CN102864410A - Preparation method of high dielectric constant gate dielectric lanthanum titanium oxide amorphous film - Google Patents
Preparation method of high dielectric constant gate dielectric lanthanum titanium oxide amorphous film Download PDFInfo
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- CN102864410A CN102864410A CN2012103189798A CN201210318979A CN102864410A CN 102864410 A CN102864410 A CN 102864410A CN 2012103189798 A CN2012103189798 A CN 2012103189798A CN 201210318979 A CN201210318979 A CN 201210318979A CN 102864410 A CN102864410 A CN 102864410A
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- titanium oxide
- amorphous film
- lanthanum
- noncrystal membrane
- lanthanum titanium
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Abstract
The invention discloses a preparation method of a high dielectric constant gate dielectric lanthanum titanium oxide amorphous film, for solving the technical problem that the leakage current density of the lanthanum titanium oxide amorphous film prepared by the existing method is high. According to the technical scheme, LaTiO3.5 particles are used as the coating material for evaporation, p-type Si(100) is used as a substrate; after the substrate is washed, a heating system is used to heat and evaporate the substrate in a vacuum chamber, wherein the temperature is kept at 100-250 DEG C, the evaporation time is 1-6min, the electronic gun beam is 70-90mA, the vacuum degree of the vacuum chamber is less than 3*10<-3>Pa, and O2 of which the purity is 99.99% is used as a reaction gas in the evaporation process; a deposited lanthanum titanium oxide amorphous film is obtained; and rapid annealing is performed on the deposited lanthanum titanium oxide amorphous film at 700-900 DEG C for 1-5min to obtain the lanthanum titanium oxide amorphous film. By optimizing the formula and technology of the lanthanum titanium oxide amorphous film, the lanthanum titanium oxide amorphous film with low leakage current density and high dielectric constant is obtained. The prepared lanthanum titanium oxide amorphous film has low leakage current density which is reduced from 10<-6>A/cm<2> in the background technology to 6.5*10<-7>A/cm<2>.
Description
Technical field
The invention belongs to the function ceramics field, relate to a kind of preparation method of lanthanum titanyl noncrystal membrane, particularly relate to a kind of preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane.
Background technology
Along with the widespread use of integrated components and parts in microelectronics, moderate in the urgent need to specific inductivity under a kind of room temperature condition, leakage current is little, have simultaneously higher voltage breakdown and the functional materials of less equivalent gate oxide thickness, lanthanum titanyl noncrystal membrane is considered to a kind of candidate material that gets a good chance of.The more high k gate insulation dielectric material that conducts a research both at home and abroad at present mainly is metal oxide, such as TiO
2, ZrO
2, HfO
2, Er
2O
3, Ta
2O
5, Y
2O
3, Al
2O
3, Gd
2O
3, La
2O
3And silicate (M-Si-O, M=Zr, Hf, La, Gd etc., aluminate (M-Al-O, M=Zr, Hf, La etc.).But the specific inductivity of these materials and leakage current can not satisfy the requirement of instrument simultaneously.
Document " M.Li, Z.Zhang, S.A.Campbell et al.Electrical and material characterizations of high-permittivity Hf
xTi
1-xO
2Gate insulatorsa.Journal of Applied Physics.2005,98:054506 " a kind of preparation method of lanthanum titanyl noncrystal membrane disclosed; and the method adopts traditional method for manufacturing thin film to prepare lanthanum titanyl noncrystal membrane; still, the leakage current density (～10 of prepared lanthanum titanyl noncrystal membrane
-6) also undesirable.
Summary of the invention
For the large deficiency of leakage current density of the lanthanum titanyl noncrystal membrane that overcomes the preparation of existing method, the invention provides a kind of preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane.The method can obtain the lanthanum titanyl noncrystal membrane that leakage current density is little, specific inductivity is high by optimizing the composition and engineering of lanthanum titanyl noncrystal membrane.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane is characterized in may further comprise the steps:
(a) with purity be 99.99% LaTiO
3.5Particle is as the coating materials of evaporation, and substrate adopts p-type Si (100);
(b) after substrate thoroughly cleans, in vacuum chamber, with heating system substrate is carried out heating evaporation, make its temperature remain on 100～250 ° of C.Evaporation time is 1～6min, and electron beam gun line size is 70～90mA.Vacuum tightness is less than 3 * 10 in the vacuum chamber
-3Pa in the evaporative process, uses the O of purity 99.99%
2As reactant gases.Obtain the lanthanum titanyl noncrystal membrane of deposited.
(c) the lanthanum titanyl noncrystal membrane of deposited obtains lanthanum titanyl noncrystal membrane at 700～900 ° of C short annealing 1～5min.
Described LaTiO
3.5The diameter of particle is 2～3mm.
The diameter of described substrate is 75mm.
The resistivity of described p-type Si (100) is 2～10 Ω cm.
The invention has the beneficial effects as follows: owing to by optimizing the composition and engineering of lanthanum titanyl noncrystal membrane, obtain the lanthanum titanyl noncrystal membrane that leakage current density is little, specific inductivity is high.The leakage current density of prepared lanthanum titanyl noncrystal membrane by background technology～10
-6A/cm
2Be reduced to～6.5 * 10
-7A/cm
2Specific inductivity has reached 19.1 simultaneously, has kept higher level.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the XRD figure spectrum of four prepared lanthanum titanyls of embodiment of the inventive method noncrystal membrane under aerobic and oxygen free condition.
Fig. 2 be four prepared lanthanum titanyls of embodiment of the inventive method noncrystal membrane under aerobic and oxygen free condition electric current with the curve of voltage change.
Fig. 3 is the time dependent curves of the inventive method embodiment 2 prepared lanthanum titanyl noncrystal membrane deposited voltage breakdowns, and voltage breakdown is 22.4V.
Fig. 4 is the time dependent curve of voltage breakdown that the inventive method embodiment 3 prepared lanthanum titanyl noncrystal membranes record after annealed, and voltage breakdown is 54.5V behind the short annealing 1min.
Fig. 5 is the time dependent curve of voltage breakdown that the inventive method embodiment 3 prepared lanthanum titanyl noncrystal membranes record after annealed, and voltage breakdown is reduced to 8.7V behind the short annealing 5min.
Embodiment
Following examples are with reference to Fig. 1～5.
Embodiment 1, and weighing purity is 99.99% LaTiO
3.5Particle is as coating materials, LaTiO
3.5Granular size is 2-3mm.Adopt diameter be the p-type Si (100) of 75mm as substrate, its resistivity is 2-10 Ω cm, thickness is 0.5mm.After substrate thoroughly cleans up, put into rapidly vacuum chamber, with heating system substrate is heated, make its temperature remain on 100 ° of C.Base vacuum is less than 3 * 10 before the evaporation
-3Pa in the evaporative process, in order to obtain higher oxygen level, uses the O of purity 99.99%
2As reactant gases.Evaporation time is 6min, and electron beam gun line size is 70mA, obtains the lanthanum titanyl noncrystal membrane of deposited.The film of deposited obtains lanthanum titanyl noncrystal membrane at 700 ° of C short annealing 5min.
Use XRD that the film phase structure is analyzed; Use XPS that the composition of film is analyzed; And adopt electric impedance analyzer and semiconductor analysis instrument test platform that dielectric properties and the I-V characteristic of film are tested.The XRD figure spectrum that obtains after the annealing when curve a is 700 ° of C among Fig. 1 can be found out for still keeping amorphous structure.Fig. 2 can find out that for the changing conditions with bias voltage of gained leakage current density under the rear different oxygen atmosphere conditions of annealing leakage current density reaches 5.5 * 10 under the oxygen free condition
-5A/cm
2
Embodiment 2, and weighing purity is 99.99% LaTiO
3.5Particle is as coating materials, LaTiO
3.5Granular size is 2-3mm.Adopt diameter be the p-type Si (100) of 75mm as substrate, its resistivity is 2-10 Ω cm, thickness is 0.5mm.After substrate thoroughly cleans up, put into rapidly vacuum chamber, with heating system substrate is heated, make its temperature remain on 150 ° of C.Base vacuum is less than 3 * 10 before the evaporation
-3Pa in the evaporative process, in order to obtain higher oxygen level, uses the O of purity 99.99%
2As reactant gases.Evaporation time is 4min, and electron beam gun line size is 80mA, obtains the lanthanum titanyl noncrystal membrane of deposited.The film of deposited obtains lanthanum titanyl noncrystal membrane at 750 ° of C short annealing 4min.
Use XRD and SEM that film phase structure and appearance structure are analyzed; Use XPS that the composition of film is analyzed; And adopt electric impedance analyzer and semiconductor analysis instrument test platform that dielectric properties and the I-V characteristic of film are measured.Fig. 2 can find out that for the changing conditions with bias voltage of gained leakage current density under the rear different oxygen atmosphere conditions of annealing leakage current density reaches 6.5 * 10 under the aerobic conditions
-7A/cm
2Under the aerobic conditions annealing after voltage breakdown change curve as shown in Figure 3, Fig. 3 represents that the deposited voltage breakdown of lanthanum titanyl noncrystal membrane is 22.4V.
Use XRD and SEM that film phase structure and appearance structure are analyzed; Use XPS that the composition of film is analyzed; And adopt electric impedance analyzer and semiconductor analysis instrument test platform that dielectric properties and the I-V characteristic of film are measured.The XRD figure spectrum that obtains after the annealing when curve b is 800 ° of C among Fig. 1 can find out that film begins to change to crystalline state from non-crystalline state.Under the aerobic conditions after the annealing change curve of voltage breakdown as shown in Figure 4, Fig. 4 represents that voltage breakdown is 54.5V behind the lanthanum titanyl noncrystal membrane short annealing 1min.
Use XRD and SEM that film phase structure and appearance structure are analyzed; Use XPS that the composition of film is analyzed; And adopt electric impedance analyzer and semiconductor analysis instrument test platform that dielectric properties and the I-V characteristic of film are measured.The XRD figure spectrum that obtains after the annealing when curve c is 900 ° of C among Fig. 1 can find out that for diffraction peak is more obvious, film begins to change to crystalline state from non-crystalline state.Under the aerobic conditions annealing after voltage breakdown change curve as shown in Figure 5, voltage breakdown was reduced to 8.7V after Fig. 5 represented lanthanum titanyl noncrystal membrane short annealing 5min.
In a word, the present invention has prepared lanthanum titanyl noncrystal membrane by traditional thin film preparation process, and through suitable oxygen atmosphere control and suitable temperature control, film keeps lower leakage current density (～6.5 * 10 under aerobic conditions
-7A/cm
2) and higher specific inductivity (19.1).Therefore lanthanum titanyl noncrystal membrane of the present invention can well satisfy the service requirements of storer and integrated component, and its prescription and preparation method are fit to industrialization promotion and production in enormous quantities.
Claims (4)
1. the preparation method of a grid medium with high dielectric lanthanum titanyl noncrystal membrane is characterized in that may further comprise the steps:
(a) with purity be 99.99% LaTiO
3.5Particle is as the coating materials of evaporation, and substrate adopts p-type Si (100);
(b) after substrate thoroughly cleans, in vacuum chamber, with heating system substrate is carried out heating evaporation, make its temperature remain on 100～250 ° of C; Evaporation time is 1～6min, and electron beam gun line size is 70～90mA; Vacuum tightness is less than 3 * 10 in the vacuum chamber
-3Pa in the evaporative process, uses the O of purity 99.99%
2As reactant gases; Obtain the lanthanum titanyl noncrystal membrane of deposited;
(c) the lanthanum titanyl noncrystal membrane of deposited obtains lanthanum titanyl noncrystal membrane at 700～900 ° of C short annealing 1～5min.
2. the preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane according to claim 1 is characterized in that: described LaTiO
3.5The diameter of particle is 2～3mm.
3. the preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane according to claim 1, it is characterized in that: the diameter of described substrate is 75mm.
4. the preparation method of grid medium with high dielectric lanthanum titanyl noncrystal membrane according to claim 1, it is characterized in that: the resistivity of described p-type Si (100) is 2～10 Ω cm.
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Cited By (1)
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|---|---|---|---|---|
| CN114197048A (en) * | 2021-12-08 | 2022-03-18 | 电子科技大学长三角研究院(湖州) | Single crystal film with two-dimensional electron gas and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060084251A1 (en) * | 2004-10-18 | 2006-04-20 | Fujitsu Limited | Plating method, semiconductor device fabrication method and circuit board fabrication method |
| CN101200794A (en) * | 2007-07-09 | 2008-06-18 | 昆山光铭光电子元件有限公司 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060084251A1 (en) * | 2004-10-18 | 2006-04-20 | Fujitsu Limited | Plating method, semiconductor device fabrication method and circuit board fabrication method |
| CN101200794A (en) * | 2007-07-09 | 2008-06-18 | 昆山光铭光电子元件有限公司 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
Non-Patent Citations (3)
| Title |
|---|
| M.LI ET.AL: "Electrical and material characterizations of high-permittivity HfxTi1-xO2 gate insulators", 《JOURNAL OF APPLIED PHYSICS》 * |
| 杨陈等: "等离子辅助电子束蒸发La2O3 薄膜的制备", 《稀有金属材料与工程》 * |
| 郭鸣等: "新一代CMOS 器件栅介质材料研究进展", 《井冈山大学学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114197048A (en) * | 2021-12-08 | 2022-03-18 | 电子科技大学长三角研究院(湖州) | Single crystal film with two-dimensional electron gas and preparation method thereof |
| CN114197048B (en) * | 2021-12-08 | 2024-04-09 | 电子科技大学长三角研究院(湖州) | Monocrystalline film with two-dimensional electron gas and preparation method thereof |
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Application publication date: 20130109 |