CN114057470A - Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material - Google Patents
Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material Download PDFInfo
- Publication number
- CN114057470A CN114057470A CN202010755647.0A CN202010755647A CN114057470A CN 114057470 A CN114057470 A CN 114057470A CN 202010755647 A CN202010755647 A CN 202010755647A CN 114057470 A CN114057470 A CN 114057470A
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- indium oxide
- target material
- oxide powder
- doped indium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3256—Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Abstract
The invention provides a preparation method of an indium oxide target material doped with molybdenum and the indium oxide target material doped with molybdenum, wherein the preparation method of the indium oxide target material doped with molybdenum comprises the following steps: grinding the target material through a two-stage grinding process to obtain slurry; granulating the slurry to obtain granules; preparing molybdenum-doped indium oxide target materials through granules; the method comprises the following steps of preparing a target raw material, wherein the target raw material comprises indium oxide powder and molybdenum oxide powder, and the step of obtaining slurry by two-stage grinding the target raw material specifically comprises the following steps: processing a target material by a ball milling process to obtain a section of slurry; treating the first-stage slurry through a sand milling process to obtain the slurry with the median particle size of 0.1-0.32 mu m, wherein the treatment time of the ball milling process is 12-18 h; the material concentration in the ball milling process is 40% to 50%. The target material is prepared by the target material preparation method, the target material has high density and good component distribution uniformity, and the transparent conductive film prepared by the target material is beneficial to the transmission of infrared band light.
Description
Technical Field
The invention relates to the technical field of targets, in particular to a preparation method of an indium oxide target doped with molybdenum and the indium oxide target doped with molybdenum.
Background
Transparent Conductive Oxide films (Transparent Conductive oxides) have been widely used in the fields of displays, solar cells, light emitting diodes, touch panels, gas sensors, microelectronics, vacuum electronics, and the like, because of their excellent metal-like conductivity, glass-like high optical transparency, infrared-region high reflectivity, and other excellent semiconductor characteristics. The infrared transparent conductive film has important application value in military and civil fields. For civil application, the method can be applied to the fields of electronics and energy industry, sensing technology, photoelectric technology and the like, for example, the method can be used as an infrared transparent electrode to be applied to an infrared solar cell and an infrared laser. For the military field, the infrared imaging system can be applied to the fields of infrared imaging, spacecraft windows and the like. Therefore, the infrared transparent conductive film is a material with high application value.
The existing transparent conductive oxide film is mostly prepared by tin oxide doped indium oxide target material, and because tin replaces indium, the target material has high electron concentration and low electron mobility, the transparent conductive oxide film prepared by the target material has poor infrared wave band light transmission capability.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art.
To this end, the invention provides a method for preparing a molybdenum-doped indium oxide target material.
In a second aspect, the invention provides a molybdenum-doped indium oxide target.
In view of the above, according to a first aspect of the present invention, there is provided a method for preparing a molybdenum-doped indium oxide target, including: grinding the target material through a two-stage grinding process to obtain slurry; granulating the slurry to obtain granules; preparing molybdenum-doped indium oxide target materials through granules; wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
According to the preparation method of the molybdenum-doped indium oxide target material, the indium oxide powder and the molybdenum oxide powder are mixed and finely ground through two-stage grinding, the slurry after full mixing and fine grinding is granulated, and the molybdenum-doped indium oxide target material can be obtained further based on the granules. According to the invention, through two-stage grinding, indium oxide powder and molybdenum oxide powder can be fully mixed, the particle sizes of the indium oxide powder and the molybdenum oxide powder are further reduced, and gaps among indium oxide powder particles, molybdenum oxide powder particles and between the indium oxide powder particles and the molybdenum oxide powder particles are reduced through reducing the particle sizes of the indium oxide powder and the molybdenum oxide powder, so that the density of the target material is improved, and the component distribution uniformity of the indium oxide and the molybdenum oxide is good. The performance of the conductive oxide film using the target material is improved.
According to the invention, molybdenum oxide powder is selected as a raw material in the preparation process of the target material, so that the light transmittance of the infrared band of the conductive oxide film using the molybdenum-doped indium oxide target material is improved, the conductive oxide film has excellent conductivity, the conductive oxide film can be used as a conductive electrode, and other physical and chemical properties of the film are consistent with those of the conventional Indium Tin Oxide (ITO) film.
Specifically, the target material relies on two important aspects to improve electrical conductivity: the first is the concentration of carriers formed by doping, and the second is the mobility of the carriers. The high doping concentration generates a large number of carriers and improves the conductivity, but the high carrier concentration causes the plasma resonance absorption edge to move towards the short wavelength direction, and the light transmittance of the infrared band is seriously reduced. Therefore, under the condition of doping proper amount of impurities, a certain amount of carriers are obtained,the electron scattering is reduced, the mobility of carriers is improved, and the light transmittance of infrared bands is improved. The conventional target material is Sn4+Doping to substitute In3+The application adopts hexavalent high-valence elements to replace In by introducing molybdenum oxide powder3+And a small amount of doping can generate high-concentration carriers, which is beneficial to improving the mobility of the carriers, so that a target material with high electron concentration and high electron mobility is finally obtained, and the transparent conductive oxide film with excellent infrared band light transmission capability can be prepared and obtained through the indium oxide target material.
It can be understood that the auxiliary agent can be added in the process of obtaining the slurry by two-stage grinding of the indium oxide powder and the molybdenum oxide powder, so as to improve the probability of the contact of the auxiliary agent with the indium oxide powder and the molybdenum oxide powder, and the auxiliary agent can play a better auxiliary role. In particular, the adjuvant may be a dispersant.
In addition, the method for preparing the molybdenum-doped indium oxide target material in the technical scheme provided by the invention can also have the following additional technical characteristics:
in the above technical solution, further, the step of obtaining the slurry by two-stage grinding the target material specifically includes: processing a target material by a ball milling process to obtain a section of slurry; and (3) treating the primary slurry by a sand grinding process to obtain the slurry with the median particle size of 0.1-0.32 μm.
In the technical scheme, the specific steps of secondary grinding are further provided, wherein the secondary grinding comprises a ball-milling process and a sand-milling process, and the indium oxide powder and the molybdenum oxide powder are treated by the ball-milling process and the sand-milling process to obtain the slurry with the median particle size of 0.1-0.32 μm. The grinding fineness of the indium oxide powder and the molybdenum oxide powder is further ensured, the indium oxide powder and the molybdenum oxide powder are fully mixed, the density and the component distribution uniformity of the molybdenum-doped indium oxide target material are further improved, and the performance of a conductive oxide film using the target material is ensured.
In any of the above technical solutions, further, the treatment time of the ball milling process is 12h to 18 h; the material concentration in the ball milling process is 40% to 50%.
In the technical scheme, the processing time and the material concentration of the ball milling process are further provided, the abrasive fineness of the indium oxide powder and the molybdenum oxide powder is further ensured by selecting the ball milling process with the processing time of 12-18 h and the material concentration of 40-50%, the indium oxide powder and the molybdenum oxide powder are fully mixed, the density and the component distribution uniformity of the molybdenum-doped indium oxide target material are further improved, and the performance of a conductive oxide film using the target material is ensured.
In any of the above technical solutions, further, the number of times of the sand-milling process is 3 to 7, and the time duration of each time is 1.5h to 2.5 h.
In the technical scheme, the treatment times of the sanding process and the time length of each sanding are further provided, so that the median particle size of solid particles in the slurry subjected to sanding is 0.1-0.32 μm, the density and the component distribution uniformity of the molybdenum-doped indium oxide target can be further improved, and the performance of a conductive oxide film using the target is guaranteed.
In any of the above technical solutions, further, the abrasive in the sand grinding process is zirconia ceramic with a particle size of 0.2mm to 0.4 mm.
In the technical scheme, the material selection and the particle size of the sanding grinding abrasive are further provided, the indium oxide powder and the molybdenum oxide powder are prevented from being polluted by the abrasive, and the purity of the target is improved.
In any of the above technical solutions, further, the step of preparing the molybdenum-doped indium oxide target material by using the pellet specifically includes: placing the granules in an isostatic pressing die, and carrying out cold isostatic pressing to obtain a biscuit; and sintering the biscuit, and cooling to obtain the molybdenum-doped indium oxide target material.
According to the technical scheme, the specific steps of preparing the molybdenum-doped indium oxide target material through the granules are further provided, the granules obtained through granulation are subjected to cold isostatic pressing to obtain a biscuit, the biscuit is sintered, and the molybdenum-doped indium oxide target material is obtained after cooling.
In any of the above technical solutions, further, the sintering temperature for sintering the biscuit is 1500 ℃ to 1570 ℃; the cold isostatic pressing pressure is 250MPa to 300 MPa.
In the technical scheme, the sintering temperature and the cold isostatic pressure are further provided, and the quality of the molybdenum-doped indium oxide target material is ensured by selecting 1500-1570 ℃ and 250-300 Mpa, so that the performance of a conductive oxide film using the target material is improved.
In any of the above technical solutions, further, the mass percentage of the molybdenum oxide powder is 1.2 to 3.2.
In the technical scheme, the usage amount of the molybdenum oxide material is further provided, the usage amount of the molybdenum oxide powder is 1.2-3.2 percent of the total mass of the target material raw material, and the selection of the formula ensures the performance of the molybdenum-doped indium oxide target material and improves the density of the molybdenum-doped indium oxide target material.
In any of the above technical solutions, further, the purity of molybdenum oxide in the molybdenum oxide powder is greater than 99.99%, and the specific surface area is 10m2G to 15m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 12m2G to 18m2/g。
In the technical scheme, the purity and the specific surface area of the molybdenum oxide powder and the indium oxide powder are further provided, the purity of the molybdenum-doped indium oxide target material is guaranteed, and the quality of the molybdenum-doped indium oxide target material is improved.
In any of the above embodiments, further the molybdenum oxide powder has a median particle size of less than or equal to 0.35 μm; the indium oxide powder has a median particle diameter of 0.56 μm or less.
In the technical scheme, the performance of the target material is that the median particle size of molybdenum powder in the target material is less than or equal to 0.35 μm; the selection of the median particle size of the indium oxide powder is less than or equal to 0.56 μm, so that the particle size of solid particles in the slurry obtained by two-stage grinding is further reduced, the density of the molybdenum-doped indium oxide target material is further improved, and the uniformity of the component distribution of the indium oxide powder and the molybdenum oxide powder is better.
Specifically, the median particle diameter of the indium oxide powder was 0.56 μm; the median particle diameter of the molybdenum oxide powder is 0.35 μm, which can reduce the cost of raw materials.
According to a second aspect of the present invention, a molybdenum-doped indium oxide target is provided, which is prepared by any one of the above-mentioned methods.
The molybdenum-doped indium oxide target material provided by the invention is prepared by adopting the target material preparation method of any one of the technical schemes, so that the molybdenum-doped indium oxide target material has all the beneficial effects of the molybdenum-doped indium oxide target material preparation method of any one of the technical schemes, and the details are not repeated herein.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic flow diagram illustrating a method for making a molybdenum-doped indium oxide target according to a first embodiment of the present invention;
FIG. 2 is a schematic flow chart showing a method of making a molybdenum-doped indium oxide target according to example two of the present invention;
FIG. 3 is a schematic flow chart showing a process for preparing a molybdenum-doped indium oxide target according to example III of the present invention;
FIG. 4 is a schematic flow chart illustrating a method of making a molybdenum doped indium oxide target according to example four of the present invention;
FIG. 5 is a schematic flow chart illustrating a method of making a molybdenum doped indium oxide target according to example V of the present invention;
FIG. 6 is a schematic flow chart illustrating a method of making a molybdenum doped indium oxide target according to an embodiment of the present invention;
FIG. 7 is a schematic flow chart showing a process for preparing a molybdenum-doped indium oxide target of comparative example 1;
FIG. 8 is a schematic flow chart showing a process for preparing a molybdenum-doped indium oxide target of comparative example 2;
fig. 9 shows a schematic of pellets placed within an isostatic mold according to one embodiment of the invention.
Wherein, the correspondence between the reference numbers and the names of the components in fig. 9 is:
100 plugs, 200 wraps, 300 cores, 400 pellets.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be described in further detail below with reference to the accompanying drawings and detailed description. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and therefore the scope of the present invention is not limited by the specific embodiments disclosed below.
Methods of preparing molybdenum-doped indium oxide targets and molybdenum-doped indium oxide targets according to some embodiments of the present invention are described below with reference to fig. 1-9.
Example one
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 102: grinding the target material through a two-stage grinding process to obtain slurry;
step 104: granulating the slurry to obtain granules;
step 106: and preparing the molybdenum-doped indium oxide target material through granules.
Wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
According to the preparation method of the molybdenum-doped indium oxide target material, the indium oxide powder and the molybdenum oxide powder are mixed and finely ground through two-stage grinding, the slurry after full mixing and fine grinding is granulated, and the molybdenum-doped indium oxide target material can be obtained further based on the granules. According to the invention, through two-stage grinding, indium oxide powder and molybdenum oxide powder can be fully mixed, the particle sizes of the indium oxide powder and the molybdenum oxide powder are further reduced, and gaps among indium oxide powder particles, molybdenum oxide powder particles and between the indium oxide powder particles and the molybdenum oxide powder particles are reduced through reducing the particle sizes of the indium oxide powder and the molybdenum oxide powder, so that the density of the target material is improved, and the component distribution uniformity of the indium oxide and the molybdenum oxide is good. The performance of the conductive oxide film using the target material is improved, and meanwhile, the production process is simple and is suitable for industrial production.
It can be understood that the auxiliary agent can be added in the process of obtaining the slurry by two-stage grinding of the indium oxide powder and the molybdenum oxide powder, so as to improve the probability of the contact of the auxiliary agent with the indium oxide powder and the molybdenum oxide powder, and the auxiliary agent can play a better auxiliary role. In particular, the adjuvant may be a dispersant.
Example two
As shown in fig. 2, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 202: processing a target material by a ball milling process to obtain a section of slurry;
step 204: treating the first-stage slurry by a sand grinding process to obtain slurry with the median particle size of 0.1-0.32 mu m;
step 206: granulating the slurry to obtain granules;
step 208: and preparing the molybdenum-doped indium oxide target material through granules.
Wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
In this embodiment, a specific step of secondary grinding is further provided, where the secondary grinding includes a ball-milling process and a sand-milling process, and the indium oxide powder and the molybdenum oxide powder are processed by the ball-milling process and the sand-milling process, so as to obtain a slurry with a median particle size of 0.1 μm to 0.32 μm. The grinding fineness of the indium oxide powder and the molybdenum oxide powder is further ensured, the indium oxide powder and the molybdenum oxide powder are fully mixed, the density and the component distribution uniformity of the molybdenum-doped indium oxide target material are further improved, and the performance of a conductive oxide film using the target material is ensured.
EXAMPLE III
As shown in fig. 3, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 302: processing a target material by a ball milling process to obtain a section of slurry;
step 304: treating the first-stage slurry by a sand grinding process to obtain slurry with the median particle size of 0.1-0.32 mu m;
step 306: granulating the slurry to obtain granules;
step 308: and preparing the molybdenum-doped indium oxide target material through granules.
Wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
Further, the processing time of the ball milling process is 12h to 18 h; the material concentration in the ball milling process is 40% to 50%.
In the embodiment, the processing time and the material concentration of the ball milling process are further provided, and the grinding fineness of the indium oxide powder and the molybdenum oxide powder is further ensured by selecting the ball milling process for 12h to 18h and the material concentration for 40% to 50%, and meanwhile, the indium oxide powder and the molybdenum oxide powder are fully mixed, so that the density and the component distribution uniformity of the molybdenum-doped indium oxide target material are further improved, and the performance of a conductive oxide film using the target material is ensured.
Example four
As shown in fig. 4, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 402: processing a target material by a ball milling process to obtain a section of slurry;
step 404: treating the first-stage slurry by a sand grinding process to obtain slurry with the median particle size of 0.1-0.32 mu m;
step 406: granulating the slurry to obtain granules;
step 408: and preparing the molybdenum-doped indium oxide target material through granules.
Wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
Further, the processing time of the ball milling process is 12h to 18 h; the material concentration in the ball milling process is 40% to 50%.
Further, the treatment times of the sand milling process are 3 to 7 times, and the time length of each time is 1.5h to 2.5 h.
In the embodiment, the treatment times of the sanding process and the time length of each sanding are further provided, so that the median particle size of solid particles in the slurry subjected to sanding is 0.1-0.32 μm, the compactness and the uniformity of the component distribution of the molybdenum-doped indium oxide target can be further improved, and the performance of a conductive oxide film using the target is guaranteed.
Further, the grinding material in the sand grinding process is zirconia ceramic with the grain diameter of 0.2mm to 0.4 mm.
In the embodiment, the material selection and the particle size of the sanding grinding abrasive are further provided, the indium oxide powder and the molybdenum oxide powder are prevented from being polluted by the abrasive, and the purity of the target material is improved.
EXAMPLE five
As shown in fig. 5, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 502: processing a target material by a ball milling process to obtain a section of slurry;
step 504: treating the first-stage slurry by a sand grinding process to obtain slurry with the median particle size of 0.1-0.32 mu m;
step 506: granulating the slurry to obtain granules;
step 508: placing the granules in an isostatic pressing die, and carrying out cold isostatic pressing to obtain a biscuit;
step 510: and sintering the biscuit, and cooling to obtain the molybdenum-doped indium oxide target material.
Wherein, the target material comprises indium oxide powder and molybdenum oxide powder.
In the embodiment, the specific step of preparing the molybdenum-doped indium oxide target material by using the granules is further provided, the granules obtained by granulation are subjected to cold isostatic pressing to obtain a biscuit, the biscuit is sintered, and the molybdenum-doped indium oxide target material is obtained after cooling.
Further, the sintering temperature for sintering the biscuit is 1500-1570 ℃; the cold isostatic pressing pressure is 250MPa to 300 MPa.
In the embodiment, the sintering temperature and the cold isostatic pressure are further provided, and the quality of the molybdenum-doped indium oxide target material is ensured by selecting 1500-1570 ℃ and 250-300 Mpa, so that the performance of the conductive oxide film using the target material is improved.
As shown in fig. 9, in the process of performing cold isostatic pressing on the granules, the sheath 200 is sleeved on the iron core 300, a granule storage gap is formed between the sheath 200 and the iron core, the granules 400 are placed in the granule storage gap, the plugs 100 are arranged at two ends of the iron core 300 to plug the granule storage gap, and then the granules 400 can be subjected to cold isostatic pressing by using cold isostatic pressing to obtain a biscuit.
EXAMPLE six
In any one of the first to fifth embodiments, the molybdenum oxide powder is 1.2 mass%.
EXAMPLE seven
In any one of the first to fifth embodiments, the molybdenum oxide powder is 3.2 mass%.
Example eight
In any one of the first to fifth embodiments, the molybdenum oxide powder is 2.2 mass%.
Example nine
In any one of the first to fifth embodiments, the molybdenum oxide powder is 1.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 10m2(ii) from/g to; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 18m2/g。
Example ten
In any one of the first to fifth embodiments, the molybdenum oxide powder is 3.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 15m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 12m2/g。
EXAMPLE eleven
In any one of the first to fifth embodiments, the molybdenum oxide powder is 2.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 12m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 15m2/g。
Example twelve
In any one of the first to fifth embodiments, the molybdenum oxide powder is 1.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 10m2(ii) from/g to; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 18m2/g。
Wherein the median particle diameter of the indium oxide powder is 0.56 μm; the median particle diameter of the molybdenum oxide powder was 0.35. mu.m.
EXAMPLE thirteen
In any one of the first to fifth embodiments, the molybdenum oxide powder is 3.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 15m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 12m2/g。
Wherein the median particle diameter of the indium oxide powder is 0.56 μm; the median particle diameter of the molybdenum oxide powder was 0.35. mu.m.
Example fourteen
In any one of the first to fifth embodiments, the molybdenum oxide powder is 2.2 mass%.
Wherein the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 12m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 14m2/g。
Wherein the median particle diameter of the indium oxide powder is 0.56 μm; the median particle diameter of the molybdenum oxide powder was 0.35. mu.m.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
As shown in fig. 6, an embodiment of the present invention provides a method for preparing a molybdenum-doped indium oxide target, including:
step 602: the purity is more than 99.99 percent and the granularity D is50＜0.56μm，BET＝10m2Indium oxide powder/g and a purity of more than 99.95%, particle size D50＜0.35μm，BET＝12m2Putting/g of molybdenum oxide powder into a ball mill for mixing for 15 h;
step 604: the slurry after ball milling is injected into a sand mill for sand milling, wherein the sand milling frequency is 5 times, and each time lasts for 2 hours;
step 606: obtaining spherical granules through spray granulation;
step 608: placing the granules in a cold isostatic pressing mould, and carrying out cold isostatic pressing at a forming pressure of 250MPa to obtain a biscuit;
step 610: and (3) placing the molded biscuit into a sintering furnace, sintering in an oxygen atmosphere at 1570 ℃, and cooling to obtain the molybdenum-doped indium oxide target material.
The molybdenum-doped indium oxide target material obtained by the embodiment has the advantages of high density, high purity, good component distribution uniformity, small grain size, simple process and suitability for large-scale production.
Comparative example 1
As shown in fig. 7, this comparative example provides a method for preparing a molybdenum-doped indium oxide target, comprising:
step 12: grinding indium oxide powder and molybdenum oxide powder by ball milling to obtain slurry;
step 14: granulating the ground pulp to obtain granules;
step 16: carrying out cold isostatic pressing on the granules to obtain a biscuit;
step 18: and sintering the biscuit, and cooling to obtain the target material.
Comparative example 2
As shown in fig. 8, this comparative example provides a method for preparing a molybdenum-doped indium oxide target, comprising:
step 22: carrying out sand grinding on the indium oxide powder and the molybdenum oxide powder to obtain slurry;
step 24: granulating the slurry to obtain granules;
step 26: carrying out cold isostatic pressing on the granules to obtain a biscuit;
step 28: and sintering the biscuit, and cooling to obtain the target material.
Test example
Selecting the targets prepared in the first to fourteenth embodiments, the specific embodiments, the comparative examples 1 and the comparative examples 2, wherein the sizes of the targets after being processed by an inner and outer circle grinder and a wire cutting machine are as follows: the inner diameter is 135mm, the height is 500mm, the wall thickness is 6mm, the density test of the target material adopts an Archimedes drainage method, the resistivity test adopts a four-probe method, the resistivity uniformity analysis adopts a Sudoku method to test the resistivity of 9 points on the surface of the target material at different positions, then the difference value between the maximum value and the average value is compared with the average value to calculate the uniformity, the density, the resistivity and the resistivity uniformity of the target material prepared in the first to sixteenth embodiments and the specific embodiments and the comparative examples 1 to 3 are respectively measured, and the test results are shown in Table 1.
Table 1 test example measurement results
Based on the measurement results of table 1, as can be seen from the comparison of the measurement results of examples one to fourteen and specific examples with the measurement results of comparative examples 1 and 2, the density and resistivity uniformity of the target materials prepared in examples one to fourteen and specific examples are significantly improved, and the resistivity of the target material is significantly reduced, so that the conductive oxide thin film using the target materialThe light transmittance of the infrared band is improved, and the conductive electrode has excellent conductivity and does not influence the use as a conductive electrode. As can be seen from comparison of the measurement results of examples six to eight with the measurement results of examples one to five, the addition of the molybdenum oxide powder in an amount of 1.2 to 3.2 by mass% can further improve the target density and the resistivity uniformity, and can further reduce the target resistivity. As can be seen from the comparison of the measurement results of examples nine to fourteen and the measurement results of examples six to eight, the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99%, and the specific surface area is 10m2G to 15m2(ii)/g; the purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 12m2G to 18m2(ii)/g and the median particle diameter of the molybdenum oxide powder is less than or equal to 0.35 μm; determination of the median particle size of the indium oxide powder to be less than or equal to 0.56 μm can further improve the target performance.
In the present invention, the terms "mounting," "connecting," "fixing," and the like are used in a broad sense, for example, "connecting" may be a fixed connection, a detachable connection, or an integral connection; "coupled" may be direct or indirect through an intermediary. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description herein, the description of the terms "one embodiment," "some embodiments," "specific embodiments," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing an indium oxide target material doped with molybdenum is characterized by comprising the following steps:
grinding the target material through a two-stage grinding process to obtain slurry;
granulating the slurry to obtain granules;
preparing the molybdenum-doped indium oxide target material through the granules;
the target material comprises indium oxide powder and molybdenum oxide powder.
2. The method for preparing a molybdenum-doped indium oxide target according to claim 1, wherein the step of obtaining the slurry by two-stage grinding the target material comprises:
processing the target material by a ball milling process to obtain a section of slurry;
and treating the section of slurry through a sand grinding process to obtain the slurry with the median particle size of 0.1-0.32 μm.
3. The method of claim 2, wherein the molybdenum-doped indium oxide target is prepared by,
the processing time of the ball milling process is 12h to 18 h;
the concentration of the materials in the ball milling process is 40-50%.
4. The method of claim 2, wherein the molybdenum-doped indium oxide target is prepared by,
the treatment times of the sand grinding process are 3-7 times, and the time length of each time is 1.5-2.5 h;
the grinding material in the sand grinding process is zirconia ceramic with the grain diameter of 0.2mm to 0.4 mm.
5. The method of claim 1, wherein the step of obtaining the molybdenum-doped indium oxide target material by the pellet fabrication comprises:
placing the granules in an isostatic pressing die, and carrying out cold isostatic pressing to obtain a biscuit;
and sintering the biscuit, and cooling to obtain the molybdenum-doped indium oxide target material.
6. The method of claim 5, wherein the molybdenum-doped indium oxide target is prepared by,
the sintering temperature for sintering the biscuit is 1500-1570 ℃;
the cold isostatic pressing pressure is 250MPa to 300 MPa.
7. The method of making a molybdenum doped indium oxide target according to any one of claims 1 to 6,
the molybdenum oxide powder is 1.2 to 3.2 mass percent.
8. The method of claim 7, wherein the molybdenum-doped indium oxide target is prepared by,
the purity of molybdenum oxide in the molybdenum oxide powder is more than 99.99 percent, and the specific surface area is 10m2G to 15m2/g；
The purity of indium oxide in the indium oxide powder is more than 99.99 percent, and the specific surface area is 12m2G to 18m2/g。
9. The method of making a molybdenum doped indium oxide target according to any one of claims 1 to 7,
the molybdenum oxide powder has a median particle diameter of less than or equal to 0.35 μm;
the indium oxide powder has a median particle diameter of 0.56 μm or less.
10. A molybdenum-doped indium oxide target material, comprising:
prepared by the method of preparing a molybdenum-doped indium oxide target according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010755647.0A CN114057470A (en) | 2020-07-31 | 2020-07-31 | Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010755647.0A CN114057470A (en) | 2020-07-31 | 2020-07-31 | Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114057470A true CN114057470A (en) | 2022-02-18 |
Family
ID=80227356
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010755647.0A Pending CN114057470A (en) | 2020-07-31 | 2020-07-31 | Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114057470A (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004323877A (en) * | 2003-04-22 | 2004-11-18 | Sumitomo Metal Mining Co Ltd | Ito thin film manufacturing target, and method for manufacturing the same |
| CN1918672A (en) * | 2004-03-09 | 2007-02-21 | 出光兴产株式会社 | Thin film transistor, thin film transistor substrate, method for producing thin film transistor substrate, liquid crystal display device using thin film transistor substrate, apparatus and method for producing thin film transistor substrate, sputtering target, transparent conductive film and transparent electrode formed by using sputtering target, and apparatus and method for producing thin film transistor substrate |
| CN101079382A (en) * | 2007-05-24 | 2007-11-28 | 复旦大学 | Near-infrared high-transmission rate and multi-crystal transparent conductive oxide film and its making method |
| US20090211903A1 (en) * | 2008-02-26 | 2009-08-27 | Samsung Corning Precision Glass Co.,Ltd. | Indium zinc oxide based sputtering target, method of manufacturing the same, and indium zinc oxide based thin film |
| CN101560642A (en) * | 2009-05-22 | 2009-10-21 | 南开大学 | Method for preparing In2O3 transparent conductive film with high mobility doped with Mo |
| JP2012126937A (en) * | 2010-12-13 | 2012-07-05 | Sumitomo Metal Mining Co Ltd | Ito sputtering target and manufacturing method thereof |
| WO2013035335A1 (en) * | 2011-09-06 | 2013-03-14 | 出光興産株式会社 | Sputtering target |
| CN103682015A (en) * | 2012-09-20 | 2014-03-26 | 海洋王照明科技股份有限公司 | Molybdenum doped indium oxide conductive film, preparation method and application thereof |
| CN111138202A (en) * | 2020-01-16 | 2020-05-12 | 洛阳晶联光电材料有限责任公司 | Method for preparing ITO (indium tin oxide) granulation powder by mixing method |
| CN111196899A (en) * | 2018-11-20 | 2020-05-26 | 江苏金石研磨有限公司 | Superfine grinding preparation process for nano silicon oxide |
-
2020
- 2020-07-31 CN CN202010755647.0A patent/CN114057470A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004323877A (en) * | 2003-04-22 | 2004-11-18 | Sumitomo Metal Mining Co Ltd | Ito thin film manufacturing target, and method for manufacturing the same |
| CN1918672A (en) * | 2004-03-09 | 2007-02-21 | 出光兴产株式会社 | Thin film transistor, thin film transistor substrate, method for producing thin film transistor substrate, liquid crystal display device using thin film transistor substrate, apparatus and method for producing thin film transistor substrate, sputtering target, transparent conductive film and transparent electrode formed by using sputtering target, and apparatus and method for producing thin film transistor substrate |
| CN101079382A (en) * | 2007-05-24 | 2007-11-28 | 复旦大学 | Near-infrared high-transmission rate and multi-crystal transparent conductive oxide film and its making method |
| US20090211903A1 (en) * | 2008-02-26 | 2009-08-27 | Samsung Corning Precision Glass Co.,Ltd. | Indium zinc oxide based sputtering target, method of manufacturing the same, and indium zinc oxide based thin film |
| CN101560642A (en) * | 2009-05-22 | 2009-10-21 | 南开大学 | Method for preparing In2O3 transparent conductive film with high mobility doped with Mo |
| JP2012126937A (en) * | 2010-12-13 | 2012-07-05 | Sumitomo Metal Mining Co Ltd | Ito sputtering target and manufacturing method thereof |
| WO2013035335A1 (en) * | 2011-09-06 | 2013-03-14 | 出光興産株式会社 | Sputtering target |
| CN103682015A (en) * | 2012-09-20 | 2014-03-26 | 海洋王照明科技股份有限公司 | Molybdenum doped indium oxide conductive film, preparation method and application thereof |
| CN111196899A (en) * | 2018-11-20 | 2020-05-26 | 江苏金石研磨有限公司 | Superfine grinding preparation process for nano silicon oxide |
| CN111138202A (en) * | 2020-01-16 | 2020-05-12 | 洛阳晶联光电材料有限责任公司 | Method for preparing ITO (indium tin oxide) granulation powder by mixing method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8941002B2 (en) | Oxide evaporation material, vapor-deposited thin film, and solar cell | |
| CN114057471A (en) | Target material preparation method and target material | |
| EP2495224B1 (en) | Indium oxide sintered body and indium oxide transparent conductive film | |
| CN114059025A (en) | Indium oxide target material and indium oxide target material preparation method | |
| JP5692224B2 (en) | Zinc oxide sintered tablet and method for producing the same | |
| JP5082928B2 (en) | ZnO vapor deposition material, method for producing the same, and ZnO film formed thereby | |
| JP5585046B2 (en) | Composite oxide sintered body, target and oxide transparent conductive film | |
| JP6500446B2 (en) | Oxide sintered body and oxide transparent conductive film | |
| JP5418752B2 (en) | ZnO vapor deposition material, method for producing the same, and method for forming the ZnO film | |
| JP2009097088A (en) | ZnO VAPOR DEPOSITION MATERIAL, PROCESS FOR PRODUCING THE SAME, AND ZnO FILM OR THE LIKE | |
| JP5082927B2 (en) | Method for producing ZnO vapor deposition material | |
| CN113735564A (en) | Nb-doped IZO target blank and preparation method thereof | |
| JP5499453B2 (en) | ZnO vapor deposition material, method for producing the same, and method for forming the ZnO film | |
| JP5418749B2 (en) | ZnO vapor deposition material, method for producing the same, and method for forming the ZnO film | |
| JP2009097086A (en) | ZnO VAPOR DEPOSITION MATERIAL, PROCESS FOR PRODUCING THE SAME, AND ZnO FILM OR THE LIKE | |
| TWI431135B (en) | Zno deposition material, method for producing the same, and zno film | |
| JP5418748B2 (en) | ZnO vapor deposition material, method for producing the same, and method for forming the ZnO film | |
| JP4962355B2 (en) | ZnO vapor deposition material and ZnO film formed thereby | |
| CN114057470A (en) | Preparation method of molybdenum-doped indium oxide target material and molybdenum-doped indium oxide target material | |
| CN114057481B (en) | Method for producing zinc oxide target material and zinc oxide target material | |
| JP5018553B2 (en) | ZnO vapor deposition material, method for producing the same, and ZnO film formed thereby | |
| JP5381724B2 (en) | Method for producing ZnO vapor deposition material | |
| KR20180116281A (en) | Oxide-sintered body and oxide-transparent conductive film | |
| JP5169313B2 (en) | Method for producing ZnO vapor deposition material | |
| JP5418750B2 (en) | ZnO vapor deposition material, method for producing the same, and method for forming the ZnO film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220218 |
|
| RJ01 | Rejection of invention patent application after publication |