CN103966566B - The preparation method of double-deck high-entropy alloy diffusion impervious layer - Google Patents
The preparation method of double-deck high-entropy alloy diffusion impervious layer Download PDFInfo
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Abstract
The preparation method that the invention discloses a kind of double-deck high-entropy alloy diffusion impervious layer, mainly comprises the steps of and single crystalline Si matrix is carried out ultrasonic waves for cleaning；Adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, adopt pre-sputter cleaning to remove the impurity in target and target sheet；It is 1:(0.65～0.9 passing into Ar and N flow-rate ratio) under condition, sputtering sedimentation HEANs thin film on single crystalline Si matrix；When HEANs thin film reaches design thickness, using Ar as working gas, sputtering sedimentation HEAs thin film on HEANs thin film；When HEAs thin film reaches design thickness, the vacuum in stove is adjusted to being not less than 10-3Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。The double-deck high-entropy alloy diffusion impervious layer that the present invention obtains improve matrix, Cu and from ought bond strength once, and improve the advantage such as overall thermal stability of diffusion impervious layer and the technology maturation that preparation technology adopts, cost is low, pollutes the features such as few。
Description
Technical field
The application belongs to semiconductor integrated circuit manufacturing process technology field, particularly to a kind of deep sub micrometer VLSI Cu interconnection film system preparation method of double-deck high-entropy alloy diffusion impervious layer。
Background technology
Along with developing rapidly of super large-scale integration (ULSI) Technology, integrated circuit feature size continues to reduce, while requiring that diffusion impervious layer is thinning as far as possible, maintaining the diffusion barrier performance under high temperature and thermal stability, this makes Al be on the rise as the RC that interconnection material the produces problem postponing to sharply increase the device performance degradation caused。Even to this day, Cu progressively replaces Al and interconnects metal material as a new generation。But, although many physical propertys of Cu self are applied to have very big advantage on Si device, but but there are some unavoidable problems in the application that Cu is in Si device, as Cu has higher diffusion rate in Si and oxide thereof, once Cu atom enters Si layer, deep energy level acceptor impurity will be become at a lower temperature, the carrier in device is had very strong trap effect, cause device performance degeneration, ultimate failure。Additionally the adhesion property of Cu and medium is more weak, easily oxidized。Therefore, Cu interconnection process must be introduced into the suitable metal or alloy rete adhesiveness with Reinforced Cu and medium, simultaneously work as the diffusion reaction stoping Cu and Si。
At present the research of Cu diffusion impervious layer is concentrated mainly on the following aspects: (1) simple substance refractory metal and alloy material, such as document [KhinMaungLATT, H.S.PARK, S.LI.JournalofMaterialsScience, 2002,37 (2002): 1,941 1949] and [J.S.FANG, T.P.HSU, H.C.CHEN.2007, JournalofElectronicMaterials, 36 (5): 614-622]。Although indissoluble elemental metals and bianry alloy have relatively low resistivity and the advantage such as better with Cu adhesiveness, but its heat stability is generally poor, namely reacts with Si and cause losing efficacy in barrier layer below 600 DEG C；(2) nitrogen/carbide of refractory metal and refractory metal ternary compound, such as document [KhinMaungLatt, C.Sher-Yi, T.Osipowicz.JournalofMaterialsScience, 2001,36 (2001): 5,705 5712] and [L.W.Lin, B.Liu, D.Renetal.SurfaceandCoatingsTechnology.2012]。Although refractory metal nitride and ternary compound have a higher heat stability, but due under hot conditions N, O, C easily diffuse to the interface on barrier layer and Cu, cause that the adhesiveness of barrier layer and Cu reduces, cause the appearance of interfacial gap。
For overcoming the shortcoming existing for above-mentioned material, seek new material and new technology to solve the problems referred to above imperative。In recent years, researcheres turn one's attention to high-entropy alloy one after another, it is desirable to utilize desirable physical that high-entropy alloy has and chemical property to solve the problems referred to above。
High-entropy alloy why have the process based prediction model of excellence depend on effect that conventional alloys do not have [Ye Junwei. the development of high-entropy alloy. magnificent ridge engineering journal, 2011,27 (2011): 1-18]。Researcher wishes that the high entropic effect that high-entropy alloy can be utilized to have, serious distortion of lattice effect are solving adhesiveness, improves stability of material simultaneously, utilizes its slow spreading effect, cocktail effect to improve diffusion impervious layer and hinders the ability of diffusion。
Just because of high-entropy alloy has good diffusion barrier performance and heat stability so that the numerous and confused Cu that high-entropy alloy and nitride thereof is applied in of researcheres interconnects in diffusion impervious layer, and achieves good effect。As 50nmAlCrTaTiZr nitride film is expanded barrier layer as Cu interconnection, invalid temperature is up to 900 DEG C [Shou-YiChang, Ming-KuChen.ThinSolidFilms, 2009,517 (2009): 4,961 4965]；For meeting the requirement of diffusion impervious layer ultrathin, Chang devises (AlCrRuTaTiZr) Nx diffusion impervious layer [ChangSY, LiCE, HuangYC, HuangYC.JAlloysCompd, 2012 that thickness is 4nm；515:4]。For reaching the purpose improving diffusion impervious layer with metal level binding ability, avoid owing to the difference of thermal expansion coefficients of nitride Yu Cu is bigger, it is easily formed cavity in interface under high temperature, cause that metal interconnecting wires lost efficacy, Chang and Chen etc. devise (AlCrTaTiZr) N/ (AlCrTaTiZr) N0.7 bilayer diffusion barrier, but (AlCrTaTiZr) N0.7 is improving the adhering resistivity too increasing system simultaneously, interconnection architecture is made to postpone to increase [ChangSY, ChenDS.MaterChemPhys, 2011；125:5]。
Summary of the invention
The state of the art and deficiency for double-deck high-entropy alloy diffusion impervious layer, the application is directed to a kind of preparation method being suitable to industrialized double-deck high-entropy alloy diffusion impervious layer, prepare Heat stability is good, resistivity by the method low, and the double-deck high-entropy alloy diffusion impervious layer of adhesion property between Cu can be improved。
The basic thought of the application is: first first depositing one layer of HEANs layer on Si matrix, its reason is in that: have, between (1) HEANs and Si matrix, adhering well to property, it can be ensured that diffusion impervious layer will not come off from Si matrix；(2) utilize the high thermal stability of HEANs layer, improve the invalid temperature of whole diffusion impervious layer。Then on HEANs layer, deposit the HEAs layer of one layer of low-resistivity, produce HEAs/HEANs low-resistance bilayer diffusion barrier。Utilizing the adhesiveness that HEAs and Cu is good, improve the binding ability of diffusion impervious layer and Cu, solving conventional nitride relatively poor with the adhesiveness of Cu, thus causing the problem that the stability of interconnection architecture reduces。Simultaneously because the high entropic effect that has of high-entropy alloy self and distortion of lattice effect so that HEAs/HEANs diffusion impervious layer due to the difference of thermal coefficient of expansion between metal and its nitride, will not cause that diffusion impervious layer comes off when device is on active service。It is the raw material constituting high-entropy alloy that the application chooses Al, Cr, Ta, Ni, Ti, is because inventors herein have recognized that the AlCrTaNiTi high entropy alloy material constituted has good high entropic effect and distortion of lattice effect。The application also further study how to obtain nano level HEANs and HEAs thin film, provides development space for meeting microelectronic product process requirements。
The preparation method of the double-deck high-entropy alloy diffusion impervious layer that the application provides, mainly includes following preparation process:
(1) single crystalline Si matrix is successively respectively placed in acetone and dehydrated alcohol, carry out ultrasonic waves for cleaning, namely first it is placed in after acetone or dehydrated alcohol carry out ultrasonic waves for cleaning, then is placed in dehydrated alcohol or acetone and carries out ultrasonic waves for cleaning, after fully cleaning, take out drying for standby。
The purpose of this step is in that to adopt ultrasonic wave concussion method to remove the impurity such as the oil stain of single crystalline Si matrix surface, dust, it is possible to adopt the above-mentioned acetone provided and dehydrated alcohol as cleanout fluid, it is also possible to take the organic solvent with phase same-action as cleanout fluid。Through fully cleaning, remove the impurity such as the oil stain of single crystalline Si matrix surface, dust completely。Scavenging period is unimportant, as long as the effect of fully cleaning can be reached。In this application, single crystalline Si matrix is sequentially placed in acetone and dehydrated alcohol ultrasonic waves for cleaning no less than 20min。
(2) insert in magnetron sputtering plating vacuum drying oven using single crystalline Si matrix with as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, Ta target is placed Ti target sheet；After magnetron sputtering plating vacuum drying oven evacuation, pass into Ar as working gas, adopting reverse sputtering to clean and remove impurity in single crystalline Si matrix, adopt pre-sputter cleaning to remove the impurity in target and target sheet, reverse sputtering and pre-sputtering operation pressure are (1～3) Pa。
The purpose of this step is in that to carry out sputter clean to single crystalline Si matrix with as the Ta target of target, Al target, Cr target, Ni target sheet, Ti target sheet, remove further the impurity in single crystalline Si matrix and Ta target, Al target, Cr target, Ni target sheet, Ti target sheet, particularly above foreign atom and the oxide skin(coating) of formation；Sputtering power is not had particular/special requirement by the application, if the impurity can removed in single crystalline Si matrix and Ta target, Al target, Cr target, Ni target sheet, Ti target sheet。
It is (160～240) W that the single crystalline Si matrix reverse sputtering provided in the application cleans power, biases as (-700～-800) V；Ta target, Al target, Cr target, Ni target sheet and Ti target sheet sputter clean power are (60～100) W。Can adjust to some extent for other magnetron sputtering plating vacuum drying oven, reverse sputtering and pre-sputtering power。
Being limited to (1～3) Pa for reverse sputtering and pre-sputtering operation pressure, its reason is in that, for the magnetron sputtering plating vacuum drying oven that the application adopts, when pressure is less than 1Pa, it is impossible to reach the cleaning performance of reverse sputtering and pre-sputtering；When pressure is more than 3Pa, will beyond equipment working range。For other magnetron sputtering plating vacuum drying oven, the operation pressure of reverse sputtering and pre-sputtering can adjust to some extent, and this adjustment relies on present invention design, will fall into the protection domain of the application。
The application is for the time not special requirement of the reverse sputtering in this step and pre-sputtering, as long as above-mentioned sputter clean purpose can be arrived。Reverse sputtering scavenging period in this step that the application provides is (8～12) min, and the pre-sputter cleaning time is (10～15) min。
In order to ensure that sputter clean maintains within the scope of operation pressure, it is possible to before passing into Ar, vacuum in magnetron sputtering plating vacuum drying oven is evacuated to and is not less than 10-3Pa, it is more preferable that 10-4Pa, so it is also ensured that to single crystalline Si matrix and Ta target, Al target, Cr target, Ni target sheet, Ti target sheet cleaning quality。
(3) Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin film of thickness, during sputtering, pass into Ar and N2, Ar and N2Flow-rate ratio be 1:(0.65～0.9), regulate deposition pressure be (0.3～0.6) Pa。
The purpose of this step is in that, sets the HEANs thin film of thickness at single crystalline Si substrate deposit。In order to obtain above-mentioned HEANs thin film, it is necessary to pass into N in magnetron sputtering plating vacuum drying oven2, and make the atomic ratio of high-entropy alloy AlCrTaTiNi and N be about 1:1, for this reason, it may be necessary to control Ar and N2Flow-rate ratio be 1:(0.65～0.9)；N2Time very few, it is impossible to ensure that the atomic ratio of high-entropy alloy AlCrTaTiNi and N is about 1:1。Preferred Ar and N in the application2Flow-rate ratio be 1:0.75, it is preferred that Ar flow be 40sccm, N2Flow is 30sccm。
Regulating deposition pressure is to obtain relatively thin HEANs thin layer, by regulating deposition pressure at (0.3～0.6) Pa, it is possible to obtain set the thickness HEANs thin film as (9～12) nm。
Deposition power is not had particular/special requirement by the application, as long as can reach on the atomic deposition on Ta target, Al target, Cr target, Ni target sheet and Ti target sheet to single crystalline Si matrix。The deposition sputtering power provided in the application is (60-100) W。For other magnetron sputtering plating vacuum drying oven, deposition sputtering power can adjust to some extent。
(4) HEANs thin film layer is to design thickness, closes N2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning to remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber in air pressure (0.3～0.6) Pa。
The purpose of this step is in that to remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber, obtains HEAs thin film for next step and prepares。It is nanoscale owing to needing the HEAs thin film obtained, if the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber is not processed, largely effecting on the double-deck high-entropy alloy diffusion impervious layer quality finally obtained, what even obtain is not the double-deck high-entropy alloy diffusion impervious layer that provides of the application。
It is noted herein that, the application is in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber are carried out pre-sputter cleaning, do so, while ensure that double-deck high-entropy alloy diffusion impervious layer HEAs/HEANs performance, decrease the energy consumption produced because extracting back end vacuum, greatly reduce production cost, it is more suitable for industrialized production, and is prone to mutually compatible with other microelectronics manufacture。
Sputtering power is not had particular/special requirement by the application, if the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber can be removed。The Ta target, Al target, Cr target, Ni target sheet and the Ti target sheet sputter clean power that provide in the application are (60-100) W。Can adjust to some extent for other magnetron sputtering plating vacuum drying oven, reverse sputtering and pre-sputtering power。
In this step, being limited to (0.3～1) Pa for pre-sputtering operation pressure, its reason is in that, for the magnetron sputtering plating vacuum drying oven that the application adopts, when pressure is less than 0.3Pa, it is impossible to reach the purpose of the cleaning of pre-sputtering；When pressure is more than 1Pa, it will increase the loss of target, increase cost。For other magnetron sputtering plating vacuum drying oven, the operation pressure of the pre-sputtering of this step can adjust to some extent, and this adjustment relies on present invention design, will fall into the protection domain of the application。
The application is for the time not special requirement of the pre-sputtering in this step, as long as above-mentioned sputter clean purpose can be arrived。The pre-sputter cleaning time in this step that the application provides is 15～25min。
(5) with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness, during sputtering, with Ar gas for working gas, regulating deposition pressure is (0.3～0.6) Pa。
The purpose of this step is in that, continues deposition one layer and set the HEAs thin film of thickness on HEANs thin film。
In this step, with Ar for working gas, regulating deposition pressure relatively low is to obtain relatively thin HEANs thin film, by regulating deposition pressure at (0.3～0.6) Pa, it is possible to obtain set the thickness HEAs thin film as (9～12) nm。
The deposition power of this step is not had particular/special requirement by the application, as long as can reach on the atomic deposition on Ta target, Al target, Cr target, Ni target sheet and Ti target sheet to HEANs thin film。The deposition sputtering power provided in the application is (60～100) W。For other magnetron sputtering plating vacuum drying oven, deposition sputtering power can adjust to some extent。
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to being not less than 10-3Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
In technique scheme, single crystalline Si matrix preferably selects N-type single crystalline Si, and single crystalline Si matrix is oriented to [100]。
In technique scheme, Al target purity is preferably not below 99.95%, and Cr target purity is preferably not below 99.95%, and Ta target purity is preferably not below 99.95%, and Ni sheet purity is preferably not below 99.95%, and Ti purity is preferably not below 99.95%。
The preparation method of the double-deck high-entropy alloy diffusion impervious layer that the application provides has the advantages that
1, double-deck high-entropy alloy diffusion impervious layer HEAs/HEANs prepared by the application, improves the bond strength on matrix, Cu and barrier layer, and improves the overall thermal stability of diffusion impervious layer。
2, the distortion of lattice effect that double-deck high-entropy alloy diffusion impervious layer HEAs/HEANs prepared by the application utilizes high-entropy alloy serious, it is ensured that the HEANs layer of preparation and HEAs layer can be effectively combined。
3, the application is in the process of the double-deck high-entropy alloy diffusion impervious layer HEAs/HEANs of preparation, do not change vacuum and target modes of emplacement, while ensureing double-deck high-entropy alloy diffusion impervious layer HEAs/HEANs performance, decrease the energy consumption produced because extracting back end vacuum, greatly reduce production cost, it is more suitable for industrialized production, and is prone to mutually compatible with other microelectronics manufacture。
4, double-deck high-entropy alloy diffusion impervious layer prepared by the application, the size of HEANs thin layer and HEAs thin layer is at below 12nm, it is possible to well meets microelectronic product processing request, and provides development space for reducing size further。
5, the preparation method of the application adopts Ni sheet and Ti sheet as raw material, is possible not only to save the target position adopted in sputter procedure, has reserved space for expanding further later, and can save in sputter procedure the saving for raw material, saves cost further。
The features such as 6, the preparation method of the application adopts popular response radiofrequency magnetron sputtering technology, has technology maturation, and cost is low, and pollutant are few。
Accompanying drawing explanation
Accompanying drawing described herein is used to provide further understanding of the present application, constitutes the part of the application, and the schematic description and description of the application is used for explaining the application, but does not constitute the improper restriction to the application。
Fig. 1 schematically shows the structural representation of the film sample with double-deck high-entropy alloy diffusion impervious layer obtained according to one embodiment of the application；Wherein, 1-Cu layer, 2-HEAs layer, 3-HEANs layer, 4-Si matrix；
Fig. 2 schematically shows scanning electron microscope (SEM) Cross Section Morphology of the film sample with double-deck high-entropy alloy diffusion impervious layer obtained according to one embodiment of the application；Wherein, (a)-deposited, (b)-700 DEG C of annealed state, (c)-800 DEG C of annealed state, (d)-900 DEG C of annealed state；
Fig. 3 schematically shows scanning electron microscope (SEM) surface topography of the film sample with double-deck high-entropy alloy diffusion impervious layer obtained according to one embodiment of the application；Wherein, (a)-deposited, (b)-700 DEG C of annealed state, (c)-800 DEG C of annealed state, the enlarged drawing of (d)-900 DEG C of annealed state and black dotted lines part；
Fig. 4 schematically shows thin film composition distribution collection of illustrative plates (EDS) of selection area in d figure in Fig. 3；And
Fig. 5 schematically shows X ray diffracting spectrum under the different annealing temperature of the film sample with double-deck high-entropy alloy diffusion impervious layer obtained according to one embodiment of the application。
Detailed description of the invention
In order to make the purpose of the application, technical scheme and advantage clearly, below in conjunction with specific embodiment, the application is described in further detail。
In the following description, " embodiment ", " embodiment ", " example ", " example " etc. quoted expression, described embodiment or example can include special characteristic, structure, characteristic, character, element or limit, but not each embodiment or example necessarily include special characteristic, structure, characteristic, character, element or limit。It addition, reuse phrase " according to the application embodiment " although it is possible to refer to identical embodiment, but it is not necessarily referring to identical embodiment。
Embodiment 1:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is first placed in acetone to be placed in dehydrated alcohol and carry out about 20min ultrasonic waves for cleaning respectively, after fully cleaning, takes out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy Cr target and the portion of Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 4.0 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 200W, biases as-700V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 60W；Reverse sputtering and pre-sputtering operation pressure are 2Pa；Reverse sputtering scavenging period is about 10min, and the pre-sputter cleaning time is about 15min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 10nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 30sccm, and adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 60W；
(4) HEANs thin film layer is to design thickness, closes N2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 0.3Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；Pre-sputtering power is 60W；The pre-sputtering time is about 20min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 10nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 60W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 4.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
In order to verify the performance of double-deck high-entropy alloy diffusion impervious layer that the present invention obtains, after prepared by above-mentioned double-deck high-entropy alloy diffusion impervious layer, when not changing magnetron sputtering plating vacuum drying oven chamber house vacuum, adopt d.c. sputtering, at double-deck high-entropy alloy diffusion impervious layer, it deposits the Cu layer (purity of Cu target is 99.95%) of 100nm, namely the film sample with double-deck high-entropy alloy diffusion impervious layer is obtained, wherein Ar operating air pressure is 0.6Pa, and sputtering power is 100W。The film sample with double-deck high-entropy alloy diffusion impervious layer of above-mentioned preparation is further divided into four groups, one of which is the deposited sample that the present embodiment provides, other three groups carry out fine vacuum annealing respectively, obtain 700 DEG C of annealing specimens, 800 DEG C of annealing specimens, 900 DEG C of annealing specimens。The base vacuum of vacuum annealing furnace is 2.0 × 10-5Pa, annealing temperature is 700 DEG C, 800 DEG C or 900 DEG C, and annealing time is 30min,
Fig. 1 schematically shows the structural representation of the above-mentioned film sample with double-deck high-entropy alloy diffusion impervious layer。As it can be seen, Si matrix 4 is in bottom, Cu layer 1 topmost, between Cu layer 1 and Si matrix 4 respectively HEAs layer 2 and HEANs layer 3, HEAs2 near Cu layer 1, HEANs layer 3 near Si matrix 4。
Fig. 2 schematically shows scanning electron microscope (SEM) Cross Section Morphology of the above-mentioned film sample with double-deck high-entropy alloy diffusion impervious layer。It can be seen that unannealed sample, architecture is complete, has good adhesion between double-deck high-entropy alloy diffusion impervious layer and Cu layer 1 and Si matrix 4；The sample of less than 800 DEG C annealing, architecture is still very complete, remains to keep good adhesion between double-deck high-entropy alloy diffusion impervious layer and Cu layer 1 and Si matrix 4。The sample of 900 DEG C of annealing, the adhesion between double-deck high-entropy alloy diffusion impervious layer and Cu layer 1 and Si matrix 4 is destroyed。As can be seen here, the double-deck high-entropy alloy diffusion impervious layer that the preparation method provided by the application is obtained has good heat stability
Fig. 3 schematically shows scanning electron microscope (SEM) surface topography of the above-mentioned film sample with double-deck high-entropy alloy diffusion impervious layer。As can be seen from the figure the sample surfaces after 700 DEG C, 800 DEG C annealing presents striated, there is certain crackle, and present certain fluctuating, striated is the result of Cu grain growth under high temperature annealing condition, further up along with annealing temperature, due to thermal stress and capillary effect, surface starts to present massif shape。And when temperature is increased to 900 DEG C, Cu surface topography starts to become coarse and discontinuous, and in local, bright taper granule (see the part that broken box provides) occurs。
Fig. 4 schematically shows thin film composition distribution collection of illustrative plates (EDS) of selection area in d figure in Fig. 3。Through the EDS energy spectrum analysis to taper particulate matter, it has been found that particulate matter mainly contains Cu and Si。XRD spectrum after annealing in conjunction with 900 DEG C, it is possible to confirm the Cu-Si phase generating high-impedance state. illustrate that Cu/AlCrTaTiNi/ (AlCrTaTiNi) N/Si sample is when 900 DEG C, double-deck high-entropy alloy diffusion impervious layer complete failure。
Fig. 5 schematically shows X ray diffracting spectrum under the different annealing temperature of the above-mentioned film sample with double-deck high-entropy alloy diffusion impervious layer。It is shown that along with the rising of annealing temperature, Cu (111) orientation is remarkably reinforced, occur with more weak Cu (200) simultaneously。But after annealing at 900 DEG C, Cu (111) and Cu (200) disappears, and occurs in that substantial amounts of Cu-Si phase, illustrates that now counterdiffusion has occurred Cu and Si, generates deep energy level phase, and diffusion impervious layer lost efficacy。
Embodiment 2:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is first placed in dehydrated alcohol it is placed in acetone and carries out about 30min ultrasonic waves for cleaning respectively, after fully cleaning, take out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy Cr target and the portion of Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 1.2 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 160W, biases as-800V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 100W；Reverse sputtering and pre-sputtering operation pressure are 1Pa；Reverse sputtering scavenging period is about 12min, and the pre-sputter cleaning time is about 10min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 12nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 36sccm, and adjustment deposition pressure is 0.6Pa；Deposition sputtering power is 80W；
(4), when HEANs thin film layer is to design thickness, N is closed2Intake valve, not changing in magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 1Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；Pre-sputtering power is 80W；The pre-sputtering time is about 15min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 12nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.6Pa；Deposition sputtering power is 80W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 1.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
Embodiment 3:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is sequentially placed in acetone and dehydrated alcohol and carries out about 25min ultrasonic waves for cleaning respectively, after fully cleaning, take out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy the upper portion of Cr target and Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 4.0 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 240W, biases as-700V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 80W；Reverse sputtering and pre-sputtering operation pressure are 3Pa；Reverse sputtering scavenging period is about 8min, and the pre-sputtering time is about 15min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 9nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 26sccm, and adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 80W；
(4), when HEANs thin film layer is to design thickness, N is closed2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 0.6Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；The pre-sputtering time is about 20min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 9nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 80W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 4.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
Embodiment 4:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is sequentially placed in acetone and dehydrated alcohol and carries out about 20min ultrasonic waves for cleaning respectively, after fully cleaning, take out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy the upper portion of Cr target and Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 4.0 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 200W, biases as-800V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 100W；Reverse sputtering and pre-sputtering operation pressure are 1.5Pa；Reverse sputtering scavenging period is about 9min, and the pre-sputter cleaning time is about 10min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 10nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 30sccm, and adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 100W；
(4), when HEANs thin film layer is to design thickness, N is closed2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 0.8Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；The pre-sputtering time is 15min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 10nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.3Pa；Deposition sputtering power is 100W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 4.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
Embodiment 5:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is sequentially placed in acetone and dehydrated alcohol and carries out about 30min ultrasonic waves for cleaning respectively, after fully cleaning, take out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy the upper portion of Cr target and Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 1.2 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 180W, biases as-700V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 80W；Reverse sputtering and pre-sputtering operation pressure are 1.5Pa；Reverse sputtering scavenging period is about 12min, and the pre-sputter cleaning time is about 15min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 11nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 30sccm, and adjustment deposition pressure is 0.45Pa；Deposition sputtering power is 100W；
(4), when HEANs thin film layer is to design thickness, N is closed2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 0.45Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；The pre-sputtering time is 25min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 11nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.45Pa；Deposition sputtering power is 100W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 4.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
Embodiment 6:
(1) the N-type single crystalline Si matrix that crystal orientation is [100] is sequentially placed in acetone and dehydrated alcohol and carries out 40min ultrasonic waves for cleaning respectively, after fully cleaning, take out drying for standby；
(2) using single crystalline Si matrix cleaned for step (1) with insert in magnetron sputtering plating vacuum drying oven as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, placing Ti target sheet on Ta target, wherein Ni target sheet and Ti target sheet only occupy the upper portion of Cr target and Ta target；Magnetron sputtering plating vacuum drying oven is evacuated to 4.0 × 10-4After Pa, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, the power that reverse sputtering cleans is 220W, biases as-800V；Adopting pre-sputter cleaning to remove the impurity of target and target sheet, the power of pre-sputter cleaning is 80W；Reverse sputtering and pre-sputtering operation pressure are 2.5Pa；Reverse sputtering scavenging period is 8min, and the pre-sputter cleaning time is 15min；
(3) after reverse sputtering cleans and terminates with pre-sputter cleaning, Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness 12nm, during sputtering, pass into Ar and N2, Ar flow is 40sccm, N2Flow is 36sccm, and adjustment deposition pressure is 0.45Pa；Deposition sputtering power is 80W；
(4), when HEANs thin film layer is to design thickness, N is closed2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning in air pressure 0.45Pa, remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber；The pre-sputtering time is 20min；
(5) after in step (4), pre-sputter cleaning terminates, with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the Si/HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness 12nm, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.45Pa；Deposition sputtering power is 80W；
(6) when HEAs thin film layer is to design thickness, close Ta target, Al target, Cr target, Ni target sheet and Ti target sheet, close Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to 4.0 × 10-4Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
Claims (10)
1. the preparation method of a double-deck high-entropy alloy diffusion impervious layer, it is characterised in that comprise the following steps:
(1) single crystalline Si matrix is successively respectively placed in acetone and dehydrated alcohol, carries out ultrasonic waves for cleaning, after fully cleaning, take out drying for standby；
(2) insert in magnetron sputtering plating vacuum drying oven using single crystalline Si matrix cleaned for step (1) with as the Ta target of target, Al target, Cr target, and on Cr target, place Ni target sheet, Ta target is placed Ti target sheet；After magnetron sputtering plating vacuum drying oven evacuation, passing into Ar as working gas, adopt reverse sputtering to clean and remove impurity in single crystalline Si matrix, adopt pre-sputter cleaning to remove the impurity in target and target sheet, reverse sputtering and pre-sputtering operation pressure are 1～3Pa；
(3) Ta target after processing using step (2) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet are as magnetic control target, the cleaned single crystalline Si matrix of step (2) reverse sputtering adopt magnetron sputtering deposition set the HEANs thin layer of thickness, during sputtering, pass into Ar and N2, Ar and N2Flow-rate ratio be 1:(0.65～0.9), adjustment deposition pressure is 0.3～0.6Pa；
(4) HEANs thin film layer is to design thickness, closes N2Intake valve, in not disrumpent feelings magnetron sputtering plating vacuum drying oven under vacuum condition, pass into Ar as working gas, adopt pre-sputter cleaning to remove the atom N of residual in Ta target, Al target, Cr target, Ni target sheet, Ti target sheet and magnetron sputtering plating vacuum drying oven chamber in air pressure 0.3～1Pa；
(5) with the Ta target after the process of step (4) pre-sputter cleaning, Al target, Cr target, Ni target sheet and Ti target sheet for magnetic control target, the HEANs thin layer that step (3) obtains adopt magnetron sputtering deposition set the HEAs thin layer of thickness, during sputtering, with Ar gas for working gas, adjustment deposition pressure is 0.3～0.6Pa；
(6), when HEAs thin film layer is to design thickness, closes Ar intake valve, make the vacuum in magnetron sputtering plating vacuum drying oven adjust to being not less than 10-3Pa, comes out of the stove after natural cooling and obtains double-deck high-entropy alloy diffusion impervious layer。
2. the preparation method of double-deck high-entropy alloy diffusion impervious layer according to claim 1, it is characterised in that described single crystalline Si matrix is N-type single crystalline Si matrix, and single crystalline Si matrix is oriented to [100]。
3. the preparation method of double-deck high-entropy alloy diffusion impervious layer according to claim 1, it is characterised in that in step (1), single crystalline Si matrix is placed in acetone and dehydrated alcohol ultrasonic waves for cleaning no less than 20min。
4. the preparation method of double-deck high-entropy alloy diffusion impervious layer according to claim 1, it is characterised in that Al target purity is not less than 99.95%, Cr target purity is not less than 99.95%, Ta target purity is 99.95%, and Ni target sheet purity is 99.95%, and Ti target sheet purity is 99.95%。
5. the preparation method of double-deck high-entropy alloy diffusion impervious layer according to claim 1, it is characterised in that be not less than 10 by being evacuated to by magnetron sputtering plating vacuum drying oven-4Pa, to ensure that sputter clean and sputtering sedimentation maintain within the scope of operation pressure。
6. the preparation method according to the arbitrary described double-deck high-entropy alloy diffusion impervious layer of claim 1 to 5, it is characterised in that the Ar flow passed in step (3) is 40sccm, N2Flow is 30sccm。
7. the preparation method according to the arbitrary described double-deck high-entropy alloy diffusion impervious layer of claim 1 to 5, it is characterised in that it is 160～240W that described single crystalline Si matrix reverse sputtering cleans power, biases as-700～-800V。
8. the preparation method according to the arbitrary described double-deck high-entropy alloy diffusion impervious layer of claim 1 to 5, it is characterised in that Ta target, Al target, Cr target, Ni target sheet and Ti target sheet sputter clean power are 60～100W。
9. the preparation method according to the arbitrary described double-deck high-entropy alloy diffusion impervious layer of claim 1 to 5, it is characterised in that Ta target, Al target, Cr target, Ni target sheet and Ti target sheet magnetron sputtering deposition sputtering power are 60～100W。
10. the preparation method according to the arbitrary described double-deck high-entropy alloy diffusion impervious layer of claim 1 to 5, it is characterised in that HEANs thin film and HEAs thin film set thickness as 9～12nm。
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| CN104911556B (en) * | 2015-05-02 | 2018-04-17 | 四川理工学院 | A kind of preparation process of Ni submicron arrays |
| CN108018550B (en) * | 2016-11-04 | 2019-12-03 | 叶均蔚 | Multi-layer film structure |
| CN109989001A (en) * | 2019-04-09 | 2019-07-09 | 西安交通大学 | A kind of method of pulsed laser deposition technique preparation high rigidity infusibility high-entropy alloy film |
| CN109988998A (en) * | 2019-04-09 | 2019-07-09 | 西安交通大学 | A kind of preparation method of polynary high-entropy alloy film |
| CN111441026A (en) * | 2020-05-14 | 2020-07-24 | 南京工业大学 | Preparation method of high-entropy alloy with dual-phase structure |
| CN112064024B (en) * | 2020-09-23 | 2021-08-31 | 广东省科学院新材料研究所 | Diffusion-resistant high-entropy alloy coating material, high-temperature-resistant coating material, and preparation method and application thereof |
| CN114032502B (en) * | 2021-11-23 | 2022-05-03 | 江西省科学院应用物理研究所 | Wear-resistant corrosion-resistant composite layer and preparation method thereof |
| CN114783980B (en) * | 2022-06-21 | 2022-09-23 | 亚芯半导体材料(江苏)有限公司 | Multilayer alloy diffusion impervious layer for Cu interconnection integrated circuit and preparation method thereof |
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