CN102392216A - Method for preparing high thermal stability double layer diffusion impervious layer material - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000009792 diffusion process Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000004544 sputter deposition Methods 0.000 claims description 21
- 230000004888 barrier function Effects 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- 229910052707 ruthenium Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000013077 target material Substances 0.000 claims description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000005477 sputtering target Methods 0.000 claims description 3
- 238000004501 airglow Methods 0.000 claims description 2
- 238000000137 annealing Methods 0.000 abstract description 8
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- 239000010949 copper Substances 0.000 description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
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- 229910052782 aluminium Inorganic materials 0.000 description 3
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention provides a method for preparing a high thermal stability double layer diffusion impervious layer material. The method is characterized in that a direct current magnetron sputtering process is employed, accurate control of N content in an amorphous TaN film is realized by regulating N air flow rate, a high performance double layer Ru/TaN diffusion impervious layer structure with different N content is prepared, the effective work is stably as high as 650 DEG C. N atoms in gap of the TaN film are diffused during the annealing process and then raise the diffusion impervious performance of the Ru/TaN bilaminar membrane. The thermal stability double layer diffusion impervious layer material can be obtained by accurately controlling the N content, and is capable of keeping excellent electrical performance and better ensuring its practical application. The invention has the advantages of simple operation, good repeatability and good realization effect.
Description
Technical field
The present invention relates to a kind of high thermal stability Ru/TaN bilayer diffusion barrier thin-film material and preparation.
Background technology
Along with advancing by leaps and bounds of science and technology, semiconductor fabrication faces variation with rapid changepl. never-ending changes and improvements.Traditional semiconductor technology mainly adopts aluminium as metal interconnection material (Interconnect), on signal lag (signal delay), is restricted.With respect to aluminium, copper has favorable conductive and electric migration performance, thereby copper has replaced aluminium and becomes main interconnection material in VLSI (ULSI) is made.Briefly, can improve the integrated level of chip as a series of semiconductor fabrication process of metal interconnection material, improve device density, improve clock requency and reduce the energy that consumes with copper.But copper-base is prone on silicon-based substrate, diffuse to form the copper silicon compound, reduces the electric property of device.In order to prevent the diffusion of copper in silica-base material, thus must be between the copper silicon deposition one deck blocking layer, and then the very thin copper seed layer of deposition one deck is as the conducting medium of electro-coppering, also as the crystal nucleation layer of the Metallic Solids growth of electro-coppering.Technology then is that chemical machinery polishes (CMP), mainly is to grind off unnecessary copper, simultaneously silicon chip surface is polished.
Along with the yardstick of semiconducter device is more and more littler, the blocking layer also becomes obvious further to the influence of device electric property in the copper interconnect structures.Widely used Ta base blocking layer is at further obvious of 32nm technology and lower yardstick defective down in the traditional industry.The surface on Ta base blocking layer is comparatively coarse, needs the thicker Cu seed layer of deposition, so that the size of whole copper interconnect structures can't be accomplished is very little.Secondly the resistance on Ta blocking layer has also influenced the electric property of copper interconnect structures greatly.Therefore, how the excellent more barrier material of processability substitutes Ta base blocking layer becomes the technical barrier that needs to be resolved hurrily at present.
Ru receives scholar's extensive concern this year as a kind of emerging barrier material.Ru is the same with Ta have HMP, high-temperature stability and and Cu good characteristics such as chemical reaction do not take place.In addition, Ru also has the not available good characteristic of Ta.Its body resistivity of Ru is 7.6 μ Ω cm, approximately is the half the of Ta resistivity, and the what is more important surfaceness of Ru in process of production obviously is superior to Ta, and can be on the Ru layer Direct Electroplating Cu and do not need to deposit in advance Cu seed layer.This advantage has reduced technology and has reduced production cost.But the Ru film itself is not a good diffusion impervious layer.Bibliographical information; Ru very easily forms in room temperature and annealing process and the vertical column crystal of substrate is that the copper diffusion provides diffusion admittance; The Ru film of 20nm is 450 ℃ as the invalid temperature of copper diffusion barrier layer in addition, and for the Ru film of 5nm, invalid temperature is merely 300 ℃.
In sum, how the thermostability that improves the Ru film is become of crucial importance, also directly influenced its safety in practical application.Method of modifying commonly used perhaps prepares methods double-deck, multilayer film for other elements that mix.
Summary of the invention
The present invention seeks to: provide a kind of magnetron sputtering method of simple controllable to prepare the Ru/TaN double membrane structure.Nitrogen flow through controlling in its sputter procedure obtains the amorphous TaN film of different N content, and then deposits the Ru film, thereby obtains the Ru/TaN double membrane structure.The object of the invention also is; The N atom of oversaturated TaN film intermediate gap can discharge in the annealed process; Ru bonding formation RuN and plug with the upper strata in the process of diffusion amass the crystal boundary place at Ru; Accurate control through to N content in the double-deck barrier material obtains high performance diffusion barrier property, has effectively stoped the diffusion of copper atom.
Technical scheme of the present invention is: high thermal stability bilayer diffusion barrier preparation methods, adopt the direct current magnetron sputtering process preparation to have the Ru/TaN double membrane structure of the TaN underlying membrane of different nitrogen contents (unsaturated and supersaturation N).Sputtering target material is that purity reaches 99.9wt% above Ta and Ru, and substrate is single crystalline Si sheet (111), before deposition, the Si sheet is cleaned, and then Vakuumkammer is vacuumized, to the preparatory sputter of Ta and the about 30min of Ru target; Adopt magnetically controlled DC sputtering when Ru and TaN membrane prepare, the Vakuumkammer base vacuum is evacuated to 6 * 10
-5More than the Pa, Vakuumkammer adds Ar gas during preparation, and the WP of Vakuumkammer is set to 1.5Pa; Underlayer temperature remains room temperature, and the sputtering power 80 ± 10W of TaN film obtains the TaN film of different N content through the flow of nitrogen in the control sputter procedure; The sputtering power of Ru film is 134 ± 10W.
The significant parameter that direct current magnetron sputtering process prepares different N content TaN film is: before preparation TaN film, take out base vacuum to 6 * 10 earlier
-5Pa feeds Ar gas then, and flow is 20sccm; Regulating vacuum degree in vacuum chamber through slide valve is 3.5Pa, begins airglow then, for the spot of removing the Ta target material surface and oxide compound etc.; Guarantee the purity of film, preparatory sputter that earlier will about 30min is after the preparatory sputter; Feed nitrogen, again vacuum tightness is transferred to about 1.5Pa TaN film that begins to grow, in order to grow the TaN film of different N content; We realize that through argon gas and nitrogen partial pressure in the adjusting sputter procedure scope of sputtering power is 80 ± 10W, and underlayer temperature is a room temperature.Same experimental procedure deposition Ru and Cu film obtain the Cu/Ru/TaN/Si interconnection structure.The sputtering power of Ru film is controlled at 134 ± 10W, and the Cu film is 80 ± 10W.The bilayer diffusion barrier material is respectively equipped with TaN, Ru and Cu film on the substrate Si, three's thickness is respectively 8 ± 2nm, 8 ± 2nm and 300 ± 30nm.
The experimental technique step that magnetically controlled DC sputtering prepares different Cu/Ru/TaN/Si interconnection structures is following:
A. substrate material is selected single crystalline Si (111) sheet for use.
B. the preparation the first layer is the TaN film of different N content earlier, and underlayer temperature is a room temperature, and the sputtering power scope is 80 ± 10W.
C. the refabrication second layer is nanocrystalline Ru, and underlayer temperature is a room temperature, and sputtering power is 134 ± 10W.
D. deposit the Cu film at last, underlayer temperature is a room temperature, and sputtering power is 80 ± 10W.
E. the TaN to different N content carries out XPS analysis.
F. the TaN that chooses saturated and unsaturated N content carries out annealing experiment as bottom.
G. two groups of samples are carried out XRD and resistivity measurement.
The higher vacuum tightness that dc sputtering had that adopts can prevent effectively that the purity of Cu, Ru and TaN film from preventing the foreign gas pollution, effectively guaranteed the intrinsic physicals of Ru and TaN.Through accurate adjusting, realized control preferably simultaneously, guaranteed its stability in practical application the N content of TaN to nitrogen flow.
The invention provides the accurate controlled TaN of a kind of N content prepares the double-deck barrier layer structure of Ru/TaN as bottom film preparation method.Separately as the shortcoming of the diffusion barrier material in the interconnecting line, deposit the TaN bottom film to metal Ru in advance, the N atom of its intermediate gap discharges in the process of high temperature annealing.The N atom that discharges plug in the process of diffusion amasss the diffusion that stops the Cu atom at Ru crystal boundary place, and the N that discharges can improve the thermostability of Ru with the Ru bonding, at high temperature still can keep the integrity of Ru membrane structure, improves the barrier properties of Ru/TaN.
Compare with existing preparation method, the present invention has following beneficial effect:
1. the present invention is the method that under a kind of condition of high vacuum degree, prepares, and can effectively avoid film oxidized.Metal Ru is very easily oxidation in air, and the primary Ru oxide compound of formation can reduce the sticking power between Cu and the Ru, makes interconnection structure very fast inefficacy in the process under arms.In our preparation, also can avoid the oxidation of Ru film fully, guarantee the quality of prepared film.
2. the present invention can realize the accurate control to N content in the metal TaN film.The method of control also is simple and easy to control very much, only need in the process of sputter, regulate the flow of nitrogen, and repeatability is also better.
3. the present invention can realize metal Ru and TaN thickness are accurately controlled.Under identical processing parameter, depositing of thin film velocity-stabilization, good reproducibility.Thickness can be controlled at nanoscale.
4. preparation technology of the present invention is simple and convenient, and controllability is good.
The present invention can realize the accurate control of N content in the double-deck barrier material is obtained high performance diffusion barrier property, and maximum operating temperature can reach 650 ℃.
Description of drawings
The XRD (a) and the XPS analysis (b) of Fig. 1 deposited amorphous phase TaN film.
The XRD analysis of Cu/Ru/TaN/Si interconnection structure after Fig. 2 deposited and the 350-650 ℃ annealing, wherein (a) TaN is unsaturated, and wherein (b) TaN is saturated.
Cu/Ru/TaN/Si interconnection structure resistivity is analyzed after Fig. 3 deposited and the 350-650 ℃ annealing.
Embodiment
Adopt direct current magnetron sputtering process to prepare the Ru/TaN film of different N content, a model is the magnetic control sputtering device of JGP350, and this equipment uses the electromagnetism target, and diameter 60mm only adds DC, and maximum sputtering power is 400W.One six station has the sample rotating disk of revolution function, but sample both can heat also water-cooled, and top temperature can arrive 550 ℃, and the heating rate variable range is applicable to the multiple differing materials film of preparation at 10 ℃/min-40 ℃/min.Vacuum system mainly is furnished with a 2XZ-8 type mechanical pump and the FB600 whirlpool molecular pump that sinks, and maximum vacuum can reach 6.6 * 10
-5Pa, the vacuum tightness of superelevation has effectively been protected the quality of film.
Material is prepared: sputtering target material is that purity reaches 99.9%Ta, 99.9%Ru, and 99.999%Cu, diameter 60mm, the about 3mm of thickness, substrate are single crystalline Si (111).In order to improve the sticking power of TaN film and substrate, before deposition, with the Si sheet successively by ethanol, acetone and ultrasonic 20min, with surface dirt and the oil stain of removing the adhesion that influences film and substrate.Before sputter, to the preparatory sputter of the about 30min of target, remove its surperficial zone of oxidation and spot earlier in addition, guaranteed the purity of film, also guarantee is provided for the quality that guarantees film.
The TaN membrane prepare: adopt direct current magnetron sputtering process, base vacuum is evacuated to 6 * 10
-5Pa, the Ar airshed is 20sccm, WP is set to 1.5Pa.The dividing potential drop of argon gas and nitrogen is come the content of N among the accuracy controlling TaN in the control sputter procedure.Control the thickness of film according to sputtering time, the thickness of all TaN films is 8 ± 2nm.The experimental basis substrate temperature remains room temperature, and the sputtering power scope is 80 ± 10W.
The preparation of Ru film: adopt direct current magnetron sputtering process, base vacuum is evacuated to 6 * 10
-5Pa, the Ar airshed is 20sccm, WP is set to 1.5Pa.Control the thickness of film according to sputtering time, the thickness of Ru film is 8 ± 2nm.The experimental basis substrate temperature remains room temperature, and the sputtering power scope is 134 ± 10W.Structural characterization and result:
Through knowing to the XRD analysis of deposited TaN film, when 3-12sccm changes any peak crystallization does not appear in the N airshed, and it is existing to have only a ripple to contract out, and shows to be entirely amorphous TaN.Through knowing the XPS analysis of deposited TaN film, when increasing the N airshed, Ta-N bond number amount constantly increases among the TaN, and Ta-O bond number amount constantly reduces.When the N airshed surpassed 5sccm, the N atomic quantity among the TaN reached supersaturation and keeps stable, and Ta/N atomicity ratio is about 0.33.XRD and XPS analysis through to deposited Ru film can know that the Ru film is nanocrystalline, and the average grain size that can calculate Ru according to the Scherrer formula is about 25nm.Do not contain O impurity among the Ru, prove at magnetron sputtering to prepare very purified Ru film, help improving the sticking power between Cu and the Ru.
The Cu/Ru/TaN/Si interconnection structure is carried out 350-650 ℃ of XRD, resistance and the tem analysis result behind 30 minutes annealing tests to be shown: the unsaturated TaN of N can improve the barrier properties to 550 ℃ of Ru; Ru/TaN in the time of 650 ℃ (unsaturated) barrier properties lost efficacy, and resistance rises rapidly.And the blocking layer of the Ru/TaN of the oversaturated TaN of N still keeps good barrier properties after 650 ℃ of annealing, and resistance rises slightly.Thermostability but also interconnection structure that the oversaturated Ru/TaN of N not only can improve Ru still keep good electric property.
Claims (3)
1. high thermal stability bilayer diffusion barrier preparation methods is characterized in that adopting direct current magnetron sputtering process to prepare the TaN film and the film of different N content, i.e. Ru/TaN double membrane structure; Sputtering target material is that purity reaches 99.9wt% above Ta and Ru, and substrate is single crystalline Si sheet (111), before deposition, the Si sheet is cleaned, and then Vakuumkammer is vacuumized, to the preparatory sputter of Ta and the about 30min of Ru target; Adopt magnetically controlled DC sputtering when Ru and TaN membrane prepare, the Vakuumkammer base vacuum is evacuated to 6 * 10
-5More than the Pa, Vakuumkammer adds Ar gas during preparation, and the WP of Vakuumkammer is set to 1.5Pa; Underlayer temperature remains room temperature, and the sputtering power 80 ± 10W of TaN film obtains the TaN film of different N content through the flow of nitrogen in the control sputter procedure; The sputtering power of Ru film is 134 ± 10W.
2. according to the preparation method of claim 1 and 2 described different N content TaN films, it is characterized in that before preparation TaN film, taking out base vacuum to 6 * 10 earlier
-5Pa feeds Ar gas then, and flow is 20sccm; Regulating vacuum degree in vacuum chamber through slide valve is 3.5Pa, begins airglow then, for the spot of removing the Ta target material surface and oxide compound etc.; Guarantee the purity of film, preparatory sputter that earlier will about 30min is after the preparatory sputter; Feed nitrogen, again vacuum tightness is transferred to about 1.5Pa TaN film that begins to grow, in order to grow the TaN film of different N content; Realize that through argon gas and nitrogen partial pressure in the adjusting sputter procedure scope of sputtering power is 80 ± 10W, underlayer temperature is a room temperature; The sputtering power of Ru film is controlled at 134 ± 10W, and the Cu film is 80 ± 10W.
3. the bilayer diffusion barrier material is respectively equipped with TaN, Ru and Cu film on the substrate Si, and three's thickness is respectively 8 ± 2nm, 8 ± 2nm and 300 ± 30nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703870A (en) * | 2012-05-09 | 2012-10-03 | 昆明贵金属研究所 | Nonmagnetic Ru film and production method thereof |
| CN103500728A (en) * | 2013-09-29 | 2014-01-08 | 武汉新芯集成电路制造有限公司 | Forming method of copper blocking layers and copper seed-crystal layer |
| CN108640092A (en) * | 2018-04-18 | 2018-10-12 | 南京大学 | The method that a kind of one step nitriding of oxygenatedchemicals auxiliary prepares metal nitride film |
| CN109763100A (en) * | 2019-01-25 | 2019-05-17 | 西安交通大学苏州研究院 | Sensitive thin film in diaphragm pressure sensor and preparation method thereof and application |
| CN113380944A (en) * | 2020-03-10 | 2021-09-10 | 铠侠股份有限公司 | Magnetic memory device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703870A (en) * | 2012-05-09 | 2012-10-03 | 昆明贵金属研究所 | Nonmagnetic Ru film and production method thereof |
| CN102703870B (en) * | 2012-05-09 | 2014-01-15 | 昆明贵金属研究所 | Nonmagnetic Ru film and production method thereof |
| CN103500728A (en) * | 2013-09-29 | 2014-01-08 | 武汉新芯集成电路制造有限公司 | Forming method of copper blocking layers and copper seed-crystal layer |
| CN103500728B (en) * | 2013-09-29 | 2016-03-02 | 武汉新芯集成电路制造有限公司 | A kind of formation method of copper barrier layer and copper seed layer |
| CN108640092A (en) * | 2018-04-18 | 2018-10-12 | 南京大学 | The method that a kind of one step nitriding of oxygenatedchemicals auxiliary prepares metal nitride film |
| CN109763100A (en) * | 2019-01-25 | 2019-05-17 | 西安交通大学苏州研究院 | Sensitive thin film in diaphragm pressure sensor and preparation method thereof and application |
| CN113380944A (en) * | 2020-03-10 | 2021-09-10 | 铠侠股份有限公司 | Magnetic memory device |
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