WO2022030455A1 - スパッタリングターゲット材及び酸化物半導体 - Google Patents
スパッタリングターゲット材及び酸化物半導体 Download PDFInfo
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- WO2022030455A1 WO2022030455A1 PCT/JP2021/028640 JP2021028640W WO2022030455A1 WO 2022030455 A1 WO2022030455 A1 WO 2022030455A1 JP 2021028640 W JP2021028640 W JP 2021028640W WO 2022030455 A1 WO2022030455 A1 WO 2022030455A1
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- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types 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
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types 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
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin 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
Definitions
- the present invention relates to a sputtering target material.
- the present invention also relates to an oxide semiconductor formed by using the sputtering target material.
- TFT thin film transistors
- FPD flat panel displays
- IGZO Oxide semiconductors represented by -Zn composite oxides
- Patent Documents 1 and 2 propose an oxide semiconductor for TFT using an In—Zn—X composite oxide composed of an indium (In) element and a zinc (Zn) element and an arbitrary element X.
- this oxide semiconductor is formed by sputtering using a target material composed of an In—Zn—X composite oxide.
- the target material is manufactured by a powder sintering method.
- the target material produced by the powder sintering method generally has a low relative density, which tends to generate particles and easily cracks in the target material during abnormal discharge. As a result, it may hinder the manufacture of high-performance TFTs.
- an oxide semiconductor exhibiting a field effect mobility higher than the field effect mobility exhibited by IGZO is desired.
- an oxide semiconductor having a threshold voltage close to 0 V is desired. Therefore, an object of the present invention is to provide a sputtering target material and an oxide semiconductor that can eliminate the drawbacks of the above-mentioned prior art.
- the present invention is composed of an oxide containing an indium (In) element, a zinc (Zn) element and an additive element (X).
- the additive element (X) consists of at least one element selected from tantalum (Ta), strontium (Sr) and niobium (Nb).
- the atomic ratio of each element satisfies the formulas (1) to (3) (X in the formula is the sum of the content ratios of the added elements).
- the present invention is an oxide semiconductor formed by using the above-mentioned sputtering target material. It is composed of an oxide containing an indium (In) element, a zinc (Zn) element and an additive element (X).
- the additive element (X) consists of at least one element selected from tantalum (Ta), strontium (Sr), and niobium (Nb).
- the atomic ratio of each element satisfies the formulas (1) to (3) (X in the formula is the sum of the content ratios of the added elements).
- the present invention is composed of an oxide containing an indium (In) element, a zinc (Zn) element and an additive element (X).
- the additive element (X) consists of at least one element selected from tantalum (Ta), strontium (Sr), and niobium (Nb).
- the atomic ratio of each element satisfies the formulas (1) to (3) (X in the formula is the sum of the content ratios of the added elements).
- the present invention provides a thin film transistor having an electrolytic effect mobility of 45 cm 2 ⁇ Vs or more.
- FIG. 1 is a schematic view showing the structure of a thin film transistor manufactured by using the sputtering target material of the present invention.
- FIG. 2 is a chart showing the results of X-ray diffraction measurement of the sputtering target material obtained in Example 1.
- FIG. 3 is a scanning electron microscope image of the sputtering target material obtained in Example 1.
- FIG. 4 is a scanning electron microscope image of the sputtering target material obtained in Example 1.
- FIG. 5 shows a qualitative analysis chart and quantitative analysis results in the EDX analysis of the In 2 O 3 phase of the sputtering target material obtained in Example 1.
- FIG. 6 is a scanning electron microscope image of the sputtering target material obtained in Example 1.
- FIG. 1 is a schematic view showing the structure of a thin film transistor manufactured by using the sputtering target material of the present invention.
- FIG. 2 is a chart showing the results of X-ray diffraction measurement of the sputtering target material obtained in Example 1.
- FIG. 7 shows a qualitative analysis chart and quantitative analysis results in the EDX analysis of the Zn 3 In 2 O 6 phase of the sputtering target material obtained in Example 1.
- FIG. 8A is an image showing the EDX analysis result of the sputtering target material obtained in Example 1
- FIG. 8B shows the EDX analysis result of the sputtering target material obtained in Comparative Example 1. It is a statue.
- the present invention relates to a sputtering target material (hereinafter, also referred to as “target material”).
- the target material of the present invention is composed of an oxide containing an indium (In) element, a zinc (Zn) element and an additive element (X).
- the additive element (X) consists of at least one element selected from tantalum (Ta), strontium (Sr) and niobium (Nb).
- the target material of the present invention contains In, Zn and an additive element (X) as the metal elements constituting the target material, but in addition to these elements, intentionally or inevitably, as long as the effect of the present invention is not impaired. It may contain trace elements.
- trace elements include elements contained in organic additives described later and media raw materials such as ball mills mixed during the production of target materials.
- Trace elements in the target material of the present invention include, for example, Fe, Cr, Ni, Al, Si, W, Zr, Na, Mg, K, Ca, Ti, Y, Ga, Sn, Ba, La, Ce, Pr, Examples thereof include Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Pb.
- Their contents are usually preferably 100 mass ppm (hereinafter, also referred to as "ppm") or less, respectively, with respect to the total mass of the oxides containing In, Zn and X contained in the target material of the present invention.
- the total amount of these trace elements is preferably 500 ppm or less, more preferably 300 ppm or less, still more preferably 100 ppm or less.
- the total mass also includes the mass of trace elements.
- the target material of the present invention is preferably composed of a sintered body containing the above-mentioned oxide.
- the shapes of the sintered body and the sputtering target material are not particularly limited, and conventionally known shapes such as a flat plate type and a cylindrical shape can be adopted.
- the formula (2). ) And (3) are the same.) 0.4 ⁇ (In + X) / (In + Zn + X) ⁇ 0.8 (1)
- Zn it is preferable to satisfy the atomic ratio represented by the following formula (2).
- the semiconductor device having an oxide thin film formed by sputtering using the target material of the present invention has high field effect mobility. It shows a low leakage current and a threshold voltage close to 0V. From the viewpoint of further enhancing these advantages, it is more preferable to satisfy the following formulas (1-2) to (1-5) for In and X.
- the additive element (X) at least one selected from Ta, Sr and Nb is used as described above. Each of these elements can be used alone, or two or more kinds can be used in combination. In particular, it is preferable to use Ta as the additive element (X) from the viewpoint of the overall performance of the oxide semiconductor device manufactured from the target material of the present invention and from the viewpoint of economic efficiency in manufacturing the target material.
- the target material of the present invention is formed from the target material of the present invention to satisfy the following formula (4) with respect to the atomic ratio of In and X. It is preferable from the viewpoint of further enhancing the field effect mobility of the oxide semiconductor device and exhibiting a threshold voltage close to 0V. 0.970 ⁇ In / (In + X) ⁇ 0.999 (4)
- the electric field effect mobility of the oxide semiconductor device formed from the target material is increased by using an extremely small amount of X with respect to the amount of In. .. This was first discovered by the present inventor.
- the amount of X used relative to the amount of In is larger than that of the present invention.
- the atomic ratio of In and X is expressed by the following equations (4-2) to (4-2). It is more preferable to satisfy 4-4). 0.980 ⁇ In / (In + X) ⁇ 0.997 (4-2) 0.990 ⁇ In / (In + X) ⁇ 0.995 (4-3) 0.990 ⁇ In / (In + X) ⁇ 0.993 (4-4)
- the TFT provided with the oxide semiconductor element formed from the target material preferably has a field effect mobility (cm 2 / Vs) of 45 cm 2 / Vs or more, preferably 50 cm 2 / Vs or more. More preferably, it is more preferably 60 cm 2 / Vs or more, further preferably 70 cm 2 / Vs or more, further preferably 80 cm 2 / Vs or more, and even more preferably 90 cm 2 / Vs or more. Is even more preferable, and 100 cm 2 / Vs or more is particularly preferable.
- the ratio of each metal contained in the target material of the present invention is measured by, for example, ICP emission spectroscopy.
- the target material of the present invention is characterized by a high relative density in addition to the atomic ratios of In, Zn and X. Specifically, the target material of the present invention exhibits a high relative density of preferably 95% or more. By exhibiting such a high relative density, when sputtering is performed using the target material of the present invention, it is possible to suppress the generation of particles, which is preferable. From this viewpoint, the target material of the present invention preferably has a relative density of 97% or more, more preferably 98% or more, further preferably 99% or more, and even more preferably 100% or more. It is particularly preferable, and it is particularly preferable that it is more than 100%. The target material of the present invention having such a relative density is suitably produced by the method described later. Relative density is measured according to the Archimedes method. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention is also characterized by a small size of pores inside the target material and a small number of pores.
- the target material of the present invention has 5 pores / 1000 ⁇ m 2 or less having an area circle equivalent diameter of 0.5 ⁇ m or more and 20 ⁇ m or less.
- the target material of the present invention has more preferably 3 holes / 1000 ⁇ m 2 or less and more preferably 2 holes / 1000 ⁇ m 2 or less having an area circle equivalent diameter of 0.5 ⁇ m or more and 20 ⁇ m or less.
- the number is 1 piece / 1000 ⁇ m 2 or less, more preferably 0.5 pieces / 1000 ⁇ m 2 or less, and particularly preferably 0.1 piece / 1000 ⁇ m 2 or less.
- the target material of the present invention having such a small number of pores is suitably produced by the method described later. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention is also characterized by its high strength.
- the target material of the present invention has a high bending strength of preferably 100 MPa or more.
- the target material of the present invention preferably has a bending strength of 120 MPa or more, and more preferably 150 MPa or more.
- the target material of the present invention having such bending strength is suitably produced by the method described later.
- the bending strength is measured according to JIS R1601. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention is also characterized by a low bulk resistivity.
- the low bulk resistivity is advantageous in that DC sputtering can be performed using the target material.
- the target material of the present invention preferably has a bulk resistance of 100 m ⁇ ⁇ cm or less, more preferably 50 m ⁇ ⁇ cm or less, and even more preferably 10 m ⁇ ⁇ cm or less at 25 ° C. It is more preferably 5 m ⁇ ⁇ cm or less, further preferably 4 m ⁇ ⁇ cm or less, particularly preferably 3 m ⁇ ⁇ cm or less, particularly preferably 2 m ⁇ ⁇ cm or less, and 1.5 m ⁇ ⁇ cm. The following is particularly preferable.
- the target material of the present invention having such a bulk resistivity is suitably produced by the method described later. Bulk resistivity is measured by the DC four-probe method. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention is also characterized by a small variation in the number of pores and a small variation in bulk resistivity within the same plane of the target material.
- the difference between the respective values of the number of pores and the bulk resistivity and the arithmetic mean value of the five points measured at any five points on the same surface is set at five points.
- the absolute value of the value divided by the arithmetic mean value and multiplied by 100 is 20% or less.
- the target material of the present invention has an absolute value of 15% or less, more preferably 10% or less, still more preferably 5% or less, and 3%. It is particularly preferably less than or equal to, and particularly preferably 1% or less.
- the target material of the present invention, in which the variation in the number of pores and the variation in the bulk resistivity is small, is suitably produced by the method described later.
- the target material of the present invention is also characterized by a small variation in the number of pores and a small variation in bulk resistivity in the depth direction of the target material.
- the difference between each value of the number of pores and bulk resistivity and the arithmetic mean value of 5 points on the surface ground every 1 mm in the depth direction from the surface is 5
- the absolute value of the value divided by the arithmetic mean value of the points and multiplied by 100 is 20% or less.
- the target material of the present invention has an absolute value of 15% or less, more preferably 10% or less, and even more preferably 5% or less. It is particularly preferably 3% or less, and particularly preferably 1% or less.
- the target material of the present invention, in which the variation in the number of pores and the variation in the bulk resistivity is small is suitably produced by the method described later.
- the target material of the present invention preferably has a standard deviation of Vickers hardness of 50 or less in the same plane of the target material. When this value satisfies the above condition, it is preferable as a target material because there is no bias in density, crystal grain size and composition.
- the standard deviation of the Vickers hardness in the same plane is preferably 40 or less, more preferably 30 or less, further preferably 20 or less, and even more preferably 10 or less.
- the target material of the present invention having such Vickers hardness is suitably produced by the method described later. Vickers hardness is measured according to JIS-R-1610: 2003. The specific measurement method will be described in detail in Examples described later.
- the arithmetic mean roughness Ra (JIS-B-0601: 2013) of the surface of the target material of the present invention can be appropriately adjusted by the number of grindstones at the time of grinding.
- the target material of the present invention preferably has an arithmetic mean roughness Ra of 3.2 ⁇ m or less, more preferably 1.6 ⁇ m or less, further preferably 1.2 ⁇ m or less, and 0. It is even more preferably 0.8 ⁇ m or less, particularly preferably 0.5 ⁇ m or less, and particularly preferably 0.1 ⁇ m or less.
- the arithmetic mean roughness Ra is measured by a surface roughness measuring instrument. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention preferably has a maximum surface color difference ⁇ E * of 5 or less. Further, it is preferable that ⁇ E * is 5 or less as the maximum color difference in the depth direction of the target material.
- Color difference ⁇ E * is an index that quantifies the difference between two colors. When this value satisfies the above condition, it is preferable as a target material because there is no bias in density, crystal grain size and composition.
- the maximum color difference ⁇ E * between the entire surface and the depth direction is preferably 4 or less, more preferably 3 or less, further preferably 2 or less, and even more preferably 1 or less.
- the target material of the present invention having such a maximum color difference ⁇ E * is suitably produced by the method described later. The specific measurement method will be described in detail in Examples described later.
- the target material of the present invention is composed of an oxide containing In, Zn and X as described above.
- This oxide can be an oxide of In, an oxide of Zn, or an oxide of X.
- this oxide can be a composite oxide of any two or more elements selected from the group consisting of In, Zn and X.
- Specific examples of the composite oxide include In—Zn composite oxide, Zn—Ta composite oxide, In—Ta composite oxide, In—Nb composite oxide, Zn—Nb composite oxide, and In—Nb composite.
- the target material of the present invention contains, in particular, the In 2 O 3 phase, which is an oxide of In, and the Zn 3 In 2 O 6 phase, which is a composite oxide of In and Zn, so that the density and strength of the target material can be determined. It is preferable from the viewpoint of increasing and reducing the resistance.
- the inclusion of the In 2 O 3 phase and the Zn 3 In 2 O 6 phase in the target material of the present invention means that In 2 O is measured by X-ray diffraction (hereinafter, also referred to as “XRD”) measurement for the target material of the present invention. It can be judged by whether or not 3 phase and Zn 3 In 2 O 6 phase are observed.
- the In 2 O 3 phase in the present invention may contain a trace amount of Zn element.
- X is contained in both the In 2 O 3 phase and the Zn 3 In 2 O 6 phase.
- the oxide semiconductor formed from the target material of the present invention uniformly contains X, and a homogeneous oxide semiconductor film can be obtained. Can be done.
- the inclusion of X in both the In 2 O 3 phase and the Zn 3 In 2 O 6 phase can be measured by, for example, energy dispersive X-ray spectroscopy (hereinafter, also referred to as “EDX”). The specific measurement method will be described in detail in Examples described later.
- the In 2 O 3 phase can satisfy a specific range in the size of its crystal grains, which determines the density and strength of the target material of the present invention. It is preferable from the viewpoint of increasing and reducing the resistance.
- the size of the crystal grains of the In 2 O 3 phase is preferably 3.0 ⁇ m or less, more preferably 2.7 ⁇ m or less, and even more preferably 2.5 ⁇ m or less. The smaller the crystal grain size is, the more preferable it is, and the lower limit is not particularly determined, but it is usually 0.1 ⁇ m or more.
- the target of the present invention is that the size of the crystal grains of the Zn 3 In 2 O 6 phase also satisfies a specific range. It is preferable from the viewpoint of increasing the density and strength of the material and reducing the resistance.
- the size of the crystal grains of the Zn 3 In 2 O 6 phase is preferably 3.9 ⁇ m or less, more preferably 3.5 ⁇ m or less, still more preferably 3.0 ⁇ m or less. It is more preferably 2.5 ⁇ m or less, further preferably 2.3 ⁇ m or less, particularly preferably 2.0 ⁇ m or less, and particularly preferably 1.9 ⁇ m or less.
- the target material may be manufactured by the method described later.
- the size of the crystal grains of the In 2 O 3 phase and the size of the crystal grains of the Zn 3 In 2 O 6 phase are measured by observing the target material of the present invention with a scanning electron microscope (hereinafter, also referred to as “SEM”). Will be done. The specific measurement method will be described in detail in Examples described later.
- the ratio of the area of the In 2 O 3 phase to the unit area (hereinafter, also referred to as “In 2 O 3 phase area ratio”) is specific.
- the range is also preferable from the viewpoint of reducing the resistance of the target material.
- the In 2 O 3 -phase area ratio is preferably 10% or more and 70% or less, more preferably 20% or more and 70% or less, and further preferably 30% or more and 70% or less. It is even more preferable that it is 35% or more and 70% or less.
- the ratio of the area of the Zn 3 In 2 O 6 phase to the unit area is preferably 30% or more and 90% or less, preferably 30% or more. It is more preferably 80% or less, further preferably 30% or more and 70% or less, and even more preferably 30% or more and 65% or less.
- the target material may be manufactured by the method described later.
- the In 2 O 3 phase area ratio and the Zn 3 In 2 O 6 phase area ratio are measured by observing the target material of the present invention by SEM. The specific measurement method will be described in detail in Examples described later.
- the In 2 O 3 phase and the Zn 3 In 2 O 6 phase are uniformly dispersed. It is preferable that these are uniformly dispersed because the composition is not biased and the film characteristics do not change when the thin film is formed by sputtering.
- the dispersion state of the crystal phase is evaluated by EDX.
- the In / Zn atom ratio of the entire field of view is obtained by EDX from a range of 200 times, 437.5 ⁇ m ⁇ 625 ⁇ m, which is randomly selected in the target material. Subsequently, the same field of view is evenly divided into 4 vertical ⁇ 4 horizontal, and the In / Zn atom ratio in each divided visual field is obtained.
- the absolute value of the difference between the In / Zn atom ratio in each divided field of view and the In / Zn atom ratio in the entire field of view is divided by the In / Zn atom ratio in the entire field of view, and the value multiplied by 100 is taken as the dispersion rate (%). It is defined and the degree of homogeneity of dispersion of In 2 O 3 phase and Zn 3 In 2 O 6 phase is evaluated based on the magnitude of the dispersion rate. The closer the dispersion ratio is to zero, the more uniformly the In 2 O 3 phase and the Zn 3 In 2 O 6 phase are dispersed.
- the maximum value of the dispersion ratio at 16 points is preferably 10% or less, more preferably 5% or less, further preferably 4% or less, still more preferably 3% or less. It is particularly preferably 2% or less, and particularly preferably 1% or less.
- an oxide powder as a raw material for a target material is molded into a predetermined shape to obtain a molded body, and the molded body is fired to obtain a target material made of a sintered body.
- a method known so far in the art can be adopted.
- the cast molding method is also called the slip cast method.
- a slurry containing a raw material powder and an organic additive is prepared using a dispersion medium.
- oxide powder it is preferable to use oxide powder, hydroxide powder, or carbonate powder as the raw material powder.
- oxide powder In oxide powder, Zn oxide powder, and X oxide powder are used.
- In oxide for example, In 2 O 3 can be used.
- ZnO can be used as the Zn oxide.
- the powder of the X oxide for example, Ta 2 O 5 , SrO and Nb 2 O 5 can be used.
- SrO may be combined with carbon dioxide in the air and exist in the state of SrCO 3 , but carbon dioxide is dissociated from SrCO 3 to become SrO in the firing process. In this production method, firing is performed after all these raw material powders are mixed.
- the amount of In oxide powder, Zn oxide powder and X oxide powder used is preferably adjusted so that the atomic ratio of In, Zn and X in the target material satisfies the above range. ..
- the particle size of the raw material powder is preferably 0.1 ⁇ m or more and 1.5 ⁇ m or less in terms of the volume cumulative particle size D50 at the cumulative volume of 50% by volume by the laser diffraction / scattering type particle size distribution measurement method.
- the above-mentioned organic additive is a substance used for appropriately adjusting the properties of a slurry or a molded product.
- the organic additive include a binder, a dispersant, a plasticizer and the like.
- the binder is added to increase the strength of the molded product.
- a binder usually used when obtaining a molded product by a known powder sintering method can be used.
- the binder include polyvinyl alcohol.
- the dispersant is added to enhance the dispersibility of the raw material powder in the slurry.
- the dispersant include a polycarboxylic acid-based dispersant and a polyacrylic acid-based dispersant.
- the plasticizer is added to increase the plasticity of the molded product.
- the plasticizer include polyethylene glycol (PEG) and ethylene glycol (EG).
- the dispersion medium used to prepare the slurry containing the raw material powder and the organic additive is not particularly limited, and may be appropriately selected from water and a water-soluble organic solvent such as alcohol depending on the purpose. can.
- the method for producing a slurry containing the raw material powder and the organic additive is not particularly limited, and for example, a method in which the raw material powder, the organic additive, the dispersion medium and the zirconia balls are placed in a pot and mixed by a ball mill can be used.
- the slurry is poured into a mold, and then the dispersion medium is removed to prepare a molded product.
- the mold that can be used include a metal mold, a gypsum mold, and a resin mold that is pressurized to remove a dispersion medium.
- a slurry similar to the slurry used in the casting molding method is spray-dried to obtain a dry powder.
- the obtained dry powder is filled in a mold and CIP molding is performed.
- Firing of the molded product can generally be performed in an oxygen-containing atmosphere. In particular, it is convenient to bake in an atmospheric atmosphere.
- the firing temperature is preferably 1200 ° C. or higher and 1600 ° C. or lower, more preferably 1300 ° C. or higher and 1500 ° C. or lower, and even more preferably 1350 ° C. or higher and 1450 ° C. or lower.
- the firing time is preferably 1 hour or more and 100 hours or less, more preferably 2 hours or more and 50 hours or less, and further preferably 3 hours or more and 30 hours or less.
- the heating rate is preferably 5 ° C./hour or more and 500 ° C./hour or less, more preferably 10 ° C./hour or more and 200 ° C./hour or less, and 20 ° C./hour or more and 100 ° C./hour or less. Is more preferable.
- a composite oxide of In and Zn for example, a phase of Zn 5 In 2 O 8 is formed for a certain period of time in the firing process promotes sintering and a dense target material. It is preferable from the viewpoint of generation. Specifically, when the raw material powder contains In 2 O 3 powder and Zn O powder, these react with each other as the temperature rises to form a phase of Zn 5 In 2 O 8 and then Zn 4 In 2 O 7 . It changes to a phase and then to a Zn 3 In 2 O 6 phase.
- volume diffusion proceeds and densification is promoted when the phase of Zn 5 In 2 O 8 is formed it is preferable to surely generate the phase of Zn 5 In 2 O 8 .
- it is preferable to maintain the temperature in the range of 1000 ° C. or higher and 1250 ° C. or lower for a certain period of time in the process of raising the temperature of firing and it is more preferable to maintain the temperature in the range of 1050 ° C. or higher and 1200 ° C. or lower for a certain period of time.
- the temperature to be maintained is not necessarily limited to the temperature of a specific point, and may be a temperature range having a certain range. Specifically, when a specific temperature selected from the range of 1000 ° C.
- T ° C.
- T ⁇ 10 ° C. as long as it is included in the range of 1000 ° C. or higher and 1250 ° C. or lower. It is also good, preferably T ⁇ 5 ° C, more preferably T ⁇ 3 ° C, still more preferably T ⁇ 1 ° C.
- the time for maintaining this temperature range is preferably 1 hour or more and 40 hours or less, and more preferably 2 hours or more and 20 hours or less.
- FIG. 1 schematically shows an example of the TFT element 1.
- the TFT element 1 shown in the figure is formed on one surface of a glass substrate 10.
- a gate electrode 20 is arranged on one surface of the glass substrate 10, and a gate insulating film 30 is formed so as to cover the gate electrode 20.
- a source electrode 60, a drain electrode 61, and a channel layer 40 are arranged on the gate insulating film 30.
- the channel layer 40 can be formed by using the target material of the present invention.
- the channel layer 40 is composed of an oxide containing an indium (In) element, a zinc (Zn) element and an additive element (X), and is composed of an indium (In) element, a zinc (Zn) element and an additive element.
- the atomic ratio of (X) satisfies the above-mentioned formula (1). Further, the above-mentioned equations (2) and (3) are satisfied. It is preferable that the oxide semiconductor device formed from the target material of the present invention has an amorphous structure from the viewpoint of improving the performance of the device.
- Example 1 In 2 O 3 powder having an average particle size D 50 of 0.6 ⁇ m, Zn O powder having an average particle size D 50 of 0.8 ⁇ m, and Ta 2 O 5 powder having an average particle size D 50 of 0.6 ⁇ m. was mixed dry with a ball mill using zirconia balls to prepare a mixed raw material powder.
- the average particle size D50 of each powder was measured using a particle size distribution measuring device MT3300EXII manufactured by Microtrac Bell Co., Ltd. At the time of measurement, water was used as a solvent, and the measurement was carried out at the refractive index of 2.20 of the measurement substance.
- the mixing ratio of each powder the atomic ratio of In, Zn and Ta was set to the value shown in Table 1 below.
- the prepared slurry was poured into a metal mold sandwiching a filter, and then the water in the slurry was discharged to obtain a molded product.
- This molded product was fired to produce a sintered body.
- the firing was carried out in an atmosphere having an oxygen concentration of 20% by volume at a firing temperature of 1400 ° C., a firing time of 8 hours, a temperature rising rate of 50 ° C./hour, and a temperature lowering rate of 50 ° C./hour. During the firing, the temperature was maintained at 1100 ° C. for 6 hours to promote the formation of Zn 5 In 2 O 8 .
- the sintered body thus obtained was machined to obtain an oxide sintered body (target material) having a width of 210 mm, a length of 710 mm, and a thickness of 6 mm.
- a # 170 grindstone was used for cutting.
- the number of pores and the variation in bulk resistivity in the same plane and in the depth direction were calculated by the above-mentioned method.
- the variations in the number of pores in the same plane calculated at any five points of the target material were 5.7%, 0.4%, 1.4%, 6.8%, and 2.2%, respectively. ..
- the variations in bulk resistivity within the same plane were 3.5%, 5.3%, 3.5%, 5.3%, and 3.5%, respectively.
- the variations in the number of pores in the depth direction calculated at any five points of the target material were 4.6%, 0.2%, 1.6%, 1.6%, and 1.6%, respectively. ..
- the variations in bulk resistivity in the depth direction were 3.5%, 3.5%, 5.3%, 5.3%, and 3.5%, respectively.
- the number of pores per 1000 ⁇ m 2 was 1.2.
- the arithmetic mean roughness Ra was 1.0 ⁇ m.
- the maximum color difference ⁇ E * on the surface was 1.1, and the maximum color difference ⁇ E * in the depth direction was 1.0.
- Example 2 In Example 1, each raw material powder was mixed so that the atomic ratios of In, Zn, and Ta were the values shown in Table 1 below. A target material was obtained in the same manner as in Example 1 except for this.
- ZnO powder having an average particle size D 50 of 0.8 ⁇ m was mixed with this mixed powder so that the atomic ratio [In / (In + Zn)] was 0.698.
- the mixed powder was supplied to a wet ball mill and mixed and pulverized for 24 hours to obtain a slurry of raw material powder.
- the slurry was filtered, dried and granulated.
- the obtained granulated product was press-molded, and further, a pressure of 2000 kgf / cm 2 was applied and molded by a cold hydrostatic pressure press.
- the molded body was charged into a firing furnace and fired at 1400 ° C. for 12 hours under atmospheric pressure and oxygen gas inflow conditions to obtain a sintered body.
- the heating rate was 0.5 ° C./min from room temperature to 400 ° C. and 1 ° C./min from 400 to 1400 ° C.
- the temperature lowering rate was 1 ° C./min.
- a target material was obtained in the same manner as in Example 1 except for these.
- Example 2 In Example 1, Ta 2 O 5 powder was not used. The raw material powders were mixed so that the atomic ratios of In and Zn were the values shown in Table 2 below. A target material was obtained in the same manner as in Example 1 except for this.
- Example 9 In Example 1, each raw material powder was mixed so that the atomic ratios of In, Zn and Ta were the values shown in Table 2 below. A target material was obtained in the same manner as in Example 1 except for this.
- Example 14 In Example 1, instead of Ta 2 O 5 powder, Nb 2 O 5 powder having an average particle size D 50 of 0.7 ⁇ m was used. The raw material powders were mixed so that the atomic ratios of In, Zn and Nb were the values shown in Table 2 below. A target material was obtained in the same manner as in Example 1 except for this.
- Example 15 In Example 1, instead of Ta 2 O 5 powder, SrCO 3 powder having an average particle size D 50 of 1.5 ⁇ m was used. The raw material powders were mixed so that the atomic ratios of In, Zn and Sr were as shown in Table 2 below. A target material was obtained in the same manner as in Example 1 except for this.
- the content (% by mass) of the constituent substances of the target material is considered to be In 2 O 3 , ZnO, Ta 2 O 5 , Nb 2 O 5 , SrO, for example, C1: In 2 O 3 of the target material.
- the mass% of In 2 O 3 , the mass% of Zn O, the mass% of Ta 2 O 5 , the mass% of Nb 2 O 5 and the mass% of SrO are obtained from the analysis results of each element of the target material by ICP emission spectroscopy. be able to.
- the in-plane color difference ⁇ E * was measured by measuring the surface of the machined target material at intervals of 50 mm in the x-axis and y-axis directions using a color difference meter (color difference meter CR-300 manufactured by Konica Minolta). The L * value, a * value and b * value of each point were evaluated in the CIE1976L * a * b * color space. Then, from the differences ⁇ L *, ⁇ a *, and ⁇ b * of the L * value, a * value, and b * value of two points among the measured points, the color difference ⁇ E * is calculated from the following equation (ii) for all the two points.
- the maximum value of the plurality of color difference ⁇ E * obtained by the combination was taken as the maximum color difference ⁇ E * in the surface.
- ⁇ E * (( ⁇ L *) 2 + ( ⁇ a *) 2 + ( ⁇ b *) 2 ) 1/2 ... (ii)
- the maximum color difference ⁇ E * in the depth direction is measured by cutting 1 mm at an arbitrary point of the machined target material and measuring at each depth up to the center of the target material using a color difference meter.
- the L * value, a * value, and b * value of each point were evaluated in the CIE1976L * a * b * color space.
- the color difference ⁇ E * was obtained from the differences ⁇ L *, ⁇ a *, and ⁇ b * of the L * value, a * value, and b * value of two points among the measured points by the combination of all the two points.
- the maximum value of a plurality of color differences ⁇ E * was defined as the maximum color difference ⁇ E * in the depth direction.
- BSE-COMP images in the range of 87.5 ⁇ m ⁇ 125 ⁇ m at a magnification of 1000 times were randomly photographed in 10 fields to obtain SEM images.
- the obtained SEM image was analyzed by image processing software: ImageJ 1.51k (http://imageJ.nih.gov/ij/, provider: National Institutes of Health (NIH)).
- image processing software ImageJ 1.51k (http://imageJ.nih.gov/ij/, provider: National Institutes of Health (NIH)).
- the specific procedure is as follows.
- the sample used for SEM image imaging was subjected to thermal etching at 1100 ° C. for 1 hour, and SEM observation was performed to obtain an image in which the grain boundaries shown in FIG. 3 appeared.
- the obtained image was first drawn along the grain boundaries of the In 2 O 3 phase (region A that looks white in FIG. 3).
- the arithmetic mean value of the area equivalent circle diameter of all the particles calculated in 10 fields of view was taken as the size of the crystal grains of the Zn 3 In 2 O 6 phase.
- the ratio of the area of the In 2 O 3 phase to the total area was calculated by performing particle analysis on the BSE-COMP image without grain boundaries before thermal etching.
- the arithmetic mean value of all the particles calculated in 10 fields of view was taken as the In 2 O 3 phase area ratio.
- the Zn 3 In 2 O 6 phase area ratio was calculated by subtracting the In 2 O 3 phase area ratio from 100. 4 and 6 are enlarged images of FIG.
- the TFT element 1 shown in FIG. 1 was manufactured by a photolithography method.
- a Mschreib thin film was formed as a gate electrode 20 on a glass substrate (OA-10 manufactured by Nippon Electric Glass Co., Ltd.) using a DC sputtering apparatus.
- a SiOx thin film was formed as the gate insulating film 30 under the following conditions.
- Film forming equipment Plasma CVD equipment PD-2202L manufactured by SAMCO Co., Ltd.
- Film formation gas SiH 4 / N 2 O / N 2 mixed gas
- Film formation pressure 110 Pa
- Substrate temperature 250-400 ° C
- the channel layer 40 was sputtered under the following conditions using the target materials obtained in Examples and Comparative Examples to form a thin film having a thickness of about 10 to 50 nm.
- Film forming equipment DC sputtering equipment SML-464 manufactured by Tokki Co., Ltd.
- the measured transfer characteristics are field effect mobility ⁇ (cm 2 / Vs), SS (Subthreshold Swing) value (V / dec), and threshold voltage Vth (V).
- the transfer characteristics were measured by a Semiconductor Navigator Device Analogizer B1500A manufactured by Agilent Technologies, Inc. The measurement results are shown in Tables 1 and 2. Although not shown in the table, the present inventor has confirmed by XRD measurement that the channel layer 40 of the TFT element 1 obtained in each embodiment has an amorphous structure.
- the field effect mobility is the channel mobility obtained from the change in the drain current with respect to the gate voltage when the drain voltage is constant in the saturation region of MOSFET (Metal-Oxide-Semiconductor Field-Effective Transistor) operation.
- MOSFET Metal-Oxide-Semiconductor Field-Effective Transistor
- the SS value is a gate voltage required to increase the drain current by an order of magnitude in the vicinity of the threshold voltage, and the smaller the value, the better the transfer characteristic.
- the threshold voltage is a voltage when a positive voltage is applied to the drain electrode and a drain current flows when either a positive or negative voltage is applied to the gate electrode and becomes 1 nA, and the value is preferably close to 0 V. .. More specifically, it is more preferably -2V or higher, further preferably -1V or higher, and even more preferably 0V or higher. Further, it is more preferably 3 V or less, further preferably 2 V or less, and even more preferably 1 V or less. Specifically, it is more preferably -2V or more and 3V or less, further preferably -1V or more and 2V or less, and further preferably 0V or more and 1V or less.
- the TFT element manufactured by using the target material obtained in each example has excellent transmission characteristics.
- the number of pores per 1000 ⁇ m 2 , the number of pores, the variation in bulk resistivity, the arithmetic mean roughness Ra, the maximum color difference, and the In / Zn atomic ratio are not shown in Tables 1 and 2, but Examples 2 to 2 to The same results as in Example 1 were obtained for the target material obtained in No. 16.
- the target material obtained in Example 1 contained In 2 O 3 phase and Zn 3 In 2 O 6 phase.
- similar results were obtained for the target materials obtained in Examples 2 to 16.
- the In 2 O 3 phase and the Zn 3 In 2 O 6 phase contained in the target material obtained in Example 1 both contain Ta. rice field. Although not shown, similar results were obtained for the target materials obtained in Examples 2 to 16.
- the sputtering target material of the present invention by using the sputtering target material of the present invention, particles can be suppressed and cracks due to abnormal discharge can be suppressed. As a result, a TFT having high field effect mobility can be easily manufactured.
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Abstract
Description
また、TFTの技術分野においては、IGZOが示す電界効果移動度よりも更に高い電界効果移動度を示す酸化物半導体が望まれている。
更に、TFTの技術分野においては、しきい電圧が0Vに近い値を示す酸化物半導体が望まれている。
したがって本発明の課題は、前述した従来技術が有する欠点を解消し得るスパッタリングターゲット材及び酸化物半導体を提供することにある。
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)及びニオブ(Nb)から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たし(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
相対密度が95%以上である、スパッタリングターゲット材を提供することによって前記の課題を解決したものである。
インジウム(In)元素、亜鉛(Zn)元素及び添加元素(X)を含む酸化物から構成され、
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)、ニオブ(Nb)の中から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たす(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
酸化物半導体を提供するものである。
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)、ニオブ(Nb)の中から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たす(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
酸化物半導体を有し、
電解効果移動度が45cm2・Vs以上である、薄膜トランジスタを提供するものである。
具体的には、In及びXに関しては以下の式(1)で表される原子比を満たすことが好ましい(式中のXは、前記添加元素の含有比の総和とする。以下、式(2)及び(3)についても同じである。)。
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
Znに関しては以下の式(2)で表される原子比を満たすことが好ましい。
0.2≦Zn/(In+Zn+X)≦0.6 (2)
Xに関しては以下の式(3)で表される原子比を満たすことが好ましい。
0.001≦X/(In+Zn+X)≦0.015 (3)
0.43≦(In+X)/(In+Zn+X)≦0.79 (1-2)
0.48≦(In+X)/(In+Zn+X)≦0.78 (1-3)
0.53≦(In+X)/(In+Zn+X)≦0.75 (1-4)
0.58≦(In+X)/(In+Zn+X)≦0.70 (1-5)
0.22≦Zn/(In+Zn+X)≦0.52 (2-3)
0.25≦Zn/(In+Zn+X)≦0.47 (2-4)
0.30≦Zn/(In+Zn+X)≦0.42 (2-5)
0.0015≦X/(In+Zn+X)≦0.013 (3-2)
0.002<X/(In+Zn+X)≦0.012 (3-3)
0.0025≦X/(In+Zn+X)≦0.010 (3-4)
0.003≦X/(In+Zn+X)≦0.009 (3-5)
0.970≦In/(In+X)≦0.999 (4)
0.980≦In/(In+X)≦0.997 (4-2)
0.990≦In/(In+X)≦0.995 (4-3)
0.990<In/(In+X)≦0.993 (4-4)
In2O3相の結晶粒のサイズ及びZn3In2O6相の結晶粒のサイズは、本発明のターゲット材を走査型電子顕微鏡(以下「SEM」ともいう。)によって観察することで測定される。具体的な測定方法は後述する実施例において詳述する。
結晶相の分散状態評価は、EDXによって行う。ターゲット材において無作為に選んだ倍率200倍、437.5μm×625μmの範囲から、EDXによって視野全体のIn/Zn原子比率を得る。続いて同視野を縦4×横4の均等に分割し、各分割視野でのIn/Zn原子比率を得る。各分割視野でのIn/Zn原子比率と視野全体のIn/Zn原子比率の差の絶対値を、視野全体のIn/Zn原子比率で除し、100を乗じた値を分散率(%)と定義し、分散率の大小に基づきIn2O3相及びZn3In2O6相の分散の均質の程度を評価する。分散率がゼロに近いほどIn2O3相及びZn3In2O6相が均質に分散していることを意味する。16箇所での分散率の最大値が10%以下であることが好ましく、5%以下であることが更に好ましく、4%以下であることが一層好ましく、3%以下であることが更に一層好ましく、2%以下であることが特に好ましく、1%以下であることがとりわけ好ましい。
本製造方法においては、これら原料粉末をすべて混合した後に焼成を行う。このこととは対照的に、従来技術、例えば特許文献2に記載の技術では、In2O3粉とTa2O5粉とを混合した後に焼成を行い、次いで得られた焼成粉とZnO粉とを混合して再び焼成を行っている。この方法では事前に焼成を実施することによって粉末を構成する粒子が粗粒となってしまい、相対密度の高いターゲット材を得ることが容易でない。これに対して本製造方法では、好ましくは、In酸化物の粉末、Zn酸化物の粉末及びX酸化物の粉末をすべて常温で混合、成形した後、焼成を行っているので、相対密度の高い緻密なターゲット材が容易に得られる。
本発明のターゲット材から形成された酸化物半導体素子はアモルファス構造を有することが、該素子の性能向上の点から好ましい。
平均粒径D50が0.6μmであるIn2O3粉末と、平均粒径D50が0.8μmであるZnO粉末と、平均粒径D50が0.6μmであるTa2O5粉末とを、ジルコニアボールによってボールミル乾式混合して、混合原料粉末を調製した。各粉末の平均粒径D50は、マイクロトラックベル株式会社製の粒度分布測定装置MT3300EXIIを用いて測定した。測定の際、溶媒には水を使用し、測定物質の屈折率2.20で測定した。各粉末の混合比率は、InとZnとTaとの原子比が、以下の表1に示す値となるようにした。
ターゲット材の任意の5点において算出した同一面内における空孔の数のバラつきは、それぞれ5.7%、0.4%、1.4%、6.8%、2.2%であった。同一面内におけるバルク抵抗率のバラつきは、それぞれ3.5%、5.3%、3.5%、5.3%、3.5%であった。
ターゲット材の任意の5点において算出した深さ方向における空孔の数のバラつきは、それぞれ4.6%、0.2%、1.6%、1.6%、1.6%であった。深さ方向におけるバルク抵抗率のバラつきは、それぞれ3.5%、3.5%、5.3%、5.3%、3.5%であった。
実施例1において、InとZnとTaとの原子比が、以下の表1に示す値となるように各原料粉末を混合した。これ以外は実施例1と同様にしてターゲット材を得た。
平均粒径D50が0.6μmであるIn2O3粉末と、平均粒径D50が0.6μmであるTa2O5粉末とを、In元素とTa元素の合計に対するIn元素の原子比〔In/(In+Ta)〕が0.993となるように混合した。混合物を湿式ボールミルに供給し、12時間混合粉砕した。
得られた混合スラリーを取り出し、濾過、乾燥した。この乾燥粉を焼成炉に装入し、大気雰囲気中、1000℃で5時間熱処理した。
以上により、In元素とTa元素を含有する混合粉を得た。
この混合粉に、平均粒径D50が0.8μmであるZnO粉末を、原子比〔In/(In+Zn)〕が0.698となるように混合した。混合粉を湿式ボールミルに供給し、24時間混合粉砕して、原料粉末のスラリーを得た。このスラリーを、濾過、乾燥及び造粒した。
得られた造粒物をプレス成形し、更に、2000kgf/cm2の圧力を加えて冷間静水圧プレスで成形した。
成形体を焼成炉に装入し、大気圧、酸素ガス流入条件で、1400℃、12時間の条件で焼成し焼結体を得た。室温から400℃までは昇温速度は0.5℃/分とし、400~1400℃までは1℃/分とした。降温速度は1℃/分とした。
これら以外は実施例1と同様にしてターゲット材を得た。
実施例1において、Ta2O5粉末を用いなかった。InとZnの原子比が、以下の表2に示す値となるように各原料粉末を混合した。これ以外は実施例1と同様にしてターゲット材を得た。
実施例1において、InとZnとTaとの原子比が、以下の表2に示す値となるように各原料粉末を混合した。これ以外は実施例1と同様にしてターゲット材を得た。
実施例1において、Ta2O5粉末に代えて、平均粒径D50が0.7μmであるNb2O5粉末を用いた。InとZnとNbとの原子比が、以下の表2に示す値となるように各原料粉末を混合した。これ以外は実施例1と同様にしてターゲット材を得た。
実施例1において、Ta2O5粉末に代えて、平均粒径D50が1.5μmであるSrCO3粉末を用いた。InとZnとSrとの原子比が、以下の表2に示す値となるように各原料粉末を混合した。これ以外は実施例1と同様にしてターゲット材を得た。
実施例1において、Ta2O5粉末に代えて、Ta2O5粉末と、Nb2O5粉末と、SrCO3粉末とを、InとZnとTaとNbとSrとの原子比が、以下の表2に示す値となるように混合した。Ta、Nb及びSrのモル比は、Ta:Nb:Sr=3:1:1とした。これ以外は実施例1と同様にしてターゲット材を得た。
実施例及び比較例で得られたターゲット材について、相対密度、抗折強度、バルク抵抗率及びビッカース硬度を以下の方法で測定した。実施例及び比較例で得られたターゲット材について以下の条件でXRD測定を行い、In2O3相及びZn3In2O6相の有無を確認した。また、実施例及び比較例で得られたターゲット材についてSEM観察を行い、In2O3相の結晶粒のサイズ、Zn3In2O6相の結晶粒のサイズ、In2O3相面積率及びZn3In2O6相面積率を以下の方法で測定した。更に、SEM観察にて確認されたIn2O3相及びZn3In2O6相に添加元素(X)の含有の有無をEDXにて測定した。それらの結果を以下の表1及び2並びに図2ないし7に示す。
ターゲット材の空中質量を体積(ターゲット材の水中質量/計測温度における水比重)で除し、下記式(i)に基づく理論密度ρ(g/cm3)に対する百分率の値を相対密度(単位:%)とした。
ρ=Σ((Ci/100)/ρi)-1 ・・・(i)
(式中Ciはターゲット材の構成物質の含有量(質量%)を示し、ρiはCiに対応する各構成物質の密度(g/cm3)を示す。)
本発明の場合、ターゲット材の構成物質の含有量(質量%)は、In2O3、ZnO、Ta2O5、Nb2O5、SrOと考え、例えば
C1:ターゲット材のIn2O3の質量%
ρ1:In2O3の密度(7.18g/cm3)
C2:ターゲット材のZnOの質量%
ρ2:ZnOの密度(5.60g/cm3)
C3:ターゲット材のTa2O5の質量%
ρ3:Ta2O5の密度(8.73g/cm3)
C4:ターゲット材のNb2O5の質量%
ρ4:Nb2O5の密度(4.60g/cm3)
C5:ターゲット材のSrOの質量%
ρ5:SrOの密度(4.70g/cm3)
を式(i)に適用することで理論密度ρを算出できる。
In2O3の質量%、ZnOの質量%、Ta2O5の質量%、Nb2O5の質量%及びSrOの質量%は、ICP発光分光測定によるターゲット材の各元素の分析結果から求めることができる。
ターゲット材を切断して得られた切断面を、エメリー紙#180、#400、#800、#1000、#2000を用いて段階的に研磨し、最後にバフ研磨して鏡面に仕上げた。鏡面仕上げ面をSEM観察した。倍率400倍、218.7μm×312.5μmの範囲のSEM像を無作為に5視野撮影しSEM像を得た。
得られたSEM像を、画像処理ソフトウェア:ImageJ 1.51k(http://imageJ.nih.gov/ij/、提供元:アメリカ国立衛生研究所(NIH:National Institutes of Health))によって解析した。具体的な手順は以下のとおりである。
得られた画像に対し、先ず空孔に沿って描画を行った。すべての描画が完了した後、粒子解析を実施(Analyze→Analyze Particles)して、空孔の数と、各空孔における面積を得た。その後、得られた各空孔における面積から、面積円相当径を算出した。5視野において確認された、面積円相当径が0.5μm~20μmの空孔の総和を5視野の総面積で除して得られた空孔の数を、1000μm2あたりに換算した。
島津製作所製のオートグラフ(登録商標)AGS-500Bを用いて測定した。ターゲット材から切り出した試料片(全長36mm以上、幅4.0mm、厚さ3.0mm)を用い、JIS-R-1601(ファインセラミックスの曲げ強度試験方法)の3点曲げ強さの測定方法に従って測定した。
三菱ケミカル製のロレスタ(登録商標)HP MCP-T410を用いて、JIS規格の直流四探針法によって測定した。加工後のターゲット材の表面にプローブ(直列四探針プローブ TYPE ESP)を当接させ、AUTO RANGEモードで測定した。測定箇所はターゲット材の中央付近及び四隅の計5か所とし、各測定値の算術平均値をそのターゲット材のバルク抵抗率とした。
表面粗さ測定器(SJ-210/株式会社ミツトヨ製)を用いて測定した。ターゲット材のスパッタリング面の5個所を測定して、その算術平均値をそのターゲット材の算術平均粗さRaとした。
面内の色差ΔE*は、切削加工したターゲット材の表面をx軸、y軸方向に50mm間隔で色差計(コニカミノルタ社製、色彩色差計CR-300)を用いて測定し、測定された各点のL*値、a*値及びb*値をCIE1976L*a*b*色空間で評価した。そして、測定された各点のうち2点のL*値、a*値及びb*値の差分ΔL*、Δa*、Δb*から、下記式(ii)より色差ΔE*をすべての2点の組み合わせで求め、求められた複数の色差ΔE*の最大値を表面内の最大色差ΔE*とした。
ΔE*=((ΔL*)2+(Δa*)2+(Δb*)2)1/2・・(ii)
また、深さ方向の最大色差ΔE*は、切削加工したターゲット材の任意の箇所において、1mmずつ切削加工し、ターゲット材の中央部までの各深さで色差計を用いて測定し、測定された各点のL*値、a*値およびb*値をCIE1976L*a*b*色空間で評価した。そして、測定された各点のうち2点のL*値、a*値およびb*値の差分ΔL*、Δa*、Δb*から色差ΔE*をすべての2点の組み合わせで求め、求められた複数の色差ΔE*の最大値を深さ方向の最大色差ΔE*とした。
株式会社マツザワのビッカース硬度計MHT-1を用いて測定した。ターゲット材を切断して得られた切断面を、エメリー紙#180、#400、#800、#1000、#2000を用いて段階的に研磨し、最後にバフ研磨して鏡面に仕上げて測定面とした。また、測定面からみて反対の面は、測定面と平行になるように、上記エメリー紙#180を用いて研磨し、試験片を得た。上記試験片を用いJIS-R-1610:2003(ファインセラミックスの硬さ試験方法)の硬さ測定方法に従って荷重1kgfでのビッカース硬度の測定を行った。測定は、1つの試験片中の異なる10箇所の位置について行い、その算術平均値をそのターゲット材のビッカース硬度とした。また、得られた測定値からビッカース硬度の標準偏差を算出した。
株式会社リガクのSmartLab(登録商標)を用いた。測定条件は以下のとおりである。実施例1で得られたターゲット材についてのXRD測定の結果を図2に示す。
・線源:CuKα線
・管電圧:40kV
・管電流:30mA
・スキャン速度:5deg/min
・ステップ:0.02deg
・スキャン範囲:2θ=5度~80度
日立ハイテクノロジーズ製の走査型電子顕微鏡SU3500を用いて、ターゲット材の表面をSEM観察するとともに、結晶の構成相や結晶形状の評価を行った。
具体的には、ターゲット材を切断して得られた切断面を、エメリー紙#180、#400、#800、#1000、#2000を用いて段階的に研磨し、最後にバフ研磨して鏡面に仕上げた。鏡面仕上げ面をSEM観察した。結晶形状の評価では、倍率1000倍、87.5μm×125μmの範囲のBSE-COMP像を無作為に10視野撮影しSEM像を得た。
得られたSEM像を、画像処理ソフトウェア:ImageJ 1.51k(http://imageJ.nih.gov/ij/、提供元:アメリカ国立衛生研究所(NIH:National Institutes of Health))によって解析した。具体的な手順は以下のとおりである。
SEM像撮影時に用いたサンプルを、1100℃で1時間サーマルエッチングを施し、SEM観察を行うことで図3に示す粒界が現れた画像を得た。得られた画像に対し、先ずIn2O3相(図3中、白く見える領域A)の粒界に沿って描画を行った。すべての描画が完了した後、粒子解析を実施(Analyze→Analyze Particles)して、各粒子における面積を得た。その後、得られた各粒子における面積から、面積円相当径を算出した。10視野において算出された全粒子の面積円相当径の算術平均値を、In2O3相の結晶粒のサイズとした。続いてZn3In2O6相(図3中、黒く見える領域B)の粒界に沿って描画を行い、同様に解析を施すことによって得られた各粒子における面積から、面積円相当径を算出した。10視野において算出された全粒子の面積円相当径の算術平均値を、Zn3In2O6相の結晶粒のサイズとした。
また、サーマルエッチング前の粒界のないBSE-COMP像について、粒子解析を行うことで総面積におけるIn2O3相の面積の比率を算出した。10視野において算出された全粒子のそれらの算術平均値を、In2O3相面積率とした。また100からIn2O3相面積率を差し引くことで、Zn3In2O6相面積率を算出した。
なお図4及び図6は、図3の拡大像である。
エダックス製のエネルギー分散型X線分析装置Octane Elite Plusを用いて、前記SEM観察にて確認されたIn2O3相及びZn3In2O6相における、各々任意の箇所での点分析によるスペクトル情報を得て、添加元素(X)含有の有無を確認した。結果を図5及び図7に示す。
実施例及び比較例のターゲット材を用いて、図1に示すTFT素子1をフォトリソグラフィー法により作製した。
TFT素子1の作製においては、最初に、ガラス基板(日本電気硝子株式会社製OA-10)10上にゲート電極20としてMо薄膜を、DCスパッタリング装置を用いて成膜した。次に、ゲート絶縁膜30としてSiOx薄膜を下記の条件で成膜した。
成膜装置:プラズマCVD装置 サムコ株式会社製 PD-2202L
成膜ガス:SiH4/N2O/N2混合ガス
成膜圧力:110Pa
基板温度:250~400℃
次に、チャネル層40を、実施例及び比較例で得られたターゲット材を用いて、下記の条件でスパッタリング成膜を行い、厚さ約10~50nmの薄膜を成膜した。
・成膜装置:DCスパッタリング装置 トッキ株式会社製 SML-464
・到達真空度:1×10-4Pa未満
・スパッタガス:Ar/O2混合ガス
・スパッタガス圧:0.4Pa
・O2ガス分圧:50%
・基板温度:室温
・スパッタリング電力:3W/cm2
更に、エッチングストッパー層50として、SiOx薄膜を、前記プラズマCVD装置を用いて成膜した。次に、ソース電極60及びドレイン電極61としてMo薄膜を、前記DCスパッタリング装置を用いて成膜した。保護層70として、SiOx薄膜を、前記プラズマCVD装置を用いて成膜した。最後に350℃で熱処理を実施した。
このようにして得られたTFT素子1について、ドレイン電圧Vd=5Vでの伝達特性の測定を行った。測定した伝達特性は、電界効果移動度μ(cm2/Vs)、SS(Subthreshold Swing)値(V/dec)及びしきい電圧Vth(V)である。伝達特性は、Agilent Technologies株式会社製Semiconductor Device Analyzer B1500Aによって測定した。測定結果を表1及び表2に示す。なお表に示していないが、各実施例で得られたTFT素子1のチャネル層40がアモルファス構造であることをXRD測定によって本発明者は確認している。
電界効果移動度とは、MOSFET(Metal-Oxide-Semiconductor Field-Effect Transistor)動作の飽和領域において、ドレイン電圧を一定としたときのゲート電圧に対するドレイン電流の変化から求めたチャネル移動度のことであり、値が大きいほど伝達特性が良好である。
SS値とは、しきい電圧近傍でドレイン電流を1桁上昇させるのに必要なゲート電圧のことであり、値が小さいほど伝達特性が良好である。
しきい電圧とは、ドレイン電極に正電圧をかけ、ゲート電極に正負いずれかの電圧をかけたときにドレイン電流が流れ、1nAとなった場合の電圧であり、値が0Vに近いことが好ましい。詳細には、-2V以上であることが更に好ましく、-1V以上であることが一層好ましく、0V以上であることが更に一層好ましい。また、3V以下であることが更に好ましく、2V以下であることが一層好ましく、1V以下であることが更に一層好ましい。具体的には、-2V以上3V以下であることが更に好ましく、-1V以上2V以下であることが一層好ましく、0V以上1V以下であることが更に一層好ましい。
更に、図2に示す結果から明らかなとおり、実施例1で得られたターゲット材は、In2O3相及びZn3In2O6相を含むものであった。図示していないが、実施例2ないし16で得られたターゲット材についても同様の結果が得られた。
更に、図5及び図7に示す結果から明らかなとおり、実施例1で得られたターゲット材に含まれるIn2O3相及びZn3In2O6相はいずれもTaを含有するものであった。図示していないが、実施例2ないし16で得られたターゲット材についても同様の結果が得られた。
実施例1及び比較例1で得られたターゲット材について、上述した方法でIn2O3相及びZn3In2O6相の分散率を測定した。その結果を以下の表3並びに図8(a)及び図8(b)に示す。
これに対して図8(b)に示す結果から明らかなとおり、比較例1で得られたターゲット材は、In2O3相及びZn3In2O6相が不均質に分散していることが分かる。
なお、表には示していないが実施例2ないし16で得られたターゲット材についても、16箇所の分散率が最大でも10%以下であったことを本発明者は確認している。
Claims (14)
- インジウム(In)元素、亜鉛(Zn)元素及び添加元素(X)を含む酸化物から構成され、
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)及びニオブ(Nb)から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たし(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
相対密度が95%以上である、スパッタリングターゲット材。 - 添加元素(X)がタンタル(Ta)である、請求項1に記載のスパッタリングターゲット材。
- 抗折強度が100MPa以上である、請求項1又は2に記載のスパッタリングターゲット材。
- バルク抵抗率が25℃において100mΩ・cm以下である、請求項1ないし3のいずれか一項に記載のスパッタリングターゲット材。
- In2O3相及びZn3In2O6相を含む、請求項1ないし4のいずれか一項に記載のスパッタリングターゲット材。
- In2O3相及びZn3In2O6相の双方に添加元素(X)が含まれる、請求項5に記載のスパッタリングターゲット材。
- In2O3相の結晶粒のサイズが0.1μm以上3.0μm以下であり、
Zn3In2O6相の結晶粒のサイズが0.1μm以上3.9μm以下である、請求項5又は6に記載のスパッタリングターゲット材。 - 式(4)を更に満たす、請求項1ないし7のいずれか一項に記載のスパッタリングターゲット材。
0.970≦In/(In+X)≦0.999 (4) - JIS-R-1610:2003に準拠して測定されたビッカース硬度の標準偏差が50以下である、請求項1ないし8のいずれか一項に記載のスパッタリングターゲット材。
- 請求項1ないし9のいずれか一項に記載のスパッタリングターゲット材を用いて形成された酸化物半導体であって、
インジウム(In)元素、亜鉛(Zn)元素及び添加元素(X)を含む酸化物から構成され、
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)、ニオブ(Nb)の中から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たす(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
酸化物半導体。 - インジウム(In)元素、亜鉛(Zn)元素及び添加元素(X)を含む酸化物から構成され、
添加元素(X)はタンタル(Ta)、ストロンチウム(Sr)、ニオブ(Nb)の中から選ばれる少なくとも1つの元素からなり、
各元素の原子比が式(1)ないし(3)を満たす(式中のXは、前記添加元素の含有比の総和とする。)、
0.4≦(In+X)/(In+Zn+X)≦0.8 (1)
0.2≦Zn/(In+Zn+X)≦0.6 (2)
0.001≦X/(In+Zn+X)≦0.015 (3)
酸化物半導体を有し、
電界効果移動度が45cm2/Vs以上である、薄膜トランジスタ。 - 前記酸化物半導体がアモルファス構造である、請求項11に記載の薄膜トランジスタ。
- 電界効果移動度が70cm2/Vs以上である、請求項11又は12に記載の薄膜トランジスタ。
- しきい電圧が-2V以上3V以下である、請求項11ないし13のいずれか一項に記載の薄膜トランジスタ。
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WO2023145497A1 (ja) * | 2022-01-31 | 2023-08-03 | 三井金属鉱業株式会社 | 電界効果トランジスタ及びその製造方法並びに電界効果トランジスタ製造用スパッタリングターゲット材 |
WO2023145499A1 (ja) * | 2022-01-31 | 2023-08-03 | 三井金属鉱業株式会社 | スパッタリングターゲット |
JP7364824B1 (ja) | 2022-01-31 | 2023-10-18 | 三井金属鉱業株式会社 | 電界効果トランジスタ及びその製造方法並びに電界効果トランジスタ製造用スパッタリングターゲット材 |
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KR20230017294A (ko) | 2023-02-03 |
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JPWO2022030455A1 (ja) | 2022-02-10 |
US20230307549A1 (en) | 2023-09-28 |
JP2023041776A (ja) | 2023-03-24 |
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