CN105209405A - Sintered oxide body and sputtering target comprising said sintered oxide body - Google Patents

Sintered oxide body and sputtering target comprising said sintered oxide body Download PDF

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CN105209405A
CN105209405A CN201580000713.0A CN201580000713A CN105209405A CN 105209405 A CN105209405 A CN 105209405A CN 201580000713 A CN201580000713 A CN 201580000713A CN 105209405 A CN105209405 A CN 105209405A
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igzo
film
phase
sintered compact
sintered body
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CN105209405B (en
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角田浩二
长田幸三
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
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    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
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Abstract

The sintered oxide body comprises indium (In), gallium (Ga), zinc (Zn), oxygen (O), and unavoidable impurities, and is characterized in that: the sintered oxide body is provided with an IGZO (111) phase comprising In, Ga and Zn at In:Ga:Zn = 1:1:1 by atom ratio and an IGZO phase containing more Zn than the IGZO (111) phase; the IGZO phase containing more Zn than the IGZO (111) phase occupies a surface area ratio of 1 to 10%, and the atom number ratio of In, Ga and Zn in the sintered oxide body is In:Ga:Zn = 1:1:(1.02 to 1.10). The objective of the present invention is to provide an IGZO sintered oxide body allowing for a reduction of oxygen concentration that is necessary during sputtering to obtain a film having a desired carrier concentration.

Description

Oxidate sintered body and the sputtering target comprising this oxidate sintered body
Technical field
The present invention relates to the oxide compound comprising indium (In), gallium (Ga), zinc (Zn), oxygen (O) and inevitable impurity (to be commonly referred to as " IGZO "; This " IGZO " is used to be described as required), particularly relate to IGZO sintered compact and the sputtering target comprising this oxidate sintered body.
Background technology
In the past, in FPD (flat-panel monitor), the TFT (thin film transistor) of its backboard uses α-Si (non-crystalline silicon) always.But α-Si can not get sufficient electronic mobility, carried out in recent years using electronic mobility higher than the research and development of the TFT of the In-Ga-Zn-O type oxide (IGZO) of α-Si.And, use the next generation's high function flat-panel monitor part of IGZO-TFT to be able to practical, and attracted attention.
IGZO film carries out sputtering and film forming mainly through using the target made by IGZO sintered compact.As IGZO sputtering target, For example, Patent Document 1 discloses comprise In, Ga and Zn and the projecting tissue of the content of In by generating, even if at high temperature do not carry out reduction treatment, the target of low-resistivity also can be manufactured.In addition, Patent Document 2 discloses by containing In, Ga, Zn with requirement ratio and two or more homology crystal that coexists, sputtering can be stablized, reduce the generation of powder.
By the way, when such IGZO film is used as the active layer of TFT, be the oxygen defect amount in film to one of factor that the electrology characteristic of film has an impact.In order to control this oxygen defect amount, when spatter film forming, generally except the rare gas elementes such as argon gas, also introduce oxygen.The sputtering yield of oxygen is lower than argon gas, and when introducing oxygen when sputtering, sputtered atomic quantity reduces, and rate of film build reduces.In the spatter film forming of IGZO film, in order to the carrier concentration of film being controlled, for desired value, need to introduce a large amount of oxygen, therefore there is rate of film build and reducing thus the problem of productivity reduction.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2011-105995 publication
Patent documentation 2: No. 5288141st, Japanese Patent
Summary of the invention
Invent problem to be solved
Problem of the present invention be to provide the film that can be reduced to and obtain there is desired carrier concentration and the sputtering needed time the IGZO oxidate sintered body of oxygen concentration.The sputtering target comprising this sintered compact can improve sputter rate, and can significantly improve productivity.
For the means of dealing with problems
In order to solve above-mentioned problem, present inventor has performed further investigation, found that, by increasing the content of Zn (zinc) in IGZO sintered compact, can reduce the carrier concentration of film, result can reduce oxygen concn during sputtering.The present inventor, based on above-mentioned discovery, provides following invention.
1) oxide sintered body, it is for comprising the oxidate sintered body of indium (In), gallium (Ga), zinc (Zn), oxygen (O) and inevitable impurity, it is characterized in that, described oxidate sintered body has with the IGZO (111) of the atomic ratio measuring In:Ga:Zn=1:1:1 of In, Ga and Zn phase and the IGZO phase containing more Zn than IGZO (111) mutually; The area ratio containing the IGZO phase of more Zn than IGZO (111) is mutually 1 ~ 10%; The atomicity of In, Ga and Zn of this oxidate sintered body is than being In:Ga:Zn=1:1:(1.02 ~ 1.10).
2) as above-mentioned 1) as described in oxidate sintered body, it is characterized in that, median size is less than 20 μm.
3) as above-mentioned 1) or 2) according to any one of oxidate sintered body, it is characterized in that, body resistance is 30m below Ω cm.
4) as above-mentioned 1) to 3) according to any one of oxidate sintered body, it is characterized in that, sintered density is 6.3g/cm 3above.
5) sputtering target, it is by above-mentioned 1) to 4) according to any one of oxidate sintered body make.
Invention effect
The IGZO phase of the present invention by having in the IGZO type oxide sintered compact comprising indium (In), gallium (Ga), zinc (Zn), oxygen (O) and inevitable impurity containing a large amount of Zn, can reduce in order to form the film with desired carrier concentration and the sputtering needed time oxygen concn, therefore there is the excellent results that can improve sputter rate.
Accompanying drawing explanation
Fig. 1 is the figure of the tissue image utilizing EPMA to obtain of the oxidate sintered body representing embodiment 1.
Fig. 2 is the figure of the tissue image utilizing EPMA to obtain of the oxidate sintered body representing embodiment 2.
Fig. 3 is the figure of the tissue image utilizing EPMA to obtain of the oxidate sintered body representing embodiment 3.
Fig. 4 is the figure of the tissue image utilizing EPMA to obtain of the oxidate sintered body representing comparative example.
Fig. 5 is the figure of the relation representing oxygen concn in film forming atmosphere and rate of film build.
Fig. 6 is the figure of the relation of the carrier concentration representing oxygen concn in film forming atmosphere and film.
Embodiment
The feature of oxidate sintered body of the present invention is: comprise (In), gallium (Ga), zinc (Zn), oxygen (O) and inevitable impurity; Have with the IGZO (111) of the atomic ratio measuring In:Ga:Zn=1:1:1 of In, Ga and Zn phase and the IGZO phase containing more Zn than IGZO (111) mutually; The area ratio containing the IGZO phase of more Zn than IGZO (111) is mutually 1 ~ 10%.Owing to having than the IGZO phase (the IGZO phase of rich Zn) of IGZO (111) mutually containing more Zn, can reduce in order to form the film with desired carrier concentration and the sputtering needed time oxygen concn, therefore can improve sputter rate (rate of film build).
Use is containing a large amount of Zn and when there is the IGZO sintered compact spatter film forming of IGZO phase, although mechanism is indefinite, the carrier concentration of film reduces.By using such target, compared with the past can being reduced to obtains desired carrier concentration and the oxygen concn introduced, and therefore can suppress the reduction of the sputter rate caused by oxygen concn.It should be noted that, from saying that oxidate sintered body of the present invention is when oxygen concentration is with equal extent in the past, have the effect that can reduce carrier concentration, sputter rate reduces and does not become important document of the present invention.
IGZO phase (the IGZO phase of the rich zinc) area ratio preferably in sintered compact containing more Zn mutually than IGZO (111) is 1 ~ 10%.When the area ratio of the IGZO phase of rich zinc is less than 1%, the effect reducing the carrier concentration of film is not enough, on the other hand, when the area ratio of the IGZO phase of rich zinc is more than 10%, and spatter film forming and the carrier concentration of film that obtains increases sometimes.
In addition, in the present invention, the atomic ratio of In, Ga and Zn of preferred oxides sintered compact is In:Ga:Zn=1:1:(1.02 ~ 1.10).Thus, effectively can generate rich Zn phase, and the carrier concentration of film can be reduced.When the atomic ratio of Zn is less than 1.02, the effect reducing the carrier concentration of film diminishes.On the other hand, when the atomic ratio of Zn is more than 1.10, compared with being the mutually single-phase situation of IGZO (111) with oxidate sintered body, although the carrier concentration of film is low, carrier concentration changes increase trend into.Therefore, the atomic ratio of In, Ga, Zn of IGZO sintered compact is preferably above-mentioned numerical range.
Oxidate sintered body of the present invention preferably its median size is less than 20 μm.By reducing median size, physical strength can be improved.When median size is more than 20 μm, physical strength reduces, and when sputtering when input excessive power, the stress that the thermal expansion difference due to the backing plate because of sputtering target (sintered compact) and this target of joint produces, likely cracks in sintered compact.
In addition, oxidate sintered body of the present invention its body resistance preferred is 30m below Ω cm.When body resistance is low, the possibility that paradoxical discharge occurs in sputtering reduces, and can suppress the generation to the powder that the film in film forming has a negative impact.On the other hand, when body resistance is more than 30m Ω cm, even if when DC sputtering can be carried out, sometimes in sputtering for a long time, there is paradoxical discharge, sometimes according to circumstances electric discharge is not caused by DC, the necessary RF that using appts cost is high, rate of film build is low sputtering.
In addition, the preferred sintered density of oxidate sintered body of the present invention is 6.3g/cm 3above.When oxidate sintered body of the present invention is used as sputtering target, the densification of sintered compact has the homogeneity that can improve sputtered film and the excellent results that significantly can reduce the powder generation when sputtering.
The typical example of the manufacturing process of oxidate sintered body of the present invention is below described.
Prepare Indium sesquioxide (In 2o 3), gallium oxide (Ga 2o 3) and zinc oxide (ZnO) as raw material.In order to avoid the disadvantageous effect to electrology characteristic caused by impurity, preferably use the raw material of more than purity 4N.Weigh each raw material to reach the ratio of components of regulation.It should be noted that, containing the impurity inevitably contained in these raw materials.
Next, add, mix each raw material and make oxidate sintered body reach the ratio of components of regulation.If now undercompounding, then each composition generation segregation in target, to cause in sputtering the paradoxical discharge such as arc-over or causes powder to produce, therefore preferably fully mixing.Then, by by powder mix Crushing of Ultrafine, granulation and improve formability and the coking property of powder mix, thus highdensity sintered compact can be obtained.As mixing, pulverizing unit, such as, can use commercially available mixing machine, ball mill, ball mill etc.; As pelletization unit, such as, can use commercially available spray-drier.
Next, mixed powder is filled in mould, at surface pressure 400 ~ 1000kgf/cm 2, keep the condition of 1 minute ~ 3 minutes under carry out single shaft compacting and obtain formed body.Surface pressure is less than 400kgf/cm 2time, the formed body that density is enough can not be obtained.In addition, even if apply too high surface pressure, the density of formed body is also difficult to bring up to more than certain numerical value, and when single shaft is suppressed, principle is easy in formed body produce density distribution, thus cause sintering time distortion, cracking, therefore 1000kgf/cm 2above surface pressure is not required especially in production.
Next, this formed body plastic vacuum is packed 2 layers, and at pressure 1500 ~ 4000kgf/cm 2, keep the condition of 1 minute ~ 3 minutes under implement CIP (cold isostatic pressing process).Pressure is less than 1500kgf/cm 2time, the effect of sufficient CIP can not be obtained, on the other hand, even if apply 4000kgf/cm 2above pressure, the density of formed body is also difficult to bring up to more than certain numerical value, therefore 4000kgf/cm 2above surface pressure is not required especially in production.
Next, by formed body 1300 ~ 1500 DEG C temperature, 5 hours ~ 24 hours hold-time, carry out sintering and obtaining sintered compact in air atmosphere or oxygen atmosphere.When sintering temperature is lower than 1300 DEG C, the sintered compact that density is enough can not be obtained; When sintering temperature is more than 1500 DEG C, the crystal grain in sintered compact oversize, likely makes the physical strength of sintered compact reduce.In addition, the hold-time is shorter than 5 constantly little, can not obtain the sintered compact that density is enough; Hold-time is longer than 24 constantly little, not preferred from the viewpoint of production cost.
In addition, in shaping/sintering circuit, in addition to the previous methods, HP (hot pressing) or HIP (hot isostatic pressing method) can also be used.The sintered compact obtained in a manner described forms target shape by mechanical workouts such as grinding, polishings, thus can make sputtering target.
When the making of oxide semiconductor film of the present invention, use the sputtering target obtained in a manner described under defined terms, implement sputtering and carry out film forming, as required, this film is annealed at an established temperature, thus can oxide semiconductor film be obtained.In addition, when making thin film transistor of the present invention, described oxide semiconductor film can be used as the grid shown in Fig. 1, thus obtain thin film transistor.
Embodiment
Below, be described based on embodiment and comparative example.It should be noted that, the present embodiment is only an example, and the present invention is not by this routine any restriction.That is, the present invention only limits by claims, comprises the various distortion outside the embodiment that comprises in the present invention.
(embodiment 1)
Weigh In 2o 3powder, Ga 2o 3powder, ZnO powder make the ratio of components of sintered compact with In, Ga and Zn atomic ratio measuring for 1.00:1.00:1.02, these powder wet types are carried out mixing/Crushing of Ultrafine afterwards, afterwards, carry out drying/granulation, thus obtain mixed powder with spray-drier.Next, by this mixed powder at 400 ~ 1000kgf/cm 2surface pressure to place an order axial compression system and obtain formed body.Then, the formed body plastic vacuum obtained is packed 2 layers, and at 1500 ~ 4000kgf/cm 2under to carry out CIP shaping, in oxygen atmosphere, at the temperature of 1430 DEG C, sinter 20 hours afterwards.
The macrograph utilizing EPMA to obtain of the IGZO sintered compact obtained in a manner described as shown in Figure 1 (in figure, the part of white corresponds to the IGZO phase of rich Zn).The sintered compact confirming embodiment 1 from the macrograph of EPMA is made up of with the IGZO phase of rich Zn mutually IGZO (111).In addition, obtain the area of the IGZO phase of rich Zn from macrograph, and calculate the area ratio of the IGZO phase of rich Zn from the ratiometer of the area with this macrograph entirety.As a result, the area ratio of the IGZO phase of rich Zn is 1.7%.
In addition, the median size obtaining sintered compact is 19.7 μm, sintered density is 6.3g/cm 3highdensity sintered compact.And, obtain low-resistance sintered compact that body resistance is 30.0m Ω cm.Above result is as shown in table 1.It should be noted that, median size is calculated by method of scoring (コ-Fa), and sintered density is obtained by Archimedes method, and body resistance is obtained by four probe method.
Next, mechanical workout is carried out to sintered compact, be finish-machined to the sputtering target of 6 inches, and use this target to sputter.Sputtering condition is: film: DC magnetron sputtering; Film-forming temperature: room temperature; Become film pressure: 0.5Pa (O 2+ Ar), power input: 2.74W/cm 2, oxygen concn during film forming becomes 2 volume %, 6 volume %, 10 volume %, respectively film forming be thickness about film.
The rate of film build each oxygen concn is calculated from the determining film thickness value obtained by cathetometer and film formation time.Result is as shown in table 1 and Fig. 4.As shown in table 1, compared with comparative example described later, confirm rate of film build and slightly improve.
In addition, each film is annealed 1 hour in an atmosphere at 400 DEG C, is measured by Hall effect, measure carrier concentration and hall mobility.Result is as shown in table 1 and Fig. 6.As shown in table 1, compared with comparative example described later, under arbitrary oxygen concn, confirm carrier concentration and reduce.It should be noted that, the mensuration of Hall effect uses the ResiTest8400 of Dongyang technology Co., Ltd..
(embodiment 2)
Weigh In 2o 3powder, Ga 2o 3powder, ZnO powder make the ratio of components of sintered compact with In, Ga and Zn atomic ratio measuring for 1.00:1.00:1.05, these powder wet types are carried out mixing/Crushing of Ultrafine afterwards, afterwards, carry out drying/granulation, thus obtain mixed powder with spray-drier.Next, by this mixed powder at 400 ~ 1000kgf/cm 2surface pressure to place an order axial compression system and obtain formed body.Then, the formed body plastic vacuum obtained is packed 2 layers, and at 1500 ~ 4000kgf/cm 2under to carry out CIP shaping, in oxygen atmosphere, at the temperature of 1430 DEG C, sinter 20 hours afterwards.
The macrograph utilizing EPMA to obtain of the IGZO sintered compact obtained in a manner described as shown in Figure 2 (in figure, the part of white corresponds to the IGZO phase of rich Zn).The sintered compact confirming embodiment 2 from the macrograph of EPMA is made up of with the IGZO phase of rich Zn mutually IGZO (111).In addition, calculate the area ratio of the IGZO phase of rich Zn, result by the method identical with embodiment 1, the area ratio of the IGZO phase of rich Zn is 5.2%.
In addition, the median size obtaining sintered compact is 14.9 μm, sintered density is 6.3g/cm 3highdensity sintered compact.And, obtain low-resistance sintered compact that body resistance is 23.0m Ω cm.Above result is as shown in table 1.It should be noted that, the mensuration of median size, sintered density, body resistance uses the method identical with embodiment 1.
Next, mechanical workout is carried out to sintered compact, be finish-machined to the sputtering target of 6 inches, and use this target to sputter.Sputtering condition is set as the condition identical with embodiment 1.Afterwards, the rate of film build each oxygen concn is calculated from the determining film thickness value obtained by cathetometer and film formation time.Result is as shown in table 1 and Fig. 5.As shown in table 1, compared with comparative example described later, confirm rate of film build and improve.
Next, each film is annealed 1 hour in an atmosphere at 400 DEG C, is measured by Hall effect, measure carrier concentration and hall mobility.Result is as shown in table 1 and Fig. 6.As shown in table 1, compared with comparative example described later, under arbitrary oxygen concn, confirm carrier concentration reduce.
(embodiment 3)
Weigh In 2o 3powder, Ga 2o 3powder, ZnO powder make the ratio of components of sintered compact with In, Ga and Zn atomic ratio measuring for 1.00:1.00:1.10, these powder wet types are carried out mixing/Crushing of Ultrafine afterwards, afterwards, carry out drying/granulation, thus obtain mixed powder with spray-drier.Next, by this mixed powder at 400 ~ 1000kgf/cm 2surface pressure to place an order axial compression system and obtain formed body.Then, the formed body plastic vacuum obtained is packed 2 layers, and at 1500 ~ 4000kgf/cm 2under to carry out CIP shaping, in oxygen atmosphere, at the temperature of 1430 DEG C, sinter 20 hours afterwards.
The macrograph utilizing EPMA to obtain of the IGZO sintered compact obtained in a manner described as shown in Figure 3 (in figure, the part of white corresponds to the IGZO phase of rich Zn).The sintered compact confirming embodiment 3 from the macrograph of EPMA is made up of with the IGZO phase of rich Zn mutually IGZO (111).In addition, calculate the area ratio of the IGZO phase of rich Zn, result by the method identical with embodiment 1, the area ratio of the IGZO phase of rich Zn is 9.8%.
In addition, the median size obtaining sintered compact is 8.9 μm, sintered density is 6.3g/cm 3highdensity sintered compact.And, obtain low-resistance sintered compact that body resistance is 21.0m Ω cm.Above result is as shown in table 1.It should be noted that, the mensuration of median size, sintered density, body resistance uses the method identical with embodiment 1.
Next, mechanical workout is carried out to sintered compact, be finish-machined to the sputtering target of 6 inches, and use this target to sputter.Sputtering condition is set as the condition identical with embodiment 1.Afterwards, the rate of film build each oxygen concn is calculated from the determining film thickness value obtained by cathetometer and film formation time.Result is as shown in table 1 and Fig. 5.As shown in table 1, compared with comparative example described later, confirm rate of film build and improve.
Next, each film is annealed 1 hour in an atmosphere at 400 DEG C, is measured by Hall effect, measure carrier concentration and hall mobility.Result is as shown in table 1 and Fig. 6.As shown in table 1, compared with comparative example described later, under arbitrary oxygen concn, confirm carrier concentration reduce.
(comparative example)
Weigh In 2o 3powder, Ga 2o 3powder, ZnO powder make the ratio of components of sintered compact with In, Ga and Zn atomic ratio measuring for 1.00:1.00:1.00, these powder wet types are carried out mixing/Crushing of Ultrafine afterwards, afterwards, carry out drying/granulation, thus obtain mixed powder with spray-drier.Next, by this mixed powder at 400 ~ 1000kgf/cm 2surface pressure to place an order axial compression system and obtain formed body.Then, the formed body plastic vacuum obtained is packed 2 layers, and at 1500 ~ 4000kgf/cm 2under to carry out CIP shaping, in oxygen atmosphere, at the temperature of 1430 DEG C, sinter 20 hours afterwards.
The macrograph utilizing EPMA to obtain of the IGZO sintered compact obtained in a manner described as shown in Figure 4 (in figure, the part of white corresponds to the IGZO phase of rich Zn).The sintered compact confirming comparative example from the macrograph of EPMA is only made up of mutually IGZO (111).
In addition, the median size of sintered compact is 24.6 μm, and sintered density is 6.3g/cm 3.And body resistance is 37.3m Ω cm.Above result is as shown in table 1.It should be noted that, the mensuration of median size, sintered density, body resistance uses the method identical with embodiment 1.
Next, mechanical workout is carried out to sintered compact, be finish-machined to the sputtering target of 6 inches, and use this target to sputter.Sputtering condition is set as the condition identical with embodiment 1.Afterwards, the rate of film build each oxygen concn is calculated from the determining film thickness value obtained by cathetometer and film formation time.Result is as shown in table 1 and Fig. 5.As shown in table 1, obtain the result that rate of film build compared with embodiment is lower.Next, each film is annealed 1 hour in an atmosphere at 400 DEG C, is measured by Hall effect, measure carrier concentration and hall mobility.Result is as shown in table 1 and Fig. 6.As shown in table 1, obtain the result that carrier concentration compared with embodiment is higher.
Can confirm from above result, consist of 1.00 compared to the Zn of comparative example, the Zn of embodiment consist of 1.02,1.05,1.10 carrier concentration all lower.In comparative example, carrier concentration is reduced to below certain level (such as, 1e + 15cm -3time below), need oxygen concn to be adjusted to more than 10%, but 2% namely enough in known embodiment 1 ~ 3.In addition, though under same oxygen concn film forming, the rate of film build of embodiment is also a little more than the rate of film build of comparative example, and (in general TFT, the carrier concentration of film is about 1e to obtain desired carrier concentration to so there is no necessary increase oxygen + 15cm -3film below), can keep high rate of film build.
Industrial applicability
Oxidate sintered body of the present invention can make sputtering target, when using this sputtering target spatter film forming, can reduce the oxygen concn in sputtering atmosphere, therefore can improve sputter rate (rate of film build).Therefore, by using described sputtering target, there is the excellent results stably can producing oxide semiconductor film and thin film transistor in a large number.Oxide semiconductor film of the present invention is particularly useful as the active layer of TFT in the backboard of flat-panel monitor or flexible panel indicating meter etc.

Claims (5)

1. an oxide sintered body, it is for comprising the oxidate sintered body of indium (In), gallium (Ga), zinc (Zn), oxygen (O) and inevitable impurity, it is characterized in that, described oxidate sintered body has with the IGZO (111) of the atomic ratio measuring In:Ga:Zn=1:1:1 of In, Ga and Zn phase and the IGZO phase containing more Zn than IGZO (111) mutually; The area ratio containing the IGZO phase of more Zn than IGZO (111) is mutually 1 ~ 10%; The atomicity of In, Ga and Zn of this oxidate sintered body is than being In:Ga:Zn=1:1:(1.02 ~ 1.10).
2. oxidate sintered body as claimed in claim 1, it is characterized in that, median size is less than 20 μm.
3. oxidate sintered body as claimed in claim 1 or 2, it is characterized in that, body resistance is 30m below Ω cm.
4. oxidate sintered body as claimed any one in claims 1 to 3, it is characterized in that, sintered density is 6.3g/cm 3above.
5. a sputtering target, its oxidate sintered body according to any one of Claims 1-4 makes.
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