃ of conditions, is then placed in annealing furnace, pass into nitrogen, by room temperature, slowly rise to 350 ℃, and keep 1h, be finally slowly down to room temperature; For further investigating the thermal stability of film, gained film is placed in to annealing furnace additional annealing 30min under 500 ℃ of conditions;
(5) adopt the method for electron beam evaporation, at the Al electrode of silicon chip back difference deposit one deck 500nm thickness of being processed by the resulting film surface of step (4) and process HF.Wherein, in order accurately to measure the capacitive surface density of film, film surface covered the mask plate that one deck has even regular pattern before deposition of electrode, then grew the electrode with regular pattern.The test structure of formed film sample (being Al-SiCOH-Si-Al structure) as shown in Figure 1, is used for the electric property of testing film, as capacitance-voltage (C-V) characteristic, current-voltage (I-V) characteristic.Meanwhile, using this structure as the hygroscopic sample of research ultralow dielectric porous SiCOH ultra-low-k film.
(6) will be placed at normal temperatures humidity by the resulting film of step (5) is 80% environment humidifying 15h, then measures the electric property after humidifying;
(7) will be placed under wide range uviol lamp and irradiate by the resulting film of step (5).Wherein wave-length coverage used is 200-400nm during ultra violet lamp, and irradiation time is 5h, and during irradiation, ambient temperature is 50 ℃, and irradiation atmosphere is atmospheric atmosphere, then measures the electric property that irradiates rear film;
(8) will be placed at normal temperatures humidity by the resulting film of step (7) is 80% environment humidifying 15h, then measures the electric property after humidifying.
As shown in Figure 2, shown the variation of the dielectric constant values of the front film moisture absorption of ultraviolet processing front and back.By this figure, can be found out, after the sample humidifying of not processing through ultraviolet, k value increases nearly 12%.
As shown in Figure 3, shown the variation of film moisture absorption front and back leak current characteristics before embodiment 1 ultraviolet is processed.By this figure, can be found out, the leakage current density of humidifying rear film significantly increases, and wherein, in electric field strength, is that in 0.5MV/cm situation, after humidifying, leakage current density is by 1.87 * 10 -9a/cm 2be increased to 2.73 * 10 -8a/cm 2, increased approximately 15 times.
As shown in Figure 4, shown the variation of the dielectric constant values before and after embodiment 1 ultraviolet is processed rear film moisture absorption.As known in the figure, after the sample humidifying of processing through ultraviolet, k value only increases less than 4%.
As shown in Figure 5, having shown the variation of processing rear film moisture absorption front and back leak current characteristics through embodiment 1 ultraviolet, from this figure, is that in 0.5MV/cm situation, after humidifying, leakage current density is by 3 * 10 in electric field strength -10a/cm 2be increased to 1.7 * 10 -9a/cm 2, only increased approximately 5 times.
As shown in table 1 below, listed the variation of film performance under different annealing temperature condition before and after embodiment 1 ultraviolet is processed.Result shows, ultraviolet processing method does not have impact substantially on dielectric constant, stability, and can improve leakage current characteristic and the mechanical property of film.
The film performance that table 1 ultraviolet is processed front and back different annealing temperature changes
Embodiment 2
Step (1)-(6) are with embodiment 1.
Step (7), is placed in the resulting film of step (5) under wide range uviol lamp and irradiates.Wherein wave-length coverage used is 200-400nm during ultra violet lamp, and irradiation time is 2h, and during irradiation, ambient temperature is 100 ℃, and irradiation atmosphere is atmospheric atmosphere, then measures the electric property that irradiates rear film;
Step (8), will be placed at normal temperatures humidity by the resulting film of step (7) is 80% environment humidifying 15h, then measures the electric property after humidifying.
Embodiment 3
Step (1)-(6) are with embodiment 1.
Step (7), is placed in the resulting film of step (5) under wide range uviol lamp and irradiates.Wherein wave-length coverage used is 200-400nm during ultra violet lamp, and irradiation time is 10h, and during irradiation, ambient temperature is 60 ℃, and irradiation atmosphere is atmospheric atmosphere, then measures the electric property that irradiates rear film;
Step (8), will be placed at normal temperatures humidity by the resulting film of step (7) is 80% environment humidifying 15h, then measures the electric property after humidifying.
As following table 2 has been listed the variation of SiCOH film performance parameter before and after moisture absorption under the different ultraviolet processing time conditions of embodiment 1-3.
Table 2 ultraviolet is processed the variation of front and back thin-film hydrophobic performance
Result shows, the sample of processing through ultraviolet its dielectric constant after moisture absorption increases not obvious, reaches 0.22, and leakage current density has also increased approximately order of magnitude.Yet for the sample after ultraviolet is processed, after moisture absorption, its dielectric constant only increases 0.05-0.09, leakage current density has also increased nearly order of magnitude, but the value of leakage current density is very low, lower one more than the order of magnitude than the sample of processing without ultraviolet, reaches 10 -9-10 -10a/cm 2.Above-mentioned experimental result shows, ultraviolet is processed the anti-moisture absorption property that can improve well film, has lower leakage current density when having guaranteed ultralow dielectric.
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 (5)

1. a method of improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property, it is characterized in that, the ultralow dielectric porous SiCOH ultra-low-k film that the method is is 1.6-2.0 by k value, at ambient temperature, be placed under ultraviolet light and irradiate, to improve the anti-moisture absorption property of film, wherein, ultraviolet wavelength scope is 200-400nm, and ambient temperature is 50-100 ℃, and irradiation time is 2-10 hour.
2. the method for improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property as claimed in claim 1, is characterized in that, described irradiation time is 3-6 hour.
3. the method for improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property as claimed in claim 1, it is characterized in that, described ultralow dielectric porous SiCOH ultra-low-k film has the structure of Al-SiCOH-Si-Al, this structure is that the upper surface at silicon substrate is provided with SiCOH thin layer, at the lower surface of silicon substrate and thin layer upper surface deposit Al electrode respectively.
4. the method for improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property as claimed in claim 3, is characterized in that, the preparation method of described ultralow dielectric porous SiCOH ultra-low-k film comprises:
Step 1, for presoma, take block copolymer P123 as pore former with 1,2-bis-(triethoxy is silica-based) ethane, take watery hydrochloric acid as catalyst, and adds ethanol as solvent, is placed in the oil bath continuous stirring 1-5 hour of 40-80 ℃, obtains transparent film forming liquid; The mol ratio of above-mentioned each component is: 1,2-bis-(triethoxy is silica-based) ethane: P 123: H 2o: HCl: EtOH=(3-10): (0.02-0.15): (100-300): (0.09-0.5): (70-250);
Step 2, by above-mentioned film forming drop to clean silicon chip, spin-coating film;
Step 3, is first placed in baking oven ageing 20-100h under 40-100 ℃ of condition by above-mentioned gained film, is then placed in annealing furnace, passes into nitrogen, slowly rises to 350 ℃-600 ℃, and keep 1h by room temperature, is finally slowly down to room temperature;
Step 4, the method for employing electron beam evaporation, at the film upper surface of step 3 gained and the Al electrode of substrate lower surface difference deposit one deck 500nm-1500nm thickness, forms Al-SiCOH-Si-Al structure.
5. the method for improving ultralow dielectric porous SiCOH ultra-low-k film anti-moisture absorption property as claimed in claim 4, is characterized in that, described spin-coating film process is divided into three phases: the first stage, with the rotating speed rotation 5-15s of 500-800 rpm; Second stage, with the rotating speed rotation 20-45s of 1500-3000 rpm; Phase III, with the rotating speed rotation 5-15s of 800-1500 rpm.
CN201310565850.1A 2013-11-14 2013-11-14 Method for improving moisture-absorption-resistance performance of ultra-low-dielectric-constant porous SiCOH film Pending CN103646913A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104022074A (en) * 2014-06-02 2014-09-03 复旦大学 Method for preparing low-dielectric-constant composite film with nanometer holes
CN108447943A (en) * 2018-03-23 2018-08-24 浙江师范大学 Simple and effective store method after a kind of Wafer Cleaning

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US20110263117A1 (en) * 2010-04-27 2011-10-27 Samsung Electronics Co., Ltd. Apparatus for manufacturing semiconductor device and method of manufacturing semiconductor device using the same
US20120083117A1 (en) * 2010-09-30 2012-04-05 Samsung Electronics Co., Ltd. Method Of Forming Hardened Porous Dielectric Layer And Method Of Fabricating Semiconductor Device Having Hardened Porous Dielectric Layer
CN102683275A (en) * 2012-06-08 2012-09-19 复旦大学 Super-low dielectric constant (k) material thin film and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110263117A1 (en) * 2010-04-27 2011-10-27 Samsung Electronics Co., Ltd. Apparatus for manufacturing semiconductor device and method of manufacturing semiconductor device using the same
US20120083117A1 (en) * 2010-09-30 2012-04-05 Samsung Electronics Co., Ltd. Method Of Forming Hardened Porous Dielectric Layer And Method Of Fabricating Semiconductor Device Having Hardened Porous Dielectric Layer
CN102683275A (en) * 2012-06-08 2012-09-19 复旦大学 Super-low dielectric constant (k) material thin film and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104022074A (en) * 2014-06-02 2014-09-03 复旦大学 Method for preparing low-dielectric-constant composite film with nanometer holes
CN104022074B (en) * 2014-06-02 2017-01-11 复旦大学 Method for preparing low-dielectric-constant composite film with nanometer holes
CN108447943A (en) * 2018-03-23 2018-08-24 浙江师范大学 Simple and effective store method after a kind of Wafer Cleaning

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