CN109879667A - The preparation method of fine and close oxygen loss zinc oxide ceramics body - Google Patents
The preparation method of fine and close oxygen loss zinc oxide ceramics body Download PDFInfo
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Abstract
The present invention provides the preparation method of fine and close oxygen loss zinc oxide ceramics body, and main includes the preparation of zinc layers coating zinc oxide granulation powder, and zinc layers coating zinc oxide granulation powder prepares ceramic body and is then sintered；Wherein zinc layers coating zinc oxide granulation powder preparation process is, zinc oxide premix is added in the liquid containing dispersing agent, slurry is made, slurry is passed through into air prilling, then zinc fume is delivered to granulation zone and realizes zinc oxide granulation powder surface zinc layers cladding, wherein the formation temperature of zinc fume is 1000~1300 DEG C.Compared with prior art, the present invention realizes the preparation of fine and close oxygen loss zinc oxide ceramics body using simple method, device therefor is simple, it is low in cost, consistency is higher, and the relative density of product has lower resistivity 95% or more, by testing its resistivity < 1 Ω cm, the sputtering demand of DC and MF can satisfy.
Description
Technical field
The present invention relates to optoelectronic materials technology, in particular to one kind can be able to achieve pair while guaranteeing high-densit
The control of zinc oxide ceramics body oxygen loss rate, can be used as the target of magnetron sputtering, meet the use need of downstream light electroplating film industry
It asks.
Background technique
Zinc oxide is passing through a fixed number as a kind of environmental-friendly, rich reserves multifunctional wide forbidden band oxide material
After the degeneracy doping (such as Al, Ga, In) of amount, the transparent conductive oxide material of high light electrical property can be become
(transparent conductive oxide, TCO) has UV Absorption, visible transparent, infrared light reflection and electricity
The advantages that characteristic is adjustable is learned, in photoelectricity such as FPD, thin-film solar cells, building energy conservation Low-E glass, intelligent glass
Message area is more and more applied, can be used as transparent electrode layer in thin-film solar cells, middle dielectric layer and
Back electrode high reflection layer, the function medium layer in energy conservation Low-E glass, the transparent electrode layer of intelligent glass and household appliance glass
Infrared reflecting layer etc..The technology of deposited oxide Zinc-based film is varied at present, wherein it is the most mature with magnetron sputtering film forming, it
Have many advantages, such as high film consistency, uniformity and it is reproducible and be easy to large area high speed deposition and by industry receiving and wide
General use.In magnetron sputtering process, ceramic target plays the role of vital, its performance and sputtering stability and most
The photoelectric characteristic of telolemma layer is closely related.Basic demand to high-performance ceramic target is: the crystal grain of high-compactness, fine uniform
And the uniformity of ingredient.Recently, the new demand for development of plated film industry can realize stringent control to the Lacking oxygen of target, full
The application demand of the novel oxidized zinc function film of foot: (1) for CIGS thin film solar cell for, need to deposit one layer of intrinsic i-
ZnO, and traditional intrinsic ZnO ceramic target electric conductivity is very poor, and expensive radio frequency (RF) power supply is needed to be sputtered, and furthermore sputters
Rate is also slow, is difficult to meet the production requirement of rapid batch, it is therefore necessary to by adjusting the Lacking oxygen in ZnO crystal,
The conductivity of target is promoted, high speed deposition can be realized using direct current (DC) or intermediate frequency (MF)；(2) more in low-E plated film etc.
Layer deposition field needs ZnO target material to have certain oxygen loss rate, allows deposited film in plated film chamber body absorption one
Fixed oxygen molecule, further protects lower metal layer, and metal layer is avoided to be oxidized in coating process.
In order to control zinc oxide ceramic target oxygen loss rate content, pertinent literature gives following technology of preparing hand
Section.Wan Dongyun etc. announces a kind of with oxygen in " Chinese Optical Letters " (the 10th phases page 103102 of volume 9 in 2011)
The preparation method of the pure ZnO target material of defect, in this approach, first by dry-pressing formed ZnO green body after 1350 DEG C of sintering 4h
It takes out, is placed in a small crucible, which is placed in inverted big crucible, and carbon dust is placed between two crucibles, heats up
Carbon dust and remnant oxygen react the CO gas to be formed with reproducibility in the process, and the gas and ZnO generation reduction reaction are fallen
It sets oxygen in ZnO lattice to lose, forms the zinc oxide ceramic target with Lacking oxygen.Ming-Wei Wu et al. is in " Journal of
Alloys and Compounds " (the 650th 514-519 pages of phase in 2015) delivered and a kind of be prepared for using the method for hot isostatic pressing
Aluminium-doped zinc oxide (AZO) ceramic target with certain oxygen loss rate, in this approach, AZO green body first air conditions in
1300 DEG C of sintering 3h, so in being placed in hot isostatic apparatus, by argon pressurization, in 1250 DEG C of sintering 3h.In addition there are uses
Special atmosphere sintering furnace forms the preparation method with certain oxygen loss rate ceramic target to the reduction treatment of ceramic material.However,
The still difficult large-scale production for being applied to large scale AZO target of above-mentioned three kinds of methods, shortcoming are as follows: (1) by crucible with
And the limitation of hot isostatic apparatus cavity, it is only used for the laboratory sample processing of small size, may not apply to the big of mass
The sintering of sized ceramics target；(2) operating procedure is cumbersome, needs first to sinter into be placed in again in an other equipment after block and carries out
Secondary treatment increases the preparation cost of target indirectly；And the surface of first sintering ceramics is relatively compact to second of sintering
Middle reducing atmosphere has certain barrier effect, is easy to appear the non-uniform phenomenon of internal and surface oxygen loss and occurs, and then influences target
The uniformity of material；(3) equipment cost of hot isostatic pressing and special atmosphere sintering is higher, also will increase the cost of target preparation.
Summary of the invention
In order to solve the above technical problems, the present invention sets about from the processing of crude zinc oxide materials powder, realize zinc layers in zinc oxide
The cladding on granulation powder surface, blank forming utilize xZn+ (1-x) ZnO → ZnO in subsequent sintering process1-xDiffusion it is anti-
It answers, realizes the preparation of fine and close oxygen loss zinc oxide ceramics body.
The technical solution of the present invention is to provide a kind of preparation methods of fine and close oxygen loss zinc oxide ceramics body, mainly include zinc layers
The preparation of coating zinc oxide granulation powder, zinc layers coating zinc oxide granulation powder prepare ceramic body and are then sintered；Wherein zinc layers
Coating zinc oxide granulation powder preparation process is that zinc oxide premix is added in the liquid containing dispersing agent, and slurry is made, will starch
Then zinc fume is delivered to granulation zone and realizes zinc oxide granulation powder surface zinc layers cladding by material by air prilling, wherein
The formation temperature of zinc fume is 1000~1300 DEG C.
Further, zinc oxide premix is mixed by Zinc oxide powder and doping oxide powder, is mixed in mixture
Miscellaneous oxidate powder weight/(oxide powder and zinc weight+doping oxide powder quality)=0~10wt%；Work as doping oxide
When powder quality score is 0, zinc oxide premix is only made of Zinc oxide powder.
Further, dispersing agent mass fraction is 0.1~3wt% in the liquid containing dispersing agent, and solvent is deionized water；
Slurry is made by ball milling, Ball-milling Time is 8~for 24 hours.
Further, in zinc oxide premix Zinc oxide powder average grain diameter be 200~500nm, purity be 99.95~
99.99%；Belong to high-purity zinc oxide powder；Doping oxide is one or both of aluminium oxide, gallium oxide, indium oxide, is put down
Equal partial size is 100~400nm, and purity is 99.95~99.99%；
Further, dispersing agent is one or both of polyvinylpyrrolidone, polyvinyl alcohol, carboxymethyl cellulose；
Further, 10~100 μm of the average grain diameter of zinc layers coating zinc oxide granulation powder, 0.5~2 μm of zinc coating thickness；
Further, above-mentioned zinc layers coating zinc oxide granulation powder preparation facilities includes: the slurry that bottom has fluid injector
Material container, the carrier gas unit with gas nozzle being distributed in around fluid injector, and gas nozzle at least one, carrier gas unit
At least one and zinc fume form pond；Angle [alpha] is between the liquid stream that wherein air-flow that gas nozzle sprays and fluid injector spray
20~90 °, so that liquid particle is crushed atomization to desired partial size；
Further, the aperture of fluid injector hole is 0.5~2mm, and the flow that slurry is flowed out from hole is 0.01
~5L/min；
Further, carrier gas unit institute's gas carrier be one of argon gas or nitrogen, gas pressure be 0.8~
30MPa, the temperature for heating carrier gas is 80~120 DEG C, and slurry liquid stream is further crushed atomization, while carrier gas by carrier gas stream
With certain temperature can moisture in evaporation section liquid particles, be conducive to subsequent zinc fume in zinc oxide granulation powder particle
The attachment on surface.
Further, the relative density of ceramic body made of zinc layers coating zinc oxide granulation powder is 60~75%, is burnt
Knot process is to be raised to 1000~1250 DEG C of first step set temperature with the heating rate of 0.5~10 DEG C/min, heat preservation 30~
90min；Then 1300~1450 DEG C of second step set temperature are raised to 10~100 DEG C/min heating rate, and keep the temperature 120~
480min, is finally down to room temperature with the rate of temperature fall of 0.5~10 DEG C/min, and sintering atmosphere is one of air, nitrogen, argon gas
Or two kinds of mixing.
Further, blank forming method be cold isostatic compaction, pressure be 120~300MPa, the dwell time be 60~
600s。
The post-processing such as can fine and close oxygen loss zinc oxide ceramics body obtained be cut, be polished according to actual needs, be passed through
Black is presented in the product colour of post-processing.
The advantages of the present invention: the system of fine and close oxygen loss zinc oxide ceramics body is realized using simple method
Standby, device therefor is simple, low in cost, and consistency is higher, and the relative density of product has lower resistance 95% or more
Rate can satisfy the sputtering demand of DC and MF by testing its resistivity < 1 Ω cm.
Detailed description of the invention
Fig. 1 is the preparation facilities schematic diagram of zinc coating zinc oxide granulation powder of the present invention.
In figure, 1- slurry container, 2- slurry, 3- carrier gas, 4- gas nozzle, 5- heating coil, 61- zinc oxide pelletizing
Body, 62- zinc layers coating zinc oxide granulation powder, 7- zinc fume, 8- zinc fume form pond
Specific embodiment
The invention will be further described With reference to embodiment.
The present invention provides a kind of preparation method of fine and close oxygen loss zinc oxide ceramics body, mainly includes that zinc layers coating zinc oxide is made
The preparation of grain powder, zinc layers coating zinc oxide granulation powder prepare ceramic body and are then sintered.Wherein zinc layers coating zinc oxide is made
Grain powder preparation process is that zinc oxide premix is added in the liquid containing dispersing agent, and slurry 2 is made, slurry 2 is passed through injection
It is granulated, zinc fume 7 is then delivered to granulation zone and realizes zinc oxide granulation powder surface zinc layers cladding, wherein zinc fume 7
Formation temperature is 1000~1300 DEG C；Preparation facilities such as Fig. 1 institute of zinc layers coating zinc oxide granulation powder of the present invention
Show, comprising: bottom has the slurry container 1 of fluid injector, at least one being distributed in around fluid injector with gas nozzle 4
Carrier gas unit, form pond 8 shown in Fig. 1 for two gas nozzles 4 and zinc fume；The wherein air-flow that gas nozzle 4 sprays
Angle [alpha] is 20~90 ° between the liquid stream sprayed with fluid injector, so that the liquid particle of slurry 2 is crushed atomization to desired grain
Diameter；Carrier gas 3 and zinc fume 7 are thermally formed by heating coil 5.
As a further improvement, the aperture of fluid injector hole is 0.5~2mm, the flow that slurry 2 is flowed out from hole is
0.01~5L/min；
As a further improvement, the carrier gas 3 of carrier gas unit be one of argon gas or nitrogen, gas pressure be 0.8~
30MPa, the temperature of heating carrier gas 3 are 80~120 DEG C, and slurry liquid stream is further crushed atomization, while carrier gas 3 by carrier gas 3
With certain temperature can moisture in evaporation section liquid particles, be conducive to subsequent zinc fume 7 in zinc oxide granulation powder
The attachment on grain surface.
Embodiment 1
The present invention provides a kind of preparation method of fine and close oxygen loss zinc oxide ceramics body, and step includes:
Step 1: the preparation of zinc layers coating zinc oxide granulation powder
1. weighing a certain amount of high-purity zinc oxide powder to mix with doping oxide powder, doping oxide in mixture
Powder quality/(oxide powder and zinc weight+doping oxide powder quality)=5wt%；Wherein high-purity zinc oxide powder is averaged
Partial size is 200nm, and purity is 99.95~99.99%, and doping oxide powder is aluminium oxide, average grain diameter 100nm, purity
It is 99.95~99.99%；
2. pouring into the deionized water containing 1wt% dispersing agent after powder mixing, slurry 2 is formed by the ball milling of 8h；Its
Middle dispersing agent is polyvinylpyrrolidone；
3. slurry 2 is placed in prilling granulator shown in FIG. 1, carrier gas 3 passes through while slurry 2 is sprayed by fluid injector
Gas nozzle 4 sprays, and gas disperses liquid particle, and since gas carries certain temperature therefore can be by liquid grain
Zinc fume 7 is then formed pond 8 from zinc fume to complete to be granulated to get to zinc oxide granulation powder 61 by the moisture evaporation of son
Powder granulation zone is delivered in (temperature is maintained at 1000~1300 DEG C, convenient for the constant formation of zinc fume 7) to realize in oxygen
Change 61 surface zinc layers of zinc pelletizing cladding, forms zinc layers coating zinc oxide granulation powder 62；Obtained zinc layers coating zinc oxide is made
10~100 μm of average grain diameter, 0.5~2 μm of zinc coating thickness of grain powder 62；
Step 2: body preparation and its sintering
1. the zinc layers coating zinc oxide granulation powder 62 that step 1 is obtained is placed in mold cold etc. through 120~300MPa
Hydrostatic profile, dwell time are 60~600s, form the ceramic body that relative density is 60~75%；
2. ceramic body is placed in atmosphere (the present embodiment sintering atmosphere uses air) sintering furnace, electric furnace is opened from room temperature
Begin to be raised to 1000~1250 DEG C of first step set temperature with the heating rate of 0.5~10 DEG C/min, keeps the temperature 30~90min.Then
1300~1450 DEG C of second step set temperature are raised to the warm rate of 10~100 DEG C/min heating, and keeps the temperature 120~480min, most
Afterwards, room temperature is down to the rate of temperature fall of 0.5~10 DEG C/min；
3. by sample cutting, being polished into predetermined size, as fine and close oxygen loss zinc oxide ceramics body；After polishing, pottery
Aterrimus is presented in porcelain body color.
Embodiment 2
The present invention provides a kind of preparation method of fine and close oxygen loss zinc oxide ceramics body, and step includes:
Step 1: the preparation of zinc layers coating zinc oxide granulation powder
1. weighing a certain amount of high-purity zinc oxide powder to mix with doping oxide powder, doping oxide in mixture
Powder quality/(oxide powder and zinc weight+doping oxide powder quality)=10wt%；Wherein high-purity zinc oxide powder is averaged
Partial size is 500nm, and purity is 99.95~99.99%, and doping oxide powder is aluminium oxide and gallium oxide, and average grain diameter is
400nm, purity are 99.95~99.99%；
2. pouring into the deionized water containing 2wt% dispersing agent after powder mixing, slurry 2 is formed by the ball milling of 16h；Its
Middle dispersing agent is polyvinyl alcohol；
3. slurry 2 is placed in prilling granulator shown in FIG. 1, carrier gas 3 passes through while slurry 2 is sprayed by fluid injector
Gas nozzle 4 sprays, and gas disperses liquid particle, and since gas carries certain temperature therefore can be by liquid grain
Zinc fume 7 is then formed pond 8 from zinc fume to complete to be granulated to get to zinc oxide granulation powder 61 by the moisture evaporation of son
Powder granulation zone is delivered in (temperature is maintained at 1000~1300 DEG C, convenient for the constant formation of zinc fume 7) to realize in oxygen
Change 61 surface zinc layers of zinc pelletizing cladding, forms zinc layers coating zinc oxide granulation powder 62；Obtained zinc layers coating zinc oxide is made
10~100 μm of average grain diameter, 0.5~2 μm of zinc coating thickness of grain powder 62；
Step 2: body preparation and its sintering
1. the zinc layers coating zinc oxide granulation powder 62 that step 1 is obtained is placed in mold cold etc. through 120~300MPa
Hydrostatic profile, dwell time are 60~600s, form the ceramic body that relative density is 60~75%；
2. ceramic body is placed in atmosphere (the present embodiment sintering atmosphere uses air) sintering furnace, electric furnace is opened from room temperature
Begin to be raised to 1000~1250 DEG C of first step set temperature with the heating rate of 0.5~10 DEG C/min, keeps the temperature 30~90min.Then
1300~1450 DEG C of second step set temperature are raised to the warm rate of 10~100 DEG C/min heating, and keeps the temperature 120~480min, most
Afterwards, room temperature is down to the rate of temperature fall of 0.5~10 DEG C/min；
3. by sample cutting, being polished into predetermined size, as fine and close oxygen loss zinc oxide ceramics body；After polishing, pottery
Aterrimus is presented in porcelain body color.
Embodiment 3
The present invention provides a kind of preparation method of fine and close oxygen loss zinc oxide ceramics body, and step includes:
Step 1: the preparation of zinc layers coating zinc oxide granulation powder
1. weighing a certain amount of high-purity zinc oxide powder, the average grain diameter of high-purity zinc oxide powder is 300nm, and purity is
99.95~99.99%, doping oxide powder be aluminium oxide and indium oxide, average grain diameter 200nm, purity be 99.95~
99.99%；
2. pouring into the deionized water containing 0.5wt% dispersing agent after powder mixing, slurry 2 is formed by ball milling for 24 hours；
Wherein dispersing agent is carboxymethyl cellulose；
3. slurry 2 is placed in prilling granulator shown in FIG. 1, carrier gas 3 passes through while slurry 2 is sprayed by fluid injector
Gas nozzle 4 sprays, and gas disperses liquid particle, and since gas carries certain temperature therefore can be by liquid grain
Zinc fume 7 is then formed pond 8 from zinc fume to complete to be granulated to get to zinc oxide granulation powder 61 by the moisture evaporation of son
Powder granulation zone is delivered in (temperature is maintained at 1000~1300 DEG C, convenient for the constant formation of zinc fume 7) to realize in oxygen
Change 61 surface zinc layers of zinc pelletizing cladding, forms zinc layers coating zinc oxide granulation powder 62；Obtained zinc layers coating zinc oxide is made
10~100 μm of average grain diameter, 0.5~2 μm of zinc coating thickness of grain powder 62；
Step 2: body preparation and its sintering
1. the zinc layers coating zinc oxide granulation powder 62 that step 1 is obtained is placed in mold cold etc. through 120~300MPa
Hydrostatic profile, dwell time are 60~600s, form the ceramic body that relative density is 60~75%；
2. ceramic body is placed in atmosphere (the present embodiment sintering atmosphere uses air) sintering furnace, electric furnace is opened from room temperature
Begin to be raised to 1000~1250 DEG C of first step set temperature with the heating rate of 0.5~10 DEG C/min, keeps the temperature 30~90min.Then
1300~1450 DEG C of second step set temperature are raised to the warm rate of 10~100 DEG C/min heating, and keeps the temperature 120~480min, most
Afterwards, room temperature is down to the rate of temperature fall of 0.5~10 DEG C/min；
3. by sample cutting, being polished into predetermined size, as fine and close oxygen loss zinc oxide ceramics body；After polishing, pottery
Aterrimus is presented in porcelain body color.
Density is measured using Archimedes method and target is calculated according to the percentage between actual density and theoretical density
The relative density of relative density, target is greater than 95%, such as the ceramic target of embodiment 1, the ceramic body is close after measured
Degree is 5.553g/cm3, theoretical density 5.58g/cm3, therefore relative density is 99.5%, other embodiments relative density knot
Fruit like and be all larger than 95%.The fine and close zinc oxide ceramics body certain for doping content, change in resistance derive from oxygen
The formation in vacancy, therefore can use the resistivity of material to characterize the quantity of Lacking oxygen, by testing ceramic target of the invention
Material resistivity < 1 Ω cm, and then meet the sputtering demand of DC and MF.
The present embodiments relate to the material arrived, reagent and experimental facilities, are to meet photoelectric material unless otherwise instructed
The commercial product in field.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to scope of patent protection of the invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (11)
1. the preparation method of fine and close oxygen loss zinc oxide ceramics body, which is characterized in that mainly include zinc layers coating zinc oxide pelletizing
The preparation of body, zinc layers coating zinc oxide granulation powder prepare ceramic body and are then sintered；Wherein zinc layers coating zinc oxide pelletizing
Production procedure is that zinc oxide premix is added in the liquid containing dispersing agent, and slurry is made, and slurry is passed through air prilling,
Then zinc fume is delivered to granulation zone and realizes zinc oxide granulation powder surface zinc layers cladding, wherein the formation temperature of zinc fume
It is 1000~1300 DEG C.
2. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the zinc oxide is pre-
Mixing is mixed by Zinc oxide powder and doping oxide powder, doping oxide powder quality/(oxide powder and zinc in mixture
Weight+doping oxide powder quality)=0~10wt%.
3. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that described to contain dispersion
Dispersing agent mass fraction is 0.1~3wt% in the liquid of agent, and solvent is deionized water；Slurry, Ball-milling Time is made by ball milling
For 8~for 24 hours.
4. the preparation method of densification oxygen loss zinc oxide ceramics body as claimed in claim 2, which is characterized in that the zinc oxide is pre-
The average grain diameter of Zinc oxide powder is 200~500nm in mixing, and purity is 99.95~99.99%；Doping oxide is oxidation
One or both of aluminium, gallium oxide, indium oxide, average grain diameter are 100~400nm, and purity is 99.95~99.99%.
5. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the dispersing agent is
One or both of polyvinylpyrrolidone, polyvinyl alcohol, carboxymethyl cellulose.
6. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the zinc layers cladding
The average grain diameter of zinc oxide granulation powder is 10~100 μm, 0.5~2 μm of zinc coating thickness.
7. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the zinc layers cladding
Zinc oxide granulation powder preparation facilities includes: that bottom has the slurry container of fluid injector, is distributed in around the fluid injector
The carrier gas unit with gas nozzle, and the gas nozzle at least one, carrier gas unit at least one and zinc fume shape
Cheng Chi；Angle [alpha] is 20~90 ° between the liquid stream that wherein air-flow that the gas nozzle sprays and fluid injector spray.
8. the preparation method of densification oxygen loss zinc oxide ceramics body as claimed in claim 7, which is characterized in that the fluid injector
The aperture of hole is 0.5~2mm, and the flow that the slurry is flowed out from hole is 0.01~5L/min.
9. the preparation method of densification oxygen loss zinc oxide ceramics body as claimed in claim 7, which is characterized in that the carrier gas unit
Institute's gas carrier is one of argon gas or nitrogen, and gas pressure is 0.8~30MPa, and the temperature for heating carrier gas is 80~120
℃。
10. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the ceramic blank
The relative density of body is 60~75%, and sintering process is to be raised to first step set temperature with the heating rate of 0.5~10 DEG C/min
1000~1250 DEG C, keep the temperature 30~90min；Then second step set temperature 1300 is raised to 10~100 DEG C/min heating rate
~1450 DEG C, and 120~480min is kept the temperature, room temperature is finally down to the rate of temperature fall of 0.5~10 DEG C/min, sintering atmosphere is sky
One of gas, nitrogen, argon gas or two kinds of mixing.
11. the preparation method of densification oxygen loss zinc oxide ceramics body as described in claim 1, which is characterized in that the ceramic blank
Body formed method is cold isostatic compaction, and pressure is 120~300MPa, and the dwell time is 60~600s.
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| CN112341168A (en) * | 2020-09-23 | 2021-02-09 | 先导薄膜材料（广东）有限公司 | Rare earth doped zinc-gallium-aluminum oxide powder and preparation method thereof |
| CN113666735A (en) * | 2021-09-10 | 2021-11-19 | 山东大学 | Method for continuously regulating and controlling light absorption property of zinc oxide ceramic, zinc oxide ceramic and preparation method |
| CN113666735B (en) * | 2021-09-10 | 2022-07-05 | 山东大学 | Method for continuously regulating and controlling light absorption property of zinc oxide ceramic, zinc oxide ceramic and preparation method |
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