WO2013065784A1 - Corps compact fritté d'oxydes et cible de pulvérisation, procédé de production correspondant - Google Patents

Corps compact fritté d'oxydes et cible de pulvérisation, procédé de production correspondant Download PDF

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WO2013065784A1
WO2013065784A1 PCT/JP2012/078325 JP2012078325W WO2013065784A1 WO 2013065784 A1 WO2013065784 A1 WO 2013065784A1 JP 2012078325 W JP2012078325 W JP 2012078325W WO 2013065784 A1 WO2013065784 A1 WO 2013065784A1
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oxide
sintered body
zno
oxide sintered
sintering
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Japanese (ja)
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英雄 畠
幸樹 田尾
守賀 金丸
旭 南部
祐紀 岩崎
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株式会社コベルコ科研
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    • 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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Definitions

  • the present invention relates to an oxide sintered body and a sputtering target used when a thin film transistor (TFT) oxide semiconductor thin film used in a display device such as a liquid crystal display or an organic EL display is formed by a sputtering method, and a method for manufacturing the oxide sintered body. It is about.
  • TFT thin film transistor
  • An amorphous (amorphous) oxide semiconductor used for a TFT has a higher carrier mobility than a general-purpose amorphous silicon (a-Si), has a large optical band gap, and can be formed at a low temperature. Therefore, it is expected to be applied to next-generation displays that require large size, high resolution, and high-speed driving, and resin substrates with low heat resistance.
  • a-Si general-purpose amorphous silicon
  • ITO In-containing amorphous oxide semiconductors
  • a sputtering method is preferably used in which a sputtering target made of the same material as the film is sputtered.
  • a sputtering target made of the same material as the film is sputtered.
  • prevention of abnormal discharge during sputtering and prevention of cracking of the target are important in order to stabilize the characteristics of the thin film as a product and increase the efficiency of production, and various techniques have been proposed.
  • Patent Document 1 proposes a technique for suppressing abnormal discharge for an ITO target by reducing the average grain size of crystal grains.
  • Patent Document 2 proposes a technique for preventing cracking of the target plate during sputtering by increasing the sintering density and reducing the crystal grain size for the ITO target.
  • Patent Document 3 discloses that an In—Zn—O-based composite oxide is annealed in a reducing atmosphere after sintering, thereby improving the conductivity of the target material, thereby preventing abnormal discharge during sputtering and cracking of the target. Suppression techniques have been proposed.
  • a sputtering target used for manufacturing an oxide semiconductor film for a display device and an oxide sintered body that is a material thereof have high carrier mobility.
  • the objective is the oxide sintered compact suitably used for manufacture of the oxide semiconductor film for display apparatuses, and a sputtering target, Comprising: It has high carrier mobility.
  • An object of the present invention is to provide an oxide sintered body, a sputtering target, and a method for producing the same, which can suppress abnormal discharge of the oxide semiconductor film and cracking of the target and can stably form a film by sputtering.
  • the oxide sintered body of the present invention that can solve the above-mentioned problems includes zinc oxide; indium oxide; an oxide of at least one metal selected from the group consisting of Ti, Mg, Al, and Nb;
  • Zn m In 2 O 3 + m m is an integer of 5 to 7
  • the relative density is 95% or more and the specific resistance is 0.1 ⁇ ⁇ cm or less.
  • the content (atomic%) of zinc, indium, Ti, Mg, Al, and Nb with respect to all metal elements in the oxide sintered body is respectively [Zn], [In], [In], [Ti], [Mg], [Al], [Nb], the ratio of [In] to [Zn], [Zn] + [In] + [Ti] + [Mg] + [Al] + [Nb] ] [Ti] + [Mg] + [Al] + [Nb] satisfy the following formulas.
  • the volume ratio of each crystal phase with respect to the total of Zn m In 2 O 3 + m , In 2 O 3 , and ZnO contained in the oxide sintered body is as follows: The expression is satisfied. 0.1 ⁇ Zn m In 2 O 3 + m / (Zn m In 2 O 3 + m + In 2 O 3 + ZnO) ⁇ 0.75 0.05 ⁇ In 2 O 3 / (Zn m In 2 O 3 + m + In 2 O 3 + ZnO) ⁇ 0.7 0.05 ⁇ ZnO / (Zn m In 2 O 3 + m + In 2 O 3 + ZnO) ⁇ 0.7 (However, Zn m In 2 O 3 + m is the total of Zn 5 In 2 O 8 , Zn 6 In 2 O 9 , and Zn 7 In 2 O 10. )
  • the sputtering target of the present invention that has solved the above-mentioned problems is a sputtering target obtained using the oxide sintered body described above.
  • the preferable manufacturing method of the said oxide sintered compact which concerns on this invention which could solve the said subject is at least 1 sort (s) selected from the group which consists of zinc oxide, indium oxide, Ti, Mg, Al, and Nb.
  • a first sintering step in which the metal oxide is mixed and set in a graphite mold and then sintered at a sintering temperature of 850 to 1050 ° C. and a holding time of 1 to 10 hours in the temperature range; After the one sintering step, the sintering temperature is 1000 to 1050 ° C. (however, higher than the sintering temperature in the first step), and the second sintering time is 0.5 to 10 hours in the temperature range. And the first sintering step and the second sintering step are performed at a pressure of 100 to 500 kgf / cm 2 .
  • an oxide sintered body and a sputtering target capable of suppressing abnormal discharge and cracking of a target in an oxide semiconductor film having high carrier mobility and stably forming a film by a sputtering method, and a method for manufacturing the same Can be provided.
  • FIG. 1 is a diagram showing a basic process for producing an oxide sintered body and a sputtering target of the present invention.
  • FIG. 2 is a graph showing an example of a sintering process (first sintering process and second sintering process) used in the production method of the present invention.
  • the present inventors have made it possible to form a stable film for a long time by suppressing the occurrence of abnormal discharge and cracking during sputtering for an oxide sintered body containing zinc oxide and indium oxide, and carrier movement
  • an oxide sintered body for a sputtering target suitable for forming an oxide semiconductor film having a high degree a study has been repeated.
  • M metal zinc oxide; indium oxide; and powders of oxides of at least one metal selected from the group consisting of Ti, Mg, Al, and Nb (hereinafter referred to as M metal) are mixed and sintered.
  • phase structure when the oxide sintered body is subjected to X-ray diffraction (i) Zn and In are Zn m In 2 O 3 + m in which they are bonded (m is an integer of 5 to 7) , And In 2 O 3 and ZnO, when such a phase configuration is adopted, abnormal discharge during sputtering can be significantly suppressed, and (ii) M metal exhibits a useful effect for improving carrier mobility. (Iii) By controlling the relative density and specific resistance, it has been found that the effect of suppressing the occurrence of cracks and abnormal discharge during sputtering can be further improved. (Iv) Then, in order to obtain an oxide sintered body having such a phase structure, it was found that the sintering should be performed under predetermined sintering conditions, and the present invention has been achieved.
  • the oxide sintered body according to the present invention when the oxide sintered body of the present invention is subjected to X-ray diffraction on the oxide sintered body, Zn m In 2 O 3 + m (m is an integer of 5 to 7), In 2 O 3 , And an oxide sintered body containing each crystal phase of ZnO.
  • the X-ray diffraction conditions in the present invention are as follows. Analysis device: “X-ray diffractometer RINT-1500” manufactured by Rigaku Corporation Analysis conditions: Target: Cu Monochromatic: Uses a monochrome mate (K ⁇ ) Target output: 40kV-200mA (Continuous measurement) ⁇ / 2 ⁇ scanning Slit: Divergence 1/2 °, Scattering 1/2 °, Received light 0.15 mm Monochromator light receiving slit: 0.6mm Scanning speed: 2 ° / min Sampling width: 0.02 ° Measurement angle (2 ⁇ ): 5 to 90 °
  • Zn 6 In 2 O 9 specifies a crystal phase having a crystal structure described in the following references (1) and (2).
  • References (1) M. Nakamura, N. Kimizuka and T. Mohri: J. Solid State Chem. 86 (1990) 16-40
  • Reference (2) M. Nakamura, N. Kimizuka, T. Mohri and M. Isobe: J. Solid State Chem. 105 (1993) 535-549
  • the Zn m In 2 O 3 + m compound (phase) is formed by combining zinc oxide and indium oxide constituting the oxide sintered body of the present invention.
  • the crystal structure of this compound is a hexagonal crystal, greatly contributing to the improvement in carrier mobility of the oxide sintered body, and by containing it together with In 2 O 3 and ZnO described later, the effect of significantly suppressing abnormal discharge Is expressed.
  • M in the Zn m In 2 O 3 + m compound is at least one of 5 (Zn 5 In 2 O 8 ), 6 (Zn 6 In 2 O 9 ), and 7 (Zn 7 In 2 O 10 ). Since the Zn m In 2 O 3 + m compound is a complex oxide crystal in which Zn, In, and M metal are dissolved, m is always an integer. If m is an integer of 4 or less or an integer of 8 or more, the semiconductor characteristics of the oxide semiconductor film are deteriorated and carrier mobility is lowered, which is not desirable.
  • the oxide sintered body of the present invention essentially contains each crystal phase (compound) of In 2 O 3 and ZnO. Abnormal discharge can be suppressed by including In 2 O 3 and ZnO in the oxide sintered body. Although the details of the mechanism are unknown, when the above phases in the oxide sintered body are more uniformly dispersed, local conductivity, or thermal conductivity is improved, and abnormal discharge and cracking are suppressed. Inferred.
  • Each crystal phase of the present invention includes a case where M metal described later is in solid solution. Further, In 2 O 3 and ZnO include a case where Zn or In is dissolved in addition to M metal.
  • M metal used in the present invention is an element useful for improving carrier mobility of a film formed by sputtering.
  • the M metal is at least one selected from the group consisting of Ti, Mg, Al, and Nb.
  • the said M metal may be used independently and may use 2 or more types together.
  • preferable M metals from the viewpoint of semiconductor characteristics are Ti, Mg, and Al.
  • M metal is an element selected as an element that greatly contributes to improving the carrier mobility of an oxide sintered body composed only of zinc oxide and indium oxide. Compared with the case where no M metal is contained, carrier mobility is improved by using an oxide sintered body containing the M metal specified in the present invention, preferably in a predetermined ratio described later.
  • the present invention is not limited to this, and a part of the M metal may be present as an oxide (for example, 5% by volume or less) as long as the effect of improving the carrier mobility of the present invention is not inhibited.
  • [Zn], [In], [Ti], [Mg], [Al] for the contents (atomic%) of zinc, indium, Ti, Mg, Al, and Nb with respect to all metal elements in the oxide sintered body, respectively.
  • [Nb] the ratio of [In] to [Zn], [Ti] + [Mg] + for [Zn] + [In] + [Ti] + [Mg] + [Al] + [Nb]
  • the ratio of [Al] + [Nb] is preferably within the following specific range from the viewpoint of obtaining the desired effect.
  • the ratio of [In] to [Zn] ([In] / [Zn]; hereinafter referred to as the ratio (1)) is preferably 0.27 or more, more preferably 0.28 or more, and preferably 0. .45 or less, more preferably 0.40 or less.
  • a complex oxide (Zn 4 In 2 O 7 etc.) with [Zn m In 2 O 3 + m ] of m ⁇ 4 is generated, and the resistivity is increased and carrier movement is increased. The degree decreases.
  • a complex oxide (Zn 8 In 2 O 11 or the like) having [Zn m In 2 O 3 + m ] of m ⁇ 8 is generated, and the carrier mobility is lowered. .
  • the lower limit of the ratio (2) is not particularly limited, but is preferably 0.001 or more, more preferably 0.005 or more from the viewpoint of stabilizing the thin film semiconductor characteristics.
  • the ratio of Zn m In 2 O 3 + m , In 2 O 3 ratio, and ZnO ratio to the sum of [Zn m In 2 O 3 + m ] + [In 2 O 3 ] + [ZnO] are respectively set to [ They are called Zn m In 2 O 3 + m ] ratio, [In 2 O 3 ] ratio, and [ZnO] ratio.
  • the [Zn m In 2 O 3 + m ] ratio is preferably 0.1 or more.
  • the [Zn m In 2 O 3 + m ] ratio is less than 0.1, abnormal discharge and cracking increase.
  • a more preferable lower limit is 0.2 or more, and further preferably 0.3 or more.
  • cracking is likely to occur even if the [Zn m In 2 O 3 + m ] ratio is too large, so it is less than 0.75, preferably 0.7 or less, more preferably 0.6 or less.
  • [In 2 O 3 ] ratio is preferably 0.05 to 0.7.
  • the [In 2 O 3 ] ratio is more preferably 0.1 or more, further preferably 0.2 or more, more preferably 0.6 or less, still more preferably 0.5 or less.
  • the [ZnO] ratio is preferably 0.05 to 0.7.
  • the [ZnO] ratio is more preferably 0.1 or more, further preferably 0.2 or more, more preferably 0.6 or less, and still more preferably 0.5 or less.
  • the crystalline phase of the oxide sintered body of the present invention is preferably substantially composed of Zn m In 2 O 3 + m , In 2 O 3 , and ZnO.
  • other crystal phases that can be included include Zn 2 TiO 4 and InNbO 4 which are inevitably produced in production, and these may be contained in a proportion of about 5% by volume.
  • generated unavoidable can be measured by XRD.
  • the oxide sintered body of the present invention and the sputtering target obtained using the oxide sintered body are characterized in that the relative density is 95% or more and the specific resistance is 0.1 ⁇ ⁇ cm or less.
  • the oxide sintered body of the present invention has a very high relative density of 95% or more, preferably 97% or more.
  • a high relative density not only can prevent the generation of cracks and nodules during sputtering, but also provides advantages such as maintaining a stable discharge continuously to the target life.
  • the oxide sintered body of the present invention has a small specific resistance and is 0.1 ⁇ ⁇ cm or less, preferably 0.01 ⁇ ⁇ cm or less. Thereby, abnormal discharge can be suppressed, film formation with suppressed abnormal discharge during sputtering can be performed, and physical vapor deposition (sputtering method) using a sputtering target can be efficiently performed on the production line of the display device.
  • the oxide sintered body of the present invention is obtained by mixing and sintering zinc oxide, indium oxide, and M metal oxide powders.
  • the sputtering target can be manufactured by processing an oxide sintered body.
  • oxide powder obtained by (a) mixing / pulverization ⁇ (b) drying / granulation ⁇ (c) preforming ⁇ (d) degreasing ⁇ (e) hot pressing The basic process until the sputtering target is obtained by bonding the body to (f) processing ⁇ (g) is shown.
  • the present invention is characterized in that the sintering conditions ((e) hot press) are appropriately controlled as described in detail below, and the other steps are not particularly limited, and are usually used steps. Can be appropriately selected.
  • this invention is not the meaning limited to this.
  • each raw material powder is the ratio of [In] to [Zn], [Ti] + [Mg] + to [Zn] + [In] + [Ti] + [Mg] + [Al] + [Nb]. It is preferable to control so that the ratio of [Al] + [Nb] is within the above-described range.
  • (A) Mixing and pulverization are preferably performed by using a pot mill and adding the raw material powder together with water.
  • the balls and beads used in these steps are preferably made of materials such as nylon, alumina, zirconia, and the like.
  • a dispersant or a binder may be mixed in order to ensure the ease of the subsequent molding process for the purpose of uniform mixing.
  • preforming is performed.
  • the powder after drying and granulation is filled in a mold having a predetermined size, and preformed by a mold press. This pre-molding is performed for the purpose of improving the handleability when setting to a predetermined mold in the hot press process, so if a pressing force of about 0.5 to 1.0 tonf / cm 2 is applied to form a molded body. Good.
  • the heating conditions are not particularly limited as long as the purpose of degreasing can be achieved.
  • the heating conditions may be maintained at about 500 ° C. in the atmosphere for about 5 hours.
  • the compact After degreasing, the compact is set in a graphite mold having a desired shape and (e) sintered by hot pressing.
  • the graphite mold is a reducing material, and since the set molded body can be sintered in a reducing atmosphere, the reduction proceeds efficiently and the specific resistance can be lowered.
  • sintering is performed in two heating steps (FIG. 2), so that the desired crystal phase structure can be obtained and the relative density can be increased.
  • FOG. 2 heating steps
  • densification and reduction of the sintered body proceed in the first sintering step
  • further densification and reduction proceed in the second sintering step
  • the sintered body can be densified and the composite oxide can be produced under optimum conditions, so that the oxide sintered body having a desired crystal phase has a high relative It is estimated that the density can be obtained, and the dispersibility is greatly improved.
  • the conditions of the first sintering step are sintering at a sintering temperature: 850 to 1050 ° C. and a holding time at the temperature: 1 to 10 hours.
  • a sintering temperature is less than 850 ° C. or more than 1050 ° C.
  • a preferable sintering temperature is 900 ° C. or higher and 1000 ° C. or lower. If the sintering time is too short, it cannot be sufficiently densified and a relative density of 95% or more cannot be achieved. Accordingly, the sintering time is 1 hour or longer, preferably 2 hours or longer, more preferably 4 hours or longer. If the sintering time is lengthened, the relative density can be increased, but the productivity deteriorates, so that it is 10 hours or less, preferably 8 hours or less, more preferably 6 hours or less.
  • the conditions of the second sintering step are the same sintering temperature range (1000 to 1050 ° C.) as the first sintering step, but the temperature is higher than the sintering temperature of the first step. Holding time: Sintering is performed for 0.5 to 10 hours. If the sintering temperature is lower than the sintering temperature in the first step, the desired composite oxide cannot be sufficiently produced, and the characteristics of the oxide semiconductor film are inferior. Therefore, the sintering temperature is higher than the sintering temperature in the first step, and is 1000 ° C. or higher, preferably 1010 ° C. or higher.
  • the sintering temperature is higher than the sintering temperature in the first step, and is 1050 ° C. or lower, preferably 1040 ° C. or lower. If the sintering time is too short, a sufficient amount of complex oxide cannot be secured. Therefore, the sintering time is 0.5 hours or longer, preferably 1 hour or longer, more preferably 2 hours or longer. On the other hand, if the sintering time is too long, the amount of zinc oxide and the like cannot be ensured due to excessive progress of the solid solution reaction. Therefore, the sintering time is 10 hours or less, preferably 8 hours or less, more preferably 6 hours or less.
  • the pressurizing condition at the time of hot pressing applies a pressure of about 100 to 500 kgf / cm 2 in both the first sintering process and the second sintering process. If the pressure is too low, densification may not proceed sufficiently. On the other hand, if the pressure is too high, the graphite mold may be damaged, the densification promoting effect is saturated, and the press equipment must be enlarged.
  • a preferable pressurizing condition is 200 kgf / cm 2 or more and 400 kgf / cm 2 or less.
  • the pressurizing condition may be the same or different pressure in the first sintering step and the second sintering step, but it is desirable to carry out at the same pressure from the viewpoint of productivity.
  • the rate of temperature increase is not particularly limited.
  • the rate of temperature increase up to the temperature range of the first sintering step is about 10 to 20 ° C./min.
  • the heating rate up to the temperature range may be about 2 to 10 ° C./min.
  • the sintering process is desirably performed in a reducing gas such as H 2 , methane, and CO, and in an inert gas atmosphere such as Ar and N 2 .
  • a reducing gas such as H 2 , methane, and CO
  • an inert gas atmosphere such as Ar and N 2 .
  • the sintering atmosphere is preferably an inert gas atmosphere in order to suppress oxidation and disappearance of graphite.
  • the atmosphere control method is not particularly limited.
  • the atmosphere may be adjusted by introducing Ar gas or N 2 gas into the furnace.
  • the pressure of the atmospheric gas is preferably atmospheric pressure in order to suppress evaporation of zinc oxide having a high vapor pressure.
  • the sputtering target of the present invention is obtained by performing (f) processing ⁇ (g) bonding by a conventional method.
  • the relative density and specific resistance of the sputtering target thus obtained are also very good as in the case of the oxide sintered body, and the preferable relative density is about 95% or more, and the preferable specific resistance is about 0. 0. 0. 1 ⁇ ⁇ cm or less.
  • Table 2 shows zinc oxide powder (purity 99.99%), indium oxide powder (purity 99.99%), and titanium oxide, magnesium oxide, aluminum oxide, and niobium oxide powders (purity 99.99%). It mix
  • the temperature was raised to 500 ° C. in an air atmosphere.
  • the mixture was warmed (temperature rising rate: 1 ° C./min), held at that temperature for 5 hours, and degreased.
  • the obtained molded body was set in a graphite mold and hot pressed under the conditions (A to E) shown in Table 3.
  • the press pressure was constant for both the first sintering process and the second sintering process.
  • N 2 gas was introduced into the hot press furnace and sintered in an N 2 atmosphere.
  • the obtained sintered body was machined and finished to ⁇ 100 ⁇ t5 mm, and bonded to a Cu backing plate to produce a sputtering target.
  • the sputtering target thus obtained was attached to a sputtering apparatus, and DC (direct current) magnetron sputtering was performed.
  • the sputtering conditions were a DC sputtering power of 150 W, an Ar / 0.1 volume% O 2 atmosphere, and a pressure of 0.8 mTorr. Further, a thin film transistor having a channel length of 10 ⁇ m and a channel width of 100 ⁇ m was formed using the thin film formed under these conditions.
  • the relative density was determined by removing the target from the backing plate, mirror polishing after sputtering, and observing with a reflection electron microscope (SEM) and measuring the porosity. Specifically, a SEM observation (1000 times) was taken to take a photograph, and the pore occupation area ratio in a 50 ⁇ m square region was measured to obtain the porosity. 20 different visual fields were observed, and the average value was taken as the average porosity of the sample. The value obtained by subtracting the porosity from 100% was taken as the relative density (%) of the sintered body. A relative density of 95% or more was evaluated as acceptable.
  • the specific resistance of the sintered body was measured by the four-terminal method for the produced sputtering target.
  • the specific resistance was evaluated to be 0.1 ⁇ ⁇ cm or less.
  • Crystal phase ratio The ratio of each crystal phase was determined by removing the target from the backing plate after sputtering, cutting out a 10 mm square test piece, and measuring the intensity of the diffraction line by X-ray diffraction.
  • Analysis device “X-ray diffractometer RINT-1500” manufactured by Rigaku Corporation Analysis conditions: Target: Cu Monochromatic: Uses a monochrome mate (K ⁇ ) Target output: 40kV-200mA (Continuous measurement) ⁇ / 2 ⁇ scanning Slit: Divergence 1/2 °, Scattering 1/2 °, Received light 0.15 mm Monochromator light receiving slit: 0.6mm Scanning speed: 2 ° / min Sampling width: 0.02 ° Measurement angle (2 ⁇ ): 5 to 90 °
  • the peak of each crystal phase shown in Table 1 was identified based on an ICDD (International Center for Diffraction Data) card, and the height of the diffraction peak was measured. Since Zn 6 In 2 O 9 is not described in the ICDD card, the peak obtained by calculating the theoretical diffraction intensity by crystal structure factor calculation based on the crystal structure shown in the above references (1) and (2) and measuring it. It was determined. These peaks were selected so that the diffraction intensity of the crystal phase was sufficiently high and the overlap with the peaks of other crystal phases was as small as possible.
  • ICDD International Center for Diffraction Data
  • the measured values of the peak height at the designated peak of each crystal phase are I (Zn m In 2 O 3 + m ), I (In 2 O 3 ), and I (ZnO), respectively (“I” is the measured value) [Zn m In 2 O 3 + m ] (“P1” in Table 4), [In 2 O 3 ] (“P2” in Table 4), [ZnO] (Table 4, the volume ratio of “P3”) was determined.
  • the ratio of crystal phases is [Zn m In 2 O 3 + m ] of 0.1 or more and less than 0.75, [In 2 O 3 ] is 0.05 to 0.7, and [ZnO] is 0.05 to 0. .7 was evaluated as acceptable.
  • Abnormal discharge / cracking Abnormal discharge was evaluated by measuring the number of abnormal discharges during sputtering. Specifically, the sputtering for 1 minute was repeated 300 times, the target taken out after the sputtering was visually observed, and the number of traces of abnormal discharge and the number of cracks was obtained. Abnormal discharge evaluated that the number of abnormal discharges was 6 or less. Moreover, the case where the crack did not generate
  • Carrier mobility The carrier mobility was measured by measuring the mobility of a thin film transistor having a channel length of 10 ⁇ m and a channel width of 100 ⁇ m formed using a thin film formed under the above sputtering conditions. Carrier mobility evaluated 15 cm ⁇ 2 > / Vs or more as the pass.
  • Nos. 1 to 5 and 9 to 11 abnormal discharge and cracking were suppressed, and high carrier mobility was exhibited. That is, when sputtering was performed, it was confirmed that abnormal discharge occurred 6 times or less, no cracks occurred, and discharge was stably performed. Moreover, the relative density and specific resistance of the sputtering target thus obtained were also good.
  • the carrier mobility of the thin film was also as high as 15 cm 2 / Vs or higher.
  • No. which does not satisfy the preferred composition of the present invention No. 6 to 8 and No. which does not satisfy the preferred production conditions.
  • Nos. 12 and 13 a desired effect could not be obtained because many abnormal discharges occurred, cracks occurred, and carrier mobility was low.
  • No. No. 12 is an example in which the holding temperature T2 in the second sintering step deviates from the definition of the present invention.
  • the relative density of the sintered body was low and the number of abnormal discharges was large.
  • No. 13 the temperature T1 in the first sintering step deviated from that of the present invention, the relative density was low, and the number of abnormal discharges was large.
  • the target was also cracked.

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Abstract

　Pour obtenir le corps compact fritté d'oxydes selon la présente invention, on mélange et on fritte de l'oxyde de zinc, de l'oxyde d'indium et un oxyde d'au moins un métal sélectionné dans un groupe formé par Ti, Mg, Al et Nb. Lorsque le corps compact fritté d'oxydes est soumis à une diffraction par rayons X, ZnmIn2O3+m (où m représente un entier compris entre 5 et 7) représente la phase principale et les phases cristallines In2O3, et ZnO sont incluses, la densité relative est égale à au moins 95% et la résistance spécifique n'excède pas 0,1Ω⋅cm. Selon la présente invention, il est possible d'obtenir un corps compact fritté d'oxydes au moyen duquel on peut réaliser la formation d'un film stable par pulvérisation avec une rupture de cible minimale et une décharge anormale minimale d'un film semiconducteur d'oxydes ayant une mobilité de porteur de charge élevée.
PCT/JP2012/078325 2011-11-04 2012-11-01 Corps compact fritté d'oxydes et cible de pulvérisation, procédé de production correspondant WO2013065784A1 (fr)

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TWI602939B (zh) * 2013-01-15 2017-10-21 出光興產股份有限公司 Sputtering targets, oxide semiconductor films, and methods of making them
WO2017090584A1 (fr) * 2015-11-25 2017-06-01 株式会社アルバック Transistor à couches minces, couche semi-conductrice d'oxyde et cible de pulvérisation
WO2022030455A1 (fr) * 2020-08-05 2022-02-10 三井金属鉱業株式会社 Matériau cible de pulvérisation cathodique et semi-conducteur oxyde

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