JP2000044236A - Article having transparent conductive oxide thin film and its production - Google Patents

Article having transparent conductive oxide thin film and its production

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Publication number
JP2000044236A
JP2000044236A JP10208948A JP20894898A JP2000044236A JP 2000044236 A JP2000044236 A JP 2000044236A JP 10208948 A JP10208948 A JP 10208948A JP 20894898 A JP20894898 A JP 20894898A JP 2000044236 A JP2000044236 A JP 2000044236A
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Prior art keywords
substrate
range
ratio
article
film
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JP10208948A
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Japanese (ja)
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JP4170454B2 (en
Inventor
Hideo Hosono
Hiroshi Kawazoe
Kiyoshi Morita
Hiromichi Ota
裕道 太田
博司 川副
清 森田
秀雄 細野
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Hoya Corp
ホーヤ株式会社
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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
    • H01L29/68Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
    • H01L29/76Unipolar devices, e.g. field effect transistors
    • H01L29/772Field effect transistors
    • H01L29/78Field effect transistors with field effect produced by an insulated gate
    • H01L29/786Thin film transistors, i.e. transistors with a channel being at least partly a thin film
    • H01L29/7869Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
    • H01L29/78693Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate the semiconducting oxide being amorphous
    • 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
    • H01L29/40Electrodes ; Multistep manufacturing processes therefor
    • H01L29/43Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/45Ohmic electrodes
    • 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
    • H01L29/66969Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials

Abstract

PROBLEM TO BE SOLVED: To obtain an oxide film having excellent transmitting property for blue light while reducing the amt. of In2O3 which is a scarse mineral resource by using an oxide having a specified compsn. of Zn, Al and Ba, In as a target and specifying the substrate temp. and pressure. SOLUTION: An oxide expressed by the general formula of ZnxMyInzO(x+3y/2+3z/2) is used as a target to form an oxide film by sputtering or laser ablation method under the conditions of from room temp. to 300 deg.C substrate temp. and 1×10-2 to 10 (Pa) pressure. In the formula, M is at least one element of Al and Ga, the proportion x/y ranges 0.2 to 12, the proportion z/y ranges 0.4 to 1.4. The conductivity of the oxide of the target is good when the carrier electron density in the conductive band ranges about 1×1018 to 1×1022/cm3. By injecting actions to the oxide, carrier electrons are injected to the conductive band to develop the conductivity.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an article having a transparent conductor film containing an amorphous oxide which has high conductivity and visible light, particularly blue light transmittance, and is easy to produce, and its production. About the method. Further, the present invention relates to an electrode comprising the article of the present invention.

[0002]

2. Description of the Related Art Light-transmitting liquid crystal panel displays are widely used in various electric appliances as thin and lightweight display devices. In particular, the introduction to OA equipment such as personal computers and word processors is active.
The demand for displays for notebook computers of about inches and space-saving desktop personal computers is increasing, and improvements are being made in the direction of larger areas, more pixels, and higher definition.

[0003] A transparent electrode is indispensable for a light transmission type liquid crystal, and ITO is mainly used as a transparent electrode material. I
TO is transparent over almost the entire ultraviolet region and has an electrical resistivity of 1 ×
Since it can be reduced to about 10 −4 Ωcm, it was suitable as a transparent electrode material such as a liquid crystal display. In recent years, an amorphous phase of ITO, so-called amorphous ITO, has been used in response to a demand for higher definition. This is because amorphous ITO has a better patterning property than crystalline ITO, so that a thin electrode pattern can be cut cleanly. Although the electrical resistivity increases as compared with the crystalline ITO, T which occupies the mainstream of the liquid crystal display.
This is because the resistance value is sufficient for an FT type pixel electrode. Further, a plastic substrate tends to be used to reduce the weight of the display, and amorphous ITO which can be formed at room temperature is considered to be suitable. This is because a temperature of 200 ° C. or higher is required for forming the crystalline ITO.

[0004]

In the amorphous ITO, 90% or more of its components are composed of In 2 O 3 . For this reason,
With the spread of liquid crystal displays in recent years, the price of In 2 O 3 has soared to about twice, which is a factor of increasing the raw material cost. Further, In 2 O 3 is a rare metal, and is expected to be depleted when mining is continued for about 30 years. For these reasons, materials having a low content of In 2 O 3, a low raw material cost, and a low environmental burden on resources have been required.

Accordingly, an object of the present invention is to reduce the content of In 2 O 3 , which has a high environmental load on resources, to easily produce the material at a temperature near room temperature, to have a low resistance and an optical absorption edge having an ultraviolet absorption edge. Another object of the present invention is to provide a novel transparent conductor material having excellent blue transmittance and a method for producing the same, and an electrode using such a transparent conductor material.

The present inventors have found that a zinc-indium oxide containing a predetermined amount of aluminum or gallium can be easily produced at a temperature near room temperature.
The inventors have found that the present invention has low resistance, has an optical absorption edge in the ultraviolet region, and has excellent blue transmittance, and has completed the present invention.

[0007] JP-A-7-235219 discloses a conductive transparent substrate provided with a transparent conductive film made of a zinc-indium oxide. This transparent conductive film is made of indium (In) and zinc (Z
n) containing an amorphous oxide having an atomic ratio of In /
(In + Zn) is in the range of 0.8 to 0.9. Further, this oxide contains aluminum, gallium, antimony or germanium as the third element, and its content is determined by the atomic ratio (total third element) / (In + Zn + total) in order to suppress a decrease in conductivity. (Third element) is 0.2 or less.

In this publication, there is no description about the absorption edge of the transparent conductive film made of the oxide, and only the light transmittance of the optical characteristics is disclosed. That is, it is not clear what kind of light transmittance spectrum the transparent conductive film has, it is not clear whether the transparent conductive film has low resistance, has an optical absorption edge in an ultraviolet region, and further has excellent blue transmittance.

[0009]

A first aspect of the article of the present invention In order to achieve the above object, according to at least a portion of at least one surface of a substrate, the general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
(In the range of 1.4). A second aspect of the article of the present invention, at least a portion of at least one surface of a substrate, the general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( in the formula, M At least one element of aluminum and gallium, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
(In the range of 1.4), and a film containing an amorphous oxide which has been implanted with cations.

The present invention further relates to an electrode comprising the article of the present invention.

[0011] The first production method of the present invention is a method of manufacturing an article of the first aspect of the present invention, the general formula Zn x M y In z
O (x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, and the ratio x / y is 0.2 to 1
2 in which the ratio z / y is in the range of 0.4 to 1.4).
An oxide film is formed by a sputtering method or a laser ablation method at a temperature of 300 ° C. and a pressure of 1 × 10 −2 [Pa] to 10 [Pa].

[0012] The second manufacturing method of the present invention is a method of manufacturing an article of the second aspect of the present invention, the general formula Zn x M y In z
O (x + 3y / 2 + 3z / 2) (where M is at least one element of aluminum and gallium, and the ratio x / y is 0.2 to 1
2 in which the ratio z / y is in the range of 0.4 to 1.4).
An oxide film is formed by a sputtering method or a laser ablation method at a temperature of 300 ° C. and a pressure of 1 × 10 −2 [Pa] to 10 [Pa], and then cations are applied to the oxide film. It is characterized by injection.

[0013]

DESCRIPTION OF THE PREFERRED EMBODIMENTSArticle of the first aspect of the invention  General formula ZnxMyInzO(x + 3y / 2 + 3z / 2)M is aluminum and
And gallium alone, and M is
Minium and gallium may coexist. aluminum
Aluminum and gallium when gallium and
Is not particularly limited. However, the ratio of aluminum
Increases, the crystallization temperature tends to increase. gallium
Increases, the crystallization temperature tends to decrease.

The ratio (x / y) is in the range of 0.2 or more and 12 or less. When x / y is less than 0.2, the cost of raw materials increases. x
If / y exceeds 12, the Zn component becomes too large and becomes chemically unstable in the atmosphere. The preferred ratio (x / y) is 1
-10, more preferably 4-10. The ratio (z / y) is in the range of 0.4 or more and 1.4 or less. When z / y is less than 0.4, In 2 O 3 becomes insufficient and electric conductivity is reduced. When z / y exceeds 1.4, Ga 2
Insufficient O 3 components reduce the transparency in the blue region. The preferred ratio (z / y) is in the range of 0.6 or more and 1.4 or less, more preferably in the range of 0.8 or more and 1.2 or less.

Further, in the article of the present invention, the ratio x / (x
+ y + z) is preferably 0.5 or more from the viewpoint of reducing raw material costs and reducing environmental load. Ratio x / (x
+ y + z) preferably ranges from 0.6 to 0.9. Further, in the film of the article of the present invention, the oxide,
It is preferable that substantially the entire amount is amorphous in terms of transmittance and conductivity. However, a crystalline oxide may be contained to such an extent that transmittance and conductivity are not impaired.

The conductivity of the oxide of the present invention becomes good when the amount of carrier electrons in the conduction band is within a predetermined range. The amount of such carrier electrons is 1 × 10 18 / cm
It is in the range of 3 to 1 × 10 22 / cm 3 . Further, the preferable amount of carrier electrons is 1 × 10 19 / cm 3 to 5 × 10 21 / cm.
cm 3 . The amount of carrier electrons can be measured by, for example, a van der Pauw electrical conductivity measuring device.

[0017]Article of the second aspect of the invention  In the article according to the second aspect of the present invention, the general formula ZnxMyInzO
(x + 3y / 2 + 3z / 2)In the formula, Zn, M, ratio (x / y) and ratio
About the rate (z / y), the thing of the said 1st aspect of this invention
Same as the product. Ratio x / (x + y + z) and amorphous
And the conductivity of the article of the first aspect of the present invention.
Same as oxide.

Further, the article according to the second aspect of the present invention is obtained by implanting cations into the oxide represented by the above general formula. In the article according to the second aspect of the present invention, in addition to introducing oxygen vacancies, carrier electrons can be injected into the conduction band by injecting cations, thereby exhibiting conductivity.

The positive ions implanted into the conductive oxide having the article of the second aspect of the present invention have the general formula Zn x M y In z O
There is no particular limitation as long as it can form a solid solution without destroying the crystal structure of the oxide represented by (x + 3y / 2 + 3z / 2) . However, ions having a small ionic radius tend to form a solid solution in the crystal lattice, and the larger the ionic radius, the more likely the crystal structure is broken. Examples of the above cations include H, Li, Be, B, C, Na,
Mg, Al, Si, K, Ca, Sc, Ti, V, Cr,
Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge,
Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, A
g, Cd, In, Sn, Sb, Cs, Ba, La, C
e, Pr, Nd, Pm, Sm, Eu, Gd, Tb, D
y, Ho, Er, Tm, Yb, Lu, Hf, Ta, W,
Re, Os, Ir, Pt, Au, Hg, Tl, Pb, B
i.

[0020]The electrode of the present invention  The electrode of the present invention is the electrode of the first or second aspect of the present invention.
Includes goods. Of the conductive layer in the electrode of the present invention
The film thickness depends on the optical characteristics, conductivity and application required for the electrode.
It can be appropriately determined in consideration of such factors. For example, for LCD panel
For poles, the lower limit is about 30 nm and the upper limit is about 1 μm.
m. However, depending on the type of element contained in the oxide
May have some absorption in the visible region, in which case
Is preferably a relatively thin film. Also, almost
For those that have little or no absorption, use membranes
By increasing the thickness, higher conductivity can be obtained
You.

Examples of the transparent substrate include transparent substrates such as glass and resin. That is, any transparent material can be used as the substrate irrespective of vitreous or polymeric properties. In addition, the form of the substrate corresponds to any form such as a flat substrate, a sheet, and a film. Glass substrates are often used for liquid crystal displays and the like. Glass substrates include soda-based glass and low-alkali glass, and soda-based glass is generally widely used. However,
Low alkali glass is excellent for color displays and high quality displays. It is preferable to use glass having high transparency in the visible region and excellent flatness.

Examples of the resin substrate include a polyester substrate and a PMMA substrate. Many uses of resin substrates, which are lighter, thinner, more flexible and more flexible in shape than glass substrates, are being studied. For example, an electrophotographic film, a liquid crystal display, an optical memory, a transparent lent switch, an antistatic film, a heat ray reflective film, a surface heating film, and the like. Liquid crystal displays have high transparency in the visible region, excellent flatness, processability,
It is preferable to use it in consideration of impact resistance, durability, compatibility with an assembly process, and the like.

Further, the electrode of the present invention can be provided on a base layer provided on the transparent substrate. Examples of the base layer include a color filter, a TFT layer, an EL light emitting layer, a metal layer, a semiconductor layer, and an insulator layer.
Further, two or more types of underlayers can be provided.

The electrode of the present invention can be used for various applications. For example, it can be suitably used as an electrode of a liquid crystal display, an EL display, a solar cell, or the like. For liquid crystal displays, TFT type, STN type and MI
There are various types such as the M type, but in each case, an electric field is applied to the liquid crystal sandwiched between the transparent electrodes, and the principle of displaying by controlling the orientation direction of the liquid crystal is used. The electrode of the present invention can be used as the transparent electrode. For example, the structure of a TFT type color liquid crystal display is composed of a backlight, a first polarizing plate, a TFT substrate, a liquid crystal, a color filter substrate, and a second polarizing plate. It is necessary to form a transparent electrode on the TFT substrate and the color filter substrate in order to control the alignment direction of the liquid crystal. The transparent electrode of the present invention is formed on the TFT substrate and the color filter substrate by the above-described method. can do. Since the transparent electrode of the present invention has high transparency and high conductivity, it is most suitable as a transparent electrode provided on a TFT substrate or a color filter substrate.

Further, the transparent electrode of the present invention can be used as an electrode for an EL display. EL displays include a dispersion type, a lumocene structure type and a double insulation structure type, and in each case, an E is provided between the transparent electrode and the back electrode.
The electrode of the present invention has a basic structure sandwiching the L light emitting layer,
It is most suitable as the above transparent electrode.

The electrode of the present invention is excellent as a solar cell electrode because of its high transparency and conductivity. Solar cells are classified into pn junction type, Schottky barrier type, hetero junction type, hetero face junction type, pin type, etc. In any case, a semiconductor or insulator is sandwiched between the transparent electrode and the back electrode. It has a basic structure. Since a solar cell is a device that converts light energy into electricity using the photovoltaic effect of a semiconductor interface, it is necessary to guide light to the semiconductor interface over as wide a spectral range as possible, and the transparency of the transparent electrode Must be high. Also,
A transparent electrode of a solar cell has a function of collecting photogenerated carriers generated at a semiconductor interface and guiding the generated carriers to a terminal. Therefore, in order to collect photogenerated carriers as effectively as possible, the conductivity of the transparent electrode must be high. The transparent electrode of the present invention,
Since light can be guided to the semiconductor interface over a wide spectral range of the entire visible region including light with a wavelength shorter than 450 nm and has high conductivity, it is excellent as an electrode for a solar cell.

[0027]Production method of the present invention  The first and second manufacturing methods of the present invention
4 is a method for manufacturing the article according to the first and second aspects of the invention. Book
In the first production method of the invention, the general formula ZnxMyInzO
(x + 3y / 2 + 3z / 2)(Where M is aluminum and gallium
At least one of which has a ratio x / y of 0.2 to 12
And the ratio z / y is in the range of 0.4 to 1.4).
The oxide to be used is used as a target. Second embodiment of the present invention
In the production method of the above, similarly to the first production method, the general formula ZnxM
yInzO(x + 3y / 2 + 3z / 2)(Where M is aluminum and gully
At least one of the elements having a ratio x / y of 0.
2 to 12, and the ratio z / y is in the range of 0.4 to 1.4.
Is used as the target.

In the manufacturing method of the present invention, the composition of the formed thin film hardly changes depending on the density of the target. However, considering the damage of the target due to laser pulse irradiation, the oxide used as the target is
The relative density is preferably at least 40%, more preferably at least 70%. For example, a sintered body can be used as the target. In addition, the composition of the thin film to be formed has little deviation from the target and is at most 5%, so that the target composition can be the same as the desired thin film composition. However, the target composition can be changed if necessary.

As the target, for example, in the range of x / y> 1, it is possible to use a mixed crystal sintered body with a ZN oxide or a homologous sintered body containing an integer multiple of the ZN oxide. it can.

In the manufacturing method of the present invention, the sputtering method is performed in an oxygen atmosphere or an oxygen radical atmosphere at a substrate temperature in the range of room temperature to 300 ° C. and a pressure in the range of 1 × 10 -2 [Pa] to 10 [Pa]. Or by laser ablation method,
An oxide film is formed. In the sputtering method and the laser ablation method, the substrate temperature is raised from room temperature to 300 ° C.
And the pressure (oxygen partial pressure) is 1 × 10 -2 [Pa] to 10
When the thickness is in the range of [Pa], an amorphous oxide film can be formed. The substrate temperature is preferably in the range of 0 to 150 ° C., and the pressure is preferably 0.01 [Pa] to 1
It is in the range of [Pa].

The sputtering method can be performed by a conventional method. In the laser ablation method, the control of the oxygen partial pressure in the thin film forming apparatus can be performed by introducing oxygen molecules into the system from an appropriate leak valve or the like. The use of a radical gun is appropriate from the viewpoint that the amount of oxygen contained in the film can be easily controlled. The radical gun is a device that generates radical species of gas such as oxygen by rf plasma and introduces the radical species into a vacuum system.

The laser used in the laser ablation method of the production method of the present invention may be any wavelength from the ultraviolet region to the infrared region, that is, 0.19 to 11 μm, preferably 0.19 to 11 μm.
0.3 μm is possible, and either continuous oscillation or pulse oscillation can be employed. Laser intensity at the time of laser irradiation, 0.0001~1000J / cm 2 · pulse, and desirably 0.1~100J / cm 2 · pulse.

In the manufacturing method of the second embodiment, cations are implanted into the oxide film formed by the above method. By injecting cations, carrier electrons are injected into the conduction band, so that conductivity can be exhibited. The ions that can be implanted with cations are as described above.

In the manufacturing method of the present invention, for example, when a sintered body of In: Ga: Zn = 1: 1: 1 is used as a target,
A thin film of 6.2 × 10 −3 [Ωcm] can be easily obtained. In this case, the main cause of the high conductivity is that the mobility shows a high value of 10 or more in spite of the amorphous substance. In addition, a homologous IGZO InGaO 3 (Zn
O) When a sintered body of m (m: an integer of 2 or more) is used, 4.3 × 10 -3
A thin film having a resistivity of [Ωcm] can be easily obtained. The reason for this is that the carrier concentration shows an exponential increase trend, while the mobility hardly changes.

If it is desired to further reduce the resistance, the conductivity can be improved by increasing the carrier density by using a gas reduction method or an ion implantation method at a low temperature (preferably 300 ° C. or less) after the film formation. . Further, the carrier density may be improved by utilizing the substitution doping effect of changing the composition of the target.

[0036]

The article of the present invention has a low content of In 2 O 3 in the material, so that the material cost is low, the environmental load is small, the visible light transmittance is 85% or more, and the absorption short wavelength is low. Since the thickness is 385 nm, the resistance can be reduced by increasing the film thickness of both a monochrome screen and a color screen. Further, since the crystallization temperature of the material constituting the film is as high as 400 ° C. or more, there is an advantage that the amorphous property is maintained and the resistivity does not fluctuate in a normal use temperature range. Since it is a stable oxide, it has excellent environmental resistance and can be used as a transparent electrode for solar cells used outdoors.

In addition, since the film is formed at a temperature around room temperature and exhibits conductivity without a reduction / annealing operation, the production efficiency is high, the apparatus is simple and the production cost can be reduced.

In particular, the article of the present invention has both excellent electric conductivity and visible light transmittance including a blue region, and has a potential as a useful transparent electrode, and therefore, is useful as an electrode for a display or a solar cell. Can be used. Further, since the film formation temperature can be set at around room temperature, the production efficiency is high. Further, the crystallization temperature of the material is high and the environment resistance is excellent.

[0039]

EXAMPLE The conditions of this example are as follows. Light source: PLD by KrF laser excitation (energy density 4J / cm 2 ) Target: In: Ga: Zn = 1: 1: 1 sintered body QZ substrate used Gas introduction O 2 5-40CCM (Pt = 7.9 × 10 -2 ~ 1.4 [Pa]) Oxygen radical applied power 0-150W Resistivity 6.2 × 10 -3 [Ωcm] Carrier concentration 8.5 × 10 19 [/ cm 3 ] Mobility 15 [cm / Vs] Target: In: Ga: Zn = 1: 1: 4 sintered body (Homologous gas InGaO 3 (ZnO) mm : integer) QZ, PMMA substrate used Gas introduction O 2 5-40CCM (Pt = 7.9 × 10 -2 to 1.4 [Pa]) Resistivity 4.3 × 10 -3 [Ωcm] Carrier concentration 2.5 × 10 20 [/ cm 3 ] Mobility 5.8 [cm / Vs]

1. Preparation of Target Each powder of In 2 O 3 , Ga 2 O 3 , and ZnO was weighed such that the ratio of the contained metals became 1. The weighed powder is wet-mixed with a planetary ball mill. After calcining at 1000 ℃ for 5 hours,
It was crushed again by a planetary ball mill. This powder was formed into a disc having a diameter of 20 mm by uniaxial pressing and then subjected to CIP. The sintered body was obtained by firing at 1550 ° C. for 2 hours in the atmosphere. In by XRD
It was confirmed that an oxide represented by GaZnO 4 was generated.

In the case of homologous InGaO 3 (ZnO) m ,
2 O 3 , Ga 2 O 3 , each powder of ZnO, the ratio of the contained metal is 1: 1: m (m
Is an integer of 2 or more). The weighed powder is wet-mixed with a planetary ball mill. After calcining at 1000 ° C. for 5 hours, the mixture was again crushed by a planetary ball mill. This powder was formed into a disc having a diameter of 20 mm by uniaxial pressing and then subjected to CIP. The sintered body was obtained by firing at 1550 ° C. for 2 hours in the atmosphere. XRD
As a result, it was confirmed that an oxide represented by InGaO 3 (ZnO) m corresponding to each m value was generated.

2. Film Formation A film formation method using a laser ablation method will be described below as an example. Example 1 Among the sintered bodies prepared above, the surface of the sintered body of In: Ga: Zn = 1: 1: 1 was polished and fixed to a holder made of Inconel with metal In. This was fixed to a laser ablation device manufactured by Japan Vacuum Co., Ltd., and a KrF excimer laser beam manufactured by Lambda Physics Co., Ltd. was irradiated onto the rotating surface at an energy density of 4 J / cm 2 and a pulse interval of 5 Hz to form a plume. Was. The atmosphere in the chamber is O 2 gas flowing at 15-25 CCM, the total pressure is 0.
8-1.0 [Pa] was set. A 10 mm square, 0.5 mm thick quartz glass substrate was placed 30 mm directly above the target, and was exposed to the plume for 30 minutes while rotating so that the film thickness became uniform, thereby obtaining a thin film of about 300 nm. The composition ratio was obtained by a fluorescent X-ray method. XRD confirmed that the film was uniform and amorphous (FIG. 1). The absorption edge was determined by calculating the optical constant from the transmission and reflection spectra of the sample. The electrical characteristics were obtained by measuring the Hall effect by the van der Pauw method.

[0043]

[Table 1]

Example 2 An amorphous IGZO thin film was obtained by using a 10 mm square, 1.0 mm thick acrylic substrate as a film-forming substrate under the same conditions as in Example 1.

[0045]

[Table 2]

Example 3 As in Example 1, the chamber atmosphere was changed to O 2 gas 5-20 [CCM].
Oxygen radicals were generated by flowing and applying RF power of 50 W using a radical gun, and the total pressure was adjusted to 0.2 to 0.4 [Pa].

[0047]

[Table 3]

Example 4 Among the sintered bodies prepared above, the surface of the sintered body of In: Ga: Zn = 1: 1: 4 was polished and fixed to a holder made of Inconel with metal In. This was fixed to a laser ablation device manufactured by Japan Vacuum Co., Ltd., and a KrF excimer laser beam manufactured by Lambda Physics Co., Ltd. was irradiated onto the rotating surface at an energy density of 4 J / cm 2 and a pulse interval of 5 Hz to form a plume. Was. The atmosphere in the chamber is O 2 gas flowing at 15-25 CCM, the total pressure is 0.
8-1.0 [Pa] was set. A 10 mm square quartz glass substrate having a thickness of 0.5 mm was placed 30 mm directly above the target, and exposed to the plume for 30 minutes while rotating so that the film thickness became uniform, thereby obtaining a thin film of about 300 nm. The composition ratio was obtained by a fluorescent X-ray method. It was confirmed by XRD that the film was uniform and amorphous. The absorption edge was determined by calculating the optical constant from the transmission and reflection spectra of the sample. The electrical characteristics were obtained by measuring the Hall effect by the van der Pauw method.

[0049]

[Table 4]

[Brief description of the drawings]

FIG. 1 is a result of XRD confirming that an oxide represented by InGaZnO 4 is generated.

[Procedure amendment]

[Submission date] October 2, 1998 (1998.10.
2)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Name of invention

[Correction method] Change

[Correction contents]

An article having a transparent conductive oxide thin film and a method for producing the same

 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Hideo Hosono 4259 Nagatsutacho, Yokohama City, Kanagawa Prefecture Inside the Tokyo Institute of Technology Applied Ceramics Research Laboratory (72) Inventor Hiroshi Kawasoe 4259 Nagatsutacho, Yokohama City, Kanagawa Prefecture Tokyo Institute of Technology Applied Ceramics Research In-house F-term (reference) 2H092 HA04 MA05 MA23 MA30 NA25 PA01 5G307 FA01 FA02 FB01 FC09 FC10 5G323 BA02 BB05 BB06 BC02 BC03

Claims (14)

    [Claims]
  1. Claims: 1. At least one surface of a substrate
    Some of the general formula ZnxMyIn zO(x + 3y / 2 + 3z / 2)(Where M is
    At least one element of aluminum and gallium
    And the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is
    (Between 0.4 and 1.4)
    An article characterized in that it has a film to be formed.
  2. 2. At least one surface of the substrate
    Some of the general formula ZnxMyIn zO(x + 3y / 2 + 3z / 2)(Where M is
    At least one element of aluminum and gallium
    And the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is
    0.4 to 1.4) and implanted with cations
    Having a film containing an amorphous oxide
    Articles characterized by the following.
  3. 3. The amount of carrier electrons is 1 × 10 18 to 1 × 10 22 / c.
    As the range of m 3, article of claim 2, wherein the selected amount of injected oxygen deficiency d and cations.
  4. 4. The article according to claim 1, wherein the ratio x / (x + y + z) is 0.5 or more.
  5. 5. The article according to claim 1, wherein the substrate is a polymer substrate, a polymer flexible substrate, or a glass substrate.
  6. 6. The article according to claim 5, wherein the substrate comprises a transparent polymer on a film or a sheet.
  7. 7. An electrode comprising the article according to any one of claims 1 to 6.
  8. 8. The electrode according to claim 7, wherein the conductive layer comprises a homogeneous amorphous oxide film.
  9. 9. The electrode according to claim 7, further comprising a base layer between the substrate and the conductive layer.
  10. 10. The electrode according to claim 9, wherein the underlayer is one or more layers selected from the group consisting of a filter layer, a TFT layer, an EL layer semiconductor layer, and an insulating layer.
  11. 11. A liquid crystal display, an EL display or a solar cell for use in any one of claims 8 to 10.
    An electrode according to the item.
  12. 12. A method of manufacturing an article of claim 1, formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( wherein, M is one of aluminum and gallium At least one element, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
    1.4), the substrate temperature should be in the range of room temperature to 300 ° C, and the pressure should be 1
    A method characterized by forming an oxide film by a sputtering method or a laser ablation method in a range of × 10 -2 [Pa] to 10 [Pa].
  13. 13. A method of manufacturing an article of claim 2, general formula Zn x M y In z O ( x + 3y / 2 + 3z / 2) ( wherein, M is one of aluminum and gallium At least one element, the ratio x / y is in the range of 0.2 to 12, and the ratio z / y is 0.4 to
    1.4), the substrate temperature should be in the range of room temperature to 300 ° C, and the pressure should be 1
    A method characterized by forming an oxide film by a sputtering method or a laser ablation method in a range of × 10 -2 [Pa] to 10 [Pa], and then implanting cations into the oxide film.
  14. 14. A heat treatment and / or reduction treatment at a temperature in the range of 10 to 300 ° C. after film formation.
    3. The production method according to 3.
JP20894898A 1998-07-24 1998-07-24 Article having transparent conductive oxide thin film and method for producing the same Expired - Lifetime JP4170454B2 (en)

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