CN107021521A - A kind of preparation method of indium gallium zinc composite powder - Google Patents
A kind of preparation method of indium gallium zinc composite powder Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of indium gallium zinc composite powder, first melting is made indium gallium kirsite, is re-dissolved in nitric acid, and then the condensate of generation indium nitrate, gallium nitrate and zinc nitrate adds ammoniacal liquor, form precipitation, and precipitation calcining is produced.Because the present invention using indium sows kirsite as raw material, by the way that indium is sowed into kirsite and nitric acid reaction, indium nitrate, gallium nitrate and the zinc nitrate realized is generated simultaneously, prior art is avoided to prepare respectively during indium oxide, gallium oxide and zinc oxide by the severe deviations for being difficult to realize granularity that sameization of control condition brought and specific surface area, it ensure that the uniform particle sizes of the indium gallium zinc composite powder of preparation, specific surface area is controllable, so that final sintering character is good.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of preparation method of indium gallium zinc composite powder.
Background technology
Indium gallium zinc oxide（IGZO）It is indium oxide, aoxidizes the composite oxides sowed with the mutual solid solution of zinc oxide.IGZO has
Have good photoelectric properties, the film containing IGZO have higher electric conductivity and visible light transmission, particularly can be homogeneous
Property splendid non-crystalline state under realize electron mobility characteristics no less than crystalline state, it is adaptable to prepare high mobility
TFT transistors, thus it is widely used in field of flat panel displays.Preparing the method for thin IGZO films has sputtering method, vacuum evaporation
Method, sol-gel process, Cluster deposition method and cladding process etc..
Sputtering method is the common method for preparing IGZO films, when using vacuum evaporation or magnetron sputtering preparation IGZO films
When, first have to prepare IGZO powder, then by powder compacting sintering into IGZO targets.Wherein, the granularity of IGZO powder, granularity model
Enclose, specific surface area and particle size uniformity are the important of influence IGZO sintered bodies, IGZO targets and final IGZO property of thin film
Parameter.If the properties such as the granularity of IGZO powder, particle shape, size distribution and uniformity cannot be guaranteed, IGZO powder
Sintering circuit sintered body can be made to occur that density is low, density uniformity is poor or the phenomenon such as coarse grains, so as to produce IGZO targets
Material electric conductivity is poor, the bad phenomenon such as arc discharge in magnetron sputtering process, ultimately results in the decline of IGZO film qualities.
In the prior art, IGZO powder generally uses following preparation method：Be utilized respectively indium metal and metal sow, metal
Zinc obtains indium oxide powder, oxidation and sows powder and alumina powder, and then indium oxide, oxidation are sowed and mixed with three kinds of powder of aluminum oxide
Close scattered, such as Chinese patent： CN 102959122A（Sputtering target manufacture method and sputtering target）.The gold of raw material due to based on
Category indium and metal are sowed, the dissolution velocity of metallic zinc, solution temperature, neutralize the control strips such as pH value, neutral temperature and mixing speed
Part is difficult to fully achieve sameization, so that indium oxide powder, oxidation sow the particle diameter and prepared target of powder and Zinc oxide powder
The density variation of material is larger, have impact on indium oxide powder, oxidation and sows the quality of powder film.
The content of the invention
In order to which small granularity, uniform particle sizes and the high indium gallium zinc composite powder of specific surface area, the purpose of the present invention is made
It is to provide a kind of preparation method of indium gallium zinc composite powder.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that indium, gallium, zinc are melted by melting, then obtains granular alloy using rotating pan；
（2）By step（1）The granular alloy of gained is dissolved in nitric acid, obtains mixed solution；
（3）Regulating step（2）The pH of gained mixed solution is 7 ~ 8, is persistently stirred to separate out precipitation, then separates, washs, does
It is dry；
（4）By step（3）Products therefrom is calcined 3 ~ 8 hours in 600 ~ 1200 DEG C, is produced.
Preferably, step（1）Middle melting uses vacuum melting furnace, and smelting temperature is 380 ~ 460 DEG C.
Preferably, step（1）The particle diameter of the middle granular alloy of gained is 4 ~ 10 millimeters.
Preferably, step（1）Described in indium, gallium, zinc mass ratio be 1：1：1.
Preferably, step（2）Specially by step（1）The granular alloy of gained is added in nitric acid, stir 6 in 120 ~ 260 DEG C ~
10 hours, it was 3600 ~ 10000g/Lh that the dosage of the granular alloy, which is 30 ~ 60 g/L and adds speed,.
Further, step（2）Described in the concentration of nitric acid be the wt% of 30 wt % ~ 60.
Preferably, step（3）Specially to step（2）Alkaline conditioner, regulation pH value to 7 are added in gained mixed solution
~ 8, stirred in 50 ~ 80 DEG C 30 ~ 80 minutes, then stand, separate, wash, dry, crush.
Further, step（3）The alkaline conditioner be it is a kind of in sodium hydroxide solution, potassium hydroxide solution and ammoniacal liquor or
It is two or more.
Preferably, the concentration of the ammoniacal liquor is the wt% of 10 wt% ~ 40, and optimal is 25 wt%.
Preferably, step（3）Described in drying use spray drying process.
Wherein, step（1）It is preferred that smelting temperature ensure that indium metal, gallium and metallic zinc while uniform dissolution
Vaporization at high temperature is not likely to produce, optimal smelting temperature is 400 DEG C；Rotating pan is that the indium gallium kirsite of melting is passed through into 1 ~ 2 milli
On nozzle drip to the conveyer belt of rice diameter, granular alloy is obtained after cooling, on the one hand granular alloy is conducive to mixed with nitric acid
Close reaction, it is ensured that being smoothed out for reaction, on the other hand avoid the reunion between reaction product, it is ensured that obtained oxidation
The uniformity of indium gallium zinc composite powder particle diameter, the optimized particle size of granular alloy is 6 millimeters.
Step（2）It is the condensate that granular alloy generates indium nitrate gallium zinc with nitric acid hybrid reaction, the step is to determine oxygen
Change the core procedure of indium gallium zinc composite powder crystallinity；First, the concentration of nitric acid can influence being smoothed out and being made for reaction
Indium gallium zinc composite powder obtain particle diameter, particle size range and specific surface area, only when nitric acid is under certain concentration, granular alloy
Just there is optimal dissolution velocity, the optimal concentration of nitric acid is 45 wt%；Secondly, dissolution velocity is to control the pass of powder crystallinity
Key factor, dissolution velocity speed directly affects the size of the condensate particle diameter of production, and indium gallium zinc ion is in co-precipitation
Concentration, so as to influence the particle size of follow-up coprecipitated product, particle size range, than surface and its uniformity；Meanwhile, in order to the greatest extent
The generation of amount control particle diameter deviation, the reactive polymeric body stablized, the present invention utilize the Automated condtrol of relative stable operation
Dissolution velocity and reaction temperature, by quantitative feeding device at the uniform velocity, quantitatively, the dissolving of granular alloy quantitative constant speed in nitric acid, gas
Body can be produced uniformly, it is suppressed that the harm to environment, so optimal is to add granular alloy in nitric acid, 8 are stirred in 200 DEG C
Hour, the dosage of granular alloy is 45 g/L.The step is generated while realizing indium nitrate, gallium nitrate and zinc nitrate solution
With uniform mixing, it is to avoid prior art is prepared during indium gallium zinc solution due to sameization for being difficult to realize control condition respectively
The deviation of the particle diameter brought, it is ensured that it is uniform that indium gallium zinc composite powder prepares that indium gallium zinc ion in initial soln is distributed
Property, so as to provide primary and preferred indium gallium zinc ion solution bar for uniformity prepared by subsequent oxidation indium gallium zinc composite powder
Part.
The good indium gallium zinc composite powder of sintering character, it is necessary to possess uniform particle size distribution range, powder diameter
Small, powder is difficult to reunite；Powder diameter is big, and the mutual solid solubility of indium oxide, gallium oxide and zinc oxide is small, and the target of preparation is easily produced
Angry hole, hole, target Density inhomogeneity are also easy to produce paradoxical discharge and are poisoned with melanism dross during sputtering.Step（3）It is prepared by precipitation
The control of condition is also the key factor for obtaining the uniform powder of particle size distribution range.The forming process of precipitation is one complicated
It is interrelated between thermodynamical reaction process, wherein influence factor, some or certain two conditions are controlled merely, can not be formed
Preferable precipitation of dissolving each other, so as to cannot get the uniform indium gallium zinc composite powder of particle diameter distribution.In order to obtain crystallization particle diameter point
The indium gallium zinc composite powder that cloth scope is uniform, sintering character is good, passes through Comprehensive Control step（3）In in mixed solution3+、
Ga3+、Zn2+The key parameters such as concentration, precipitation pH value, precipitation temperature, sedimentation time, so as to obtain desired uniform chemical combination powder
Body.Due to step（2）In in mixed solution3+、Ga3+、Zn2+Concentration is higher than 70g/L, and powder crystallization particle diameter diminishes during precipitation, easily
Reunite；In in mixed solution3+、Ga3+、Zn2+Concentration be less than 30g/L, powder crystallization particle diameter becomes big during precipitation, and precipitation reaction is slow,
So step（2）The dosage control of granular alloy is 30 ~ 60 g/L.Step（3）During generation precipitation, pH value is high, the powder of preparation
Last crystallization particle diameter is big, and powder is hard, therefore pH should be controlled to be 7 ~ 8, and optimal pH is 7.8；Secondly, precipitation temperature is higher than 80 DEG C, powder
Crystallization particle diameter becomes big；Precipitation temperature is less than 50 DEG C, and crystallization particle diameter diminishes, and precipitation is difficult filtering, and optimal is 65 DEG C；Sedimentation time
Long, the powder crystallization particle diameter of preparation becomes big；Sedimentation time is short, and crystallization particle diameter diminishes, and powder is easily reunited, so the sedimentation time is preferred
For 30~80 minutes, more preferably 40~60 minutes, most preferably 50 minutes sedimentation times.
Step（3）After stirring produces precipitation, water can also be added while stirring, obtain slurries, control the slurry
The solids content of liquid is the wt% of 10 wt% ~ 70 wt%, more preferably 20 wt% ~ 60；After stirring, in order that particle diameter in precipitation solution
Growth more complete, purity is higher, and the standing precipitation that can also carry out precipitation solution preferably is handled, and stands the time of precipitation processing
Preferably more than 6 hours, more preferably more than 12 hours.Will precipitation and liquid when being separated, can use suction filtration, press filtration,
The modes such as centrifugation, filter press, ceramic membrane washing are carried out；Then distilled water, deionized water, ammoniacal liquor, alcohol is recycled to carry out
The removal of impurity is gone in washing；Then drying mode is the key factor for preparing the uniform powder of IGZO particle size distributions, preferably by
Slurries drying machine is spray-dried to the zinc-aluminium hydroxide precipitation solution, is allowed to the powder of generation co-precipitation hydroxide
Body.The drying of slurry drying machine is than traditional heating, drying method, and the precipitation powder reclaimed water point content of preparation is uniform, powder is loose
Soft soilless sticking, particle diameter distribution are uniform, and this will provide good precondition for the uniformity that oxide powder is calcined.Can before calcining
Using rod mill or gas shock to step（3）Products therefrom, which is ground to particle diameter, is less than 150 μm.
Step（4）If calcining be less than 600 DEG C, be calcined insufficient, step（3）Products therefrom conversion is incomplete；If being higher than
1200 DEG C, obtained indium gallium zinc composite powder particle diameter is big, hardness is big.So more preferably, prior to 800 DEG C ~ 1000 DEG C
Calcining 3 ~ 4 hours, is calcined 2 ~ 3 hours then at 850 ~ 950 DEG C；More preferably calcined 4 hours in 900 DEG C.For calcination atmosphere, nothing
Especially limitation, can be carried out under the atmosphere of hydrogen halides, halogen, air, oxygen, nitrogen or argon gas, wherein, hydrogen halides can be
Hydrogen chloride, hydrogen bromide, hydrogen iodide etc..Halogen is chlorine, bromine, iodine etc.；It is preferred that, calcining is carried out in air atmosphere.
The invention provides a kind of preparation method of indium gallium zinc composite powder, the indium gallium kirsite obtained using melting as
Raw material, nitric acid is dissolved in by indium gallium kirsite, and then the condensate of generation indium nitrate, gallium nitrate and zinc nitrate adds ammoniacal liquor, shape
Into mixing indium hydroxide, gallium hydroxide, zinc hydroxide precipitation, indium gallium zinc composite powder is obtained after sediment is calcined.
The present invention by indium by sowing kirsite and nitric acid reaction, and indium nitrate, gallium nitrate and the zinc nitrate realized is simultaneously raw
Due to being difficult to realize the same of control condition during indium oxide, gallium oxide and zinc oxide being prepared respectively into, it is to avoid prior art
Granularity and the severe deviations of specific surface area that sample is brought, it is ensured that the particle diameter of the indium gallium zinc composite powder of preparation is equal
Even, specific surface area is controllable, so that final sintering character is good.The Fei Shi particle mean sizes that indium gallium zinc composite powder is made are 20
~80nm；D10：0.1~0.2um, D50：0.4~0.6um, D90：0.8~1.0um；Primary partical（Step 1 gained grain
Shape alloy）The m of specific surface area 15~402/ g, secondary dough particle（Step 4 gained indium gallium zinc composite powder）Specific surface area
6~10 m2/ g。
Embodiment
Embodiment 1
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that 10 kg indiums, 10 kg galliums, 10 kg zinc are melted in 400 DEG C of meltings, then passes through 1 ~ 2
On nozzle drip to the conveyer belt of mm diameters, the granular alloys of 30 kg are obtained；
（2）In under 200 DEG C of stirring condition, by step（1）The granular alloy of gained passes through quantitative feeding device with 6 kg/h speed
At the uniform velocity add in the nitric acid that 50 L mass concentrations are 45 wt%, stir 8 hours, remove residue with filter-cloth filtering, and add pure water
It is 270 L to volume, temperature is 40 DEG C, and pH value is 2~4, obtains mixed solution；Wherein, the width of mesh of the filter cloth is 150
μm；
（3）By step（2）Gained mixed solution is placed in closed container, low whipping speed be 180 rpm under conditions of add 20
Wt% ammoniacal liquor carries out neutralization reaction, and regulation mixing speed is 240rpm when beginning with Precipitation, continuously adds 20 wt% ammoniacal liquor
So that the pH value of solution remains 7.8, stirred 50 minutes in 65 DEG C, it is complete to precipitation reaction.Precipitation 10 is stood at 40 DEG C small
When, plus pure water repeatedly stirs, and obtains the slurries of solids content 50%；Slurries are filtered, sunk with concentration for 20 wt% ammonia scrubbing
Form sediment, then it is 5 ~ 100 mS/cm to be washed with the alcoholic solution that concentration is 22 wt% to filtrate electrical conductivity, filtering, spray drying；
（4）By step（3）Products therefrom is calcined 4 hours in 900 DEG C, is produced.
Indium gallium zinc composite powder obtained above is detected, as a result as shown in table 1.
The results of property of IGZO powder prepared by the embodiment 1 of table 1
Embodiment 2
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that 10 kg indiums, 10 kg galliums, 10 kg zinc are melted in 380 DEG C of meltings, then passes through 1 ~ 2
On nozzle drip to the conveyer belt of mm diameters, the granular alloys of 30 kg are obtained；
（2）In under 120 DEG C of stirring condition, by step（1）The granular alloy of gained passes through quantitative feeding device with 6 kg/h speed
At the uniform velocity add in the nitric acid that 50 L mass concentrations are 30 wt%, stir 6 hours, remove residue with filter-cloth filtering, and add pure water
It is 270 L to volume, temperature is 40 DEG C, and pH value is 2~4, obtains mixed solution；Wherein, the width of mesh of the filter cloth is 150
μm；
（3）By step（2）Gained mixed solution is placed in closed container, low whipping speed be 180 rpm under conditions of add 20
Wt% ammoniacal liquor carries out neutralization reaction, when beginning with Precipitation, and regulation mixing speed is 240rpm, continuously adds ammoniacal liquor and causes
The pH value of solution remains 7.0, is stirred 30 minutes in 50 DEG C, to precipitation reaction completely, and precipitation 10 hours are stood at 40 DEG C, plus
Pure water is repeatedly stirred, and obtains the slurries of solids content 50%；Slurries are filtered, precipitated with concentration for 20 wt% ammonia scrubbing, then
It is 5 ~ 100 mS/cm to be washed with the alcoholic solution that concentration is 22 wt% to filtrate electrical conductivity, filtering, spray drying；
（4）By step（3）Products therefrom is calcined 4 hours in 600 DEG C, is produced.
Indium gallium zinc composite powder obtained above is detected, as a result as shown in table 2.
The results of property of IGZO powder prepared by the embodiment 1 of table 2
Embodiment 3
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that 10 kg indiums, 10 kg galliums, 10 kg zinc are melted in 380 DEG C of meltings, then passes through 1 ~ 2
On nozzle drip to the conveyer belt of mm diameters, the granular alloys of 30 kg are obtained；
（2）In under 260 DEG C of stirring condition, by step（1）The granular alloy of gained passes through quantitative feeding device with 6 kg/h speed
At the uniform velocity add in the nitric acid that 50 L mass concentrations are 60 wt%, stir 6 hours, remove residue with filter-cloth filtering, and add pure water
It is 270 L to volume, temperature is 40 DEG C, and pH value is 2~4, obtains mixed solution；Wherein, the width of mesh of the filter cloth is 150
μm；
（3）By step（2）Gained mixed solution is placed in closed container, low whipping speed be 180 rpm under conditions of add 20
Wt% ammoniacal liquor carries out neutralization reaction, when beginning with Precipitation, and regulation mixing speed is 240rpm, continuously adds ammoniacal liquor and causes
The pH value of solution remains 7.8, is stirred 80 minutes in 80 DEG C, to precipitation reaction completely, and precipitation 10 hours are stood at 40 DEG C, plus
Pure water is repeatedly stirred, and obtains the slurries of solids content 50%；Slurries are filtered, precipitated with concentration for 20 wt% ammonia scrubbing, then
It is 5 ~ 100 mS/cm to be washed with the alcoholic solution that concentration is 22 wt% to filtrate electrical conductivity, filtering, spray drying；
（4）By step（3）Products therefrom is calcined 4 hours in 1200 DEG C, is produced.
Indium gallium zinc composite powder obtained above is detected, as a result as shown in table 3.
The results of property of IGZO powder prepared by the embodiment 1 of table 3
The specific surface area of a primary partical is larger in table 1 ~ 3, embodiment 1 ~ 3, in nanoparticle range, therefore
Surface-active is high, and activated sintering is densified during being conducive to follow-up sintering.And secondary dough specific grain surface product diminishes, then flow
Dynamic property increase, is conducive to the raising and the control of sintering blank deformation of powder compacting and biscuit density.
Comparative example 1
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that 10 kg indiums, 10 kg galliums, 10 kg zinc are melted in 380 DEG C of meltings, then passes through 1 ~ 2
On nozzle drip to the conveyer belt of mm diameters, the granular alloys of 30 kg are obtained；
（2）In under 100 DEG C of stirring condition, by step（1）The granular alloy of gained passes through quantitative feeding device with 6 kg/h speed
At the uniform velocity add in the nitric acid that 50 L mass concentrations are 30 wt%, stir 5 hours, remove residue with filter-cloth filtering, and add pure water
It is 270 L to volume, temperature is 40 DEG C, and pH value is 2~4, obtains mixed solution；Wherein, the width of mesh of the filter cloth is 150
μm；
（3）By step（2）Gained mixed solution is placed in closed container, low whipping speed be 180 rpm under conditions of add 20
Wt% ammoniacal liquor carries out neutralization reaction, and regulation mixing speed is 240rpm when beginning with Precipitation, continuously adds ammoniacal liquor so that molten
The pH value of liquid remains 7.8, is stirred 20 minutes in 45 DEG C, to precipitation reaction completely, precipitation 10 hours is stood at 40 DEG C, plus pure
Water is repeatedly stirred, and obtains the slurries of solids content 50%；Slurries are filtered, precipitated with concentration for 20 wt% ammonia scrubbing, then use
It is 5 ~ 100 mS/cm that the alcoholic solution that concentration is 22 wt%, which is washed to filtrate electrical conductivity, filtering, spray drying；
（4）By step（3）Products therefrom is calcined 4 hours in 600 DEG C, is produced.
Indium gallium zinc composite powder obtained above is detected, as a result as shown in table 4.
The results of property of IGZO powder prepared by the comparative example 1 of table 4
Comparative example 2
A kind of preparation method of indium gallium zinc composite powder, comprises the following steps：
（1）The indium gallium kirsite that 10 kg indiums, 10 kg galliums, 10 kg zinc are melted in 380 DEG C of meltings, then passes through 1 ~ 2
On nozzle drip to the conveyer belt of mm diameters, the granular alloys of 30 kg are obtained；
（2）In under 280 DEG C of stirring condition, by step（1）The granular alloy of gained passes through quantitative feeding device with 6 kg/h speed
At the uniform velocity add in the nitric acid that 50 L mass concentrations are 65 wt%, stir 10 hours, remove residue with filter-cloth filtering, and add pure water
It is 270 L to volume, temperature is 40 DEG C, and pH value is 2~4, obtains mixed solution；Wherein, the width of mesh of the filter cloth is 150
μm；
（3）By step（2）Gained mixed solution is placed in closed container, low whipping speed be 180 rpm under conditions of add 20
Wt% ammoniacal liquor carries out neutralization reaction, and regulation mixing speed is 240rpm when beginning with Precipitation, continuously adds ammoniacal liquor so that molten
The pH value of liquid remains 8.0, is stirred 90 minutes in 90 DEG C, to precipitation reaction completely, precipitation 10 hours is stood at 40 DEG C, plus pure
Water is repeatedly stirred, and obtains the slurries of solids content 50%；Slurries are filtered, precipitated with concentration for 20 wt% ammonia scrubbing, then use
It is 5 ~ 100 mS/cm that the alcoholic solution that concentration is 22 wt%, which is washed to filtrate electrical conductivity, filtering, spray drying；
（4）By step（3）Products therefrom is calcined 4 hours in 1200 DEG C, is produced.
Indium gallium zinc composite powder obtained above is detected, as a result as shown in table 5.
The results of property of IGZO powder prepared by the comparative example 2 of table 5
It can be seen that from table 4 and table 5：When flouring technology condition changes, even if the minor alteration of key process parameter,
Primary particle and second particle can be caused more thicker than time primary partical of surface and the great variety of average grain diameter, especially one, meeting
The activity of follow-up sintering is had a strong impact on, the reduction of sintered blank density and strength character is caused.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
1. a kind of preparation method of indium gallium zinc composite powder, it is characterised in that comprise the following steps：
（1）The indium gallium kirsite that indium, gallium, zinc are melted by melting, then obtains granular alloy using rotating pan；
（2）By step（1）The granular alloy of gained is dissolved in nitric acid, obtains mixed solution；
（3）Regulating step（2）The pH of gained mixed solution is 7 ~ 8, is persistently stirred to separate out precipitation, then separates, washs, does
It is dry；
（4）By step（3）Products therefrom is calcined 3 ~ 8 hours in 600 ~ 1200 DEG C, is produced.
2. the preparation method of indium gallium zinc composite powder according to claim 1, it is characterised in that：Step（1）Middle melting
Using vacuum melting furnace, smelting temperature is 380 ~ 460 DEG C.
3. the preparation method of indium gallium zinc composite powder according to claim 1, it is characterised in that：Step（1）Middle gained
The particle diameter of granular alloy is 4 ~ 10 millimeters.
4. the preparation method of indium gallium zinc composite powder according to claim 1, it is characterised in that：Step（1）Described in
Indium, gallium, the mass ratio of zinc are 1：1：1.
5. the preparation method of indium gallium zinc composite powder according to claim 1, it is characterised in that：Step（2）Specially
By step（1）The granular alloy of gained is added in nitric acid, is stirred 6 ~ 10 hours in 120 ~ 260 DEG C, is obtained mixed solution；Wherein, grain
It is 3600 ~ 10000g/Lh that the dosage of shape alloy, which is 30 ~ 60 g/L and adds speed,.
6. the preparation method of indium gallium zinc composite powder according to claim 5, it is characterised in that：Step（2）Described in
The concentration of nitric acid is the wt% of 30 wt % ~ 60.
7. the preparation method of indium gallium zinc composite powder according to claim 1, it is characterised in that：Step（3）Specially
To step（2）Add alkaline conditioner in gained mixed solution, regulation pH value to 7 ~ 8 stirs 30 ~ 80 minutes in 50 ~ 80 DEG C, so
Stand, separate, wash, dry, crush afterwards.
8. the preparation method of indium gallium zinc composite powder according to claim 7, it is characterised in that：Step（3）The alkali
Property conditioning agent be one or more kinds of in sodium hydroxide solution, potassium hydroxide solution and ammoniacal liquor.
9. the preparation method of indium gallium zinc composite powder according to claim 8, it is characterised in that：The concentration of the ammoniacal liquor
For the wt% of 10 wt% ~ 40.
10. the preparation method of indium gallium zinc composite powder according to claim 7, it is characterised in that：Step（3）Described in
Drying uses spray drying process.
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| CN201710137910.8A Pending CN107021521A (en) | 2017-03-09 | 2017-03-09 | A kind of preparation method of indium gallium zinc composite powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102959122A (en) * | 2010-08-05 | 2013-03-06 | 三菱综合材料株式会社 | Method for producing sputtering target, and sputtering target |
| CN103193262A (en) * | 2013-04-09 | 2013-07-10 | 桂林电子科技大学 | Indium-gallium-zinc oxide powder and preparation method of ceramic target thereof |
| JP2013166661A (en) * | 2012-02-14 | 2013-08-29 | Ulvac Japan Ltd | Method for producing ito powder and method for producing ito sputtering target |
| CN103482679A (en) * | 2013-07-17 | 2014-01-01 | 南开大学 | Aluminum zinc oxide (AZO) nano powder and preparation method of AZO sintered bodies |
-
2017
- 2017-03-09 CN CN201710137910.8A patent/CN107021521A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102959122A (en) * | 2010-08-05 | 2013-03-06 | 三菱综合材料株式会社 | Method for producing sputtering target, and sputtering target |
| JP2013166661A (en) * | 2012-02-14 | 2013-08-29 | Ulvac Japan Ltd | Method for producing ito powder and method for producing ito sputtering target |
| CN103193262A (en) * | 2013-04-09 | 2013-07-10 | 桂林电子科技大学 | Indium-gallium-zinc oxide powder and preparation method of ceramic target thereof |
| CN103482679A (en) * | 2013-07-17 | 2014-01-01 | 南开大学 | Aluminum zinc oxide (AZO) nano powder and preparation method of AZO sintered bodies |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
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