CN110002853A - The method that twice sintering process prepares IGZO ceramic target - Google Patents
The method that twice sintering process prepares IGZO ceramic target Download PDFInfo
- Publication number
- CN110002853A CN110002853A CN201910351001.3A CN201910351001A CN110002853A CN 110002853 A CN110002853 A CN 110002853A CN 201910351001 A CN201910351001 A CN 201910351001A CN 110002853 A CN110002853 A CN 110002853A
- Authority
- CN
- China
- Prior art keywords
- igzo
- temperature
- sintering
- sintering temperature
- green body
- 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
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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
-
- 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
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
-
- 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
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
-
- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- 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
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses a kind of methods that twice sintering process prepares IGZO target, comprising: quantifies In in proportion2O3、Ga2O3It with tri- kinds of oxide powders of ZnO, is mixed with deionized water, diluent and binder, is prepared into the IGZO slurry of high solids content；IGZO sizing material forming is IGZO ceramic green body；The degreasing at 600~800 DEG C of temperature of IGZO ceramic green body；IGZO ceramic green body after degreasing is warming up to 1400~1500 DEG C of first step sintering temperature, then, is cooled to 1320~1360 DEG C of second step sintering temperature, keeps the temperature 8~14 hours under second step sintering temperature.Mold is simple, technological operation is easy, convenient for preparing the target of various sizes, green sintering is good, can prepare the tiny IGZO ceramic target of high density, low-resistivity, crystal grain, relative density is up to 99.5%, resistivity is down to 1.59m Ω cm, and for crystallite dimension down to 4.78 μm, reduced sintering temperature can reduce production cost accordingly, extend service life of equipment, is suitable for industrialized production.
Description
Technical field
The invention belongs to target preparation technical fields, and in particular to a kind of twice sintering process prepares IGZO ceramic target
Method.
Background technique
Thin Film Transistor-LCD (thin film transistor-liquid crystal display,
TFT-LCD) it is applied to a kind of technology on display device.With the mobile terminals such as mobile phone, tablet computer towards more high definition,
Colorfulness is more saturated, more lightening development, and then developing amorphous oxide indium gallium zinc (IGZO) display material of new generation is film
Transistor technology growth requirement.
Current most of TFT-LCD are using α-Si as active channel layer material, and amorphous silicon technology (α-Si) has
The advantages that technically simple, low in cost, but with the continuous increase of display sizes, there is electricity in amorphous silicon film transistor
Transport factor is insufficient, and homogeneity is poor, while also taking up elemental area, the defect for causing transmitance to reduce.As consumer is to aobvious
Show that the requirement of product steps up, the mobile terminals such as mobile phone, tablet computer are more saturated towards more high definition, colorfulness, are more lightening
Development, α-Si technology obviously cannot reach the requirement of newest display effect, at this moment just arisen IGZO and LTPS this
Two kinds of technologies.Compared to amorphous silicon technology, IGZO is high with mobility, homogeneity is good, lower power consumption, very strong bendability
Can, it can be used for Flexible Displays.
IGZO ceramic target is the critical material for preparing IGZO film, can plate IGZO by magnetron sputtering technique with large area
Film, and its ingredient, grain uniformity, microstructure etc. are easily controllable in preparing thin-film process.Prepare IGZO ceramic target
The technical process of material mainly includes oxide powder synthesis, ceramic green forming and three key links of high temperature sintering.
The common sintering method for preparing IGZO oxide ceramics target is using conventional sintering process at present.For the sintering
Technique, if maximum sintering temperature is lower than 1350 DEG C, IGZO oxide ceramics target can not densify completely, interior microscopic
Tissue still suffers from many holes；And its maximum sintering temperature is when being higher than 1400 DEG C, and will appear coarse grains and uniformity is poor
The defects of.
I-Wei Chen proposes a kind of two-step method technique (CHEN I W, WANG X H.Sintering dense
nanocrystalline ceramics without final-stage grain growth[J].Nature,2000,404
(6774): 168-71.), with Y2O3To be sintered object, sintering temperature is risen into relatively high sintering temperature T1 first, in the sintering
At a temperature of sintered body achieve certain relative density, relatively low sintering temperature T2 is then cooled to rapidly, then at this
At a temperature of long-time heat preservation finally obtain the tiny Y of crystal grain until ceramic body densifies completely2O3Ceramic sintered bodies, it is brilliant
Grain size is 122nm.
With yttrium oxide (Y2O3) ceramics unlike, indium gallium zinc (IGZO) ceramics are a kind of multicomponent system material, object
Phase structure variation is more complicated, causes its sintering mechanism to have very big difference, and the sintering temperature of the two has very big difference.
Summary of the invention
In order at least solve one of above-mentioned technical problem of the existing technology, the invention discloses a kind of two steps
The method that sintering process prepares IGZO ceramic target, comprising:
Slurry preparation: In is quantified in proportion2O3、Ga2O3With tri- kinds of oxide powders of ZnO, with deionized water, diluent and
Binder mixing, is prepared into the IGZO slurry of high solids content；
Blank forming: IGZO sizing material forming is IGZO ceramic green body；
Base substrate degreasing: IGZO ceramic green body degreasing at 600~800 DEG C of temperature；
Blank sintering: the IGZO ceramic green body after degreasing is warming up to 1400~1500 DEG C of first step sintering temperature, so
Afterwards, 1320~1360 DEG C of second step sintering temperature are cooled to, keeps the temperature 8~14 hours under second step sintering temperature, sintering atmosphere
Including air, oxygen or argon gas.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, In2O3、Ga2O3With
The atomicity molar ratio of element In, Ga and Zn are 1:1:1 or 2:2:1 in ZnO.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, diluent include poly-
Acrylic compounds or polycarboxylic acid, binder include gum arabic, polyvinyl alcohol or acrylic resin.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, base substrate degreasing and base
Body sintering integratedization carries out.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, first step sintering temperature
The heating rate of degree is 2~5 DEG C/min.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target is sintered from the first step
The rate of temperature fall of temperature to second step sintering temperature is set as 8~12 DEG C/min.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, the work of blank forming
Skill includes slip casing by pressure technique, molding-isostatic pressing process.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, it is solid in IGZO slurry
Content is not less than 60%, by quality ratio.
The method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, oxide powder with
Deionized water, diluent and the binder ball milling mixing under subnormal ambient.
Further, the method that twice sintering process disclosed in some embodiments of the invention prepares IGZO ceramic target, negative pressure
The pressure of environment is not more than 9Pa.
Method disclosed by the embodiments of the present invention, mold is simple, and technological operation is easy, convenient for preparing the target of various sizes,
Green sintering is good, can prepare the tiny IGZO ceramic target of high density, low-resistivity, crystal grain, and relative density is reachable
99.5%, resistivity is down to 1.59m Ω cm, and down to 4.78 μm, reduced sintering temperature can reduce crystallite dimension accordingly
Production cost extends service life of equipment, is suitable for industrialized production.
Detailed description of the invention
Crystal grain distribution under IGZO ceramic target scanning electron microscope (SEM) photograph and BSED mode in Fig. 1 embodiment 1-3
Crystal grain distribution under IGZO ceramic target scanning electron microscope (SEM) photograph and BSED mode in Fig. 2 comparative example 1-3
Specific embodiment
Dedicated word " embodiment " herein, should not necessarily be construed as being better than as any embodiment illustrated by " exemplary " or
It is better than other embodiments.Testing performance index in this law embodiment, unless stated otherwise, using this field conventional methods.
It should be understood that it is to describe special embodiment that heretofore described term, which is only, it is not intended to limit disclosed by the invention
Content.
Unless otherwise stated, technical and scientific terms used herein has the common of the technical field of the invention
The normally understood identical meanings of technical staff.As other not specifically specified raw material, the reagent, test method in the present invention
The usually used raw material and reagent of those skilled in the art, and the experiment side generallyd use are referred both to technological means
Method and technological means.
Term used in the disclosure " basic " and " about " are for describing small fluctuation.It is less than for example, they can refer to
Or be equal to ± 5%, such as less than or equal to ± 2%, such as less than or equal to ± 1%, such as less than or equal to ± 0.5%, such as less than or
Equal to ± 0.2%, such as less than or equal to ± 0.1%, such as less than or equal to ± 0.05%.Concentration, amount and other numeric datas exist
It can indicate or present with range format herein.Such range format only uses for convenience and for the sake of brief, therefore Ying Ling
Work is construed to not only include the numerical value clearly enumerated as the boundary of the range, further includes include all independent within the scope of this
Numerical value or subrange.For example, the numberical range of " 1% to 5% " should be construed to include 1% to 5% clearly enumerating
Value, further includes independent values in the range shown and subrange.It therefore, include independent values in this numberical range, such as 2%,
3.5% and 4% and subrange, such as 1%~3%, 2%~4% and 3%~5%.This principle is equally applicable to only enumerate
The range of one numerical value.In addition, width or the feature regardless of the range, such explanation is all suitable for.Herein,
One step sintering temperature is labeled as T1, and second step sintering temperature is labeled as T2.
In the disclosure, including claims, all conjunctions, as "comprising", " comprising ", " having ", " having ",
" containing ", " being related to ", " receiving " etc. are understood to be open, that is, refer to " including but not limited to ".Only conjunction
" by ... constitute " and " by ... constitute " it is closing conjunction.
The present invention discloses in some embodiments, and the method that twice sintering process prepares IGZO ceramic target includes slurry system
Standby step, in proportion quantitative In2O3、Ga2O3With tri- kinds of oxide powders of ZnO, mixed with deionized water, diluent and binder,
It is prepared into the IGZO slurry of high solids content；In some embodiments, In2O3、Ga2O3With the ratio root of tri- kinds of oxide powders of ZnO
According to metallic atom required in ceramic target molar ratio determine, such as can set the atomicity molar ratio of In, Ga and Zn as
1:1:1 or 2:2:1.In some embodiments, In2O3、Ga2O3With tri- kinds of oxide powders of ZnO and deionized water, diluent and
Binder mixing, ball milling mixing obtain IGZO slurry；In some embodiments, ball milling carries out under negative pressure, for example, can set
The pressure of subnormal ambient is set no more than 9Pa.
In some embodiments, diluent uses polyacrylic or polycarboxylic acid, and binder uses gum arabic, gathers
Vinyl alcohol or acrylic resin.In some embodiments, the solid content of oxide powder in IGZO slurry is controlled, to control ball
Effect is ground, such as the solid content not less than 60% is conducive to the IGZO slurry to be suited the requirements.The solid content addressed herein is logical
Refer to the mass percent of oxide powder in the slurry.
In some embodiments, the method that twice sintering process prepares IGZO ceramic target includes blank forming step,
IGZO sizing material forming is IGZO ceramic green body.In some embodiments, the IGZO slurry obtained using slip casing by pressure technique at
Type injects in mold, such as in gypsum mold under certain raised pressure, and molding obtains green.In some embodiments
In, IGZO slurry is used and is first molded, then carries out isostatic pressing process, prepares green.
In some embodiments, the method that twice sintering process prepares IGZO ceramic target includes base substrate degreasing step,
Usual IGZO ceramic green body needs to carry out ungrease treatment at a certain temperature, for example, the skimming temp of some embodiments selection
Between 600~800 DEG C.
In some embodiments, the method that twice sintering process prepares IGZO ceramic target includes blank sintering step,
It is generally necessary to which the IGZO ceramic green body after degreasing is sintered at a higher temperature, ceramic target is obtained；In some embodiments
In, using two-step method process, target material blank body is warming up to higher first sintering temperature first, then cool the temperature to compared with
The second low sintering temperature, held for some time obtain ceramic target.In some embodiments, target material blank body is heated up first
To 1400~1500 DEG C of first step sintering temperature, then, 1320~1360 DEG C of second step sintering temperature are cooled to, are burnt in second step
8~14 hours are kept the temperature under junction temperature.Sintering process usually carries out in air, oxygen or argon atmosphere.In some embodiments,
Control is warming up to the heating rate of the first sintering temperature, to reach better sintering effect, for example, the liter of first step sintering temperature
When warm rate is 2~5 DEG C/min, it is more advantageous to obtain the tiny target of consistency high resistance and low resistance rate, grain particles.Some
In embodiment, control is cooled to the rate of temperature fall of the second sintering temperature from the first sintering temperature, to control sintering effect, such as
The rate of temperature fall of first step sintering temperature to second step sintering temperature is set as 8~12 DEG C/min, when, it is more advantageous to obtain densification
Spend the tiny target of high resistance and low resistance rate, grain particles.
In some embodiments, base substrate degreasing step and blank sintering step integration carry out.In some embodiments,
The skimming processes and two-step sintering process of IGZO green body carry out in degreasing sintered integrated normal pressure atmosphere sintering furnace, primary to complete to take off
Rouge and two-step sintering process.
Below in conjunction with specific embodiment, prepared by the implementation detail of the method for IGZO ceramic target into one to twice sintering process
Step description, and be compared with the result of the comparative example using a step sintering process, experimental results are referring to attached drawing 1-2.Figure
In, abscissa (Grain size, μm) indicating grain size, ordinate (Frequency, %) indicates the corresponding crystalline substance of crystallite dimension
Grain percentage composition.
Embodiment 1
The method that the present embodiment 1 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, rises to the with 3 DEG C/min heating rate
One 1400 DEG C of step sintering temperature, is then down to 1340 DEG C of second step sintering temperature with 10 DEG C/min rate of temperature fall, in the second sintering
At a temperature of keep the temperature 12 hours, sintering atmosphere is air.The relative density of obtained IGZO ceramic target is 99.5%, and resistivity is
2.31m Ω cm, average grain size are 4.73 μm.Grain morphology and particle diameter distribution are shown in Fig. 1 (b).(to data information in figure into
Row explanation.)
Embodiment 2
The method that the present embodiment 2 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, rises to the with 3 DEG C/min heating rate
One 1450 DEG C of step sintering temperature, is then down to 1340 DEG C of second step sintering temperature with 10 DEG C/min rate of temperature fall, in the second sintering
At a temperature of keep the temperature 12 hours, sintering atmosphere is air.
The relative density of obtained IGZO ceramic target is 99.2%, and resistivity is 1.78m Ω cm, average grain size
It is 5.81 μm.Grain morphology and particle diameter distribution are shown in Fig. 1 (a).
Embodiment 3
The method that the present embodiment 3 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, rises to the with 3 DEG C/min heating rate
One 1500 DEG C of step sintering temperature, is then down to 1340 DEG C of second step sintering temperature with 10 DEG C/min rate of temperature fall, in the second sintering
At a temperature of keep the temperature 12 hours, sintering atmosphere is air.
The relative density of obtained IGZO ceramic target is 99.1%, and resistivity is 1.59m Ω cm, average grain size
It is 6.56 μm.Grain morphology and particle diameter distribution are shown in Fig. 1 (c).
Comparative example 1
The method that this comparative example 1 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, burning is risen to 3 DEG C/min heating rate
1400 DEG C of junction temperature, 12 hours are kept the temperature at a sintering temperature, sintering atmosphere is air.
The relative density of obtained IGZO ceramic target is 97.6%, and resistivity is 3.38m Ω cm, average grain size
It is 10.32 μm.Grain morphology and particle diameter distribution are shown in Fig. 2 (c).
Comparative example 2
The method that this comparative example 2 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, burning is risen to 3 DEG C/min heating rate
1450 DEG C of junction temperature, 12 hours are kept the temperature at a sintering temperature, sintering atmosphere is air.
The relative density of obtained IGZO ceramic target is 97.8%, and resistivity is 2.92m Ω cm, average grain size
It is 12.08 μm.Grain morphology and particle diameter distribution are shown in Fig. 2 (b).
Comparative example 3
The method that this comparative example 3 prepares highdensity IGZO target includes:
Weigh 73.7g In respectively2O3Oxide powder, 49.75g Ga2O3Oxide powder and 43.21g ZnO aoxidize powder
Body；Polyacrylic acid 2.83g, gum arabic 0.5g, acrylamide 1.67g and deionized water 26.67g form premixed liquid；
Ball grinder is added in oxide powder and premixed liquid, the vacuum degree of ball grinder is evacuated to~9Pa, ball milling 48 hours,
Obtain the IGZO slurry that powder solid mass content is 60%；
Slurry is injected in gypsum mold, is shaped under the conditions of pressure is 0.2MPa, obtains IGZO ceramic green body；
IGZO ceramic green body is dry, it is put into degreasing sintered all-in-one oven later, burning is risen to 3 DEG C/min heating rate
1500 DEG C of junction temperature, 12 hours are kept the temperature at a sintering temperature, sintering atmosphere is air.
The relative density of obtained IGZO ceramic target is 98.7%, and resistivity is 2.27m Ω cm, average grain size
It is 12.96 μm.Grain morphology and particle diameter distribution are shown in Fig. 2 (a).
Relative to embodiment 1-3, the IGZO ceramic target contrast that comparative example 1-3 is obtained is small, and resistivity is high, crystal grain ruler
It is very little big.
Method disclosed by the embodiments of the present invention, mold is simple, and technological operation is easy, convenient for preparing the target of various sizes,
Green sintering is good, can prepare the tiny IGZO ceramic target of high density, low-resistivity, crystal grain, and relative density is reachable
99.5%, resistivity is down to 1.59m Ω cm, and down to 4.78 μm, reduced sintering temperature can reduce crystallite dimension accordingly
Production cost extends service life of equipment, is suitable for industrialized production.
Technical detail disclosed in technical solution and embodiment disclosed by the invention, is merely illustrative structure of the invention
Think, and does not constitute a limitation of the invention, it is all not have a creative change to what technical detail disclosed by the invention was made, it is right
Presently disclosed techniques scheme is applied in combination, all with present invention inventive concept having the same, all in the claims in the present invention
Protection scope within.
Claims (10)
1. the method that twice sintering process prepares IGZO ceramic target characterized by comprising
Slurry preparation: In is quantified in proportion2O3、Ga2O3With tri- kinds of oxide powders of ZnO, with deionized water, diluent and binder
Mixing, is prepared into the IGZO slurry of high solids content；
Blank forming: IGZO sizing material forming is IGZO ceramic green body；
Base substrate degreasing: IGZO ceramic green body degreasing at 600~800 DEG C of temperature；
Blank sintering: being warming up to 1400~1500 DEG C of first step sintering temperature for the IGZO ceramic green body after degreasing, then, drop
Temperature keeps the temperature 8~14 hours under second step sintering temperature to 1320~1360 DEG C of second step sintering temperature, and sintering atmosphere includes sky
Gas, oxygen or argon gas.
2. the method according to claim 1, wherein In2O3、Ga2O3With the atom of element In, Ga and Zn in ZnO
Number molar ratio is 1:1:1 or 2:2:1.
3. the method according to claim 1, wherein the diluent includes polyacrylic or polycarboxylic acid,
The binder includes gum arabic, polyvinyl alcohol or acrylic resin.
4. the method according to claim 1, wherein the base substrate degreasing and the blank sintering integration into
Row.
5. the method according to claim 1, wherein the heating rate of the first step sintering temperature is 2~5
℃/min。
6. the method according to claim 1, wherein from first step sintering temperature to the drop of second step sintering temperature
Warm rate is set as 8~12 DEG C/min.
7. the method according to claim 1, wherein the technique of the blank forming include slip casing by pressure technique,
Molding-isostatic pressing process.
8. the method according to claim 1, wherein solid content is not less than 60% in the IGZO slurry, with matter
Amount is than meter.
9. the method according to claim 1, wherein the oxide powder and deionized water, diluent and viscous
Tie agent ball milling mixing under subnormal ambient.
10. according to the method described in claim 9, it is characterized in that, the pressure of the subnormal ambient is not more than 9Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910351001.3A CN110002853A (en) | 2019-04-28 | 2019-04-28 | The method that twice sintering process prepares IGZO ceramic target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910351001.3A CN110002853A (en) | 2019-04-28 | 2019-04-28 | The method that twice sintering process prepares IGZO ceramic target |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110002853A true CN110002853A (en) | 2019-07-12 |
Family
ID=67174828
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910351001.3A Pending CN110002853A (en) | 2019-04-28 | 2019-04-28 | The method that twice sintering process prepares IGZO ceramic target |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110002853A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111394706A (en) * | 2020-03-06 | 2020-07-10 | 郑州大学 | Preparation method of ITO ceramic target material with controllable grain size |
| CN113354393A (en) * | 2021-07-13 | 2021-09-07 | 江苏迪丞光电材料有限公司 | Preparation method for preparing IGZO (indium gallium zinc oxide) rotary target material by gel casting |
| CN113354407A (en) * | 2021-07-14 | 2021-09-07 | 郑州大学 | Variable-temperature fast-sintering process of aluminum-doped zinc oxide target material |
| CN115894010A (en) * | 2022-11-28 | 2023-04-04 | 郑州大学 | Tubular indium gallium zinc (In) oxide 2 Ga 2 ZnO 7 ) Preparation method of fine-grain high-density crack-free target material |
| CN115925416A (en) * | 2023-01-17 | 2023-04-07 | 丰联科光电(洛阳)股份有限公司 | Preparation method of tantalum oxide target material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101578245A (en) * | 2007-08-06 | 2009-11-11 | 三井金属矿业株式会社 | ITO sintered body and ITO sputtering target |
| CN101622208A (en) * | 2007-08-06 | 2010-01-06 | 三井金属矿业株式会社 | ITO sintered body and ITO sputtering target |
| CN101845614A (en) * | 2010-05-07 | 2010-09-29 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-based sputtering target material |
| US20120279856A1 (en) * | 2009-10-15 | 2012-11-08 | Medvedovski Eugene | Tin Oxide Ceramic Sputtering Target and Method of Producing It |
| CN107522483A (en) * | 2017-06-26 | 2017-12-29 | 广西新未来信息产业股份有限公司 | A kind of preparation method of AZO targets |
| CN109665834A (en) * | 2019-03-01 | 2019-04-23 | 郑州大学 | The controllable indium gallium zinc target and preparation method thereof of phase composition |
-
2019
- 2019-04-28 CN CN201910351001.3A patent/CN110002853A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101578245A (en) * | 2007-08-06 | 2009-11-11 | 三井金属矿业株式会社 | ITO sintered body and ITO sputtering target |
| CN101622208A (en) * | 2007-08-06 | 2010-01-06 | 三井金属矿业株式会社 | ITO sintered body and ITO sputtering target |
| US20120279856A1 (en) * | 2009-10-15 | 2012-11-08 | Medvedovski Eugene | Tin Oxide Ceramic Sputtering Target and Method of Producing It |
| CN101845614A (en) * | 2010-05-07 | 2010-09-29 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-based sputtering target material |
| CN107522483A (en) * | 2017-06-26 | 2017-12-29 | 广西新未来信息产业股份有限公司 | A kind of preparation method of AZO targets |
| CN109665834A (en) * | 2019-03-01 | 2019-04-23 | 郑州大学 | The controllable indium gallium zinc target and preparation method thereof of phase composition |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111394706A (en) * | 2020-03-06 | 2020-07-10 | 郑州大学 | Preparation method of ITO ceramic target material with controllable grain size |
| CN113354393A (en) * | 2021-07-13 | 2021-09-07 | 江苏迪丞光电材料有限公司 | Preparation method for preparing IGZO (indium gallium zinc oxide) rotary target material by gel casting |
| CN113354407A (en) * | 2021-07-14 | 2021-09-07 | 郑州大学 | Variable-temperature fast-sintering process of aluminum-doped zinc oxide target material |
| CN115894010A (en) * | 2022-11-28 | 2023-04-04 | 郑州大学 | Tubular indium gallium zinc (In) oxide 2 Ga 2 ZnO 7 ) Preparation method of fine-grain high-density crack-free target material |
| CN115925416A (en) * | 2023-01-17 | 2023-04-07 | 丰联科光电(洛阳)股份有限公司 | Preparation method of tantalum oxide target material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110002853A (en) | The method that twice sintering process prepares IGZO ceramic target | |
| CN109665834B (en) | Phase-composition-controllable indium gallium zinc oxide target and preparation method thereof | |
| CN101268211B (en) | Sputtering target, transparent conductive film, and transparent electrode | |
| CN108706965B (en) | A kind of short flow process of indium gallium zinc tubular target | |
| CN109133911A (en) | A kind of method of ultra-low temperature cold sintering zno-based ceramics | |
| CN108218419B (en) | Preparation method of indium tin oxide ceramic target material | |
| JPH02149459A (en) | Oxide sintered body, production and use thereof | |
| CN107130217B (en) | A kind of inexpensive, high-density ITO targe material preparation method | |
| US20130206590A1 (en) | Manufacture of High Density Indium Tin Oxide (ITO) Sputtering Target | |
| JP2021138595A (en) | Method for preparing ito ceramic target material with controllable grain size | |
| CN113149613B (en) | ITWO target material and preparation method thereof | |
| Choi et al. | Microwave dielectric properties and sintering behaviors of scheelite compound CaMoO4 | |
| WO2023093025A1 (en) | Hexagonal ferrite thick film with high remanence ratio and low porosity, and preparation method therefor and application thereof | |
| CN115745573A (en) | Preparation method of fine-grain IZO target material | |
| Wang et al. | Synthesis of doped ZnO nanopowders in alcohol–water solvent for varistors applications | |
| CN106145927A (en) | A kind of manufacture method of gallium doped zinc oxide target | |
| Liu et al. | Preparation and properties of 0.79 ZnAl2O4-0.21 TiO2 microwave dielectric ceramics via digital light processing | |
| CN101343729A (en) | Method for preparing lanthanum nickelate conductive metallic oxide nano-film | |
| CN112390637A (en) | High dielectric constant microwave ferrite material without yttrium formula and preparation method and device thereof | |
| CN112479707A (en) | Cold isostatic pressing preparation method of tungsten oxide-based ceramic target material | |
| CN106145928A (en) | A kind of manufacture method of tubular ZnO electronic ceramics | |
| CN109305811A (en) | A kind of microwave-assisted zinc oxide ceramics sintering method | |
| KR101436468B1 (en) | High strength Aluminum Nitride ceramics and the method of low temperature sintering thereof | |
| CN116813324B (en) | Composite ferrite material and preparation method thereof | |
| CN113072380B (en) | Lanthanum cobaltate ceramic target material for PLD, and preparation method and application thereof |
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: 20190712 |
|
| RJ01 | Rejection of invention patent application after publication |