CN104425213B - A kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate - Google Patents

A kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate Download PDF

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CN104425213B
CN104425213B CN201310377507.4A CN201310377507A CN104425213B CN 104425213 B CN104425213 B CN 104425213B CN 201310377507 A CN201310377507 A CN 201310377507A CN 104425213 B CN104425213 B CN 104425213B
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gaas substrate
strontium titanate
barium strontium
gaas
prepared
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CN201310377507.4A
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CN104425213A (en
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魏贤华
黄文�
郝建华
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香港理工大学
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L29/00Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof; Multistep manufacturing processes therefor
    • H01L29/66Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/66007Multistep manufacturing processes
    • H01L29/66075Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials
    • H01L29/66227Multistep manufacturing processes of devices having semiconductor bodies comprising group 14 or group 13/15 materials the devices being controllable only by the electric current supplied or the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched, e.g. three-terminal devices
    • H01L29/66409Unipolar field-effect transistors
    • H01L29/66477Unipolar field-effect transistors with an insulated gate, i.e. MISFET
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02107Forming insulating materials on a substrate
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02107Forming insulating materials on a substrate
    • H01L21/02225Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02107Forming insulating materials on a substrate
    • H01L21/02225Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/324Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering

Abstract

The invention discloses a kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate, comprise the following steps:S1:Surface treatment is done to GaAs substrates and forms clean surface of the arsenic atom of atomically flating for termination face;S2:Prepare barium strontium titanate colloidal sol;S3:Above-mentioned steps S2 is prepared to obtained barium strontium titanate sol solution to be added dropwise on the GaAs substrate that above-mentioned steps S1 is obtained, whirl coating is carried out;S4:Dry;S5:Baking pretreatment;S6:The pretreated GaAs substrate of above-mentioned steps S5 bakings is placed in quartz ampoule and is passed through in a certain proportion of protective atmosphere, is made annealing treatment under specified temp, barium strontium titanate dielectric film is made.The barium strontium titanate dielectric film crystalline quality prepared using the chemical method of the present invention is good, surfacing and dielectric properties keep stable with frequency, in the range of 100KHz 1MHz, dielectric constant is higher than 250, and the making requirement of MOSFET device can be met in structure.

Description

A kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate

Technical field

The present invention relates to ferroelectric properties field of material technology, prepared more specifically to one kind on GaAs substrate The chemical method of barium strontium titanate dielectric film.

Background technology

GaAs(GaAs)With characteristics such as electron mobility height, broad-band gap and high strike electric fields, it has also become prepare at a high speed, greatly The important materials of power solid device.In recent years, people wish ferroelectricity functional oxide dielectric film material, such as metatitanic acid always Strontium barium (BST)The mos field effect transistor (MOSFET) to form GaAs bases is integrated with GaAs materials. Polarized using ferroelectric material, the characteristic such as electric light, piezoelectricity, dielectric tunable characteristic and GaAs high mobilities, direct band gap, exploitation provides There are electric light coupling, the multi-functional, integrated of waveguide properties, high frequency semiconductor devices.

At present, the SiO commonly used relative to semi-conductor industry2For/Si is as substrate, GaAs semiconductors are binary chemical combination Thing, its surface and interface has higher activity, and GaAs is unable to autoxidation and forms natural chemical passivation layer, therefore in GaAs bases Grown on piece during ferroelectric oxide dielectric film, very high interface state density can be caused by interfacial reaction or diffusion, these Electric charge is directly injected into semiconductor during highdensity interfacial state can make fermi level pinning in band gap center or cause ferroelectric material Big leakage current is caused, the development of GaAs related device technologies is hindered.Meanwhile, these interfacial states greatly enhance surface recombination center Non-radiative recombination speed, destroy GaAs proper semiconductor's characteristic, the operation of serious limitation GaAs devices.

As can be seen here, the problem of interface growth is incompatible between ferroelectric material barium strontium titanate and binary compound GaAs, leads Cause can not grow high-quality functional oxide barium strontium titanate dielectric film, the hair of restriction semiconductor devices industry on GaAs Exhibition.

The content of the invention

The technical problem to be solved in the present invention is, for the above-mentioned ferroelectric material barium strontium titanate and dualization of prior art Presence of an interface growth is incompatible between compound GaAs, causes that high-quality functional oxide metatitanic acid can not be grown on gallium There is provided a kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate for the defect of strontium barium dielectric film.

The technical solution adopted for the present invention to solve the technical problems is:Construction one kind prepares metatitanic acid on GaAs substrate The chemical method of strontium barium dielectric film, comprises the following steps:

S1, GaAs substrate pretreatment:First successively with trichloro ethylene solution, acetone soln and alcoholic solution to arsenic Gallium substrate carries out sonic oscillation cleaning, then GaAs substrate is cleaned with deionized water and hydrofluoric acid solution to remove successively The oxide layer of GaAs substrate surface is gone, GaAs substrate is finally dried up;

S2, barium strontium titanate colloidal sol preparation:Using barium acetate, strontium acetate and butyl titanate as initiation material, glacial acetic acid and second Acyl acetone is that solvent prepares barium strontium titanate colloidal sol;

S3, whirl coating film forming:It will be placed on by the above-mentioned steps S1 GaAs substrates handled on sol evenning machine, then will pass through upper State step S2 and prepare obtained barium strontium titanate sol solution dropwise addition on the GaAs substrate, carry out whirl coating;, will after whirl coating terminates The GaAs substrate is placed in culture dish, is wiped the barium strontium titanate colloidal sol for being thrown out of substrate with alcohol swab, is placed to making arsenic Change the barium strontium titanate colloidal sol solidification on gallium substrate;

S4, drying:GaAs substrate after above-mentioned steps S3 whirl coatings is placed in vacuum drying chamber and is dried;

S5, baking pretreatment:The dried GaAs substrates of above-mentioned steps S4 are placed in Muffle furnace and carry out toasting pre- place Reason, then naturally cools to room temperature by the GaAs substrate.

S6, annealing:Pretreated GaAs substrate will be toasted to be positioned in quartz ampoule, the constant temperature of tube furnace is pushed to Area, anneals 150~180 minutes, whole process is passed through the protective gas containing inert gas and oxygen, described at 450~650 DEG C The flow velocity of protective gas is 600 ml/mins, and after tubular type furnace temperature is down to room temperature, sample is taken out, is positioned in drying box Preserve.

It is described to contain inertia in the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate In the protective gas of gas and oxygen, the volume ratio of the inert gas and oxygen is 90:10~98:2.

In the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate, the step S1 Also include:In the vacuum cavity that the GaAs substrate of drying is sent into RIE reactive ion etching machines, in nitrogen and argon gas Product is than being 4:Ion etching is carried out in 1 mixed gas.

In the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate, the GaAs Substrate carries out ion etching 10 minutes under the conditions of the sputtering power of the RIE reactive ion etching machines is 50 milliwatts.

In the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate, the step S2 Barium strontium titanate colloidal sol preparation, prepare according to the following steps:

S21, according to 8:2 mol ratios weigh a certain amount of barium acetate and strontium acetate, add glacial acetic acid and heat and be sufficiently stirred for Dissolve it;

S22, measure equimolar and mixed than butyl titanate and acetylacetone,2,4-pentanedione;

S23, solution made from above-mentioned steps S21 mixed with solution made from step S22 in 50 DEG C~70 DEG C stirrings, plus It is 2 to enter mass ratio:1 ethylene glycol monomethyl ether and ethylene glycol solution dilutes above-mentioned mixed solution, finally gives 0.01mol/L Barium strontium titanate sol solution.

In the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate, the step S3 Described in GaAs substrate rotating speed be 2500~3500r/ minutes under the conditions of whirl coating 30s.

In the chemical method of the present invention that barium strontium titanate dielectric film is prepared on GaAs substrate, the step S5 It is middle that Muffle furnace is warming up to 300~380 DEG C, the GaAs substrate is incubated 15~30 minutes under the temperature conditionss.

Implement the chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate of the present invention, with following beneficial Effect:Surface treatment is done by GaAs substrate and forms clean surface of the arsenic atom of atomically flating for termination face, and is passed through Whirl coating film forming, drying, bake, the pretreated GaAs substrate of baking is placed in quartz ampoule and is passed through a certain proportion of protection gas In atmosphere, made annealing treatment under specified temp, make to grow high-quality barium strontium titanate dielectric film on GaAs substrate, solve titanium The problem of Presence of an interface growth is incompatible between sour strontium barium and GaAs.The barium strontium titanate prepared using the inventive method is situated between Conductive film crystalline quality is good, and surfacing and dielectric properties keep stable with frequency, in the range of 100KHz-1MHz, dielectric Constant is higher than 250, and the making requirement of MOSFET device can be met in structure.In addition, with Sol-gal process prepares barium strontium titanate dielectric film, and making apparatus is simple, and cost of material is relatively low, it is not necessary to expensive vacuum equipment Such as sputtering, molecular beam epitaxy, and it is adapted to large area film forming, be conducive to business application.

Brief description of the drawings

Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:

Fig. 1 is a kind of flow chart for the chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate of the present invention;

Fig. 2 is the barium strontium titanate that the present invention is grown into by step S6 present invention process(BST)Dielectric film is moved back with other The X-ray diffraction comparison diagram of BST dielectric films prepared by fiery condition;

Fig. 3 is the BST dielectric film surface regional area AFM surface topography maps that the present invention is grown into by step S6;

Fig. 4 is dielectric constant-frequency survey that the present invention grows into BST dielectric films/GaAs substrate samples by step S6 Measure curve.

Embodiment

In order to which technical characteristic, purpose and effect to the present invention are more clearly understood from, now compare accompanying drawing and describe in detail The embodiment of the present invention.

As shown in figure 1, preparing barium strontium titanate on GaAs substrate for one kind that the present invention is provided(BST)Dielectric film The flow chart of chemical method, is mainly included the following steps that:S1:Pretreatment → S2 of GaAs substrate:Barium strontium titanate colloidal sol is matched somebody with somebody System → S3:Whirl coating film forming → S4:Drying → S5:Toast pretreatment → S6:Annealing.It will be illustrated below with specific embodiment.

Embodiment one:The specific steps of the above-mentioned chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate are such as Under:

S1, GaAs(GaAs)The pretreatment of substrate:

GaAs substrates are surface-treated, first successively with trichloro ethylene solution, acetone soln and alcoholic solution to GaAs Substrate carries out sonic oscillation cleaning, every time cleaning 5 minutes;Then GaAs substrates are cleaned 5 minutes with deionized water, then uses hydrogen fluorine Acid(HF)Solution(HF:H2O=l:50)GaAs substrates are cleaned 1 minute, the oxide layer of GaAs substrate surfaces is removed, uses nitrogen(N2) Dry up GaAs substrates;Then the GaAs substrates of drying are sent into the vacuum cavity of RIE reactive ion etching machines, in nitrogen and argon Air volume ratio is 4:Ion etching 10 minutes is carried out in 1 mixed gas, the RIE reactive ion etching machines sputtering power is 50 millis Watt, etched substrate surface is more cleaned, closer to atomically flating, so as to obtain the interface of high-quality in growth course;

Wherein, the material of GaAs substrates is 2 inches of Si doped p-type(Concentration is 1 × 1018cm-3)GaAs(100)For lining Bottom, the Europe of sheet resistance about 6.

S2, barium strontium titanate colloidal sol preparation:Barium acetate, strontium acetate and butyl titanate are used for initiation material, glacial acetic acid and Acetylacetone,2,4-pentanedione is that solvent prepares barium strontium titanate colloidal sol, is prepared according to the following steps:

S21, according to 8:2 mol ratios weigh a certain amount of barium acetate(2.0436 gram)And strontium acetate(0.4294 gram), add Glacial acetic acid is stirred 120 minutes at 120 DEG C dissolves it;

S22, equimolar is measured again compare butyl titanate(3.5 milliliter)And acetylacetone,2,4-pentanedione(1 milliliter)60 points are stirred at 60 DEG C Clock is sufficiently mixed;

S23, solution made from above-mentioned steps S21 mixed with solution made from step S22 in 50~70 DEG C of stirrings, obtained The mixed solution of yellow transparent;In order to promote the hydrolytic polymerization of above-mentioned mixed solution, a small amount of deionized water is added(Content does not surpass Cross 5%), and the PVDF miillpore filters for being 200nm with aperture are filtered, to remove molecule and dust in the solution, finally It is 2 to add mass ratio:1 ethylene glycol monomethyl ether(4 grams)And ethylene glycol(2 grams)Solution is diluted, and finally gives 0.01mol/L's Barium strontium titanate sol solution, and barium strontium titanate sol solution is placed on progress low temperature maturation 48 hours at 5~10 DEG C;

S3, whirl coating film forming:

GaAs substrate after being surface-treated through above-mentioned steps S1 is put on sol evenning machine, then above-mentioned steps S2 is prepared Obtained barium strontium titanate sol solution is added dropwise on the GaAs substrate after above-mentioned steps S1 surface treatments, starts sol evenning machine GaAs substrate is driven to rotate, under 3000 revs/min of rotating speed, whirl coating 30 seconds;After whirl coating terminates, culture dish is placed the substrate in In, the barium strontium titanate colloidal sol being thrown out of is wiped with alcohol swab, places 15 minutes, makes the barium strontium titanate on GaAs substrate molten The abundant gel of glue.

S4, drying:

GaAs substrate after above-mentioned steps S3 whirl coatings is placed in vacuum drying chamber, 20 points are first dried at a temperature of 80 DEG C Clock;Vavuum pump is then turned on, under vacuum, temperature is 150 DEG C, dries 20 minutes, finally naturally cools to room temperature.

S5, baking pretreatment:

GaAs substrate made from above-mentioned steps S4 is placed in Muffle furnace, 380 DEG C are warming up to, 30 minutes are incubated, it is natural It is cooled to room temperature;

S6, GaAs substrate is positioned in quartz ampoule, is placed on the flat-temperature zone of tube furnace, heating process parameter is set, it is whole Individual process is passed through the protective gas containing argon gas and oxygen, argon gas:Oxygen volume ratio is 94:6, the flow velocity of protective gas is 600 millis Liter/min;550~600 DEG C of annealing temperature.

Wherein heating process parameter is specially:

A.60 minute rises to 500 DEG C from room temperature;

B. 90 minutes are incubated under the conditions of 500 DEG C;

C. pass through 15 minutes, 600 DEG C are warming up to from 550 DEG C, then be incubated 30 minutes;

D. it is naturally cooling near room temperature.

The micro-structural and Electrical Analysis of BST/GaAs dielectric films obtained as above use following instrument:

RIE reactive ion etching machines, the FA2000Reactive Ion Etching of MRICO companies production;

X-ray diffraction, the production of Rigaku company;

AFM, the SPA300HV of Japanese SEIKO companies production;

Electric impedance analyzer, the HP4284 of Hewlett-Packard Corporation of U.S. production.

Below by structure and the performance test design sketch of the sample shown in Fig. 2 to Fig. 4 carry out the further present invention can be real The property applied and effect.

Fig. 2 is the BST dielectric films of the annealing process growth by step S6 of the present invention, with being prepared under other annealing conditions BST dielectric film X-ray diffraction comparison diagrams;Wherein,

(a)For the GaAs substrate XRD spectrums of unannealed non-deposited dielectric films,

(b)For in pure oxygen atmosphere 600 DEG C annealing BST/GaAs sample XRD spectrums,

(c)For in pure argon atmosphere 600 DEG C annealing BST/GaAs sample XRD spectrums,

(d)For argon gas:Oxygen=94:The BST/GaAs sample XRD spectrums of 550 DEG C of annealings in 6 atmosphere;

(a)For the GaAs substrate XRD spectrums of unannealed non-deposited dielectric films, clearly GaAs seen from the figure(200)'s XRD characteristic peaks;(b)For the BST/GaAs sample XRD spectrums of 600 DEG C of annealings in pure oxygen atmosphere, as seen from the figure BST dielectrics The XRD characteristic peaks of film(Marked in figure with *), illustrate that dielectric film has been crystallized, with figure(a)On GaAs(200)XRD features Peak is compared, figure(b)Middle GaAs substrates XRD feature peak stretchings, illustrate that GaAs substrates are destroyed, surface is by severe oxidation;(c)Figure For the BST/GaAs sample XRD spectrums for 600 DEG C of annealings in pure argon atmosphere, clearly GaAs seen from the figure(200)XRD The characteristic peak of BST dielectric films is had no in characteristic peak, but figure, this explanation anneals BST dielectric films for amorphous under this atmosphere, The purpose of Annealing Crystallization is not reached;(d)For argon gas:Oxygen=94:The BST/GaAs samples XRD of 550 DEG C of annealings in 6 atmosphere , as seen from the figure, only there is the diffraction of BST dielectric films in the BST/GaAs diffraction spectra that 550 DEG C are annealed in argon atmospher in collection of illustrative plates Peak:BST(100)、BST(110)、BST(111)、BST(200), Er Qieyan(110)Direction(High preferred orientation)Diffraction it is most strong, Illustrate on GaAs substrates, BST dielectric films edge(011)Direction(Crystallographic axis is orientated)Preferred orientation grows.Sum it up, by this BST dielectric films prepared by invention preparation method have good crystallization property.

Fig. 3 is the BST dielectric film surface regional area AFM surface topography maps that the present invention is grown into by step S6.By Scheme visible dielectric film surface even compact, surface roughness is 12nm.Even compact illustrates dielectric film stable electrical properties, It is difficult electric leakage or breakdown.Roughness reflects the flatness of dielectric film, and the smaller explanation dielectric film of roughness is more smooth, the sample The roughness of product dielectric film is only 12nm, illustrates surfacing, has reached and has prepared micro-nano electronic device to surface smoothness It is required that.

Fig. 4 is dielectric constant-frequency that the present invention grows into BST dielectric films/GaAs substrate structures by step S6(C- f)Experiment curv.Abscissa Frequence represents that test b ST dielectric films are used test frequency, ordinate in figure Dieletric constant represent the dielectric constant that BST dielectric films are obtained under test frequency.BST dielectrics are thin as seen from the figure Film dielectric constant in 100KHz to 10MHz frequency spectrums is stable, and about 340, reach and manufacture metal oxide semiconductor field-effect crystalline substance Body pipe(MOSFET)The requirement of device.

As shown in above-mentioned Fig. 1 to Fig. 3, it may be said that the bright method by the present invention prepares orientation life on GaAs substrate The feasibility of long barium strontium titanate dielectric film, the crystalline quality of gained strontium titanates dielectric film is good, surfacing and dielectric Performance keeps stable with frequency, in the range of 100KHz-1MHz, and dielectric constant is higher than 250.

Embodiment two:The step of barium strontium titanate dielectric dielectric film is prepared on GaAs substrate is as follows:

The pretreatment of S1, GaAs substrate:Step S1 in be the same as Example one;

S2, barium strontium titanate colloidal sol preparation:Step S2 in be the same as Example one;

S3, whirl coating film forming:

GaAs substrate after being surface-treated through above-mentioned steps S1 is put on sol evenning machine, then above-mentioned steps S2 is prepared Obtained barium strontium titanate sol solution is added dropwise on the GaAs substrate after above-mentioned steps S1 surface treatments, starts sol evenning machine GaAs substrate is driven to rotate, under 2500 revs/min of rotating speed, whirl coating 30 seconds;After whirl coating terminates, culture dish is placed the substrate in In, the barium strontium titanate colloidal sol being thrown out of is wiped with alcohol swab, places 15 minutes, makes the barium strontium titanate on GaAs substrate molten The abundant gel of glue.

S4, drying:Step S4 in be the same as Example one;

S5, baking pretreatment:

GaAs substrate made from above-mentioned steps S4 is placed in Muffle furnace, 350 DEG C are warming up to, 30 minutes are incubated, it is natural It is cooled to room temperature;

S6, GaAs substrate is positioned in quartz ampoule, is placed on the flat-temperature zone of tube furnace, heating process parameter is set, it is whole Individual process is passed through the protective gas containing argon gas and oxygen, Krypton:Oxygen volume ratio is 90:10, the flow velocity of protective gas is 600 millis Liter/min;450~580 DEG C of annealing temperature;Wherein heating process parameter is specially:

A.60 minute rises to 450 DEG C from room temperature;

B. 90 minutes are incubated under the conditions of 500 DEG C;

C. pass through 15 minutes, 580 DEG C are warming up to from 550 DEG C, then be incubated 30 minutes;

D. it is naturally cooling near room temperature.

The BST dielectric films prepared by present invention process processing procedure have good crystallization property, dielectric film table Face is smooth, even compact, and dielectric constant is stable in 100KHz to 10MHz frequency spectrums, and dielectric constant is higher than 250, reaches and manufactures gold Belong to oxide semiconductor field effect transistor(MOSFET)The requirement of device.The method by the present invention can be illustrated in GaAs The feasibility of the barium strontium titanate dielectric film of oriented growth, the microstructure and property of gained strontium titanates dielectric film are prepared on substrate Expected Results can have been reached.

Embodiment three:The step of barium strontium titanate dielectric film is prepared on GaAs substrate is as follows:

The pretreatment of S1, GaAs substrate:Step S1 in be the same as Example one;

S2, barium strontium titanate colloidal sol preparation:Step S2 in be the same as Example one;

S3, whirl coating film forming:

GaAs substrate after being surface-treated through above-mentioned steps S1 is put on sol evenning machine, then above-mentioned steps S2 is prepared Obtained barium strontium titanate sol solution is added dropwise on the GaAs substrate after above-mentioned steps S1 surface treatments, starts sol evenning machine GaAs substrate is driven to rotate, under 3500 revs/min of rotating speed, whirl coating 30 seconds;After whirl coating terminates, culture dish is placed the substrate in In, the barium strontium titanate colloidal sol being thrown out of is wiped with alcohol swab, places 15 minutes, makes the barium strontium titanate on GaAs substrate molten The abundant gel of glue.

S4, drying:Step S4 in be the same as Example one;

S5, baking pretreatment:

GaAs substrate made from above-mentioned steps S4 is placed in Muffle furnace, 300 DEG C are warming up to, 15 minutes are incubated, it is natural It is cooled to room temperature;

S6, GaAs substrate is positioned in quartz ampoule, is placed on the flat-temperature zone of tube furnace, heating process parameter is set, it is whole Individual process is passed through the protective gas containing argon gas and oxygen, radon gas:Oxygen volume ratio is 98:2, the flow velocity of protective gas is 600 millis Liter/min;500~650 DEG C of annealing temperature;Wherein heating process parameter is specially:

A.60 minute rises to 500 DEG C from room temperature;

B. 90 minutes are incubated under the conditions of 500 DEG C;

C. pass through 15 minutes, 650 DEG C are warming up to from 500 DEG C, then be incubated 30 minutes;

D. it is naturally cooling near room temperature.

The BST dielectric films prepared by present invention process processing procedure have good crystallization property, dielectric film table Face is smooth, even compact, and dielectric constant is stable in 100KHz to 10MHz frequency spectrums, and dielectric constant is higher than 250, reaches and manufactures gold Belong to oxide semiconductor field effect transistor(MOSFET)The requirement of device.The method by the present invention can be illustrated in GaAs The feasibility of the barium strontium titanate dielectric film of oriented growth, the microstructure and property of gained strontium titanates dielectric film are prepared on substrate Expected Results can have been reached.

Embodiments of the invention are described above in conjunction with accompanying drawing, but the invention is not limited in above-mentioned specific Embodiment, above-mentioned embodiment is only schematical, rather than restricted, one of ordinary skill in the art Under the enlightenment of the present invention, in the case of present inventive concept and scope of the claimed protection is not departed from, it can also make a lot Form, these are belonged within the protection of the present invention.

Claims (7)

1. a kind of chemical method that barium strontium titanate dielectric film is prepared on GaAs substrate, it is characterised in that including following step Suddenly:
S1, GaAs substrate pretreatment:First successively with trichloro ethylene solution, acetone soln and alcoholic solution to GaAs base Piece carries out sonic oscillation cleaning, then GaAs substrate is cleaned with deionized water and hydrofluoric acid solution to remove arsenic successively Change the oxide layer of gallium substrate surface, finally dry up GaAs substrate;
S2, barium strontium titanate colloidal sol preparation:Using barium acetate, strontium acetate and butyl titanate as initiation material, glacial acetic acid and levulinic Ketone is that solvent prepares barium strontium titanate colloidal sol;
S3, whirl coating film forming:It will be placed on by the above-mentioned steps S1 GaAs substrates handled on sol evenning machine, then will pass through above-mentioned step Rapid S2 prepares obtained barium strontium titanate sol solution and is added dropwise on the GaAs substrate, carries out whirl coating;After whirl coating terminates, by the arsenic Change gallium substrate to be placed in culture dish, wiped the barium strontium titanate colloidal sol for being thrown out of substrate with alcohol swab, place to GaAs base Barium strontium titanate colloidal sol solidification on piece;
S4, drying:GaAs substrate after above-mentioned steps S3 whirl coatings is placed in vacuum drying chamber and is dried;
S5, baking pretreatment:The dried GaAs substrates of above-mentioned steps S4 are placed in progress baking pretreatment in Muffle furnace, so The GaAs substrate is naturally cooled into room temperature afterwards;
S6, annealing:Above-mentioned steps S5 is toasted into pretreated GaAs substrate to be positioned in quartz ampoule, tube furnace is pushed to Flat-temperature zone, anneals 150~180 minutes at 450~650 DEG C, and be continually fed into whole annealing process containing inert gas with The protective gas of oxygen, and flow velocity of the protective gas containing inert gas and oxygen when being passed through is 600 ml/mins, is treated The flat-temperature zone temperature of tube furnace is down to after room temperature, and sample is taken out, and is positioned in drying box and is preserved.
2. the chemical method according to claim 1 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is, in the protective gas containing inert gas and oxygen, the volume ratio of the inert gas and oxygen is 90:10~98: 2。
3. the chemical method according to claim 1 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is, the step S1 also includes:The GaAs substrate of drying is sent into the vacuum cavity of RIE reactive ion etching machines It is interior, it is 4 in nitrogen and argon gas volume ratio:Ion etching is carried out in 1 mixed gas.
4. the chemical method according to claim 3 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is, the GaAs substrate carries out sputtering work(during ion etching in the vacuum cavity of the RIE reactive ion etching machines Rate is 50 milliwatts, and the duration for carrying out ion etching is 10 minutes.
5. the chemical method according to claim 1 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is that the preparation of the barium strontium titanate colloidal sol of the step S2 is prepared according to the following steps:
S21, according to 8:2 mol ratios weigh a certain amount of barium acetate and strontium acetate, add glacial acetic acid and heat and be sufficiently stirred for making it Dissolving;
S22, measure equimolar and mixed than butyl titanate and acetylacetone,2,4-pentanedione;
S23, solution made from above-mentioned steps S21 mixed with solution made from step S22 in 50 DEG C~70 DEG C stirrings, add matter Amount is than being 2:1 ethylene glycol monomethyl ether and ethylene glycol solution dilutes above-mentioned mixed solution, finally gives 0.01 mol/L Barium strontium titanate sol solution.
6. the chemical method according to claim 1 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is, in the step S3, the rotating speed when GaAs substrate carries out whirl coating is 2500~3500 revolutions per seconds, the whirl coating time is 30 seconds.
7. the chemical method according to claim 1 that barium strontium titanate dielectric film is prepared on GaAs substrate, its feature It is, Muffle furnace is warming up to 300 DEG C~380 DEG C in the step S5, and be incubated 15~30 minutes.
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