CN108516820A - A kind of short route sintering process of tin indium oxide target material - Google Patents
A kind of short route sintering process of tin indium oxide target material Download PDFInfo
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- CN108516820A CN108516820A CN201810722380.8A CN201810722380A CN108516820A CN 108516820 A CN108516820 A CN 108516820A CN 201810722380 A CN201810722380 A CN 201810722380A CN 108516820 A CN108516820 A CN 108516820A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The present invention provides a kind of short route sintering process of tin indium oxide target material, including：Indium oxide powder and tin oxide powder are mixed, mixed powder is obtained；Water, forming agent, dispersant and antifoaming agent are added into mixed powder, is mixed to get slurry；Slurry is used into slurry moulding by casting, obtains tin indium oxide biscuit；The progress integration of tin indium oxide biscuit is degreasing sintered, obtains tin indium oxide target material.Using degreasing sintered integral process, sintering temperature reduces, sintering time greatly shortens, it is only necessary to can be completed within 5 days from degreasing sintered and cooling entire sintering process.It realizes fast activating sintering, crystal grain is inhibited to grow up, ensure that the crystal grain of the tin indium oxide target material prepared is tiny, uniform, mean grain size is 4~5 μm；Consistency is high, and relative density has higher strength character, bending strength >=200MPa up to 99.7% or more.
Description
Technical field
The application belongs to metal oxide target material technical field, and in particular to a kind of short route burning of tin indium oxide target material
Knot technique.
Background technology
ITO, i.e. tin-doped indium oxide (Indium Tin Oxide), or be tin indium oxide, it is a kind of n-type semiconductor material
Material, ITO target is the raw material that magnetron sputtering prepares transparent conductive film.This transparent conductive film is to visible light transmittance>
85%, infrared reflectivity>90%, and good conductivity, there are excellent chemical stability, thermal stability and etching property, is a kind of
The very unique thin-film material of purposes, is widely used in the fields such as flat-panel monitor, non-browning glass, thin-film solar cells.
The preparation method of ITO target has pressure sintering, hot isostatic pressing method and sintering process.Pressure sintering and hot isostatic pressing method are deposited because of it
It is gradually eliminated the defects of die size is controlled, oxygen-free atmosphere condition easily causes oxygen loss problem.Currently a popular technique master
If oxygen atmosphere sintering method, especially low pressure or normobaric oxygen atmosphere sintering process are successfully developed by more companies, such as Japan three
There is lot of advantages, danger that is simple for process, easy to operate, avoiding high pressure oxygen to close for well and Kuang companies, normal pressure-sintered technique
Key, which is normal pressure or non-pressure sintering technology effect, so that target blankss is densified completely.However the sintering process of these companies exploitation is always
Individually carried out using degreasing and sintering circuit, degreasing finishes be cooled to room temperature after, then move to sintering furnace again, heating sintering.Cause
Biscuit is cold-pressed after completing degreasing process for ITO target, blank strength is very low, slightly shakes, i.e., can cause fracture or crackle, this
Defect once occurs, since ITO sintering densifications poor performance will remain in final target.And normal pressure in the prior art
(it is resistant to 1kg/cm2) high concentration high throughput oxygen atmosphere sintering technique, oxygen flow in 30L/min or more, high temperature up to 1600 DEG C,
Soaking time is long, is 12 hours, as a result causes that target crystalline grains are coarse, intensity is low and the waste of oxygen, is not real
Non-pressure sintering technology in meaning, thus sintering equipment design is excessively complicated, independent degreasing and sintering time are long, it usually needs
8 days or more or even 10 days, the serious waste of electric power, oxygen and manpower is caused, the production cost is very high for final products.
Invention content
At least for one of problems described above, the present disclosure provides a kind of sintering of the short route of tin indium oxide target material
Technique, the technique is degreasing sintered by the progress integration of tin indium oxide biscuit, obtains tin indium oxide target material.
The short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, integration are degreasing sintered specific
Including in air atmosphere, degreasing at elevated temperatures；Then it in oxygen atmosphere, is sintered at elevated temperatures；It is cooling
To room temperature, tin indium oxide target material is obtained.
Further, the short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, integrated degreasing
Sintering specifically includes, and 600~800 DEG C are warming up to 0.1~3 DEG C/min heating rates under air atmosphere, carries out degreasing, keeps 36
~48 hours；Oxygen is then passed to, 4 hours are kept the temperature at 800 DEG C, then 1500 are warming up to 1~5 DEG C/min heating rates~
It 1600 DEG C, is sintered, keeps the temperature 4~10 hours；Stopping is passed through oxygen, is cooled to 200 DEG C with 1~3 DEG C/min cooling rates, so
Cooled to room temperature afterwards obtains tin indium oxide target material.
Further, the short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, it is de- in integration
In fat sintering process, the flow set that is passed through of oxygen is 1~20L/min.
On the other hand, some embodiments of the invention also disclose in the short route sintering process of tin indium oxide target material, oxidation
The preparation method of indium tin biscuit, specifically comprises the following steps：
Indium oxide powder and tin oxide powder are mixed, mixed powder is obtained；
Water, forming agent, dispersant and antifoaming agent are added into mixed powder, mixing obtains slurry；
Slurry is used into slurry moulding by casting, obtains tin indium oxide biscuit.
Further, the short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, tin indium oxide element
In base preparation process, the mass content of mixed powder is arranged between 50~80% in slurry, phosphoric acid setting 120~
Between 3800mpa.s, pH value is arranged between 7~9.
It is prepared by the short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, tin indium oxide biscuit
Cheng Zhong, indium oxide powder and the mass ratio of the tin oxide powder are set as 9:1.
The short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, the preparation of tin indium oxide biscuit
In the process, slurry moulding by casting specifically includes：Slurry is injected by pump pressure in gypsum mold cavity, by standing, demoulding, is done
It is dry, obtain tin indium oxide biscuit.
Further, the short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, tin indium oxide element
In the preparation process of base, the grouting pressure of slurry moulding by casting is arranged between 0.1~0.4MPa, and the setting of slip casting dwell time exists
Between 5~20 minutes.
The short route sintering process of tin indium oxide target material disclosed in some embodiments of the invention, the preparation of tin indium oxide biscuit
In the process, the relative density of tin indium oxide biscuit is arranged between 58~72%.
The short route sintering process of tin indium oxide target material disclosed by the embodiments of the present invention, using degreasing sintered integrated chemical industry
Skill, sintering temperature reduces, sintering time greatly shortens, it is only necessary to can be completed within 5 days from degreasing sintered and cooling entire sintering
Process.It realizes fast activating sintering, crystal grain is inhibited to grow up, ensure that the crystal grain of the ITO target prepared is tiny, uniform, average crystal grain
Degree is 4~5 μm；Consistency is high, and relative density has a higher strength character up to 99.7% or more, and bending strength >=
200Mpa。
Description of the drawings
Fig. 1 present invention discloses tin indium oxide target material short route sintering process flow chart
1 mixed powder scanning electron microscope (SEM) photograph of Fig. 2 embodiment of the present invention
1 tin indium oxide target material scanning electron microscope (SEM) photograph of Fig. 3 embodiment of the present invention
1 tin indium oxide target material Fracture scan electron microscope of Fig. 4 embodiment of the present invention
Specific implementation mode
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 heretofore described term is only to describe special embodiment, being 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 in the present invention, reagent, test method
The experiment side of the usually used raw material and reagent and generally use of those skilled in the art is referred both to technological means
Method and technological means；The chronomere that h is indicated is hour, and the chronomere that min is indicated is minute, the mixing speed that rpm is indicated
Unit be rev/min；Slurry liquid refers to the liquid composition for forming slurry with mixed powder, using water as main component,
Added with other auxiliary agents, such as forming agent, dispersant, antifoaming agent, the content of auxiliary agent is contained with its mass percent in slurry
Amount indicates；Integration is degreasing sintered to be further referred to as degreasing sintered integration, typically refer to the skimming processes of target biscuit with
Sintering process is carried out continuously, i.e., is directly carried out at further raised temperature after skimming processes at elevated temperatures
Sintering process.
Term " basic " and " about " used in the disclosure is for describing small fluctuation.For example, they can refer to being less than
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 include not only 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 " 1~5% " should be construed to include 1% to 5% the value clearly enumerated,
Further include independent values in the range shown and subrange.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, the width regardless of the range or the feature, such explanation is all suitable for.
In the disclosure, including claims, all conjunctions, as "comprising", " comprising ", " carrying ", " 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 " consist of " should be closing or semiclosed conjunction.
Below in conjunction with specific implementation mode and short flow process flow chart disclosed by the invention, Fig. 1 is seen, to the present invention
Disclosed preparation method further illustrates, so that those skilled in the art implement.
In some embodiments, the short route sintering process of tin indium oxide target material is carried out according to following steps flow：
S1, indium oxide powder and tin oxide powder are mixed, obtains mixed powder；
S2, water, forming agent, dispersant and antifoaming agent are added into mixed powder, mix 2~6 hours, obtains slurry；
S3, slurry is used into slurry moulding by casting, obtains tin indium oxide biscuit；
S4, the progress integration of tin indium oxide biscuit are degreasing sintered, obtain tin indium oxide target material.
In some embodiments, the present invention discloses the indium oxide powder of use and tin oxide powder material uses common city
Sell product, you can be made by the either method in acid system, electrolysis, hydrothermal synthesis and physical evaporation method, it is generally the case that oxygen
Changing the pattern of indium powder and tin oxide powder can also be not limited, i.e., the pattern of powder can be powdered, spherical, piece shape or
It is rodlike etc..In some embodiments, by indium oxide powder and tin oxide powder, ball milling mixing, when mixing, add in ball milling barrel
Enter mill ball and pure water, ratio of grinding media to material selection 4:1~2:1；Large and small ball mass ratio selection 3:1~2:Between 1；Large and small bulb diameter point
It Xuan Ze not 3~10mm and 0.5~1.6mm.
In some embodiments, in slurry preparation process, it is polyvinyl alcohol to mix the forming agent being added in powder,
Mass content in slurry is arranged between 1~2%, and dispersant is ammonium polyacrylate, and the mass content setting in slurry exists
Between 0.1~0.2%, antifoaming agent is polyethers, and the mass content in slurry is arranged between 0.1~0.2%.In some realities
It applies in mode, the mass content of mixed powder is arranged between 50~80% in slurry.
In some embodiments, the method for slurry being used slip casing by pressure, is injected into the cavity of gypsum mold, stands
After a period of time, mold is sloughed, obtains tin indium oxide biscuit, biscuit is placed in climatic chamber dry.
Usual slurry casting process parameters, such as solid concentration, phosphoric acid, grouting pressure are to forming of green body and most last phase
To density important.Usual solid concentration is high, is conducive to obtain high biscuit density, during reducing follow-up sintering,
The various sintering defects caused by deformation is excessive, such as warpage, fracture, density is low, allowance is big.However, solid concentration is too high
The control of phosphoric acid can be influenced, phosphoric acid is too high or too low can to make mouldability be deteriorated, as more preferred embodiment,
Select relatively mild solid concentration and viscosity number.In addition, grouting pressure is higher, can make slip casting it is rapid uniformly and can reduce because
Density inhomogeneity phenomenon caused by part quickly solidifies, but gypsum mold carrying is limited, can only generally bear 6kg/cm2The limit
Pressure.As more preferred embodiment, the solid concentration of slurry controls between 50~80%, more preferably embodiment
In, the solid content of slurry controls between 60~70%.As more preferred embodiment, phosphoric acid control 120~
3800mpa.s, more preferably in embodiment, phosphoric acid controls between 200~1000mpa.s, further preferred
In embodiment, phosphoric acid controls between 300~700mpa.s, can also be preferably between 400~600mpa.s.As
More preferred embodiment, the pH value of slurry is arranged between 7~9, or sets the arbitrary value in the section, such as 7.4,7.6,
7.8,8.0,8.2,8.4 etc..As optional embodiment, the grouting pressure of slurry cast is arranged between 0.1~0.4MPa, compared with
In preferred embodiment, to be arranged between 0.2~0.3MPa.As more preferred embodiment, the slip casting dwell time sets
It sets between 5~20 minutes, is more highly preferred between 6~10 minutes.The solid phase that the present invention addresses in disclosing, typically refers in slurry
Powder component, i.e. mixed powder, including indium oxide powder and tin oxide powder.
In some embodiments, slurry casting biscuit is neatly positioned on trolley, trolley is pushed into sintering furnace, i.e.,
It can implement degreasing sintered auto-programming.Degreasing sintered is the critical process for preparing high quality ITO target, the ginseng that each section of process curve
Number is crucial, such as heating, degreasing, sintering, heat preservation, cooling and logical oxygen parameter etc., interrelated between parameter and shadow
It rings, mistake or deviation occurs in a parameter, i.e., can cause the failure of sintering.Degreasing heating rate is too fast, it is easy to cause biscuit
Interior forming agent fierceness volatilization, expansion, which is overflowed, causes the fracture of biscuit body or underbead crack, once being formed fracture or underbead crack, can be tight
It is difficult to avoid that ghost image, which rings subsequent sintering process, sintered density meeting degradation, and sintering crack and shrinks phenomenon of rupture,；So
And degreasing heating rate can extend the sintering period slowly excessively, reduce sintering efficiency, improve manufacturing cost.As more preferred implementation side
Formula, degreasing heating rate is arranged between 0.1~3 DEG C/min, in highly preferred embodiment, is arranged in 0.5~2 DEG C/min
Between.Skimming temp is too low, is unable to that degreasing is totally thorough, and the remnants of any binder can seriously affect follow-up sintering process,
Remaining binders continue volatilization and can induce green body underbead crack, however skimming temp is too high, can cause to be pre-sintered phenomenon too early
Occur, biscuit sintering activity is made to substantially reduce, usual ITO target ceramics are difficult sintering, are sintered the decline of driving force, are caused final
Sintering process be difficult to realize be densified completely.In some embodiments, degreasing maximum temperature setting 600~800 DEG C it
Between；In other embodiments, degreasing maximum temperature is arranged between 700~800 DEG C, in some other embodiment,
Degreasing maximum temperature is arranged between 750~800 DEG C.It is not significant effects factor to be sintered heating rate, can be selected quickly
Heating, such as some more preferred heating rates are 1~5 DEG C/min, are more highly preferred to 2~4 DEG C/min.Implementation disclosed herein
Example the result shows that, being sintered maximum temperature and soaking time has sintering effect an even more important influence, and sintering temperature improves can be with
Sintered density is improved, but the volatilization of target can be accelerated, because ITO belongs to the material of highly volatile, in addition high-temperature can cause gold
Belong to being precipitated again for tin, seriously affect the internal organizational structure of ITO target, then follow-up magnetron sputtering membrane process is generated serious
It influences.Sintering temperature is very sensitive to the density and microstructure of target, and temperature is slightly lower, i.e., can cause underburnt, sintered density is not
Enough, porosity has detrimental effects to follow-up sputter coating.Maximum temperature soaking time has similar influence, and soaking time is too
Short, density is not achieved；Soaking time is too long, is easy burning, coarse grains, target embrittlement is serious, and subsequent back of the body target welding connects and splashes
Target phenomenon of rupture is susceptible to during penetrating plated film.Due to ITO highly volatiles decompose, in sintering process the presence of oxygen become
Inevitable, this technique overcomes the obstacle of high pressure and high flow capacity oxygen, operates using entirely without the logical oxygen under pressure state, not only obtains
The ITO target of high quality, and safe operation were obtained, the various dangerous hidden danger of high pressure-temperature oxygen are avoided.It is more excellent at some
In the embodiment of choosing, sintering temperature is arranged between 1500~1600 DEG C, and in other embodiment, sintering temperature is set
It sets between 1540~1580 DEG C；In some more preferred embodiment, soaking time was arranged between 4~10 hours,
It is more highly preferred between 5~8 hours, further preferably between 6~7 hours.Oxygen flow is too low in sintering process, it is difficult to press down
The decomposition of ITO processed, the excessively high pressure that can increase process equipment manipulation of flow, and expensive gas is wasted, increase production cost.
In some embodiments, oxygen flow is preferably provided between 1~20L/min in sintering process, more preferably embodiment
In, oxygen flow is arranged between 5~15L/min, further preferably between 8~12L/min.In some embodiments,
In degreasing sintered integrated process, temperature changing process includes multiple stages, for example, in degreasing temperature-rise period, it can be most
Multiple step-up temperature sections are set before high skimming temp, and temperature is kept for the different time in different calefactive interzones,
To reach more preferably degreasing effect, for example, can be set between maximum sintering temperature more in being sintered temperature-rise period
A step-up temperature section, temperature is kept for the different time in different calefactive interzones, and sintering process is made to reach more preferably
Sintering is as a result, equally, in temperature-fall period, be also provided with different cooling sections, rationally to control cooling rate, to temperature change
The multi-phase containment of change process is arranged, and is conducive to the density and intensity that control grain size and target in tin indium oxide target material.
The short route sintering process of tin indium oxide target material disclosed by the embodiments of the present invention, using degreasing sintered integrated chemical industry
Skill, sintering temperature reduces, sintering time greatly shortens, it is only necessary to the entire sintering from degreasing to sintering cooling can be completed within 5 days
Process.Realize fast activating sintering, it is suppressed that crystal grain is grown up, and ensure that the crystal grain of the ITO target of preparation is tiny, uniform, is put down
Equal grain size is 4~5 μm；Consistency is high, and relative density has higher strength character, bending strength up to 99.7% or more
≥200MPa。
In order to better illustrate the content of present invention, concrete details is given in specific embodiment below.This field
It will be appreciated by the skilled person that without certain details, the present invention can equally be implemented.In embodiment, for this field skill
Certain methods, means, instrument, equipment, raw material composition, molecular structure etc. known to art personnel are not described in detail, in order to convex
Show the purport of the present invention.
Embodiment 1
In the present embodiment 1, the short route preparation process of tin indium oxide target material, including：
By 9kg indium oxide powders and 1kg stannic oxide powder ball milling mixings, 10kg mixed powders are obtained；Wherein, when ball milling,
Ratio of grinding media to material selection 3:1, large and small ball mass ratio selection 2:1, large and small bulb diameter selects 3mm and 0.5mm respectively；
Water, forming agent, dispersant and antifoaming agent are added into mixed powder, continues ball milling mixing 4 hours, obtains slurry；
Wherein, forming agent is polyvinyl alcohol, mass content 1%；Dispersant is ammonium polyacrylate, mass content 0.1%；Disappear
Infusion is polyethers antifoaming agent, and mass content 0.1%, the mass percent of mixed powder is 62% in gained slurry；
Gained slurry is sprayed by pump pressure in gypsum mold, grouting pressure is set as 0.3MPa, and the slip casting dwell time 6 divides
Clock stands 6 minutes, sloughs gypsum grinding tool, obtain moist biscuit, then biscuit is placed in climatic chamber, keeps temperature 20
DEG C, humidity 55% obtains biscuit until being completely dried, wherein the relative density of biscuit is 58%.
Biscuit is sent into electrical heating sintering furnace, 800 DEG C of degreasings, degreasing period are warming up to 1 DEG C/min under air atmosphere
72 hours, oxygen is then passed through with the flow of 10L/min and is warming up to 1540 DEG C with 3 DEG C/min, 6 hours is kept the temperature, stops being passed through
Oxygen is simultaneously cooled to 200 DEG C with 2 DEG C/min, is come out of the stove after cooled to room temperature to get to sintered body；Wherein, oxygen is pure
Degree is 99.5%, and the relative pressure of oxygen remains 0, i.e. atmospheric pressure state in whole sintering process.
In the present embodiment 1, it further will heat up and be set as multiple temperature stages with temperature-fall period, it is degreasing sintered to optimize
The technique effect of integrated process.Wherein, skimming processes include six stages of serial number 1~6, and sintering process includes serial number 7
With 8 two stages, temperature-fall period includes seven stages of serial number 9~15, the temperature setting in each stage, the retention time,
Heating rate and oxygen flux setting are shown in Table 1, and oxygen flux zero, expression atmosphere is air.
1 degreasing sintered process condition list of table
The relative density that the tin indium oxide target material of the present embodiment 1 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
In the present embodiment 1, the mixed powder stereoscan photograph that indium oxide powder and tin oxide powder are mixed to get is shown in figure
2, the stereoscan photograph of tin indium oxide target material is shown in that Fig. 3, the stereoscan photograph of tin indium oxide target material section are shown in Fig. 4.
Embodiment 2
In the present embodiment 2, with embodiment 1, wherein sintering temperature is set as the short route sintering process of tin indium oxide target material
1580 DEG C, the oxygen flux of sintering stage is 5L/min, and the sintered heat insulating time is set as 10 hours.
The relative density that the tin indium oxide target material of the present embodiment 2 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
Embodiment 3
In the present embodiment 3, with embodiment 1, wherein sintering temperature is set as the short route sintering process of tin indium oxide target material
1560 DEG C, the sintered heat insulating time is set as 10 hours.
The relative density that the tin indium oxide target material of the present embodiment 3 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
Comparative example 1
In this comparative example 1, with embodiment 1, wherein sintering temperature is set as the short stream sintering process of tin indium oxide target material
1460 DEG C, the oxygen flux of sintering stage is set as 2L/min, and the sintered heat insulating time is set as 10 hours.
The relative density that the tin indium oxide target material of this comparative example 1 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
Comparative example 2
In this comparative example 2, tin indium oxide target material short route sintering process is set as with embodiment 1, wherein sintering temperature
1480 DEG C, the oxygen flux of sintering stage is set as 2L/min, and the sintered heat insulating time is set as 10 hours.
The relative density that the tin indium oxide target material of this comparative example 2 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
Comparative example 3
In this comparative example 3, with embodiment 1, wherein sintering temperature is set as the short route sintering process of tin indium oxide target material
1620 DEG C, the oxygen flux of sintering stage is set as 5L/min, and the sintered heat insulating time is set as 10 hours.
The relative density that the tin indium oxide target material of this comparative example 3 is measured with Archimedes's drainage, uses scanning electron microscopy
Mirror (SEM) measures crystallite dimension and as a result sees list 2 with its bending strength of stretching test machine determination.
2 Examples 1 to 3 of table, 1~3 the performance test results list of comparative example
The short route sintering process of tin indium oxide target material disclosed by the embodiments of the present invention, using degreasing sintered integrated chemical industry
Skill, sintering temperature reduces, sintering time greatly shortens, it is only necessary to can be completed within 5 days from degreasing sintered and cooling entire sintering
Process, oxygen consumption decline to a great extent, and yield rate improves 20% or more.Realizing fast activating sintering, it is suppressed that crystal grain is grown up,
It ensure that the crystal grain of the tin indium oxide target material of preparation is tiny, uniform, mean grain size is 4~5 μm；Consistency is high, relative density
Up to 99.7% or more, there is higher strength character, bending strength >=200MPa.
Technical detail disclosed in technical solution and embodiment disclosed by the invention is merely illustrative the structure of the present invention
Think, does not constitute limitation of the invention, it is every 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 domain within.
Claims (10)
1. a kind of short route sintering process of tin indium oxide target material, which is characterized in that it is de- that tin indium oxide biscuit is carried out integration
Fat is sintered, and obtains tin indium oxide target material.
2. the short route sintering process of tin indium oxide target material according to claim 1, which is characterized in that the integration is de-
Fat sintering specifically includes：
In air atmosphere, degreasing at elevated temperatures；Then it in oxygen atmosphere, is sintered at elevated temperatures；It is cooling
To room temperature, tin indium oxide target material is obtained.
3. the short route sintering process of tin indium oxide target material according to claim 2, which is characterized in that the integration is de-
Fat sintering specifically includes：
600~800 DEG C are warming up to 0.1~3 DEG C/min heating rates under air atmosphere, carries out degreasing, is kept for 36~48 hours；
Oxygen is then passed to, 4 hours are kept the temperature at 800 DEG C, is then warming up to 1500~1600 DEG C with 1~5 DEG C/min heating rates, is carried out
Sintering keeps the temperature 4~10 hours；Stopping is passed through oxygen, is cooled to 200 DEG C with 1~3 DEG C/min cooling rates, then natural cooling
To room temperature.
4. the short route sintering process of tin indium oxide target material according to claim 3, which is characterized in that the oxygen leads to
Inbound traffics are set as 1~20L/min.
5. the short route sintering process of tin indium oxide target material according to claim 1, which is characterized in that the tin indium oxide
The preparation of biscuit includes the following steps：
Indium oxide powder and tin oxide powder are mixed, mixed powder is obtained；
Water, forming agent, dispersant and antifoaming agent are added into mixed powder, mixing obtains slurry；
Slurry is used into slurry moulding by casting, obtains tin indium oxide biscuit.
6. the short route sintering process of tin indium oxide target material according to claim 5, which is characterized in that mixed in the slurry
The mass content for closing powder is arranged between 50~80%, and phosphoric acid is arranged between 120~3800mpa.s, pH value setting
Between 7~9.
7. the short route sintering process of tin indium oxide target material according to claim 5, which is characterized in that the indium oxide powder
The mass ratio of body and the tin oxide powder is set as 9:1.
8. the short route sintering process of tin indium oxide target material according to claim 5, which is characterized in that the slurry cast
Molding specifically includes：Slurry is injected by pump pressure in gypsum mold cavity, by standing, demoulding, drying, obtains tin indium oxide
Biscuit.
9. the short route sintering process of tin indium oxide target material according to claim 5, which is characterized in that the slurry cast
Molding grouting pressure is arranged between 0.1~0.4MPa, and the slip casting dwell time was arranged between 5~20 minutes.
10. the short route sintering process of tin indium oxide target material according to claim 5, which is characterized in that the indium oxide
The relative density of tin biscuit is arranged between 58%~72%.
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| CN112592172A (en) * | 2020-12-15 | 2021-04-02 | 株洲火炬安泰新材料有限公司 | Method for preparing ITO sintered body |
| CN113354407A (en) * | 2021-07-14 | 2021-09-07 | 郑州大学 | Variable-temperature fast-sintering process of aluminum-doped zinc oxide target material |
| CN113788669A (en) * | 2021-10-20 | 2021-12-14 | 南宁西桂微电子有限公司 | Preparation method of ITO sputtering target material |
| CN115894009A (en) * | 2022-11-14 | 2023-04-04 | 先导薄膜材料（广东）有限公司 | Rapid sintering and degreasing method for ITO (indium tin oxide) planar target and supporting plate used by rapid sintering and degreasing method |
| CN116375463A (en) * | 2023-04-17 | 2023-07-04 | 湘潭大学 | Indium tin cerium oxide target material and preparation method and application thereof |
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| CN113354407A (en) * | 2021-07-14 | 2021-09-07 | 郑州大学 | Variable-temperature fast-sintering process of aluminum-doped zinc oxide target material |
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| CN116444263B (en) * | 2023-03-15 | 2024-02-27 | 先导薄膜材料(安徽)有限公司 | Sintering process of indium tin oxide target |
| CN116375463A (en) * | 2023-04-17 | 2023-07-04 | 湘潭大学 | Indium tin cerium oxide target material and preparation method and application thereof |
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