CN108218419A - A kind of preparation method of indium tin oxide ceramic target - Google Patents
A kind of preparation method of indium tin oxide ceramic target Download PDFInfo
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- CN108218419A CN108218419A CN201810034431.8A CN201810034431A CN108218419A CN 108218419 A CN108218419 A CN 108218419A CN 201810034431 A CN201810034431 A CN 201810034431A CN 108218419 A CN108218419 A CN 108218419A
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Abstract
The invention discloses a kind of preparation methods of indium tin oxide ceramic target, it is in ceramic body forming process, with 150 ~ 220 DEG C of 10 ~ 50min of heat preservation while to mold pressurize, realize the microcell hydro-thermal reaction between green body internal particle, reach the purpose of mass transfer, particle is round and smooth；Mold is made to be warming up to 270 ~ 400 DEG C later and continues 10 ~ 50min of heat-insulation pressure keeping at such a temperature, realize overcriticalization of an intergranular water, the inorganic matter dissolved in water is uniformly precipitated in crystal boundary, it is finally reached the effect of intercrystalline mutually " welding ", so as to effectively promote the consistency of green body sample block, help to reduce the consistency and sintering temperature of final ITO target obtained；The present invention realizes the dense sintering less than 1500 DEG C, and the crystallite dimension of obtained ITO target is 5 ~ 10 μm, and relative density is more than 99.5%, and cube phase structure of all indium oxides of internal structure is generated without any second phase substance.
Description
Technical field
The invention belongs to optoelectronic materials technologies, and in particular to one kind can be at a lower temperature（<1500 ℃）It realizes
The preparation method of the densification sintering of indium tin oxide ceramic target.
Background technology
With the oxidation phosphide material of 10 wt% doped sno_2s（Referred to as：Indium tin oxide material, Indium Tin Oxide,
ITO）Have many advantages, such as that UV Absorption, visible transparent, infrared light reflection and electrology characteristic are adjustable, in FPD, thin
It is more and more applied in the fields such as film solar cell, intelligent glass, heating glass, heat-reflecting glass.Deposition ITO at present
The technology of film is varied, wherein the most ripe with magnetron sputtering film forming, it has high film consistency, uniformity and repetition
Property it is good and received and widely used by industrial quarters the advantages that be easy to large area high speed deposition.In magnetron sputtering process, ceramics
Target play the role of it is vital, its performance and sputtering stability and final film layer photoelectric characteristic it is closely related.It is right
The basic demand of high-performance indium tin-oxide ceramic target is：High-compactness, the crystal grain of fine uniform, ingredient uniformity with
And low-resistivity.
At present, it is the means of mainstream using the ITO target of normal pressure in oxygen atmosphere or minute-pressure sintering preparation high quality, but
It is that typical ITO target sintering temperature is usually relatively high, generally at 1550 ~ 1650 DEG C, so high sintering temperature can be brought
Following problem：（1）Indium oxide and the material that tin oxide is easy vaporization at high temperature, at such high temperatures, oxygen loss increases, defect
Increase, target density is difficult to control；（2）Sintering temperature is excessively high, can promote coarse grains, and sputtering uniformity reduces；（3）In high temperature
Under the conditions of, the tin element being solid-solubilized in indium oxide lattice can segregate to crystal boundary, form such as In4Sn3O12Deng the second phase, cause to make pottery
Porcelain solute segregation is no longer single indium oxide cube phase structure, brings dross and paradoxical discharge etc. unfavorable in sputtering process
It influences；（4）Excessively high sintering temperature can accelerate the volatilization of the elements such as silicon, the aluminium in burner hearth material and load bearing board, these substances
It can penetrate into sintered body, pollute ITO target, the adverse effects such as dross and paradoxical discharge can be also brought in sputtering process；（5）
Higher sintering temperature, to the more demanding of equipment, equipment price is also costly, and then influence the ultimate cost of target.
Invention content
The technical problems to be solved by the invention are in view of the deficiencies of the prior art, to provide a kind of indium tin oxide ceramics
The preparation method of target, the preparation method can be with lower temperatures（<1500 ℃）Realize the densification of indium tin oxide ceramic target
Change sintering.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of preparation of indium tin oxide ceramic target
Method includes the following steps：
Step 1: the molding of indium tin oxide ceramic body：
（1）It weighs a certain amount of high-purity tin oxide powder to mix with high-purity indium oxide powder, obtains mixed powder, the mixed powder
The mass ratio of tin oxide powder and indium oxide powder is 1 in body:9；
（2）Mixed powder is poured into the deionized water containing 0.1 ~ 3 wt% dispersants, slurry is formed by the ball milling of 8 ~ 24 h
Material；
（3）Slurry is taken out, be placed in 60 ~ 100 DEG C of baking oven dry then ground and forms dry powder after sieving with 100 mesh sieve
A；
（4）1 part of powder A is taken uniformly to be mixed containing 0 ~ 0.001 part of lewis acidic deionized water with 0.05 ~ 0.2 part, is formed aqueous
Powder B；
（5）Powder B is placed in a closed mold with heating and heat preserving function, using uniaxial press to mould pressurizing, with 2
Pressure is risen to 50 ~ 300 MPa by the rate of pressure rise of ~ 5 MPa/s, while opens heating function, and mold is made to be warming up to 150 ~ 220
DEG C and under 50 ~ 300 MPa pressure keep the temperature 10 ~ 50 min, mold is then made to be warming up to 270 ~ 400 DEG C and in 50 ~ 300 MPa
10 ~ 50 min are kept the temperature under pressure, hereafter natural cooling mold, release after mold temperature is cooled to room temperature is removed from the molds
Green body sample block C；
（6）Green body sample block C is placed in 60 ~ 100 DEG C of baking oven the dry not aqueous green body D of formation, green body D is indium tin oxygen
Compound ceramic body, relative density are 65 ~ 80 %；
Step 2: the high temperature sintering of indium tin oxide ceramic body：
Green body D is placed in atmosphere chamber type electric resistance furnace, oxygen pressure is passed through in oxygen to stove into stove up to 0.01 ~ 0.1 MPa, so
Regulation resistance stove afterwards makes the furnace temperature of resistance furnace rise to first step setting since room temperature with the heating rate of 0.5 ~ 10 DEG C/min
900 ~ 1100 DEG C of temperature simultaneously keeps the temperature 30 ~ 90 min, then the furnace temperature of resistance furnace is made to be risen to the heating rate of 10 ~ 100 DEG C/min
1350 ~ 1480 DEG C of second step set temperature simultaneously keeps the temperature 60 ~ 300 min, finally makes the furnace temperature of resistance furnace with 0.5 ~ 10 DEG C/min
Rate of temperature fall be down to room temperature, obtain indium tin oxide ceramic semi-finished product；
Step 3: by the cutting of indium tin oxide ceramic semi-finished product, predetermined size is polished into get to the indium tin with high-compactness
Oxide ceramics target, relative density are more than 99.5 %.
Preferably, the crystalline form of high-purity indium oxide powder be cube phase structure, grain size be 200 ~ 500 nm, purity
>99.99 %。
Preferably, the grain size of high-purity tin oxide powder is 50 ~ 200 nm, purity>99.99 %.
Preferably, the dispersant is one kind in polyvinylpyrrolidone, polyvinyl alcohol and carboxymethyl cellulose
Or two kinds.
Preferably, the lewis acid is one or both of nitric acid, citric acid and acetic acid.
Preferably, the mold is planar targets mold or rotary target material mold.
Compared with prior art, the advantage of the invention is that：
（1）In indium tin oxide ceramic body forming process, with 150 ~ 220 DEG C of heat preservations 10 ~ 50 while to mold pressurize
Min realizes the microcell hydro-thermal reaction between green body internal particle, reaches the purpose of mass transfer, particle is round and smooth；Make mold liter later
Temperature continues 10 ~ 50 min of heat-insulation pressure keeping to 270 ~ 400 DEG C and at such a temperature, realizes overcriticalization of an intergranular water, molten in water
The inorganic matter of solution is uniformly precipitated in crystal boundary, is finally reached the effect of intercrystalline mutually " welding ", so as to effectively promote green body sample block
Consistency, help to reduce the consistency and sintering temperature of final obtained ITO target；
（2）In the method for the present invention, the sintering temperature of indium tin oxide ceramic body is less than 1500 DEG C, relative to traditional sintering
Technique, the method for the present invention realize the dense sintering less than 1500 DEG C, and the crystallite dimension of obtained ITO target is 5 ~ 10 μm,
Relative density is more than 99.5 %, and cube phase structure of all indium oxides of target internal structure is led without any high temperature sintering
Cause the second phase substance generate, these characteristics be beneficial to target in follow-up coating process stablize, equably deposition ITO it is thin
Film；
（3）The method of the present invention can be reduced further and agglomerating plant, burner hearth material are wanted to the of less demanding of agglomerating plant
It asks, so as to further reduce the manufacturing cost of indium tin oxide ceramic target.
Description of the drawings
Fig. 1 is the SEM microsctructural photographs of existing commercially available ITO target；
Fig. 2 is the SEM microsctructural photographs of the ITO target of embodiment 1；
Fig. 3 is the XRD analysis curve of the ITO target of embodiment 1.
Specific embodiment
The present invention is described in further detail below in conjunction with attached drawing embodiment.
The preparation method of the indium tin oxide ceramic target of embodiment 1, includes the following steps：
Step 1: the molding of indium tin oxide ceramic body：
（1）It weighs a certain amount of high-purity indium oxide powder to mix with high-purity tin oxide powder, obtains mixed powder, the mixed powder
The mass ratio of tin oxide powder and indium oxide powder is 1 in body:9, wherein, the crystalline form of high-purity indium oxide powder is cubic phase knot
Structure, grain size be 250 nm, purity>99.99 %；The grain size of high-purity tin oxide powder be 50 nm, purity>99.99 %；
（2）Mixed powder is poured into the deionized water containing 1.5 wt% polyvinylpyrrolidones, is formed by the ball milling of 12 h
Slurry；
（3）Slurry is taken out, be placed in 80 DEG C of baking oven dry then ground and forms dry powder A after sieving with 100 mesh sieve；
（4）1 part of powder A is taken uniformly to be mixed with 0.1 part of deionized water containing 0.0005 part of acetic acid, forms aqueous powder B；
（5）Powder B is placed in a closed planar targets mold with heating and heat preserving function, using uniaxial press to mold
Pressurization, rises to 80 MPa by pressure, while open heating function with the rate of pressure rise of 2 MPa/s, mold is made to be warming up to 150 DEG C
And keep the temperature 45 min under 80 MPa pressure, mold is then made to be warming up to 300 DEG C and keep the temperature 45 min under 80 MPa pressure,
Hereafter natural cooling mold, release after mold temperature is cooled to room temperature are removed from the molds green body sample block C；
（6）Green body sample block C is placed in 85 DEG C of baking oven the dry not aqueous green body D of formation, green body D is indium tin oxide
Ceramic body；
Step 2: the high temperature sintering of indium tin oxide ceramic body：
Green body D is placed in atmosphere chamber type electric resistance furnace, oxygen pressure in oxygen to stove is passed through into stove and, up to 0.05 MPa, is then adjusted
Resistance furnace is saved, the furnace temperature of resistance furnace is made to rise to first step set temperature 1000 since room temperature with the heating rate of 1 DEG C/min
DEG C and keep the temperature 80 min, then the furnace temperature of resistance furnace is made to rise to 1420 DEG C of second step set temperature with the heating rate of 15 DEG C/min
And 180 min are kept the temperature, the furnace temperature of resistance furnace is finally made to be down to room temperature with the rate of temperature fall of 8 DEG C/min, obtains indium tin oxide pottery
Porcelain semi-finished product；
Step 3: by the cutting of indium tin oxide ceramic semi-finished product, predetermined size is polished into get to the indium tin with high-compactness
Oxide ceramics target sample.
The preparation method of the indium tin oxide ceramic target of embodiment 2, includes the following steps：
Step 1: the molding of indium tin oxide ceramic body：
（1）It weighs a certain amount of high-purity indium oxide powder to mix with high-purity tin oxide powder, obtains mixed powder, the mixed powder
The mass ratio of tin oxide powder and indium oxide powder is 1 in body:9, wherein, the crystalline form of high-purity indium oxide powder is cubic phase knot
Structure, grain size be 350 nm, purity>99.99 %；The grain size of high-purity tin oxide powder be 150 nm, purity>99.99 %；
（2）Mixed powder is poured into the deionized water containing 0.5 wt% polyvinyl alcohol, slurry is formed by the ball milling of 8 h；
（3）Slurry is taken out, be placed in 60 DEG C of baking oven dry then ground and forms dry powder A after sieving with 100 mesh sieve；
（4）1 part of powder A is taken uniformly to be mixed with 0.05 part of deionized water containing 0.0008 part of nitric acid, forms aqueous powder B；
（5）Powder B is placed in a closed rotary target material mold with heating and heat preserving function, using uniaxial press to mold
Pressurization, rises to 150 MPa by pressure, while open heating function with the rate of pressure rise of 3 MPa/s, mold is made to be warming up to 180 DEG C
And 30 min are kept the temperature under 150 MPa pressure, mold is then made to be warming up to 300 DEG C and keep the temperature 30 under 150 MPa pressure
Min, hereafter natural cooling mold, release after mold temperature is cooled to room temperature are removed from the molds green body sample block C；
（6）Green body sample block C is placed in 70 DEG C of baking oven the dry not aqueous green body D of formation, green body D is indium tin oxide
Ceramic body；
Step 2: the high temperature sintering of indium tin oxide ceramic body：
Green body D is placed in atmosphere chamber type electric resistance furnace, oxygen pressure in oxygen to stove is passed through into stove and, up to 0.06 MPa, is then adjusted
Resistance furnace is saved, the furnace temperature of resistance furnace is made to rise to 900 DEG C of first step set temperature since room temperature with the heating rate of 3 DEG C/min
And 60 min are kept the temperature, then the furnace temperature of resistance furnace is made to rise to 1350 DEG C of second step set temperature simultaneously with the heating rate of 25 DEG C/min
120 min are kept the temperature, the furnace temperature of resistance furnace is finally made to be down to room temperature with the rate of temperature fall of 4 DEG C/min, obtain indium tin oxide ceramics
Semi-finished product；
Step 3: by the cutting of indium tin oxide ceramic semi-finished product, predetermined size is polished into get to the indium tin with high-compactness
Oxide ceramics target sample.
The preparation method of the indium tin oxide ceramic target of embodiment 3, includes the following steps：
Step 1: the molding of indium tin oxide ceramic body：
（1）It weighs a certain amount of high-purity indium oxide powder to mix with high-purity tin oxide powder, obtains mixed powder, the mixed powder
The mass ratio of tin oxide powder and indium oxide powder is 1 in body:9, wherein, the crystalline form of high-purity indium oxide powder is cubic phase knot
Structure, grain size be 450 nm, purity>99.99 %；The grain size of high-purity tin oxide powder be 200 nm, purity>99.99 %；
（2）Mixed powder is poured into the deionized water containing 2.7 wt% carboxymethyl celluloses, slurry is formed by the ball milling of 18 h
Material；
（3）Slurry is taken out, be placed in 95 DEG C of baking oven dry then ground and forms dry powder A after sieving with 100 mesh sieve；
（4）1 part of powder A is taken uniformly to be mixed with 0.18 part of deionized water containing 0.001 part of citric acid, forms aqueous powder B；
（5）Powder B is placed in a closed planar targets mold with heating and heat preserving function, using uniaxial press to mold
Pressurization, rises to 260 MPa by pressure, while open heating function with the rate of pressure rise of 5 MPa/s, mold is made to be warming up to 220 DEG C
And 20 min are kept the temperature under 260 MPa pressure, mold is then made to be warming up to 380 DEG C and keep the temperature 20 under 260 MPa pressure
Min, hereafter natural cooling mold, release after mold temperature is cooled to room temperature are removed from the molds green body sample block C；
（6）Green body sample block C is placed in 100 DEG C of baking oven the dry not aqueous green body D of formation, green body D is indium tin oxide
Ceramic body；
Step 2: the high temperature sintering of indium tin oxide ceramic body：
Green body D is placed in atmosphere chamber type electric resistance furnace, oxygen pressure in oxygen to stove is passed through into stove and, up to 0.1 MPa, is then adjusted
Resistance furnace is saved, the furnace temperature of resistance furnace is made to rise to first step set temperature 1100 since room temperature with the heating rate of 6 DEG C/min
DEG C and keep the temperature 40 min, then the furnace temperature of resistance furnace is made to rise to 1450 DEG C of second step set temperature with the heating rate of 50 DEG C/min
And 70 min are kept the temperature, the furnace temperature of resistance furnace is finally made to be down to room temperature with the rate of temperature fall of 2 DEG C/min, obtains indium tin oxide pottery
Porcelain semi-finished product；
Step 3: by the cutting of indium tin oxide ceramic semi-finished product, predetermined size is polished into get to the indium tin with high-compactness
Oxide ceramics target sample.
The color of indium tin oxide ceramic target sample made from embodiment 1 is in aterrimus.To target sample obtained, lead to
Metallography microscope sem observation its crystallite dimension is crossed, crystallite dimension is 5 ~ 10 μm；Target density, and root are measured using Archimedes method
According to the percentage between actual density and theoretical density, the relative density of target is calculated, the relative degree for obtaining target is more than 99.5
%；The phase structure of target is measured using X-ray diffractometer, cube phase structure of all indium oxides of target internal structure is found, does not have
There is the second phase substance caused by any high temperature sintering to generate.
The SEM microsctructural photographs of existing commercially available ITO target are shown in Fig. 1, indium tin oxide ceramic target made from embodiment 1
The SEM microsctructural photographs of sample are shown in Fig. 2.Comparison diagram 1 and Fig. 2 as it can be seen that the ITO target that the method for the present invention is prepared it is microcosmic
Structure has high-compactness.By density measurement, the density of two kinds of targets is 7.13 g/cm3, it is the 99.6 of theoretical density
%, but the crystallite dimension of ITO target that the method for the present invention is prepared is 5 ~ 10 μm, hence it is evident that less than existing commercially available ITO target
20 ~ 30 μm of crystallite dimension, and grain size distribution is uniform.
Fig. 3 is the XRD analysis curve of the ITO target of embodiment 1, from figure 3, it can be seen that this passes below 1500 DEG C
Low sintering ITO target all indium oxides of internal structure cube phase structure, without caused by any high temperature sintering
The second phase substance generate.
Claims (6)
1. a kind of preparation method of indium tin oxide ceramic target, it is characterised in that include the following steps：
Step 1: the molding of indium tin oxide ceramic body：
（1）It weighs a certain amount of high-purity tin oxide powder to mix with high-purity indium oxide powder, obtains mixed powder, the mixed powder
The mass ratio of tin oxide powder and indium oxide powder is 1 in body:9；
（2）Mixed powder is poured into the deionized water containing 0.1 ~ 3 wt% dispersants, slurry is formed by the ball milling of 8 ~ 24 h
Material；
（3）Slurry is taken out, be placed in 60 ~ 100 DEG C of baking oven dry then ground and forms dry powder after sieving with 100 mesh sieve
A；
（4）1 part of powder A is taken uniformly to be mixed containing 0 ~ 0.001 part of lewis acidic deionized water with 0.05 ~ 0.2 part, is formed aqueous
Powder B；
（5）Powder B is placed in a closed mold with heating and heat preserving function, using uniaxial press to mould pressurizing, with 2
Pressure is risen to 50 ~ 300 MPa by the rate of pressure rise of ~ 5 MPa/s, while opens heating function, and mold is made to be warming up to 150 ~ 220
DEG C and under 50 ~ 300 MPa pressure keep the temperature 10 ~ 50 min, mold is then made to be warming up to 270 ~ 400 DEG C and in 50 ~ 300 MPa
10 ~ 50 min are kept the temperature under pressure, hereafter natural cooling mold, release after mold temperature is cooled to room temperature is removed from the molds
Green body sample block C；
（6）Green body sample block C is placed in 60 ~ 100 DEG C of baking oven the dry not aqueous green body D of formation, green body D is indium tin oxygen
Compound ceramic body；
Step 2: the high temperature sintering of indium tin oxide ceramic body：
Green body D is placed in atmosphere chamber type electric resistance furnace, oxygen pressure is passed through in oxygen to stove into stove up to 0.01 ~ 0.1 MPa, so
Regulation resistance stove afterwards makes the furnace temperature of resistance furnace rise to first step setting since room temperature with the heating rate of 0.5 ~ 10 DEG C/min
900 ~ 1100 DEG C of temperature simultaneously keeps the temperature 30 ~ 90 min, then the furnace temperature of resistance furnace is made to be risen to the heating rate of 10 ~ 100 DEG C/min
1350 ~ 1480 DEG C of second step set temperature simultaneously keeps the temperature 60 ~ 300 min, finally makes the furnace temperature of resistance furnace with 0.5 ~ 10 DEG C/min
Rate of temperature fall be down to room temperature, obtain indium tin oxide ceramic semi-finished product；
Step 3: by the cutting of indium tin oxide ceramic semi-finished product, predetermined size is polished into get to the indium tin with high-compactness
Oxide ceramics target.
A kind of 2. preparation method of indium tin oxide ceramic target according to claim 1, it is characterised in that the height
The crystalline form of pure zirconia indium powder be cube phase structure, grain size be 200 ~ 500 nm, purity>99.99 %.
A kind of 3. preparation method of indium tin oxide ceramic target according to claim 1, it is characterised in that the height
The grain size of pure zirconia glass putty body be 50 ~ 200 nm, purity>99.99 %.
A kind of 4. preparation method of indium tin oxide ceramic target according to claim 1, it is characterised in that point
Powder is one or both of polyvinylpyrrolidone, polyvinyl alcohol and carboxymethyl cellulose.
A kind of 5. preparation method of indium tin oxide ceramic target according to claim 1, it is characterised in that the road
Lewis acid is one or both of nitric acid, citric acid and acetic acid.
A kind of 6. preparation method of indium tin oxide ceramic target according to claim 1, it is characterised in that the mould
Have for planar targets mold or rotary target material mold.
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Cited By (6)
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| CN109279873A (en) * | 2018-11-21 | 2019-01-29 | 郑州大学 | The ultralow temperature preparation method of tin indium oxide target material |
| CN111359541A (en) * | 2020-03-14 | 2020-07-03 | 桂林电子科技大学 | Device and method for preparing ceramic by hydrothermal method |
| CN111548144A (en) * | 2020-06-03 | 2020-08-18 | 福建阿石创新材料股份有限公司 | ITO sputtering target material not prone to nodulation and preparation method thereof |
| CN112456989A (en) * | 2020-12-22 | 2021-03-09 | 宁波江丰电子材料股份有限公司 | Preparation method of silicon dioxide target blank |
| CN113461420A (en) * | 2021-06-21 | 2021-10-01 | 桂林电子科技大学 | Preparation method of high-density ITO target material |
| CN113666736A (en) * | 2021-07-29 | 2021-11-19 | 广州市尤特新材料有限公司 | ITO target material applied to heterojunction and preparation method thereof |
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| CN107200562A (en) * | 2017-06-12 | 2017-09-26 | 安徽拓吉泰新型陶瓷科技有限公司 | The preparation method of ITO evaporation targets |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279873A (en) * | 2018-11-21 | 2019-01-29 | 郑州大学 | The ultralow temperature preparation method of tin indium oxide target material |
| CN109279873B (en) * | 2018-11-21 | 2021-05-25 | 郑州大学 | Ultralow temperature preparation method of indium tin oxide target material |
| CN111359541A (en) * | 2020-03-14 | 2020-07-03 | 桂林电子科技大学 | Device and method for preparing ceramic by hydrothermal method |
| CN111359541B (en) * | 2020-03-14 | 2022-04-12 | 桂林电子科技大学 | Method for preparing ceramic device by hydrothermal method |
| CN111548144A (en) * | 2020-06-03 | 2020-08-18 | 福建阿石创新材料股份有限公司 | ITO sputtering target material not prone to nodulation and preparation method thereof |
| CN111548144B (en) * | 2020-06-03 | 2022-05-17 | 福建阿石创新材料股份有限公司 | ITO sputtering target material not prone to nodulation and preparation method thereof |
| CN112456989A (en) * | 2020-12-22 | 2021-03-09 | 宁波江丰电子材料股份有限公司 | Preparation method of silicon dioxide target blank |
| CN113461420A (en) * | 2021-06-21 | 2021-10-01 | 桂林电子科技大学 | Preparation method of high-density ITO target material |
| CN113666736A (en) * | 2021-07-29 | 2021-11-19 | 广州市尤特新材料有限公司 | ITO target material applied to heterojunction and preparation method thereof |
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