CN108546993A - A kind of rutile structure tantalum doping tin oxide monocrystal thin films and preparation method thereof of edge [101] crystal orientation growth - Google Patents
A kind of rutile structure tantalum doping tin oxide monocrystal thin films and preparation method thereof of edge [101] crystal orientation growth Download PDFInfo
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Abstract
The present invention relates to a kind of rutile structure tantalum doping tin oxide monocrystal thin films and preparation method thereof of edge [101] crystal orientation growth.The present invention uses organometallic chemical vapor deposition (MOCVD) technology, with tetraethyl tin (Sn (C2H5)4) it is the sources organic metal Sn, ethanol tantalum (Ta (C2H5O)5) it is the sources organic metal Ta, using oxygen as oxide, nitrogen buffer gas, the epitaxial growth tantalum doping tin oxide monocrystal thin films in R surface sapphire substrates.The tantalum doping tin oxide film for the rutile structure that substrate can be prepared along the growth of [101] crystal orientation is done using R surface sapphires, the tantalum doping tin oxide film of preparation is monocrystal thin films, and mobility is up to 58.1cm2V‑1s‑1, the lattice structure and electrical properties of prepared tantalum doping tin oxide monocrystal thin films are superior to tin oxide polycrystal film, therefore are the important materials for manufacturing transparent semiconductor device and ultraviolet photoelectron device.
Description
Technical field
The present invention relates to a kind of rutile structure tantalum doping tin oxide monocrystal thin films of edge [101] crystal orientation growth and its preparations
Method belongs to Semiconductor Optoeletronic Materials technical field.
Technical background
In recent years, broad stopband oxide semiconductor material tin oxide (SnO2) cause to grind with its unique optics electrical properties
Study carefully the extensive concern of personnel.(ZnO, Eg~3.37eV, exciton bind energy are with gallium nitride (GaN, Eg~3.4eV) and zinc oxide
~60meV) compare, tin oxide have broader band gap and higher exciton bind energy (be respectively at room temperature~3.7eV and~
130meV), and stannic oxide materials have many advantages, such as that preparation temperature is low, physical and chemical performance is stablized.SnO 2 thin film material at present
Material is mainly used in transparent conductive electrode, thin-film solar cells, gas sensor and building glass etc..
In order to obtain the SnO 2 thin film with excellent electrical properties, people are dedicated to research and prepare with high mobility
With the SnO 2 thin film of low-resistivity.Intrinsic tin oxide is n-type semiconductor, and there are auto-compensations, if system
Standby tin oxide is polycrystal film, is difficult to obtain the p-type SnO 2 thin film material of function admirable and stabilization by doping
Material.
Currently with the tantalum doping tin oxide film of conventional method preparation, there are the following problems：
(1) SnO 2 thin film prepared by the conventional methods such as spray pyrolysis and magnetron sputtering method is generally polycrystalline structure, ties
Brilliant second-rate, the defect inside film is more, there are great number of grains boundary, to the carrier scattering effect inside film compared with
By force, it is difficult to obtain the film of high mobility performance.
(2) in carrying out N-shaped doping research to SnO 2 thin film, it is that the doping of metal Sb elements is ground to study at present more
Study carefully.In recent years, the sight of researcher turns to the doping of Nb and Ta elements again.It can be difficult to obtaining the single-crystal doped thin of high quality
The thin-film material of film and high hall mobility significantly limits application of the SnO 2 thin film in photoelectric material devices field.
(3) with pulsed laser deposition system (PLD) although the methods of can realize on a sapphire substrate Ta doping oxidation
The growth of tin thin film material, but crystalline quality is undesirable, film forming area is small, it is difficult to realize industrialization production.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of Rutile structure tantalum doping of edge [101] crystal orientation growth
The preparation method of tin-oxide mono-crystal film material.
Term is explained：
MOCVD：Organometallic chemical vapor deposition.
Ta adulterates ratio：Ta atoms account for the percentage of the sum of Ta and Sn atoms, Ta/ (Ta+Sn), and atomic ratio is abbreviated as：%
atm。
Summary of the invention：
The present invention uses organometallic chemical vapor deposition (MOCVD) technology, with tetraethyl tin (Sn (C2H5)4) it is organic
The sources metal Sn, ethanol tantalum (Ta (C2H5O)5) it is the sources organic metal Ta, using oxygen as oxide, nitrogen buffer gas, in the faces R indigo plant
Epitaxial growth tantalum doping tin oxide monocrystal thin films on jewel substrate.
Detailed description of the invention：
Technical scheme is as follows：
The preparation method of above-mentioned tantalum doping tin oxide monocrystal thin films, steps are as follows：
(1) MOCVD reative cells are pumped into high vacuum state, vacuum degree 4 × 10-5Pa~6 × 10-4Pa, by R surface sapphires
Substrate is placed in reative cell and is heated to 580~700 DEG C of growth temperature；
(2) nitrogen bottle valve is opened, background N is passed through to reative cell2, background N2Flow is 200~800sccm, reacts chamber pressure
Strong 10~100Torr is kept for 30~35 minutes；
(3) oxygen container valve is opened, oxygen flow is 30~100sccm, is kept for 8~12 minutes；
(4) sources organic metal Sn bottle valve is opened, carrier gas N is adjusted210~40sccm of flow is kept for 8~12 minutes；Cold-trap
10~25 DEG C of temperature；
(5) sources organic metal Ta bottle valve is opened, carrier gas N is adjusted22~15sccm of flow is kept for 8~12 minutes；It is organic
15-50 DEG C of the sources metal Ta condenser temperature；
(6) by the oxygen of step (3), the carrying organic metal Sn source carrier gas N of step (4)2The sources Ta are carried with step (4)
Carrier gas N2It is passed through reative cell simultaneously, the retention time is 180~300 minutes, and epitaxial growth tantalum adulterates in R surface sapphire substrates
Tin-oxide mono-crystal film；
(7) reaction terminates, and closes the sources organic metal Sn bottle, the sources Ta bottle and oxygen container valve, pipeline 20-30 is purged with nitrogen
Minute.
According to currently preferred, the epitaxial growth rate of tantalum doping tin oxide monocrystal thin films described in above-mentioned steps (6)
For 0.5~3.5nm/min；It is further preferred that the epitaxial growth rate of the tantalum doping tin oxide monocrystal thin films is 1~3nm/
min；Most preferably, the epitaxial growth rate of the tantalum doping tin oxide monocrystal thin films is 1.5~2.5nm/min.
According to currently preferred, the Ta doping of the tantalum doping tin oxide monocrystal thin films of above-mentioned preparation is than being 1~10%
atm；It is further preferred that the Ta doping of the tantalum doping tin oxide monocrystal thin films is than being 2~8%atm；Most preferably, described
The Ta doping of tantalum doping tin oxide monocrystal thin films is than being 4%atm.
According to currently preferred, the thickness of the tantalum doping tin oxide monocrystal thin films of above-mentioned preparation is 450~500nm.
According to currently preferred, the tantalum doping tin oxide monocrystal thin films of above-mentioned preparation are single-orientated along [101] crystal face
Monocrystal thin films, the mobility of film can reach 58.1cm2V-1s-1。
According to currently preferred, the sources the organic metal Sn are 99.9999% high-purity tetraethyl tin (Sn (C2H5)4),
The sources the organic metal Ta are 99.9999% high-purity ethanol tantalum (Ta (C2H5O)5), the oxygen is 99.999% high pure oxygen
Gas, the carrier gas N2It is the ultra-pure nitrogen purified by the 99.999% purified device of high pure nitrogen as 99.9999999%.
According to currently preferred, the aufwuchsplate of the R surface sapphire substrates isCrystal face, the crystal face is by two-sided
Polishing treatment.
According to currently preferred, the process conditions of a preferred preparation method are as follows：
Chamber pressure 30Torr is reacted,
620 DEG C of growth temperature,
Background N2Flow 500sccm,
10 DEG C of the sources organic metal Sn condenser temperature, carrier gas N2Flow 15.7sccm,
29.5 DEG C of the sources organic metal Ta condenser temperature, carrier gas N2Flow 6.7sccm,
Oxygen flow 50sccm,
The epitaxial growth rate of tin-oxide mono-crystal film is 1.7nm/min,
The Ta doping ratios of prepared tantalum doping tin oxide monocrystal thin films are 4%atm,
Prepared tantalum doping tin oxide monocrystal thin films thickness is 470nm.
Tantalum doping tin oxide film prepared by the present invention is the monocrystal thin films of the cubic rutile structure along [101] crystal orientation；
The X ray diffracting spectrum of products obtained therefrom shows only rutile structure tin oxide (101) crystal face occur, when Ta doping is than being 4%,
(101) halfwidth of crystal face is 1.04 degree；As shown in Figure 1.Prepared tantalum doping tin oxide monocrystal thin films lattice structure is complete,
Its { 110 }
The X-ray original position φ scanning results in face show, occur (110) andThere is twin knot in the diffraction maximum of crystal face
Structure, it is consistent with undoped with sample structure；As shown in Figure 2.
The hall mobility of tantalum doping tin oxide monocrystal thin films prepared by the present invention is 35.7~58.1cm2V-1s-1；It is preferred that
, when Ta doping is than being 2.5~5%, tantalum doping tin oxide monocrystal thin films hall mobility is in 51.7~58.1cm2V-1s-1, most
It is preferred that monocrystal thin films hall mobility reaches 58.1cm when Ta doping is than being 4%atm2V-1s-1, the average phase of visible-range at this time
It is more than 90% to transmitance, optical band gap 4.1eV.
Tantalum doping tin oxide film prepared by the present invention is monocrystal thin films, and hall mobility is high, is used to prepare transparent half
Conductor device and ultraviolet photoelectron device.
It is equal with reference to the prior art for what is be particularly limited in the method for the present invention.
The excellent results of the present invention：
1, the inventors discovered that, the rutile knot along the growth of [101] crystal orientation can be prepared by doing substrate using R surface sapphires
The tantalum doping tin oxide film of the tantalum doping tin oxide film of structure, preparation is monocrystal thin films, and mobility is up to 58.1cm2V-1s-1.And under the same terms, it is in the single crystal quartz substrate of polishing or the tantalum doping tin oxide film of monocrystalline silicon piece Grown
Polycrystalline structure, and mobility is below 30cm2V-1s-1.On the other hand, the prior art using pulsed laser deposition (PLD), etc.
Tantalum doping tin oxide film prepared by ion sputtering is polycrystalline or non crystalline structure film, and mobility is low.
2, the technology of the present invention method is condenser temperature by changing the sources organic metal Sn and the sources Ta and flow accurately to control
It is formed with the molar flow in the sources machine Sn and the sources Ta, the atom doped ratios of Ta are precisely controlled with this, to obtain the tantalum of high mobility
Doped stannum oxide monocrystal thin films.Wherein condenser temperature has an impact the saturated vapor pressure of organic source, and then influences whether organic source
Molar flow.
3, the method for the present invention selection is in sapphireHigh quality tin oxide monocrystal thin films are grown on crystal face.System of the present invention
Standby tantalum doping tin oxide film is the monocrystal thin films of the cubic rutile structure along [101] crystal orientation epitaxial growth, and film is suddenly
That mobility is up to 58.1cm2V-1s-1, corresponding resistivity is 1 × 10-3Ω·cm.Prepared tantalum doping tin oxide monocrystalline is thin
The lattice structure and electrical properties of film are superior to tin oxide polycrystal film, therefore are manufacture transparent semiconductor device and ultraviolet light photo
The important materials of sub- device.
4, the excellent optical performance for the tin-oxide mono-crystal film that Ta doping ratios are 4%, it is seen that being averaged for optical range is opposite
Transmitance is more than 90%, optical band gap 4.1eV, and band gap width is more than GaN and ZnO film, and it is ultraviolet to may be utilized in fabricating tin oxide
Opto-electronic device and transparent semiconductor device.
5, present invention process condition is easy to accurately control, and prepares the uniformity of film and reproducible, is convenient for industry metaplasia
Production.Prepared material photoelectric properties are excellent, and stability is high, has a extensive future.
Description of the drawings
Fig. 1 is the X-ray diffraction spectrum of the SnO 2 thin film of the undoped SnO 2 thin film prepared and different Ta doping ratios,
Wherein, abscissa Degree：Degree, ordinate Intensity/a.u.：Intensity (arbitrary unit).
Fig. 2 is the X-ray mirror that embodiment 1 prepares tantalum doping tin oxide film { 110 } face and substrate R surface sapphires { 0001 }
As φ scan test results, wherein abscissa Degree：Degree, ordinate Intensity/a.u.：Intensity (arbitrary unit).
Fig. 3 is the SnO 2 thin film that Ta doping ratios prepared by embodiment 1 are 4% through spectrum, abscissa
(Wavelength/nm) it is wavelength/nm, ordinate (Transmittance/%) is transmitance/%.
Fig. 4 is that embodiment 2 prepares the SnO 2 thin film of different Ta doping ratios and the Hall undoped with SnO 2 thin film moves
Shifting rate and resistivity with doping ratio change curve, wherein abscissa (Ta concentration/%) is Ta doping
Than/%atm, ordinate (the Hall mobility/cm on the left side2V-1s-1) it is mobility/cm2V-1s-1, the ordinate on the right
(Resistivity/ Ω cm) is resistivity/Ω cm.
Specific implementation mode
With reference to the accompanying drawings and examples, the present invention will be further described for comparative example, but not limited to this.
Embodiment 1：Ta doping is than being 4%
MOCVD technologies prepare tantalum doping tin oxide thin-film material, with the sapphire of polishingFace is substrate, uses Sn
(C2H5)4As organic metal tin source, Ta (C2H5O)5As organic metal tantalum source, steps are as follows：
(1) MOCVD device reative cell is evacuated to high vacuum state 5 × 10 first-4Pa, by silicon to 620 DEG C；
(2) nitrogen bottle valve is opened, nitrogen (background N is passed through to reative cell2) 500sccm, 30 minutes, make reaction chamber pressure
It is 30Torr by force；
(3) oxygen container valve is opened, the flow 50sccm of oxygen is adjusted, is kept for 10 minutes；
(4) sources organic metal Sn bottle valve is opened, carrier gas N is adjusted2Flow 15.7sccm is kept for 10 minutes；
(5) sources organic metal Ta bottle valve is opened, carrier gas (N is adjusted2) flow 6.7sccm, it is kept for 10 minutes；
(6) oxygen and the sources organic metal Sn, the sources Ta are passed through reative cell simultaneously, it is 300 minutes to keep film growth time；
(7) tin source and tantalum source bottle and oxygen container valve are closed after reaction, and pipeline is purged with nitrogen and terminates after twenty minutes.
Thin film growth process condition is as follows：
The sources organic metal Sn condenser temperature is that 10 DEG C, carrier gas flux 15.7sccm, organic metal Ta source condenser temperatures are
29.5 DEG C, carrier gas flux 6.7sccm；The epitaxial growth rate of SnO 2 thin film is 1.7nm/min.
The tantalum doping tin oxide film that the present embodiment 1 is prepared under the conditions of 620 DEG C is the mono-crystalline structures being orientated along [101],
Ta doping ratios are 4%, film thickness 470nm.Carrier mobility is 58.1cm2V-1s-1, resistivity is 1 × 10-3Ω·
Cm, it is seen that the average relative permeability of optical range is more than 90%.
The X ray diffracting spectrum of tantalum doping tin oxide film prepared by the present embodiment 1 is as shown in Figure 1, X ray diffracting spectrum
Only there is rutile structure tin oxide (101) crystal face, 1.04 degree of the halfwidth of (101) crystal face in display.Prepared tin oxide is thin
Film has the film along the single-orientated growth of (110) crystal face, it may be determined that tantalum doping tin oxide film is mono-crystalline structures.
Tantalum doping tin oxide film lattice structure prepared by the present embodiment 1 is complete, and the X-ray mirror image φ in { 110 } face is swept
Retouch that the results are shown in Figure 2, the results show that occur in scanning process (110) andThe diffraction maximum of crystal face, shows inside film
The crystal face arrangement of complete rule is presented.Epitaxial relationship is in face
Tantalum doping tin oxide film prepared by the present embodiment 1 penetrates spectrum as shown in figure 3, in Ta doping than being 4%atm
When, the average relative permeability of film is more than 90%, and illustration is the band gap diagram of the sample, and being computed its optical band gap width is about
4.1eV。
Embodiment 2：MOCVD technologies prepare tantalum doping tin oxide monocrystal thin films material, change Ta and adulterate ratio
Preparation process is as described in Example 1, the difference is that changing Ta source fluxs, Ta doping ratios is made to be 1.5%,
2.5%, 5%, 6% and 8%, prepared film is the mono-crystalline structures being orientated along [101], the carrier mobility point of film
It is not 35.7cm2V-1s-1、51.7cm2V-1s-1、45.8cm2V-1s-1And 23.1cm2V-1s-1, resistivity is respectively 1.3 × 10-2
Ω·cm、1.8×10-3Ω·cm、6×10-4Ω·cm、4×10-4Ω cm and 6.5 × 10-4Ω·cm.Hall mobility and
Resistivity is with the change curve of doping ratio as shown in figure 4, being shown in figure, with the raising of Ta doping ratios, the Hall of film
Mobility first increases and then decreases, when Ta doping ratios are 4%, mobility reaches as high as 58.1cm2V-1s-1, and the resistance of film
It takes the lead in increasing after reducing, when Ta doping ratios are 4%, resistivity is 1 × 10-3Ω·cm。
Comparative example 1：Mocvd method prepares tin-oxide mono-crystal epitaxial thin film material.
With the sapphire of polishingFace is substrate material, with Sn (C2H5)4As organometallic sources, in 660 DEG C of conditions
The SnO 2 thin film of lower preparation is the mono-crystalline structures being orientated along [101], as shown in Figure 1.The hall mobility of film is
18.7cm2V-1s-1, resistivity is 1.05 Ω cm.
Comparative example 2：Quartz substrate, mocvd method prepare tantalum doping tin oxide thin-film material
Preparation method is same as Example 1, except that using quartz (001) face of polishing as substrate material, at 660 DEG C
Under the conditions of the tantalum doping tin oxide film for preparing, film growth time is 120 minutes, and the tantalum doping tin oxide film of preparation is more
Crystal structure.Film carrier mobility is 28cm2V-1s-1, resistivity is 3.5 × 10-3Ω cm, it is seen that the average phase of optical range
It is 78% to transmitance.
Comparative example 3：Silicon chip substrate, mocvd method prepare tantalum doping tin oxide thin-film material
Preparation method is same as Example 1, except that：Using silicon chip as substrate material, chamber pressure 40Torr, lining are reacted
620 DEG C of bottom temperature, film growth time are 120 minutes, and the tantalum doping tin oxide film of preparation is polycrystalline structure, the current-carrying of film
Transport factor is 25cm2V-1s-1, resistivity is 5 × 10-3Ω·cm。
Claims (10)
1. a kind of preparation method of tantalum doping tin oxide monocrystal thin films, which is characterized in that steps are as follows：
(1) MOCVD reative cells are pumped into high vacuum state, vacuum degree 4 × 10-5Pa~6 × 10-4Pa sets R surface sapphire substrates
In reative cell and it is heated to 580~700 DEG C of growth temperature；
(2) nitrogen bottle valve is opened, background N is passed through to reative cell2, background N2Flow is 200~800sccm, reacts chamber pressure 10
~100Torr is kept for 30~35 minutes；
(3) oxygen container valve is opened, oxygen flow is 30~100sccm, is kept for 8~12 minutes；
(4) sources organic metal Sn bottle valve is opened, carrier gas N is adjusted210~40sccm of flow is kept for 8~12 minutes；Condenser temperature
10~25 DEG C；
(5) sources organic metal Ta bottle valve is opened, carrier gas N is adjusted22~15sccm of flow is kept for 8~12 minutes；Organic metal Ta
15-50 DEG C of source condenser temperature；
(6) by the oxygen of step (3), the carrying organic metal Sn source carrier gas N of step (4)2The load in the sources Ta is carried with step (4)
Gas N2It is passed through reative cell simultaneously, the retention time is 180~300 minutes, the epitaxial growth tantalum doping oxidation in R surface sapphire substrates
Tin monocrystal thin films；
(7) reaction terminates, and closes the sources organic metal Sn bottle, the sources Ta bottle and oxygen container valve, 20-30 points of pipeline is purged with nitrogen
Clock.
2. preparation method as described in claim 1, which is characterized in that tantalum doping tin oxide monocrystal thin films described in step (6)
Epitaxial growth rate be 0.5~3.5nm/min.
3. preparation method as described in claim 1, which is characterized in that the Ta of the tantalum doping tin oxide monocrystal thin films adulterates ratio
For 1~10%atm.
4. preparation method as described in claim 1, which is characterized in that the thickness of the tantalum doping tin oxide monocrystal thin films is
450~500nm.
5. preparation method as described in claim 1, which is characterized in that the tantalum doping tin oxide monocrystal thin films are along [101]
The single-orientated monocrystal thin films of crystal face.
6. preparation method as described in claim 1, which is characterized in that the sources the organic metal Sn be 99.9999% it is high-purity
Tetraethyl tin (Sn (C2H5)4), the sources the organic metal Ta are 99.9999% high-purity ethanol tantalum (Ta (C2H5O)5), the oxygen
Gas is 99.999% high purity oxygen gas, the carrier gas N2It is to be by the 99.999% purified device purifying of high pure nitrogen
99.9999999% ultra-pure nitrogen.
7. preparation method as described in claim 1, which is characterized in that the aufwuchsplate of the R surface sapphire substrates isIt is brilliant
Face, the crystal face are handled by twin polishing.
8. preparation method as described in claim 1, which is characterized in that process conditions are as follows：
Chamber pressure 30Torr is reacted,
620 DEG C of growth temperature,
Background N2Flow 500sccm,
10 DEG C of the sources organic metal Sn condenser temperature, carrier gas N2Flow 15.7sccm,
29.5 DEG C of the sources organic metal Ta condenser temperature, carrier gas N2Flow 6.7sccm,
Oxygen flow 50sccm,
The epitaxial growth rate of tin-oxide mono-crystal film is 1.7nm/min,
The Ta doping ratios of prepared tantalum doping tin oxide monocrystal thin films are 4%atm,
Prepared tantalum doping tin oxide monocrystal thin films thickness is 470nm.
9. tantalum doping tin oxide monocrystal thin films prepared by any one of claim 1-8, hall mobility is 35.7~58.1cm2V- 1s-1, it is seen that the average relative permeability of optical range is more than 90%, optical band gap 4.1eV.
10. tantalum doping tin oxide monocrystal thin films prepared by any one of claim 1-8, are used to prepare transparent semiconductor device and purple
Outer opto-electronic device.
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| CN114822987A (en) * | 2022-04-22 | 2022-07-29 | 厦门大学 | Ultraviolet-visible-near infrared transparent high-conductivity Ta-doped SnO 2 Film and preparation method |
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