CN116283270A - ZnO-BaTiO 3 Preparation method of composite target material - Google Patents
ZnO-BaTiO 3 Preparation method of composite target material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 239000013077 target material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000005498 polishing Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 230000006835 compression Effects 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 19
- 239000011787 zinc oxide Substances 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000008846 dynamic interplay Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
The invention belongs to the technical field of composite target preparation, and in particular relates to ZnO-BaTiO 3 A preparation method of a composite target. The invention uses ZnO powder and BaTiO 3 Mixing the powder and the binder uniformly, drying, pressing into sheets, and then rapidly heating, sintering at high temperature and polishing to obtain ZnO-BaTiO 3 And (3) a composite target material. The ZnO-BaTiO with the purity higher than 99.95 percent and the relative density higher than 95 percent is prepared by adopting an improved normal pressure sintering process 3 A composite target; meanwhile, the preparation process of the composite target material has the advantages of greatly reduced operation steps, low cost and convenient manufacture, and is more suitable for preparing high-quality ZnO-BaTiO 3 The composite film has important academic value and wide application prospect in the fields of thermistors, photoelectric conversion, resistance change storage and the like.
Description
Technical Field
The invention belongs to the technical field of composite target preparation, and in particular relates to ZnO-BaTiO 3 A preparation method of a composite target.
Background
Zinc oxide (ZnO) is a direct band gap wide forbidden band semiconductor material, has a hexagonal wurtzite crystal structure, and a ZnO film has excellent crystal lattice, electrical and optical characteristics and unique piezoelectric coupling characteristics, and has wide application in the fields of solar cells and piezoelectric devices at present. Barium titanate (BaTiO) 3 ) Is a ferroelectric compound material, which itself hasHas excellent dielectric, piezoelectric and ferroelectric properties, and is one of the most widely used materials in electronic ceramics. Thus, from ZnO and BaTiO 3 Composite ZnO-BaTiO 3 The composite film has excellent performances and coupling characteristics in the aspects of light, electricity, magnetism and the like, is hopeful to realize multifunctionality and new physical properties, and can generate special physical phenomena through multi-degree-of-freedom coupling at the two-phase interface.
At present, common methods for preparing the composite film mainly comprise a sol-gel method, a chemical vapor deposition method, a physical vapor deposition method and the like. The physical vapor deposition method has the advantages of stable preparation process, high density and good uniformity of the obtained film, strong binding force with a substrate and the like, but the quality of the film prepared by the method is fundamentally limited by the state of a target. Thus, a high quality ZnO-BaTiO is produced 3 The key premise of the composite film is a high-quality composite target. In addition, although the single crystal target material with higher quality can be obtained by the techniques of pulling single crystal method, the complex dynamic interaction between two phases or multiple phases causes difficult acquisition of the composite target material, thereby severely restricting ZnO-BaTiO 3 And (3) preparing and researching the composite film.
Therefore, how to obtain ZnO-BaTiO with high purity, high density, good uniformity, few defects and difficult cracking 3 High quality targets become a critical scientific problem to be solved by researchers in the field.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a ZnO-BaTiO 3 The preparation method of the composite target prepares the high-quality ZnO-BaTiO with high purity and relative density of more than 95 percent by adopting an improved normal pressure sintering process 3 A composite target; thereby overcoming the defect of high quality ZnO-BaTiO prepared at present 3 The composite target material is difficult.
The invention is realized by the following technical scheme:
the first aspect of the present invention provides a ZnO-BaTiO 3 The preparation method of the composite target material specifically comprises the following steps: znO powder and BaTiO 3 The powder and the binder are mixed evenly and then,drying, pressing into sheet, quickly heating, sintering at high temperature, and polishing to obtain ZnO-BaTiO 3 And (3) a composite target material.
Preferably, the high-temperature sintering is to heat up to 400-600 ℃ at 4-6 ℃/min for 4-6 hours, and then heat up to 1200-1400 ℃ at 4-6 ℃/min for 3-4 hours.
The invention prepares ZnO-BaTiO with purity higher than 99.95 percent and relative density higher than 95 percent by adopting an improved normal pressure sintering process 3 A composite target; meanwhile, the preparation process of the composite target material has the advantages of greatly reduced operation steps, low cost and convenient manufacture, and is more suitable for preparing high-quality ZnO-BaTiO 3 The composite film has important academic value and wide application prospect in the fields of thermistors, photoelectric conversion, resistance change storage and the like.
More preferably, the Gao Wenshao knots are firstly heated to 500 ℃ at 5 ℃/min and then are preserved for 4 to 6 hours; then heating to 1200-1400 ℃ at 5 ℃/min, and preserving heat for 2-3h.
Preferably, the ZnO powder and BaTiO 3 The molar ratio of the powder is 1-3: 1 to 3.
Preferably, the ZnO powder and BaTiO 3 The granularity of the powder is 100-500 meshes.
Preferably, the binder is polyvinyl butyral solution with a mass fraction of 1-10% and the solvent is absolute ethanol.
Preferably, the drying atmosphere is air or nitrogen, the temperature is 80-120 ℃, and the pressure is 0.5-2 atmospheres.
More preferably, the drying atmosphere is atmospheric air at 100 ℃.
Preferably, the diameter of the tabletting mould used for compression is 0.5-1.5, the compression pressure is 20-60 Mpa, and the compression time is 10-15 minutes.
More preferably, the pressing is performed using a tabletting die having an internal diameter of 1 inch at a pressure of 40Mpa for 10 to 15 minutes.
In a second aspect, the invention provides ZnO-BaTiO prepared by the preparation method in the first aspect 3 And (3) a composite target material.
ZnO-BaTiO prepared by the method 3 The composite target material has high crystallization quality, good compactness, uniform components and belongs to ZnO-BaTiO with high quality 3 And (3) a composite target material.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a ZnO-BaTiO 3 The preparation method of the composite target material comprises the steps of preparing ZnO powder and BaTiO 3 Mixing the powder and the binder uniformly, drying, pressing into sheets, and then rapidly heating, sintering at high temperature and polishing. According to the invention, after the glue discharge of the prefabricated sheet is finished, the rapid temperature rise and the high-temperature sintering are directly carried out, so that the binder is discharged efficiently, the density (the relative density is more than 95%) of the target material can be effectively improved, and the prepared ZnO-BaTiO 3 The composite target material has high purity and uniform components, and reaches high quality ZnO-BaTiO 3 The standard of the composite film ensures that the composite film has important academic value and wide application prospect in the fields of thermistors, photoelectric conversion, resistance change storage and the like. In addition, the invention greatly simplifies the operation flow by adopting the improved normal pressure sintering process, and has the advantages of fewer steps, low cost and convenient manufacture. In addition, the ZnO-BaTiO prepared by the invention 3 The composite target material can be widely applied to the growth of ZnO-BaTiO by adopting the process methods of pulse laser deposition, magnetron sputtering and the like 3 The composite film has important academic value and application prospect in the fields of microelectronics, military industry, photovoltaic energy sources and the like.
Drawings
FIG. 1 is a view of ZnO-BaTiO 3 A preparation process flow chart of the composite target;
FIG. 2 is a view of ZnO-BaTiO 3 X-ray diffraction pattern of composite target;
FIG. 3 is a view of ZnO-BaTiO 3 High resolution SEM pictures of the composite targets.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1 ZnO-BaTiO 3 Preparation method of composite target material
As shown in FIG. 1, znO-BaTiO was prepared 3 The method for compounding the target material comprises the following steps:
(1) ZnO powder and BaTiO 3 Preparing and mixing the powder according to the molar ratio of 2:1, and ball-milling for 24 hours on a ball mill;
(2) Adding 15mL of PVB solution (absolute ethyl alcohol as solvent) with the mass fraction of 6% into the powder which is uniformly mixed by ball milling as a binder, fully grinding, and then drying in a normal pressure air atmosphere at 100 ℃;
(3) Placing the dried powder into a tabletting mold with the inner diameter of 1 inch, and pressing for 10 minutes under the pressure of 40 Mpa;
(4) Placing the pressed sheet into a tube furnace, keeping normal pressure in the air, heating to 500 ℃ at a speed of 5 ℃/min, and preserving heat for 6 hours to discharge the binder; then heating to 1250 ℃ at 5 ℃/min and preserving heat for 4 hours; cooling along with the furnace after heat preservation is finished; taking out ZnO-BaTiO after finishing 3 The sheet material is polished to obtain high-density ZnO-BaTiO 3 And (3) a composite target material.
To ZnO-BaTiO 3 The quality of the composite target is researched, the X-ray diffraction analysis is carried out on the target, and the target is characterized by utilizing a field emission electron microscope. As shown in figure 2, the XRD spectrum peak position of the target material is sharp and clear, and no gentle slope amorphous peak exists, which indicates that the target material has high crystallinity and good crystallization quality. As shown in fig. 3, the surface of the target material is compact, the particles are uniform and smaller, and the component uniformity is high. These results show that ZnO-BaTiO prepared in this example 3 The composite target material has high crystallization quality, good compactness, uniform components and high quality ZnO-BaTiO 3 And (3) a composite target material.
Example 2 ZnO-BaTiO 3 Preparation method of composite target material
(1) ZnO powder and BaTiO 3 Preparing and mixing the powder according to a molar ratio of 1:1, and ball-milling for 24 hours on a ball mill;
(2) Adding PVB solution (absolute ethyl alcohol as solvent) with the mass fraction of 6% into the powder which is uniformly mixed by ball milling as a binder, fully grinding, and then drying in a normal pressure air atmosphere at 100 ℃;
(3) Placing the dried powder into a tabletting mold with the inner diameter of 1 inch, and pressing for 15 minutes under the pressure of 40 Mpa;
(4) Placing the pressed sheet into a tube furnace, keeping normal pressure in the air, heating to 500 ℃ at a speed of 5 ℃/min, and preserving heat for 5 hours to discharge the binder; then heating to 1200 ℃ at 5 ℃/min and preserving heat for 3 hours; cooling along with the furnace after heat preservation is finished; taking out ZnO-BaTiO after finishing 3 The sheet material is polished to obtain high-density ZnO-BaTiO 3 And (3) a composite target material.
As in example 1, znO-BaTiO prepared in this example 3 The composite target material has high crystallization quality, good compactness, uniform components and high quality ZnO-BaTiO 3 And (3) a composite target material.
Example 3 ZnO-BaTiO 3 Preparation method of composite target material
(1) ZnO powder and BaTiO 3 Preparing and mixing the powder according to a molar ratio of 3:1, and ball-milling for 24 hours on a ball mill;
(2) Adding PVB solution (absolute ethyl alcohol as solvent) with the mass fraction of 6% into the powder which is uniformly mixed by ball milling as a binder, fully grinding, and then drying in a normal pressure air atmosphere at 100 ℃;
(3) Placing the dried powder into a tabletting mold with the inner diameter of 1 inch, and pressing for 15 minutes under the pressure of 40 Mpa;
(4) Placing the pressed sheet into a tube furnace, keeping normal pressure in the air, heating to 500 ℃ at a speed of 5 ℃/min, and preserving heat for 5 hours to discharge the binder; then rise at 5 ℃/minHeating to 1400 ℃ and preserving heat for 3 hours; cooling along with the furnace after heat preservation is finished; taking out ZnO-BaTiO after finishing 3 The sheet material is polished to obtain high-density ZnO-BaTiO 3 And (3) a composite target material.
As in example 1, znO-BaTiO prepared in this example 3 The composite target material has high crystallization quality, good compactness, uniform components and high quality ZnO-BaTiO 3 And (3) a composite target material.
Example 4 ZnO-BaTiO 3 Preparation method of composite target material
(1) ZnO powder and BaTiO 3 Preparing and mixing the powder according to a molar ratio of 3:1, and ball-milling for 24 hours on a ball mill;
(2) Adding PVB solution (absolute ethyl alcohol as solvent) with mass fraction of 6% into the powder which is uniformly mixed by ball milling as a binder, fully grinding, and then drying in nitrogen atmosphere with the temperature of 100 ℃ and the pressure of 1.5 atmospheres;
(3) Placing the dried powder into a tabletting mold with the inner diameter of 1 inch, and pressing for 12 minutes under the pressure of 50 Mpa;
(4) Placing the pressed sheet into a tube furnace, keeping normal pressure in the air, heating to 500 ℃ at a speed of 5 ℃/min, and preserving heat for 5 hours to discharge the binder; then heating to 1350 ℃ at 5 ℃/min and preserving heat for 3 hours; cooling along with the furnace after heat preservation is finished; taking out ZnO-BaTiO after finishing 3 The sheet material is polished to obtain high-density ZnO-BaTiO 3 And (3) a composite target material.
As in example 1, znO-BaTiO prepared in this example 3 The composite target material has high crystallization quality, good compactness, uniform components and high quality ZnO-BaTiO 3 And (3) a composite target material.
In summary, the invention directly and rapidly heats up and sinters at high temperature after the glue discharge of the prefabricated sheet is finished, so that the density of the target material can be effectively improved, and the prepared ZnO-BaTiO 3 The composite target material has high purity and uniform components. And the improved normal pressure sintering process has simple operation flow and less steps. ZnO-BaTiO prepared by the invention 3 The composite target material can be widely applied to miningZnO-BaTiO is grown by pulse laser deposition, magnetron sputtering and other technological methods 3 The composite film has important academic value and application prospect in the fields of microelectronics, military industry, photovoltaic energy sources and the like.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (8)
1. ZnO-BaTiO 3 A process for producing a composite target, characterized by mixing ZnO powder and BaTiO 3 Mixing the powder and the binder uniformly, drying, pressing into sheets, then rapidly heating and sintering at high temperature, and finally polishing to obtain the ZnO-BaTiO 3 And (3) a composite target material.
2. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the high-temperature sintering is to heat up to 400-600 ℃ for 4-6 hours at 4-6 ℃/min, and then heat up to 1200-1400 ℃ for 3-4 hours at 4-6 ℃/min.
3. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the ZnO powder and the BaTiO powder 3 The molar ratio of the powder is 1-3: 1 to 3.
4. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the ZnO powder and the BaTiO powder 3 The granularity of the powder is 100-500 meshes.
5. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the binder is polyvinyl butyral solution, the mass fraction is 1-10%, and the solvent is absolute ethyl alcohol.
6. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the dry atmosphere is air or nitrogen, the temperature is 80-120 ℃, and the pressure is 0.5-2 atmospheres.
7. A ZnO-BaTiO according to claim 1 3 The preparation method of the composite target material is characterized in that the diameter of a tabletting mould used for compression is 0.5-1.5, the compression pressure is 20-60 Mpa, and the compression time is 10-15 minutes.
8. ZnO-BaTiO prepared by the preparation method of any one of claims 1-7 3 And (3) a composite target material.
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| CN103964843A (en) * | 2014-05-07 | 2014-08-06 | 武汉理工大学 | Preparation method for large-size dense barium titanate ceramic target material |
| CN107162582A (en) * | 2017-05-22 | 2017-09-15 | 天津大学 | Zinc oxide doped barium calcium zirconate titanate leadless piezoelectric ceramics |
| CN112500155A (en) * | 2020-11-09 | 2021-03-16 | 中国科学院宁波材料技术与工程研究所 | Preparation method of lanthanum-doped barium titanate target |
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| CN103964843A (en) * | 2014-05-07 | 2014-08-06 | 武汉理工大学 | Preparation method for large-size dense barium titanate ceramic target material |
| CN107162582A (en) * | 2017-05-22 | 2017-09-15 | 天津大学 | Zinc oxide doped barium calcium zirconate titanate leadless piezoelectric ceramics |
| CN112500155A (en) * | 2020-11-09 | 2021-03-16 | 中国科学院宁波材料技术与工程研究所 | Preparation method of lanthanum-doped barium titanate target |
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