CN102583533A - Synthetic method of anhydrous hafnium zirconium composite nitrate and application of synthetic method to atomic layer deposition (ALD) high-dielectric composite oxide film - Google Patents

Synthetic method of anhydrous hafnium zirconium composite nitrate and application of synthetic method to atomic layer deposition (ALD) high-dielectric composite oxide film Download PDF

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CN102583533A
CN102583533A CN2011100097041A CN201110009704A CN102583533A CN 102583533 A CN102583533 A CN 102583533A CN 2011100097041 A CN2011100097041 A CN 2011100097041A CN 201110009704 A CN201110009704 A CN 201110009704A CN 102583533 A CN102583533 A CN 102583533A
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hafnium zirconium
synthetic method
anhydrous hafnium
nitrate salt
anhydrous
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李爱东
章闻奇
黄柳英
邵起越
吴迪
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Nanjing University
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Nanjing University
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Abstract

The invention discloses a synthetic method of anhydrous hafnium zirconium composite nitrate and application of the synthetic method to an atomic layer deposition (ALD) high-dielectric composite oxide film. The synthetic method comprises the steps that firstly fuming nitric acid reacts with phosphorus pentoxide, generated nitric oxide gas becomes solid nitrogen pentoxide at the low temperature, the solid nitrogen pentoxide is gradually liquefied, dinitrogen tetroxide gas is generated along with the liquefaction of the solid nitrogen pentoxide, the dinitrogen tetroxide fully reacts with mixed metal chloride to finally obtain a white powder-shaped head product of the anhydrous hafnium zirconium composite nitrate, and the anhydrous hafnium zirconium composite nitrate is obtained by means of the head product through a sublimation purification device. The synthetic method successfully prepares the anhydrous hafnium zirconium composite nitrate with good volatility and free of carbon, a simple source serves as an ALD double-metal precursor, the hafnium zirconium composite oxide film is successfully deposited through an ALD method, and good performance is obtained.

Description

The compound method of the compound nitrate salt of a kind of anhydrous hafnium zirconium and deposit the application in the high dielectric composite oxide film at ALD
 
Technical field
The present invention relates to the preparation method of compound nitrate salt, specifically is the compound method of the compound nitrate salt of a kind of anhydrous hafnium zirconium, and uses this compound nitrate salt to deposit the application in the high dielectric composite oxide film at ALD.
Background technology
Metal-oxide-semicondutor FET (MOSFET) is the elementary cell that constitutes memory cell, microprocessor and logical circuit in the silicon-based semiconductor unicircuit, and its volume is directly connected to the integrated level of VLSI.Along with constantly dwindling of feature sizes of semiconductor devices, traditional SiO 2Gate dielectric material can't overcome the influence that the MOSFET device feature size dwindles the quantum tunneling effect that is brought.As the approach of further raising microelectronic device integrated level, seek novel grid dielectric material and replace SiO with high-k (high-k) 2Become the focus of current microelectronic material research.
Hafnia (HfO 2), zirconium white (ZrO 2) film is because it has suitably big specific inductivity, bigger energy gap and the thermodynamic stability of the excellence that contacts with Si, and become one of election contest material the most likely of grid medium with high dielectric of future generation, be the focus of current high-k investigation of materials.But oxygen is at ZrO 2And HfO 2Diffusivity is higher in the film, and the very easy Si substrate surface that is diffused into forms the low-k interfacial layer, cause the ultrathin oxide thin-film dielectric constant of actual fabrication on the low side (k ~ 10-15).In order to improve ZrO 2, HfO 2The specific inductivity of film, people consider to prepare (the hafnium zirconium mixed oxide Hf of k ~ 30-40) of cube phase with high-k xZr 1-xO 2Film, thus the microelectronic device integrated level further improved.
(Atomic layer deposition ALD) because of the three-dimensional stickiness and the uniform big area film forming characteristics of its accurate gauge control, excellence, becomes the prefered method of preparation high-k film to ald.The ALD deposition of MOX, the common metal organic cpds is as metal precursor.These precursors contain elements such as C, Cl, F usually, are prone to remain in worsen film performance in the film.The anhydrous nitrate that it is found that metal has good volatility, can be used for the depositing metal oxide film as a kind of novel carbon-free inorganic precursor.The nitrate radical group only contains N and O element, has avoided the pollution of elements such as C, Cl to film, and the by product oxynitride when being used for the ALD deposition process also is easy to remove.These characteristics make the metal anhydrous nitrate be well suited for the deposition of high k grid dielectric film as novel ALD precursor.In addition, with ALD method deposition binary metal oxide film, the mismatch problem between the metal precursor, like different volatilization temperatures, different heat decomposition temperature and pre-reaction mutually, the successful deposition of binary oxide film that can the remarkably influenced specific components.The composite precursor that employing comprises two kinds of metal constituent elements is kind of an effective solution; This type precursor vapor can stably transport two kinds of metallic elements simultaneously; Therefore the component of deposit film is decided by metal component ratio in the precursor simply, has solved the mismatch problem between the single precursor effectively.The present invention has successfully prepared the compound nitrate salt (Hf of anhydrous hafnium zirconium through a kind of simple and feasible synthesis technique xZr 1-x(NO 3) 4), and,, still do not have the report of relevant this precursor at present with ALD method deposition Hf-Zr-O composite oxide film as metal precursor.
Summary of the invention
Technical problem to be solved by this invention provides a kind of simple and feasible compound nitrate salt synthesis technique of anhydrous hafnium zirconium, and this nitrate salt is in the application that deposits with the ALD method in the high dielectric composite oxide film.
The compound method of the compound nitrate salt of anhydrous hafnium zirconium of the present invention, it may further comprise the steps:
1) 80 ~ 100ml nitrosonitric acid slowly is added dropwise in the Vanadium Pentoxide in FLAKES of about 200 ~ 250g, produces brown oxides of nitrogen gas, remove moisture through drying tube, the HfCl that total mass is 1 ~ 2g is equipped with in input at last 4+ ZrCl 4The muriatic Glass tubing of hybrid metal in, and Glass tubing places liquid nitrogen, nitrogen pentoxide gas is condensed into solid-state at the Glass tubing tube wall at low temperatures gradually;
2) stop to drip nitrosonitric acid, slowly remove liquid nitrogen, let Glass tubing slowly get warm again after a cold spell, solid-state nitrogen pentoxide is liquefied gradually, follow a large amount of brown nitrogen tetroxide gases to produce simultaneously; At room temperature magnetic agitation 1-3 hour then, let nitrogen tetroxide and hybrid metal muriate fully react; Take out oxynitride remaining in the Glass tubing at last, obtain the compound nitrate salt head product of anhydrous hafnium zirconium of white powder;
3) through the further compound nitrate salt head product of anhydrous hafnium zirconium of purifying of sublimation purification device, sublimation temperature is 110 oC, pressure is about 90-100 handkerchiefs, and cold finger adopts the cryosel cooling, and temperature is about-10 oC, the outer tube wall distillation condensation at cold finger at last obtains the compound nitrate salt of the crystalline anhydrous hafnium zirconium of white.
Above-mentioned steps 1) drop rate of nitrosonitric acid is preferably 1ml/min in.
The compound nitrate salt of anhydrous hafnium zirconium that the present invention also requires to protect method for preparing is in the application that deposits with the ALD method in the high dielectric composite oxide film.
The present invention adopts a kind of simple and feasible synthesis technique; Successfully prepared and had good volatility and the compound nitrate salt of carbon-free anhydrous hafnium zirconium; And with this single source as ALD bimetal precursor, successfully deposited hafnium zirconium mixed oxide film with the ALD method, obtained preferable performance.This type of composition metal source synthesis technique is simple, in the unique advantage of ALD depositing ultrathin complex metal oxides grid dielectric film, has important application prospects in the microelectronics industry field.
Description of drawings
Fig. 1 is the synthesizer of the compound nitrate salt of anhydrous hafnium zirconium;
Fig. 2 is the sublimation purification device of the compound nitrate salt of anhydrous hafnium zirconium;
Fig. 3 is the FTIR of the compound nitrate salt of anhydrous hafnium zirconium;
Fig. 4 is that the x-ray photoelectron of hafnium zirconium mixed oxide film is composed entirely;
Fig. 5 a is the x-ray photoelectron power spectrum of hafnium zirconium mixed oxide film O 1s;
Fig. 5 b is the x-ray photoelectron power spectrum of hafnium zirconium mixed oxide film Hf 4f;
Fig. 5 c is the x-ray photoelectron power spectrum of hafnium zirconium mixed oxide film Zr 3d;
Fig. 6 is the capacitance-voltage curve of hafnium zirconium mixed oxide film;
Fig. 7 is the current density-voltage curve of hafnium zirconium mixed oxide film.
Embodiment
One, the embodiment of the synthetic compound nitrate salt of anhydrous hafnium zirconium:
Synthesizer is as shown in Figure 1, and the ground interface is all adopted in all connections, and through Vanadium Pentoxide in FLAKES drying tube and atmosphere, moisture gets into system in the environment to avoid.The compound nitrate salt of anhydrous hafnium zirconium is by liquid nitrogen pentoxide (N 2O 5) and HfCl 4+ ZrCl 4Mixture react generation at normal temperatures, Fig. 2 is the sublimation purification device of the compound nitrate salt of anhydrous hafnium zirconium.
Embodiment 1:
1) like Fig. 1, in synthesizer, 90ml nitrosonitric acid 1 slowly is added dropwise in the Vanadium Pentoxide in FLAKES 2 of about 200g, produce brown oxides of nitrogen gas, remove moisture through drying tube, 0.65g HfCl is equipped with in input at last 4+ 0.48g ZrCl 4In the muriatic Glass tubing 3 of 4 hybrid metal, and Glass tubing places liquid nitrogen 5, and nitrogen pentoxide gas is condensed into solid-state nitrogen pentoxide at the Glass tubing tube wall at low temperatures gradually;
2) stop to drip nitrosonitric acid, slowly remove liquid nitrogen, let Glass tubing slowly get warm again after a cold spell, solid-state nitrogen pentoxide is liquefied gradually, follow a large amount of brown nitrogen tetroxide gases to produce simultaneously; Magnetic agitation 2 hours at room temperature lets nitrogen tetroxide and hybrid metal muriate fully react then; Take out oxynitride remaining in the Glass tubing at last, obtain the compound nitrate salt head product of anhydrous hafnium zirconium of white powder;
3) through the further compound nitrate salt head product of anhydrous hafnium zirconium of purifying of sublimation purification device, sublimation temperature is 110 oC, pressure is about 90-100 handkerchiefs, and cold finger adopts the cryosel cooling, and temperature is about-10 oC, the outer tube wall distillation condensation at cold finger at last obtains the compound nitrate salt of the crystalline anhydrous hafnium zirconium of white.
Embodiment 2:
1) the 95ml nitrosonitric acid slowly is added dropwise in the Vanadium Pentoxide in FLAKES of about 220g, produces brown oxides of nitrogen gas, remove moisture through drying tube, 0.70g HfCl is equipped with in input at last 4+ 0.51g ZrCl 4The muriatic Glass tubing of hybrid metal in, and Glass tubing places liquid nitrogen, nitrogen pentoxide gas is condensed into solid-state at the Glass tubing tube wall at low temperatures gradually;
2) stop to drip nitrosonitric acid, slowly remove liquid nitrogen, let Glass tubing slowly get warm again after a cold spell, solid-state nitrogen pentoxide is liquefied gradually, follow a large amount of brown nitrogen tetroxide gases to produce simultaneously; Magnetic agitation 3 hours at room temperature lets nitrogen tetroxide and hybrid metal muriate fully react then; Take out oxynitride remaining in the Glass tubing at last, obtain the compound nitrate salt head product of anhydrous hafnium zirconium of white powder;
3) through the further compound nitrate salt head product of anhydrous hafnium zirconium of purifying of low pressure distillation device, sublimation temperature is 110 oC, pressure is about 90-100 handkerchiefs, and cold finger adopts the cryosel cooling, and temperature is about-10 oC, the outer tube wall distillation condensation at cold finger at last obtains the compound nitrate salt of the crystalline anhydrous hafnium zirconium of white.
Embodiment 3 :
1) the 100ml nitrosonitric acid slowly is added dropwise in the Vanadium Pentoxide in FLAKES of about 250g, produces brown oxides of nitrogen gas, remove moisture through drying tube, 0.81g HfCl is equipped with in input at last 4+ 0.58g ZrCl 4The muriatic Glass tubing of hybrid metal in, and Glass tubing places liquid nitrogen, nitrogen pentoxide gas is condensed into solid-state at the Glass tubing tube wall at low temperatures gradually;
2) stop to drip nitrosonitric acid, slowly remove liquid nitrogen, let Glass tubing slowly get warm again after a cold spell, solid-state nitrogen pentoxide is liquefied gradually, follow a large amount of brown nitrogen tetroxide gases to produce simultaneously; Magnetic agitation 3 hours at room temperature lets nitrogen tetroxide and hybrid metal muriate fully react then; Take out oxynitride remaining in the Glass tubing at last, obtain the compound nitrate salt head product of anhydrous hafnium zirconium of white powder;
3) through the further compound nitrate salt head product of anhydrous hafnium zirconium of purifying of low pressure distillation device, sublimation temperature is 110 oC, pressure is about 90-100 handkerchiefs, and cold finger adopts the cryosel cooling, and temperature is about-10 oC, the outer tube wall distillation condensation at cold finger at last obtains the compound nitrate salt of the crystalline anhydrous hafnium zirconium of white.
Two, the ALD growth technique of hafnium zirconium mixed oxide film
With the compound nitrate salt of the anhydrous hafnium zirconium of synthetic is the bimetal precursor, deionized water H 2O is as oxygen source, and the source metal temperature is made as 120 oC, reaction chamber temperature are 200 oC.An ALD loop cycle is the compound nitrate salt source metal of anhydrous hafnium zirconium pulse+N of 0.6 second successively by duration 2Clean pulse+H 2O oxygen source pulse+N 2Cleaning pulse four parts forms.The ALD loop cycle is 130 times.
Measure through the inductively coupled plasma spectrographic, confirm that the hafnium zirconium is than being 1.8:1 in the compound nitrate salt of anhydrous hafnium zirconium.Because anhydrous nitrate is very easily suction in air, the present invention adopts " pasty state method " to measure its FTIR.Compound nitrate salt of anhydrous hafnium zirconium and Nujol mull are mixed, in detesting water anaerobism glove box, grind evenly, sealing is preserved to send to and is carried out IR survey.As shown in Figure 3, the nitrate radical absorption peak of the compound nitrate salt of anhydrous hafnium zirconium respectively 1562,1298,1018,773cm -1, the infrared absorption peak of Hf-O key and Zr-O key is very approaching, is positioned at 500cm -1About, INFRARED SPECTRUM has confirmed that the success of the compound nitrate salt of anhydrous hafnium zirconium is synthetic.
As shown in Figure 4, be metal precursor with the compound nitrate salt of the anhydrous hafnium zirconium of synthetic, with ALD method deposition hafnium zirconium mixed oxide Hf xZr 1-xO 2Film.X-ray photoelectron spectroscopy (XPS) analytical table is understood Hf xZr 1-xO 2Film is in the successful deposition of Si substrate.To Hf xZr 1-xO 2Film is surveyed XPS and is composed (Fig. 4) entirely, can see the peak of tangible O, Hf, Zr, and does not have the peak of N to occur, and shows Hf xZr 1-x(NO 3) 4Precursor decomposes in the ALD deposition process fully, does not have the N element residual in film.(Fig. 5 a), Hf 4f (Fig. 5 b), Zr 3d (Fig. 5 c) be XPS and carefully sweep, and can see the 4f of the peak of Hf 4f by 18.1eV to the O 1s of film 5/24f with 16.5eV 7/2Two inferior peaks are formed, corresponding to the bonding of Hf and O; And the peak of Zr 3d is by the 3d of 184.2eV 3/23d with 181.8eV 5/2Two inferior peaks are formed, corresponding to the bonding of Zr and O.The peak of O 1s is carried out match can be found, this peak is that two peaks of 531.2eV and 529.6eV are formed by peak value in fact, corresponds respectively to Hf-O and Zr-O key.Thus, further confirmed hafnium zirconium mixed oxide Hf xZr 1-xO 2The successful deposition of film.
Fig. 6 and Fig. 7 have showed hafnium zirconium mixed oxide Hf xZr 1-xO 2The capacitance-voltage of film (C-V) and current density-voltage (J-V) curve.The survey frequency of C-V curve is 1MHz (Fig. 5), is 6.9nm through the equivalent oxide thickness (CET) that calculates film, flat-band voltage (V Fb) be 1.34V.The shape that can see the C-V curve is tending towards perfect, shows Hf xZr 1-xO 2The interface of film and Si substrate is good.(Fig. 6) reads film at V from the J-V curve FbLeakage current density under the+1V is 8.9 * 10 -6A/cm 2
The above only is a preferred implementation of the present invention, should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvement, and these improvement also should be regarded as protection scope of the present invention.

Claims (3)

1. the compound method of the compound nitrate salt of anhydrous hafnium zirconium is characterized in that may further comprise the steps:
1) 80 ~ 100ml nitrosonitric acid slowly is added dropwise in the Vanadium Pentoxide in FLAKES of about 200 ~ 250g, produces brown oxides of nitrogen gas, remove moisture through drying tube, the HfCl that total mass is 1 ~ 2g is equipped with in input at last 4+ ZrCl 4The muriatic Glass tubing of hybrid metal in, and Glass tubing places liquid nitrogen, nitrogen pentoxide gas is condensed into solid-state at the Glass tubing tube wall at low temperatures gradually;
2) stop to drip nitrosonitric acid, slowly remove liquid nitrogen, let Glass tubing slowly get warm again after a cold spell, solid-state nitrogen pentoxide is liquefied gradually, follow a large amount of brown nitrogen tetroxide gases to produce simultaneously; At room temperature magnetic agitation 1-3 hour then, let nitrogen tetroxide and hybrid metal muriate fully react; Take out oxynitride remaining in the Glass tubing at last, obtain the compound nitrate salt head product of anhydrous hafnium zirconium of white powder;
3) through the further compound nitrate salt head product of anhydrous hafnium zirconium of purifying of sublimation purification device; Sublimation temperature is 110 ℃, and pressure is about 90-100 handkerchiefs, and cold finger adopts the cryosel cooling; Temperature is about-10 ℃, and the outer tube wall distillation condensation at cold finger at last obtains the compound nitrate salt of the crystalline anhydrous hafnium zirconium of white.
2. the compound method of the compound nitrate salt of anhydrous hafnium zirconium according to claim 1, the drop rate that it is characterized in that nitrosonitric acid in the step 1) is 1ml/min.
3. the compound nitrate salt of the described anhydrous hafnium zirconium of claim 1 is adopting the ALD method to deposit the application in the high dielectric composite oxide film.
CN2011100097041A 2011-01-18 2011-01-18 Synthetic method of anhydrous hafnium zirconium composite nitrate and application of synthetic method to atomic layer deposition (ALD) high-dielectric composite oxide film Pending CN102583533A (en)

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CN1693533A (en) * 2005-02-28 2005-11-09 南京大学 Lomposite metallic inorganic source of zirconium hafnium and titanium composited anhydrous nitrate and its synthesis method
CN101290883A (en) * 2008-05-29 2008-10-22 南京大学 Soft chemistry method for preparing ultrathin HfO* or ZrO* gate dielectric membrane
CN101555591A (en) * 2008-04-11 2009-10-14 气体产品与化学公司 Preparation of metal oxide thin film via cyclic cvd or ald

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1396638A (en) * 2001-06-28 2003-02-12 夏普公司 Method for dipositing high-dielectric constant material on chip using atomic layer diposition method
CN1693533A (en) * 2005-02-28 2005-11-09 南京大学 Lomposite metallic inorganic source of zirconium hafnium and titanium composited anhydrous nitrate and its synthesis method
CN101555591A (en) * 2008-04-11 2009-10-14 气体产品与化学公司 Preparation of metal oxide thin film via cyclic cvd or ald
CN101290883A (en) * 2008-05-29 2008-10-22 南京大学 Soft chemistry method for preparing ultrathin HfO* or ZrO* gate dielectric membrane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WENQI ZHANG ET.AL: "Properties of Hf0.7Zr0.3O2Thin Films Chemical Vapor Deposited Using a Single-Source Precursor of Anhydrous HfxZrl-x(NO3)4 Precursors", 《NEXT-GENERATION ELECTRONICS（ISNE）2010 INTERNATIONAL SYMPOSIUM ON》, 19 November 2010 (2010-11-19) *

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Application publication date: 20120718