CN107010654A - A kind of preparation method of single dispersing gallium oxide powder and its high density ceramic target - Google Patents
A kind of preparation method of single dispersing gallium oxide powder and its high density ceramic target Download PDFInfo
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- CN107010654A CN107010654A CN201710311705.9A CN201710311705A CN107010654A CN 107010654 A CN107010654 A CN 107010654A CN 201710311705 A CN201710311705 A CN 201710311705A CN 107010654 A CN107010654 A CN 107010654A
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Abstract
The invention discloses the preparation method of a kind of single dispersing gallium oxide powder and its high density ceramic target, purity is dissolved in acid by it for more than 99.99% metallic gallium feedstock, prepare the gallium salting liquid of clarification, add precipitating reagent produce sediment, by the precipitation of acquisition it is scrubbed, filtering, dry, calcining monodisperse superfine gallium oxide powder is made；With the single dispersing gallium oxide powder of synthesis as raw material, gallium oxide green compact are obtained through compression molding and isostatic cool pressing reinforcing, green compact are placed in high temperature furnace and sintered, the uniform gallium oxide ceramic target of high density, microstructure is made.The present invention have the advantages that technique be simple and convenient to operate, yield it is high, suitable industrialized production.
Description
Technical field
The invention belongs to gallium oxide powder and gallium oxide ceramic target preparation field, more particularly, to a kind of single dispersing
The preparation method of gallium oxide powder and its high density ceramic target.
Background technology
Gallium oxide is a kind of broad stopband transparent oxide semiconductor material, and its room temperature energy gap is up to 4.9eV, with excellent
Different chemistry, physically and thermally stability.Because it is to oxygen and day blind ultraviolet-sensitive, be at present prepare high-temperature gas sensors and
The optimal optional monophase materialses of solar blind ultraviolet detector.In current flat-panel monitor (FPD) in the market, thin film transistor (TFT) (TFT)
Display occupies absolute leading position, the global hundreds billion of members of annual value of production.Wherein, IGZO (Indium Gallium Zinc
Oxide, indium gallium zinc oxide), because it has the advantages that carrier concentration is low, mobility is high, it gradually instead of traditional amorphous
Silicon and polysilicon, are widely used in TFT channel layer materials.As the gallium oxide of one of constitutive material important IGZO, still
A kind of potential luminous host material, the different rare earth atom by adulterating can prepare a variety of electroluminescent materials, in light
Electrical domain shows very big application prospect.
In thin film preparation process, to have that depositing temperature is low, sedimentation rate is high, quality of forming film is high etc. excellent because of it for sputter coating
Point is widely used, and sputtering prepares the stable function film of uniform, performance, and high fine and close ceramic target is its prerequisite.Target
Powder used is typically unable to direct sintering shaping in material preparation, also needs through ball-milling treatment, adds the means acquisition such as binding agent granulation
High fine and close ceramic target, this process inevitably introduces exogenous impurity, but also needs degreasing process, extends target
Production cycle, add financial cost.Therefore, it is to solve this to prepare uniform particle sizes, monodispersed high-purity gallium oxide powder
The key technology of problem.Some gallium oxide raw powder's production technologies are disclosed in the prior art, and such as patent CN102978649A is public
Open and prepared gallium oxide powder using electrolysis, CN104276597A is disclosed prepares gallium oxide powder using oxidation fusion metal method
Body, wherein electrolysis prepare powder electrolysis time in more than 30h, and the production cycle is long, add financial cost, and oxidation fusion is golden
Category method is raw material using gases at high pressure, adds the danger of production.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of single dispersing gallium oxide powder and its
The preparation method of high density ceramic target, its gallium oxide powder for using chemical direct precipitation method to prepare is not required to through ball milling, addition
The means such as binding agent, granulation, just can direct weighting shaping, and then sinter the gallium oxide sintered body of high density, even structure into, it is full
Sufficient industrialized production, it is adaptable to the light such as high-temperature gas sensing, luminous substrate, field-effect transistor, thin film transistor (TFT), crystalline ceramics
Electrical domain.
To achieve the above object, according to one aspect of the present invention, it is proposed that a kind of preparation of single dispersing gallium oxide powder
Method, its gallium using purity as more than 99.99% as raw material, and by the dissolution of raw material in acid solution it is molten to prepare gallium salt
Liquid, then adds precipitating reagent to occur precipitation reaction and then obtain white depositions in the gallium salting liquid, finally will be described white
Color sediment is scrubbed, filtering, dries, prepare single dispersing gallium oxide powder after calcining.
As it is further preferred that the acid solution is preferably nitric acid, hydrochloric acid or sulfuric acid；The concentration of the gallium salting liquid is preferred
For 0.1mol/L~1mol/L；The precipitating reagent is preferably ammonia spirit.
As it is further preferred that the temperature control of the precipitation reaction is at 20 DEG C~80 DEG C, the pH value of reaction is controlled 7
~11.
As it is further preferred that the temperature of the precipitation reaction is preferably controlled in 30 DEG C~70 DEG C, the pH value of reaction is excellent
Selected control system is 7~9.
As it is further preferred that the temperature of the drying is preferably 60 DEG C~100 DEG C, drying time be preferably 12h~
24h；Calcining heat is preferably 800 DEG C~900 DEG C, and calcination time is preferably 1~3h, and calcination atmosphere is air.
As it is further preferred that the cleaning solution used that washs is deionized water or absolute ethyl alcohol.
As it is further preferred that the granule content of particle diameter≤8 μm exists in the single dispersing gallium oxide powder prepared
More than 98%, and median D50 scope is 0.5 μm~2.5 μm.
It is another aspect of this invention to provide that there is provided a kind of preparation method of high density gallium oxide ceramic target, it is with list
Scattered gallium oxide powder is the raw material for preparing target, and by the first compression molding of the gallium oxide powder material again isostatic cool pressing reinforcing
Gallium oxide green compact are made in reason, and the green compact finally are positioned over into sintering in high temperature furnace is made high density gallium oxide ceramic target.
As it is further preferred that the pressure of the compression molding is preferably 20MPa~50MPa, the isostatic cool pressing is strong
The pressure for changing processing is preferably 120MPa~300MPa.
As it is further preferred that the temperature of the sintering is preferably 1350 DEG C~1550 DEG C, soaking time is preferably
30min~20h, sintering atmosphere is air.
In general, possess following compared with prior art, mainly by the contemplated above technical scheme of the present invention
Technological merit：
1. the gallium oxide powder that the present invention is prepared using chemical direct precipitation method, with monodispersity, high-purity phase structure,
The granule content of particle diameter≤8 μm is up to more than 98% in the features such as pattern and controllable granularity, the single dispersing gallium oxide powder of preparation,
Median D50 scope is 0.5 μm~2.5 μm, in addition the precipitation method of the invention there is technique to be simple and convenient to operate, yield
High the advantages of, it is adapted to industrialized production.
2. the single dispersing gallium oxide powder that is prepared through direct precipitation method of the present invention, without follow-up ball milling, addition binding agent,
High fine and close, the uniform gallium oxide ceramic target of microstructure just can be obtained after the PROCESS FOR TREATMENTs such as granulation, direct pressing shaping sintering,
Meet the application of the optoelectronic devices such as sputter coating.
3. the present invention also each technological parameter being related in preparation method is studied and set, such as precipitation reaction, do
The setting of the technological parameters such as dry, calcining, molding, isostatic cool pressing intensive treatment and sintering, to obtain optimal preparation parameter, so as to make
It is standby to obtain single dispersing, median D50The high density oxidation of≤2.5 μm of ultra-fine gallium oxide powder and its relative density >=99%
Gallium ceramic target.
Brief description of the drawings
Fig. 1 is the gallium oxide powder XRD shown in embodiment 2；
Fig. 2 is the gallium oxide diameter of particle distribution map shown in embodiment 2；
Fig. 3 is the gallium oxide powder SEM figures shown in embodiment 2；
Fig. 4 is the gallium oxide powder SEM figures shown in embodiment 3；
Fig. 5 is the gallium oxide powder SEM figures shown in embodiment 4；
Fig. 6 is the gallium oxide powder SEM figures shown in embodiment 5；
Fig. 7 is the gallium oxide target section SEM figures shown in embodiment 6；
Fig. 8 is the gallium oxide target material surface SEM figures shown in embodiment 7；
Fig. 9 is the gallium oxide target material surface SEM figures shown in embodiment 8.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
A kind of single dispersing gallium oxide raw powder's production technology provided in an embodiment of the present invention, its using purity as 99.99% with
On gallium as raw material, and by the dissolution of raw material in acid solution to prepare gallium salting liquid, then in the gallium salting liquid plus
Enter precipitating reagent to occur precipitation reaction and then obtain white depositions, finally by the white depositions are scrubbed, it is filtering, dry
Single dispersing gallium oxide powder is prepared after dry, calcining.In the single dispersing gallium oxide powder being prepared by the method for the present invention
The granule content of particle diameter≤8 μm is more than 98%, and median D50 scope is 0.5 μm~2.5 μm.
Specifically, the acid solution is preferably nitric acid, hydrochloric acid or sulfuric acid；The concentration of the gallium salting liquid is preferably 0.1mol/L
~1mol/L；The precipitating reagent is preferably ammonia spirit.It has been investigated that when concentration used is less than 0.1mol/L, yielding poorly, reaching
Less than demand of industrial production；When concentration used is more than 1mol/L, because the concentration of gallium ion in solution is excessive, easily cause office
Portion's nucleation rate is excessive, causes generation precipitation uneven.
Further, it has been investigated that when precipitation reaction temperature be less than 20 DEG C, reaction rate is low, generate precipitation needed for when
Between extend, add the production cycle；After reaction temperature is more than 80 DEG C, the evaporation of reaction solution ammoniacal liquor is serious, consumes raw material, increases
Add financial cost, therefore by the temperature control of precipitation reaction at 20 DEG C~80 DEG C, be preferably controlled in 30 DEG C~70 DEG C, reaction
PH value is controlled 7~11, is further optimized, and pH value is controlled 7~9；The temperature of the drying is preferably 60 DEG C~100 DEG C,
Drying time is preferably 12h~24h；Calcining heat is preferably 800 DEG C~900 DEG C.
Another embodiment of the present invention provides a kind of preparation method of high density gallium oxide ceramic target, and it is with the present invention
The single dispersing gallium oxide powder of preparation, and will be cold etc. quiet after the gallium oxide powder material compression molding as the raw material for preparing target
Press intensive treatment that gallium oxide green compact are made, then the green compact are positioned over sintering in high temperature furnace and high density gallium oxide ceramic target is made
Material.
Wherein, the pressure of compression molding is preferably 20MPa~50MPa, and the pressure of isostatic cool pressing intensive treatment is preferably
120MPa~300Mpa；The temperature of sintering is preferably 1350 DEG C~1550 DEG C, and soaking time is preferably 30min~20h, sinters gas
Atmosphere is air.
It is below the specific embodiment of the present invention.
Embodiment 1
It is raw material for 99.999% gallium to use purity, weighs gallium 13.95g (0.2mol).With 65% it is dense
Nitric acid is in 50 DEG C of dissolving galliums of water-bath, and after gallium is completely dissolved, the gallium nitrate that solution is diluted into 0.1mol/L with deionized water is molten
Liquid.Above-mentioned solution is placed in water-bath, under mechanical stirring, the ammonia spirit (25%) of 10 times of dilution is added dropwise with peristaltic pump,
Reaction temperature is controlled at 20 DEG C.When the pH value of reaction solution is 9, stop that ammoniacal liquor is added dropwise.Continue to stir the reaction solution, aging 3h
More than, ammoniacal liquor is added in this process keeps pH stable 9 ± 0.2.The sediment of 3 acquisitions is washed with deionized, will
100 DEG C of insulation 12h are dried after precipitation filtering.The drying powder obtained is calcined into 3h at 800 DEG C, gallium oxide powder is obtained.
The meso-position radius D of the powder50For 0.85 μm, the granule content of particle diameter≤6 μm is more than 99.9%.
Embodiment 2
It is raw material for 99.999% gallium to use purity, weighs gallium 13.95g (0.2mol).With 65% it is dense
Nitric acid is in 50 DEG C of dissolving galliums of water-bath, and after gallium is completely dissolved, the gallium nitrate that solution is diluted into 0.2mol/L with deionized water is molten
Liquid.Above-mentioned solution is placed in water-bath, under mechanical stirring, the ammonia spirit (25%) of 10 times of dilution is added dropwise with peristaltic pump,
Reaction temperature is controlled at 30 DEG C.When the pH value of reaction solution is 8, stop that ammoniacal liquor is added dropwise.Continue to stir the reaction solution, aging 3h
More than, ammoniacal liquor is added in this process keeps pH stable 8 ± 0.2.The sediment of 3 acquisitions is washed with deionized, will
100 DEG C of insulation 12h are dried after precipitation filtering.The drying powder obtained is calcined into 1h at 900 DEG C, gallium oxide powder is obtained.
The meso-position radius D of the powder50For 1.12 μm, the granule content of particle diameter≤6 μm is more than 99.9%, and its XRD diffraction pattern is shown in Fig. 1, grain
Footpath distribution map is shown in Fig. 2, and shape appearance figure is shown in Fig. 3.
Embodiment 3
It is raw material for 99.999% gallium to use purity, weighs gallium 13.95g (0.2mol).With 65% it is dense
Nitric acid is in 50 DEG C of dissolving galliums of water-bath, and after gallium is completely dissolved, the gallium nitrate that solution is diluted into 0.2mol/L with deionized water is molten
Liquid.Above-mentioned solution is placed in water-bath, under mechanical stirring, the ammonia spirit (25%) of 10 times of dilution is added dropwise with peristaltic pump,
Reaction temperature is controlled at 80 DEG C.When the pH value of reaction solution is 8, stop that ammoniacal liquor is added dropwise.Continue to stir the reaction solution, aging 3h
More than, ammoniacal liquor is added in this process keeps pH stable 8 ± 0.2.The sediment of 3 acquisitions is washed with deionized, will
60 DEG C of insulation 24h are dried after precipitation filtering.The drying powder obtained is calcined into 2h at 900 DEG C, gallium oxide powder is obtained.Should
The meso-position radius D of powder50For 2.06 μm, the granule content of particle diameter≤6 μm is more than 99.9%, and its morphology microstructure is as shown in Figure 4.
Embodiment 4
It is raw material for 99.999% gallium to use purity, weighs gallium 34.86g (0.5mol).With 65% it is dense
Nitric acid is in 50 DEG C of dissolving galliums of water-bath, and after gallium is completely dissolved, the gallium nitrate that solution is diluted into 0.5mol/L with deionized water is molten
Liquid.Above-mentioned solution is placed in water-bath, under mechanical stirring, the ammonia spirit (25%) of 10 times of dilution is added dropwise with peristaltic pump,
Reaction temperature is controlled at 70 DEG C.When the pH value of reaction solution is 8, stop that ammoniacal liquor is added dropwise.Continue to stir the reaction solution, aging 3h
More than, ammoniacal liquor is added in this process keeps pH stable 8 ± 0.2.The precipitation of 3 acquisitions is washed with deionized, by this
90 DEG C of insulation 20h are dried after precipitation filtering.The drying powder obtained is calcined into 3h at 900 DEG C, gallium oxide powder is obtained.The powder
The meso-position radius D of body50For 1.38 μm, the granule content of particle diameter≤4 μm is more than 99.9%, and its morphology microstructure is as shown in Figure 5.
Embodiment 5
It is raw material for 99.99% gallium to use purity, weighs gallium 34.86g (0.5mol).With 65% dense nitre
After gallium is completely dissolved, 1mol/L gallium nitrate solution is diluted to deionized water in 50 DEG C of dissolving galliums of water-bath by acid for solution.Will
Above-mentioned solution is placed in water-bath, under mechanical stirring, and the ammonia spirit (25%) of 10 times of dilution, reaction temperature are added dropwise with peristaltic pump
Degree control is at 70 DEG C.When the pH value of reaction solution is 7, stop that ammoniacal liquor is added dropwise.The continuation stirring reaction solution, more than aging 3h,
Ammoniacal liquor is added in this process keeps pH stable 7 ± 0.2.The precipitation of 3 acquisitions is washed with deionized, this was precipitated
100 DEG C of insulation 12h are dried after filter.The drying powder obtained is calcined into 3h at 900 degree, gallium oxide powder is obtained.The powder
Meso-position radius D50For 2.43 μm, the granule content of particle diameter≤8 μm is more than 98%, and its morphology microstructure is as shown in Figure 6.
Understood that by the process conditions of the present invention monodispersed micron gallium oxide powder can be prepared according to embodiment 1-4
Body, the diameter of particle narrow distribution range.When reaction temperature is at 20~30 DEG C, the powder of generation is in spheroid shape, and reaction temperature is 30
DEG C~powders of 80 DEG C of preparations are in shaft-like.The powder of preparation is the β-Ga of high-purity monocline2O3。
Embodiment 6
Using embodiment 1 synthesis technique prepare gallium oxide powder as the raw material for preparing target, take 2g gallium oxide powder
Body, compression molding prepares Φ 18mm green compact, and briquetting pressure is 20MPa, then with 300MPa isostatic cool pressing reinforcing green compact.Will
The green compact of shaping, which are placed in high temperature furnace, sinters 1400 DEG C of insulation 1h, and sintering atmosphere is air.The relative density of sintered body is
99.1%, its cross-section morphology is shown in Fig. 7, and it has fine and close and uniform microscopic appearance.
Embodiment 7
Using embodiment 2 synthesis technique prepare gallium oxide powder as the raw material for preparing target, take 2g gallium oxide powder
Body, compression molding prepares Φ 18mm green compact, and briquetting pressure is 36MPa, then with 200MPa isostatic cool pressing reinforcing green compact.Will
The green compact of shaping, which are placed in high temperature furnace, sinters 1450 DEG C of insulation 1h, and sintering atmosphere is air.The relative density of sintered body is
99.5%, its surface topography is ground, polishing, see Fig. 8 after heat erosion, understands that the target material structure is fine and close and size of microcrystal is equal from figure
It is even.
Embodiment 8
Using embodiment 2 synthesis technique prepare gallium oxide powder as the raw material for preparing target, take 2g gallium oxide powder
Body, compression molding prepares Φ 18mm green compact, and briquetting pressure is 50MPa, then with 120MPa isostatic cool pressing reinforcing green compact.Will
The green compact of shaping, which are placed in high temperature furnace, sinters 1550 DEG C of insulation 30min, and sintering atmosphere is air.The relative density of sintered body is
99.9%, its surface topography is ground, polishing, see Fig. 9 after heat erosion, and the target material structure is fine and close as can be seen from Figure 9 and size of microcrystal
Uniformly.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of single dispersing gallium oxide raw powder's production technology, it is characterised in that make by more than 99.99% gallium of purity
For raw material, and by the dissolution of raw material in acid solution to prepare gallium salting liquid, precipitating reagent is then added in the gallium salting liquid to send out
Raw precipitation reaction and then obtain white depositions, finally by the white depositions are scrubbed, filtering, dry, prepare after calcining
Obtain single dispersing gallium oxide powder.
2. single dispersing gallium oxide raw powder's production technology according to claim 1, it is characterised in that the acid solution is preferably
Nitric acid, hydrochloric acid or sulfuric acid；The concentration of the gallium salting liquid is preferably 0.1mol/L~1mol/L；The precipitating reagent is preferably ammoniacal liquor
Solution.
3. single dispersing gallium oxide raw powder's production technology according to claim 1 or 2, it is characterised in that the precipitation is anti-
The temperature control answered is at 20 DEG C~80 DEG C, and the pH value of reaction is controlled 7~11.
4. single dispersing gallium oxide raw powder's production technology according to claim 3, it is characterised in that the precipitation reaction
Temperature is preferably controlled in 30 DEG C~70 DEG C, and the pH value of reaction is preferably controlled in 7~9.
5. single dispersing gallium oxide raw powder's production technology according to claim 4, it is characterised in that the temperature of the drying
Preferably 60 DEG C~100 DEG C, drying time is preferably 12h~24h；Calcining heat is preferably 800 DEG C~900 DEG C, calcination time
Preferably 1~3h, calcination atmosphere is air.
6. single dispersing gallium oxide raw powder's production technology according to claim 5, it is characterised in that what the washing was used
Cleaning solution is deionized water or absolute ethyl alcohol.
7. the single dispersing gallium oxide raw powder's production technology according to claim any one of 1-6, it is characterised in that preparation
The granule content of particle diameter≤8 μm is more than 98% in the single dispersing gallium oxide powder, and median D50Scope be 0.5 μm
~2.5 μm.
8. a kind of preparation method of high density gallium oxide ceramic target, it is characterised in that with described in claim any one of 1-7
Single dispersing gallium oxide powder is the raw material for preparing target, and isostatic cool pressing is strengthened again by the first compression molding of the gallium oxide powder material
Gallium oxide green compact are made in processing, and the green compact finally are positioned over into sintering in high temperature furnace is made high density gallium oxide ceramic target.
9. the preparation method of high density gallium oxide ceramic target according to claim 8, it is characterised in that described to be molded into
The pressure of type is preferably 20MPa~50MPa, and the pressure of the isostatic cool pressing intensive treatment is preferably 120MPa~300MPa.
10. the preparation method of high density gallium oxide ceramic target according to claim 8 or claim 9, it is characterised in that the burning
The temperature of knot is preferably 1350 DEG C~1550 DEG C, and soaking time is preferably 30min~20h, and sintering atmosphere is air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710311705.9A CN107010654B (en) | 2017-05-05 | 2017-05-05 | A kind of preparation method of monodisperse gallium oxide powder and its high density ceramic target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710311705.9A CN107010654B (en) | 2017-05-05 | 2017-05-05 | A kind of preparation method of monodisperse gallium oxide powder and its high density ceramic target |
Publications (2)
| Publication Number | Publication Date |
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| CN107010654A true CN107010654A (en) | 2017-08-04 |
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| CN108046311A (en) * | 2017-12-25 | 2018-05-18 | 清远先导材料有限公司 | The preparation method of high-purity gallium oxide |
| CN110627481A (en) * | 2019-10-18 | 2019-12-31 | 先导薄膜材料（广东）有限公司 | High-purity Ga2O3Preparation method of target material |
| CN111592033A (en) * | 2020-05-21 | 2020-08-28 | 广东先导稀材股份有限公司 | Preparation method of target-grade gallium oxide |
| CN111592034A (en) * | 2020-05-25 | 2020-08-28 | 先导薄膜材料（广东）有限公司 | Gallium oxide particle and preparation method thereof |
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| CN108046311A (en) * | 2017-12-25 | 2018-05-18 | 清远先导材料有限公司 | The preparation method of high-purity gallium oxide |
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| CN111592033A (en) * | 2020-05-21 | 2020-08-28 | 广东先导稀材股份有限公司 | Preparation method of target-grade gallium oxide |
| CN111592034A (en) * | 2020-05-25 | 2020-08-28 | 先导薄膜材料（广东）有限公司 | Gallium oxide particle and preparation method thereof |
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