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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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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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  • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
  • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/02104—Forming layers
  • H01L21/02365—Forming inorganic semiconducting materials on a substrate
  • H01L21/02518—Deposited layers
  • H01L21/02521—Materials
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  • H01L21/02104—Forming layers
  • H01L21/02365—Forming inorganic semiconducting materials on a substrate
  • H01L21/02612—Formation types
  • H01L21/02617—Deposition types
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  • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
  • H10D30/00—Field-effect transistors [FET]
  • H10D30/60—Insulated-gate field-effect transistors [IGFET]
  • H10D30/67—Thin-film transistors [TFT]
  • H10D30/674—Thin-film transistors [TFT] characterised by the active materials
  • H10D30/6755—Oxide semiconductors, e.g. zinc oxide, copper aluminium oxide or cadmium stannate
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  • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
  • H10D86/00—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates
  • H10D86/40—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs
  • H10D86/60—Integrated devices formed in or on insulating or conducting substrates, e.g. formed in silicon-on-insulator [SOI] substrates or on stainless steel or glass substrates characterised by multiple TFTs wherein the TFTs are in active matrices
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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
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • 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
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
  • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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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

Definitions

• the present invention relates to an oxide sintered body and an oxide semiconductor thin film useful for manufacturing a thin film transistor in a display device.
• Oxide semiconductors are used as active layers of thin film transistors in display devices such as liquid crystal display devices, plasma display devices, and organic EL display devices, as well as electrodes for solar cells and touch panels.
• display devices such as liquid crystal display devices, plasma display devices, and organic EL display devices, as well as electrodes for solar cells and touch panels.
• IGZO-based transparent In—Ga—Zn—O-based
• Patent Documents 1 and 2 There is also a report on a system to which Sn) is added (see Patent Documents 1 and 2).
• gallium (Ga) which is an essential component of these systems, is a rare element and has a large limitation in terms of industrial use because of its high price.
• Patent Document 3 As a transparent oxide semiconductor not using Ga, an In—Zn—O system (see Patent Document 3), an In—Zn—Sn—O system (see Patent Document 4), and a Zn—Sn—O system (Patent Document 5). Report).
• the IGZO-based alternative candidate materials described in Patent Documents 3 to 5 above have been limited to only the material system of elements that are transparent as oxides because the IGZO-based material is a transparent semiconductor.
• the IGZO system is used as a channel layer of a transistor, and in most cases, transparency is not necessarily required. Therefore, a material system that is not transparent but can be used as a channel layer of a transistor has not been studied as an alternative material for IGZO.
• an object of the present invention is to provide an oxide sintered body for manufacturing an oxide semiconductor film which is a scarce resource and does not contain expensive gallium (Ga).
• Another object of the present invention is to provide an oxide semiconductor thin film having the same composition as the oxide sintered body.
• trivalent indium ions (In 3+ ), trivalent iron ions (Fe 3+ ), and divalent X ions (X 2+ ) (where X is Cu, Zn, And an oxide sintered body composed of oxygen ions (O 2 ⁇ ) and trivalent indium ions (In 3+ ),
• the atomic ratio of iron ions (Fe 3+ ) and divalent X ions (X 2+ ) is 0.2 ⁇ (In 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2 + ) ⁇ ⁇ 0.8, 0.1 ⁇ (Fe 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ ⁇ 0.5, 0.1 ⁇ (X 2+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ ⁇ 0.5.
• the oxide sintered body according to the present invention has a relative density of 98% or more.
• the oxide sintered body according to the present invention has a bulk resistance of 3 m ⁇ or less.
• a trivalent indium ion (In 3+ ), a trivalent iron ion (Fe 3+ ), and a divalent X ion (X 2+ ) (where X is Cu,
• the atomic ratio of iron ions (Fe 3+ ) and divalent X ions (X 2+ ) is 0.2 ⁇ (In 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ ⁇ 0.8, 0.1 ⁇ (Fe 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ ⁇ 0.5, and 0.1 ⁇
• the oxide semiconductor thin film satisfies (X 2+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ ⁇ 0.5.
• the oxide semiconductor thin film according to the present invention is amorphous.
• the oxide semiconductor thin film according to the present invention has a carrier concentration of 10 16 to 10 18 cm ⁇ 3 .
• the oxide semiconductor thin film according to the present invention has a mobility of 1 cm 2 / Vs or more.
• the present invention is a thin film transistor including the oxide semiconductor thin film as an active layer.
• the present invention is an active matrix drive display panel including the thin film transistor.
• an oxide sintered body for producing an oxide semiconductor film that does not contain gallium (Ga) can be provided.
• This oxide sintered body is useful as a sputtering target.
• An oxide semiconductor film can be formed by sputtering using this target.
• the oxide sintered body according to the present invention includes a trivalent indium ion (In 3+ ), a trivalent iron ion (Fe 3+ ), and a divalent X ion (X 2+ ) (where X is It represents one or more elements selected from Cu, Zn, and Fe.) And oxygen ions (O 2 ⁇ ).
• X is It represents one or more elements selected from Cu, Zn, and Fe.
• oxygen ions O 2 ⁇
• elements that are inevitably included in the purification process of raw materials that are usually available, and impurity elements that are inevitably mixed in the oxide sintered body manufacturing process, are inevitably contained at a concentration, for example, each element. What contains about 10 ppm is included in the sintered compact which concerns on this invention.
• the number ratio (In 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is preferably 0.2 to 0.8. If (In 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is less than 0.2, the carrier concentration of the film becomes too small, and the relative value during target fabrication Density decreases, bulk resistance increases, and abnormal discharge during sputtering is likely to occur.
• the ratio of numbers (Fe 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is preferably 0.1 to 0.5 (Fe 3+ ) / ⁇ (In 3 + ) + (Fe 3+ ) + (X 2+ ) ⁇ is less than 0.1, the carrier concentration of the film obtained by sputtering the target having that composition becomes too high, and the channel layer of the transistor As a result, the on / off ratio becomes small.
• (Fe 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ exceeds 0.5, the carrier concentration of the film becomes too small, and the target is produced. The relative density of the metal becomes small, the bulk resistance becomes high, and abnormal discharge during sputtering is likely to occur.
• (Fe 3+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is more preferably in the range of 0.15 to 0.4, and more preferably 0.2 to 0. .35 range.
• Ratio of total number of atoms of metal element X to total number of trivalent indium ions (In 3+ ), trivalent iron ions (Fe 3+ ), and divalent X ions (X 2+ ) (X 2 + ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is preferably 0.1 to 0.5. If (X 2+ ) / ⁇ (In 3+ ) + (Fe 3+ ) + (X 2+ ) ⁇ is less than 0.1, the carrier concentration of the film becomes too large.
• iron ions Fe 2+
• the only types of metal ions are indium and iron.
• divalent and trivalent types of iron ions which are present in the oxide sintered body.
• Iron is a transition metal and can take a plurality of valences, and iron ions having different valences may exist in a certain compound.
• the compound is formed in advance by controlling the valence of iron ions. Thus, desired characteristics can be obtained more easily.
• the relative density of the oxide sintered body correlates with the generation of joules on the surface during sputtering. If the oxide sintered body has a low density, the oxide sintered body is processed into a target to form a sputter film. At the same time, a high-resistance portion called a protruding nodule, which is a lower oxide of indium, is generated on the surface as the film formation of the sputtering is performed, and it tends to be a starting point of abnormal discharge during the subsequent sputtering.
• a protruding nodule which is a lower oxide of indium
• the relative density of the oxide sintered body can be set to 98% or more by optimizing the appropriate range of the composition, and if this density is high, there is almost no adverse effect due to nodules during sputtering.
• the relative density is preferably 99% or more, more preferably 99.5% or more.
• the relative density of the oxide sintered body is obtained by dividing the density calculated from the weight and outer dimensions after processing the oxide sintered body into a predetermined shape by the theoretical density of the oxide sintered body. Can be sought.
• the bulk resistance of the oxide sintered body has a correlation with the ease of occurrence of abnormal discharge during sputtering, and when the bulk resistance is high, abnormal discharge is likely to occur during sputtering.
• the bulk resistance can be reduced to 3 m ⁇ cm or less by optimizing the appropriate range of the composition and the manufacturing conditions. With such a low bulk resistance, there is almost no adverse effect on the occurrence of abnormal discharge during sputtering.
• the bulk resistance is preferably 2.7 m ⁇ cm or less, more preferably 2.5 m ⁇ cm or less. Bulk resistance can be measured using a resistivity meter by the four-probe method.
• the oxide sintered body having various compositions according to the present invention includes, for example, raw materials such as indium oxide (In 2 O 3 ), iron oxide (Fe 2 O 3 as a supply source of trivalent iron, and a supply source of divalent iron. Conditions such as mixing ratio of raw material powders such as FeO), zinc oxide (ZnO), copper oxide (CuO), particle size of raw material powder, pulverization time, sintering temperature, sintering time, kind of sintering atmosphere gas, etc. Can be obtained by adjusting.
• raw materials such as indium oxide (In 2 O 3 ), iron oxide (Fe 2 O 3 as a supply source of trivalent iron, and a supply source of divalent iron.
• Conditions such as mixing ratio of raw material powders such as FeO), zinc oxide (ZnO), copper oxide (CuO), particle size of raw material powder, pulverization time, sintering temperature, sintering time, kind of sintering atmosphere gas, etc. Can be obtained by adjusting.
• the raw material powder preferably has an average particle size of 1 to 2 ⁇ m.
• the average particle diameter exceeds 2 ⁇ m, the density of the sintered body is difficult to improve. Therefore, wet pulverization or the like is performed as the raw material powder alone or as a mixed powder, and the average particle diameter is preferably reduced to about 1 ⁇ m.
• wet pulverization or the like is performed as the raw material powder alone or as a mixed powder, and the average particle diameter is preferably reduced to about 1 ⁇ m.
• it is also effective to perform calcination.
• raw materials having a particle size of less than 1 ⁇ m are difficult to obtain, and if the particle size is too small, agglomeration between particles tends to occur and handling becomes difficult.
• the average particle diameter of the raw material powder refers to the median diameter in the volume distribution measured by a laser diffraction particle size distribution measuring apparatus.
• the molded product is sintered to obtain a sintered body.
• the sintering is preferably performed at 1400 to 1600 ° C. for 2 to 20 hours. Thereby, a relative density can be 98% or more. If the sintering temperature is less than 1400 ° C., the density is difficult to improve. Conversely, if the sintering temperature exceeds 1600 ° C., the composition of the sintered body changes due to volatilization of the constituent elements, and voids are generated due to volatilization. May cause a decrease in density. Air can be used as the atmosphere gas during sintering, and the amount of oxygen vacancies in the sintered body can be increased to reduce the bulk resistance. However, depending on the composition of the sintered body, a sufficiently high density sintered body can be obtained even if the atmospheric gas is oxygen.
• the oxide sintered body obtained as described above can be used as a sputtering target by performing processing such as grinding and polishing, and by using this film, the same composition as that of the target can be obtained. It is possible to form an oxide film having At the time of processing, it is desirable that the surface roughness (Ra) be 5 ⁇ m or less by grinding the surface by a method such as surface grinding. By reducing the surface roughness, the starting point of nodule generation that causes abnormal discharge can be reduced.
• the sputtering target is affixed to a backing plate made of copper or the like, placed in a sputtering apparatus, and sputtered under appropriate conditions such as an appropriate degree of vacuum, atmospheric gas, and sputtering power, so that the film has almost the same composition as the target. Can be obtained.
• the degree of vacuum reached in the chamber before film formation is 2 ⁇ 10 ⁇ 4 Pa or less. If the pressure is too high, the mobility of the obtained film may decrease due to the influence of impurities in the residual atmospheric gas.
• a mixed gas of argon and oxygen can be used as the sputtering gas.
• a gas cylinder with 100% argon and a gas cylinder with 2% oxygen in argon are used, and the supply flow rate from each gas cylinder to the chamber is appropriately set by mass flow.
• the oxygen concentration in the mixed gas means oxygen partial pressure / (oxygen partial pressure + argon partial pressure), and is equal to the oxygen flow rate divided by the sum of oxygen and argon flow rates.
• the oxygen concentration may be appropriately changed according to the desired carrier concentration, but it can typically be 1 to 3%, more typically 1 to 2%.
• the total pressure of the sputtering gas is about 0.3 to 0.8 Pa. If the total pressure is lower than this, the plasma discharge is difficult to stand up, and even if it stands, the plasma becomes unstable. On the other hand, if the total pressure is higher than this, the film formation rate becomes slow, which causes inconveniences such as adversely affecting productivity.
• the film is formed with a sputtering power of about 200 to 1200 W. If the sputtering power is too low, the film forming speed is low and the productivity is poor. Conversely, if the sputtering power is too high, problems such as cracking of the target occur. 200 ⁇ 1200 W when converted to a sputtering power density is 1.1W / cm 2 ⁇ 6.6W / cm 2, it is desirable that the 3.2 ⁇ 4.5W / cm 2.
• the sputtering power density is a value obtained by dividing the sputtering power by the area of the sputtering target, and even with the same sputtering power, the power actually received by the sputtering target varies depending on the sputtering target size, and the film formation speed differs. It is an index for uniformly expressing the power applied to the sputtering target.
• a vacuum deposition method As a method for obtaining a film from an oxide sintered body, a vacuum deposition method, an ion plating method, a PLD (pulse laser deposition) method, or the like can be used.
• This is a DC magnetron sputtering method that satisfies requirements such as film formation and discharge stability.
• the substrate there is no need to heat the substrate during sputter deposition. This is because a relatively high mobility can be obtained without heating the substrate, and it is not necessary to spend time and energy for raising the temperature.
• the resulting film becomes amorphous.
• the film since the same effect as annealing after film formation at room temperature can be expected by heating the substrate, the film may be formed by heating the substrate.
• carrier concentration of oxide film correlates with various characteristics of the transistor when the film is used for the channel layer of the transistor. If the carrier concentration is too high, a minute leakage current is generated even when the transistor is turned off, and the on / off ratio is lowered. On the other hand, if the carrier concentration is too low, the current flowing through the transistor becomes small.
• the carrier concentration of the oxide film can be set to 10 16 to 10 18 cm ⁇ 3 depending on an appropriate range of the composition and the like, and a transistor with favorable characteristics can be manufactured within this range.
• the mobility is one of the most important characteristics of the transistor, and the oxide semiconductor has a mobility of 1 cm 2 / Vs or more which is the mobility of amorphous silicon which is a competitive material used as a channel layer of the transistor. Is desirable. Basically, the higher the mobility, the better.
• the oxide film according to the present invention can have a mobility of 1 cm 2 / Vs or more, preferably a mobility of 3 cm 2 / Vs or more, more preferably 5 cm 2 depending on an appropriate range of the composition. It can have a mobility of / Vs or higher. Thereby, it becomes a characteristic superior to amorphous silicon, and industrial applicability is further increased.
• the oxide semiconductor thin film according to the present invention can be used, for example, as an active layer of a thin film transistor.
• the thin film transistor obtained by using the above manufacturing method can be used as an active element and used for an active matrix drive display panel.
• the physical properties of the sintered bodies and films were measured by the following methods.
• A Relative density of sintered body It was determined from the measurement results of weight and outer dimensions and the theoretical density from the constituent elements.
• B Bulk resistance of sintered body The bulk resistance was determined by a four probe method (JIS K7194) using a model ⁇ -5 + apparatus manufactured by NPS.
• C Composition of sintered body and film It was determined by an ICP (high frequency inductively coupled plasma) analysis method using a model SPS3000 manufactured by SII Nanotechnology.
• D Film thickness It was determined using a step meter (Veeco, Model Dektak8 STYLUS PROFILER).
• Example 1 Indium oxide (In 2 O 3 ) powder (average particle size 1.0 ⁇ m), iron oxide (Fe 2 O 3 ) powder (average particle size 1.0 ⁇ m), and zinc oxide (ZnO) powder (average particle size 1.0 ⁇ m) ) was weighed so that the atomic ratio of metal elements (In: Fe: Zn) was 0.4: 0.3: 0.3, and wet mixed and pulverized. The average particle size of the mixed powder after pulverization was 0.8 ⁇ m. After this mixed powder was granulated with a spray dryer, the mixed powder was filled in a mold, subjected to pressure molding, and then sintered in an air atmosphere at a high temperature of 1450 ° C. for 10 hours.
• the obtained sintered body was processed into a disk shape having a diameter of 6 inches and a thickness of 6 mm, and was subjected to surface grinding to obtain a sputtering target.
• the relative density was calculated from the measurement results of the weight and the external dimensions, and the theoretical density, which was 99.6%.
• the bulk resistance of the sintered body measured by the four probe method was 2.0 m ⁇ cm.
• ICP high frequency inductively coupled plasma
• the sputtering target prepared above was attached to a copper backing plate using indium as a brazing material, and was installed in a DC magnetron sputtering apparatus (APLVA SPL-500 sputtering apparatus).
• the glass substrate uses Corning 1737, and the sputtering conditions are as follows: substrate temperature: 25 ° C., ultimate pressure: 1.2 ⁇ 10 ⁇ 4 Pa, atmospheric gas: Ar 99%, oxygen 1%, sputtering pressure (total pressure): 0.
• a thin film having a thickness of about 100 nm was prepared at 5 Pa and input power of 500 W. No abnormal discharge was observed during the formation of the oxide semiconductor thin film.
• Example 2 to Example 12 An oxide sintered body and an oxide semiconductor thin film were obtained in the same manner as in Example 1 except that the composition ratio of the raw material powder was set to the respective values shown in Table 1. The relative density, bulk resistance, carrier concentration, and mobility of each were as shown in Table 1. The composition of the sintered body and the film was the same as the composition ratio of the raw material powder.
• the indium oxide as a supply source of In 3+ (In 2 O 3) powder (average particle size 1.0 .mu.m), iron oxide as a source of Fe 3+ (Fe 2 O 3) powder (average particle size 1.0 .mu.m ), Zinc 2+ (ZnO) powder (average particle size: 1.0 ⁇ m) as a source of Zn 2+ , (CuO) powder (average particle size: 1.0 ⁇ m) as a source of Cu 2+, and a source of Fe 2+ As an iron oxide (FeO) powder (average particle size 1.0 ⁇ m) was used.
• the oxide sintered bodies according to the examples of the present invention have a high relative density and a low bulk resistance.
• an oxide semiconductor thin film having an appropriate carrier concentration and high mobility can be obtained.

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