CN108998771A - The preparation method of thin-film capacitor based on high-k dielectric material - Google Patents
The preparation method of thin-film capacitor based on high-k dielectric material Download PDFInfo
- Publication number
- CN108998771A CN108998771A CN201810774072.XA CN201810774072A CN108998771A CN 108998771 A CN108998771 A CN 108998771A CN 201810774072 A CN201810774072 A CN 201810774072A CN 108998771 A CN108998771 A CN 108998771A
- Authority
- CN
- China
- Prior art keywords
- film
- layer
- sio
- tio
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003990 capacitor Substances 0.000 title claims abstract description 44
- 239000010409 thin film Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000003989 dielectric material Substances 0.000 title claims abstract description 10
- 239000010408 film Substances 0.000 claims abstract description 95
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910020286 SiOxNy Inorganic materials 0.000 claims abstract description 46
- 238000000151 deposition Methods 0.000 claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 22
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 18
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 17
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims description 31
- 238000004544 sputter deposition Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 18
- 239000004411 aluminium Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 230000008020 evaporation Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 13
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 8
- 230000005611 electricity Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 238000007738 vacuum evaporation Methods 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical group 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical group [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000000427 thin-film deposition Methods 0.000 description 2
- -1 as shown in Figure 1 Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0676—Oxynitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/10—Metal-oxide dielectrics
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Composite Materials (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of preparation methods of thin-film capacitor based on high-k dielectric material.The following steps are included: preparing thin-film capacitor bottom nano aluminum layer film using evaporation coating, bottom conductive layer is formed；Utilize reactive sputter-deposition SiOxNyFilm layer, then pass through r. f. magnetron sputtering TiO2Layer, prepares high k TiO2/SiOxNyIntermediate insulating layer TiO2Film forms intermediate dielectric layer；Preparation top nano aluminum layer film, forms top conductive layer；Finally, can be prepared by high-k dielectric base film capacitor by annealing.High-k dielectric base film capacitor preparation process of the invention is simple, low in cost, and is not necessarily to specific template；The size of intermediate dielectric layer k value can be regulated and controled by depositing operation, and thin-film capacitor frequency characteristic and dielectric properties are excellent, and stability is high, and consistency is good, is applicable to high-frequency section.
Description
Technical field
The present invention relates to the technologies of preparing of high-k dielectric material base film capacitor, can be right by changing deposition process parameters
The k value of dielectric film is regulated and controled, and is that a kind of frequency characteristic and dielectric properties are excellent, and stability is high, is applicable to high-frequency section
Thin-film capacitor.
Background technique
Thin dielectric film plays a key effect to the performance of capacitor.From the nineties in last century, after proposing High k concept,
High-k dielectric is had been investigated as there are many material, mainly there is metal oxide, nitrogen oxides and pseudobinary alloy.Metal oxygen
In compound, TiO2With high dielectric constant, by extensive concern.Pseudobinary alloy refers to that two kinds of metal oxides are mixed through technique
It obtains, crystallinity is improved, and leakage current reduces, but is compared to original metal oxide, and dielectric constant reduces.Nitrogen oxygen
Compound is a kind of high-k dielectric, can not only improve thermal stability, moreover it is possible to solve the diffusion problem in technique.Currently, research compared with
More nitrogen oxides dielectrics are SiOxNy。
In addition to the property factor of material itself, performance of the thin film deposition processes to high-k dielectric, it may have many shadows
It rings.SiOxNyElectrolyte can realize the regulation to film performance by changing ratio of nitrogen to oxygen.With the increase of nitrogen atom content,
Dielectric constant increases to 7.9 from 3.9.But as nitrogen-atoms further increases, defect state density also be will increase.Therefore, it is necessary to
Dielectric constant and defect state density are had both, by rationally designing nitrogen oxygen atom ratio, while obtaining high k, avoids biggish defect
Density.Currently, deposition SiOxNyThe main method of film is CVD technique.However, the defect of this kind of technique is to be easy in the film
Generate impurity.Reactive sputtering is as a kind of low temperature deposition process, and preparation is easy and parameter is controllable, and still, film deposition rate is slow.
Therefore, for reactive sputtering process, how SiO is improvedxNyThe deposition rate of film is current problem to be solved.
TiO2Crystal structure decide the size of its dielectric constant, anatase structured TiO2Dielectric constant is 30, and golden red
Stone structure TiO2Up to 80.However, it is contemplated that fringing field effect, not the higher the better for dielectric constant.And TiO2The lattice knot of film
Structure is controlled by preparation process, therefore, changes thin film preparation process, it can be achieved that TiO2The regulation of dielectric constant.Stepped construction conduct
A kind of special structure can be good at improving TiO2Thin film dielectric performance.Therefore, it is badly in need of exploitation new process, prepares high k's
TiO2/SiOxNyStepped construction improves the comprehensive performance of thin-film capacitor.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of thin-film capacitor based on high-k dielectric material, using anti-
Answer sputtering sedimentation SiOxNyFilm layer optimizes film performance, technique is overcome to synthesize defect by adjusting nitrogen oxygen atom ratio；Using penetrating
Frequency magnetron sputtering depositing Ti O2Layer, by changing technological parameter, the TiO of preparation2/SiOxNyIntermediate insulating layer TiO2 film is formed
Intermediate dielectric layer is laminated, solves the problems, such as high k；Thin-film capacitor bottom nano aluminum layer film is prepared using evaporation coating；Finally, passing through
Annealing, can be prepared by high-k dielectric base film capacitor.Preparation process is simple, low in cost；The size of k value can be by heavy
Product technique is regulated and controled, and thin-film capacitor frequency characteristic and dielectric properties are excellent, and stability is high.
To achieve the above object, the invention provides the following technical scheme: using single crystalline Si substrate, vacuum degree is not less than 10-3
Pa, coiling speed are 100-200 m/min, by being evaporated in vacuo aluminium, deposit nano aluminum layer film, form bottom conductive layer；It will
The Si substrate that deposited aluminium film, in Ar/O2/ N2Gas flow is respectively under the atmosphere of 10.5,0.4-1,0.4-1 sccm, into
Row reactive sputtering, SiO in depositionxNyFilm layer；In the sputtering power of 200-500 W, 150-300 DEG C of underlayer temperature and
Under the Ar sputtering pressure of 0.2-0.6 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNyIntermediate insulation
Layer TiO2 film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo aluminium, shape under conditions of coiling speed is 100-200 m/min
At bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, it is thin to can be prepared by high-k dielectric base
Membrane capacitance；
Further, the SiOxNyFilm, using single crystalline Si as substrate, on sputtering platform, Ar/O2/ N2Under atmosphere, carry out
Reactive sputtering deposits SiOxNyFilm；Argon gas stream is 8-10.5 sccm, and oxygen stream is 0.4-1 sccm, nitrogen stream 0.4-1
Sccm, vacuum degree are not less than 10-3Pa；Sputtering power is stablized in 400 W, and target-substrate distance is 100 mm；In reactive sputter-deposition
SiOxNyBefore film, in reaction system, ultraviolet radiation facility is added, improves the ionization level of nitrogen oxygen precursor, it is anti-to improve nitrogen oxygen
Answer the doping efficiency of gas；
Further, the TiO2/SiOxNyIntermediate insulating layer TiO2Film, deposited SiOxNyThe Si piece of film is as base
Bottom carries out rf magnetron sputtering, depositing Ti O on rf magnetron sputtering platform2/SiOxNyInterlevel dielectric layer film；Sputter function
Rate is 200-500 W, and underlayer temperature is 150-300 DEG C, and Ar sputtering pressure is 0.2-0.6 Pa, and target-substrate distance is 100 mm；In order to
Convenient for the control of membrane structure, to TiO2Film carries out 2% Pt particle doping, while preventing TiO2The dielectric constant mistake of film
It is high；
Further, the bottom and top conductive layer are all Al film, by being evaporated in vacuo Al block, are deposited as Al film；
Vacuum degree is not less than 10-3Pa, coiling speed are 120 m/min.
Further, the Al/TiO2/SiOxNy/ Al thin-film capacitor is made annealing treatment, atmosphere N2, annealing temperature
Degree is at 400 DEG C, and annealing time is 1 h.
Further, the substrate is that single crystalline Si has carried out following cleaning: a. immerses Si piece in cleaning solution, and ingredient is
H2SO4And KMnO4Mixed solution, ebuillition of heated simultaneously keep 2 h, remove substrate on oxide；B. deionized water is used, and is led to
Ultrasonic cleaning Si piece 3 times are crossed, every time 10 min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；
D. Si piece is put into deionized water again, is cleaned by ultrasonic 5 min, is put into vacuum oven and dries.
Further, the intermediate dielectric layer TiO2/SiOxNyK value size, can be adjusted by thin film deposition processes
Control is realized to Al/TiO2/SiOxNyThe optimization of/Al thin-film capacitor dielectric properties.
Compared to the prior art, the invention has the following advantages: it is thin to develop high k lamination by optimization preparation process
Film；Thin-film capacitor bottom nano aluminum layer film is prepared using evaporation coating, forms bottom conductive layer；Utilize reactive sputter-deposition
SiOxNyFilm layer, then pass through r. f. magnetron sputtering TiO2Layer, prepares high k TiO2/SiOxNyIntermediate insulating layer TiO2It is thin
Film forms intermediate dielectric layer, solves the problems, such as high K thin film preparation process；Preparation top nano aluminum layer film, forms top conductive
Layer；Finally, can be prepared by high-k dielectric base film capacitor by annealing.High-k dielectric base film capacitor of the invention
Preparation process is simple, low in cost；The size of intermediate dielectric layer k value can be regulated and controled by depositing operation, thin-film capacitor frequency
Characteristic is excellent with dielectric properties, and stability is high, is applicable to high-frequency section.
Detailed description of the invention
A kind of structural schematic diagram of the thin-film capacitor based on high-k dielectric material in Fig. 1 present invention.
A kind of preparation flow figure of the thin-film capacitor based on high-k dielectric material in Fig. 2 present invention.
Specific embodiment
A kind of preparation method of the thin-film capacitor based on high-k dielectric material, as shown in Figure 1, composition is led by aluminum film layer
Electric layer, high k TiO2/SiOxNyFilm layer, as intermediate dielectric layer；Fig. 2 is the preparation flow of thin-film capacitor.Below in conjunction with this
Attached drawing in invention, technical scheme in the embodiment of the invention is clearly and completely described.
Embodiment 1
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.4,0.4 sccm；In the sputtering power of 200 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 2
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.6,0.6 sccm；In the sputtering power of 200 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 3
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.8,0.8 sccm；In the sputtering power of 200 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 4
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,1.0,1.0 sccm；In the sputtering power of 200 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Detect SiO under different nitrogen oxygen reaction gas flowsxNyRatio shared by oxygen atom in film.As shown in table 1, with
Nitrogen oxygen reaction gas flow increases, SiOxNyRatio shared by oxygen atom rises in film.
Ratio shared by oxygen atom in SiOxNy film under the different nitrogen oxygen reaction gas flows of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Oxygen atom ratio | 0.41 | 0.56 | 0.64 | 0.78 |
Table 2 is the situation of change of thin-film dielectric constant deposition rate as oxygen flow changes.When oxygen flow is from 0.4 sccm
1.0 sccm are increased to, dielectric constant is reduced to 3.6 by 7.3.When oxygen flow is 0.4 sccm, deposition rate highest,
Reach 22.1 nm/min.As oxygen flow increases to 0.6 sccm, deposition rate is still higher, is maintained at 15 nm/min.
However, deposition rate is lower, is reduced to 7.6 nm/min when oxygen flow is further increased to 1.0 sccm.
The situation of change of 2 thin-film dielectric constant deposition rate of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Dielectric constant | 6.5 | 5.9 | 5.2 | 4.7 |
| It deposits digit rate (nm/min) | 17.6 | 15.1 | 14.4 | 12.5 |
Embodiment 5
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.8,0.8 sccm；In the sputtering power of 200 W, 250 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 6
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.8,0.8 sccm；In the sputtering power of 200 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.2 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 7
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.8,0.8 sccm；In the sputtering power of 200 W, 300 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.6 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Embodiment 8
The preparation flow of thin-film capacitor: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, heating
It boils and keeps 2 h, remove the oxide in substrate；B. deionized water is used, and by ultrasonic cleaning Si piece 3 times, every time 10
min；C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again,
It is cleaned by ultrasonic 5 min, is put into vacuum oven and dries；Then, vacuum evaporation, deposited bottom Al conductive layer, vacuum degree are utilized
Not less than 10-3 Pa, coiling speed are 150 m/min；By reactive sputtering, in the Si substrate that deposited aluminium film, in deposition
SiOxNyFilm layer, Ar/O2/ N2Gas flow is respectively 10.5,0.8,0.8 sccm；In the sputtering power of 400 W, 150 DEG C
Under the Ar sputtering pressure of underlayer temperature and 0.5 Pa, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/SiOxNy
Intermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa is evaporated in vacuo under conditions of coiling speed is 150 m/min
Aluminium forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, high k electricity is can be prepared by and is situated between
Matter base film capacitor.
Table 3 is resulting TiO under different sputtering pressures, underlayer temperature and sputtering power2The dielectric constant of film, this
Technique in invention can be by TiO2The dielectric constant of film is efficiently controlled in 30-80.
Gained TiO under the different sputtering pressures of table 3, underlayer temperature and sputtering power2The dielectric constant of film
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Dielectric constant | 30 | 45 | 52 | 67 |
Using technical solution of the present invention or those skilled in the art under the inspiration of technical solution of the present invention, design
Similar technical solution, and reach above-mentioned technical effect, it is to fall into protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the thin-film capacitor based on high-k dielectric material, which is characterized in that use single crystalline Si substrate, very
Reciprocal of duty cycle is not less than 10-3 Pa, coiling speed are 100-200 m/min, by being evaporated in vacuo aluminium, deposit nano aluminum layer film, are formed
Bottom conductive layer；The Si substrate of aluminium film will be deposited, in Ar/O2/ N2Gas flow is respectively 10.5,0.4-1,0.4-1
Under the atmosphere of sccm, reactive sputtering, SiO in deposition are carried outxNyFilm layer；In the sputtering power of 200-500 W, 150-300 DEG C
Underlayer temperature and 0.2-0.6 Pa Ar sputtering pressure under, pass through rf magnetron sputtering, depositing Ti O2Layer, prepares TiO2/
SiOxNyIntermediate insulating layer TiO2Film；It is not less than 10 in vacuum degree-3Pa, under conditions of coiling speed is 100-200 m/min,
It is evaporated in vacuo aluminium, forms bottom conductive layer；Finally, in N2In atmosphere, at 400 DEG C, the annealing of 1 h is carried out, can be prepared by
High-k dielectric base film capacitor.
2. preparation method according to claim 1, wherein the SiOxNyFilm is flat in sputtering using single crystalline Si as substrate
On platform, Ar/O2/ N2Under atmosphere, reactive sputtering is carried out, deposits SiOxNyFilm；Argon gas stream is 8-10.5sccm, and oxygen stream is
0.4-1 sccm, nitrogen stream are 0.4-1 sccm, and vacuum degree is not less than 10-3Pa；Sputtering power is stablized in 400 W, and target-substrate distance is
100 mm；In reactive sputter-deposition SiOxNyBefore film, in reaction system, ultraviolet radiation facility is added, improves nitrogen oxygen precursor
Ionization level, to improve the doping efficiency of nitrogen oxygen reaction gas.
3. preparation method according to claim 1, wherein the TiO2/SiOxNyIntermediate insulating layer TiO2Film, with deposition
SiOxNyThe Si piece of film is as substrate, on rf magnetron sputtering platform, carries out rf magnetron sputtering, depositing Ti O2/
SiOxNyInterlevel dielectric layer film；Target-substrate distance is 100 mm；For the ease of the control of membrane structure, to TiO2Film carries out 2%
The doping of Pt particle, while preventing TiO2The dielectric constant of film is excessively high.
4. preparation method according to claim 1 passes through vacuum wherein the bottom and top conductive layer are all Al film
Al block is evaporated, Al film is deposited as.
5. preparation method according to claim 1, first to single crystalline Si substrate, is oriented to before making thin-film capacitor
<1ll>, is cleaned as follows: a. immerses Si piece in cleaning solution, ingredient H2SO4And KMnO4Mixed solution, ebuillition of heated
And 2 h are kept, remove the oxide in substrate；B. deionized water is used, and passes through ultrasonic cleaning Si piece 3 times, every time 10 min；
C. ethanol solution is used, and passes through ultrasonic cleaning Si piece 3 times, every time 15 min；D. Si piece is put into deionized water again, ultrasound is clear
5 min are washed, is put into vacuum oven and dries.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810774072.XA CN108998771A (en) | 2018-07-15 | 2018-07-15 | The preparation method of thin-film capacitor based on high-k dielectric material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810774072.XA CN108998771A (en) | 2018-07-15 | 2018-07-15 | The preparation method of thin-film capacitor based on high-k dielectric material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108998771A true CN108998771A (en) | 2018-12-14 |
Family
ID=64599093
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810774072.XA Pending CN108998771A (en) | 2018-07-15 | 2018-07-15 | The preparation method of thin-film capacitor based on high-k dielectric material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108998771A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696091A (en) * | 2008-06-30 | 2010-04-21 | 肖特股份有限公司 | Device for reflecting heat radiation, a method for production of and use of same |
| US20160216419A1 (en) * | 2015-01-23 | 2016-07-28 | Materion Corporation | Near infrared optical interference filters with improved transmission |
-
2018
- 2018-07-15 CN CN201810774072.XA patent/CN108998771A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696091A (en) * | 2008-06-30 | 2010-04-21 | 肖特股份有限公司 | Device for reflecting heat radiation, a method for production of and use of same |
| US20160216419A1 (en) * | 2015-01-23 | 2016-07-28 | Materion Corporation | Near infrared optical interference filters with improved transmission |
Non-Patent Citations (1)
| Title |
|---|
| 徐文彬: "TiO2/ SiO2和TiO2/ SiOx Ny 层叠结构高k 栅介质比较研究", 《半导体技术》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5581527B2 (en) | Transparent conductive film, manufacturing method thereof, transparent electrode and solar cell | |
| WO2017045398A1 (en) | Low-temperature deposition method for vanadium dioxide thin film | |
| CN110595084A (en) | Metal gradual-change high-temperature solar energy absorption coating and preparation method thereof | |
| CN107058962A (en) | A kind of method that low temperature magnetic sputtering prepares low-resistivity titanium nitride membrane | |
| Chandra et al. | Structural and electrical properties of radio frequency magnetron sputtered tantalum oxide films: Influence of post-deposition annealing | |
| CN101323946A (en) | Preparation of nanocrystalline metal Ta film having out phase structure | |
| CN108281414A (en) | A kind of capacitance and preparation method thereof, semiconductor equipment | |
| CN113186528B (en) | Platinum film and preparation method and application thereof | |
| CN102097209A (en) | Method for preparing capacitor with composite titanium dioxide thin film as dielectric | |
| CN108998771A (en) | The preparation method of thin-film capacitor based on high-k dielectric material | |
| CN102157262B (en) | Method for preparing capacitor with Ta205 thin film as dielectric film | |
| JP5516438B2 (en) | Thermochromic body and method for producing the same | |
| CN103215556A (en) | Rapid deposition process for combined-type spectrally selective absorption film layer | |
| CN106431012A (en) | Temperable high-transparency and low-radiation coated glass and manufacturing method thereof | |
| CN108441833B (en) | Multilayer transparent conductive film and preparation method thereof | |
| CN111063724A (en) | Vertical AlN Schottky diode based on drift region multi-layer gradient doping and manufacturing method | |
| CN101831618B (en) | Gate dielectric film with TiO2/ZrO2 two-layer stack structure and high dielectric constant and preparation method thereof | |
| CN109536904B (en) | Doped TiO (titanium dioxide)2Barrier layer film and preparation method thereof | |
| CN101527264B (en) | Gate dielectric taking TiO2 as MOS structure and preparation method thereof | |
| CN104538113B (en) | Superconducting coating Y2Ce2O7The preparation method of transition layer film | |
| CN109065715B (en) | Memristive switching device based on a-TSC-O ceramic film and preparation method thereof | |
| CN102779845A (en) | Laminated metallic oxide gate dielectric layer and preparation method thereof | |
| CN106328821B (en) | A kind of method for preparing perovskite solar cell hole transmission layer cobalt oxide films | |
| CN104532186A (en) | Method for preparing BTS film by virtue of radio frequency magnetron sputtering | |
| CN100431157C (en) | Oxide ferroelectric memory cell and prepn process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181214 |