CN116143512B - High-purity titanium dioxide planar target material and preparation method thereof - Google Patents
High-purity titanium dioxide planar target material and preparation method thereof Download PDFInfo
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- CN116143512B CN116143512B CN202310115496.6A CN202310115496A CN116143512B CN 116143512 B CN116143512 B CN 116143512B CN 202310115496 A CN202310115496 A CN 202310115496A CN 116143512 B CN116143512 B CN 116143512B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 68
- 239000013077 target material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- 239000010439 graphite Substances 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 8
- 229910052738 indium Inorganic materials 0.000 claims description 8
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000009489 vacuum treatment Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 238000003825 pressing Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000006057 Non-nutritive feed additive Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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Abstract
The invention discloses a high-purity titanium dioxide planar target and a preparation method thereof, and belongs to the technical field of semiconductors. The preparation method of the high-purity titanium dioxide planar target material does not add any auxiliary agent at all, and the high-purity titanium dioxide planar target material is prepared only through the steps of sintering, pressing and the like. The method also does not need special equipment or complicated processing procedures, and can ensure that the density and purity of the finally prepared product reach the use level after ensuring that the purity of the raw materials reaches the standard.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a high-purity titanium dioxide planar target and a preparation method thereof.
Background
The titanium dioxide planar target is an important raw material for preparing AR glass (anti-reflection and anti-reflection glass), and in the preparation process of the AR glass, a layer of titanium dioxide film is required to be sputtered on common glass by the titanium dioxide planar target. In order to make the film have excellent light transmittance and high refractive index, the titanium dioxide planar target material used for preparation needs to have higher density and purity, but in the prior art, certain processing aids are often introduced for processing properties and density such as formability, stability and the like of the target material, and the purity of the prepared planar target material is influenced by the aids, so that the processing properties, the density and the purity of the target material are difficult to be simultaneously considered.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide a preparation method of a high-purity titanium dioxide planar target, which is a method for preparing the high-purity titanium dioxide planar target by steps of sintering, pressing and the like without adding any auxiliary agent. The method also does not need special equipment or complicated processing procedures, and can ensure that the density and purity of the finally prepared product reach the use level after ensuring that the purity of the raw materials reaches the standard.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the high-purity titanium dioxide planar target comprises the following steps:
(1) Placing 4N titanium dioxide powder into a graphite die, maintaining the pressure for 5-10 min under the pressure of 50-100T, and then decompressing to 5-10T;
(2) Vacuum treatment is carried out on the graphite mould until the vacuum degree is less than 10Pa, then the graphite mould is heated to 900-1000 ℃ for 10-60 min, and then the graphite mould is heated to 1000-1200 ℃ for 30-120 min;
(3) Pressurizing the graphite mold to 250-300T, maintaining the pressure for 1-3 h, cooling and introducing protective atmosphere, and cutting and polishing the obtained coarse target;
(4) And (3) heating the crude target material obtained in the step (3) to 1500-1600 ℃ in a sealing way under normal pressure, preserving heat for 10-50 h, and cooling to room temperature to obtain the high-purity titanium dioxide planar target material.
In the preparation method of the high-purity titanium dioxide planar target material, in order to avoid the influence of an auxiliary agent introduced by the traditional processing technology on the purity of the target material product, 4N-purity titanium dioxide powder is used as a raw material, and then the powder is subjected to special program treatment at specific pressure and temperature to be converted into the planar target material, the operation steps are simple, no additional special equipment is needed, in the process, the pre-pressing process can effectively remove gas impurities in the raw material titanium dioxide powder, and the subsequent vacuum treatment and two-stage heating processes can effectively reduce the melting point of the powder, so that the density of the prepared target material is effectively improved; and the final pressure maintaining process can further improve the density of the product. In the pressure maintaining and heat preserving processes, if the set temperature or pressure is improper, the quality of the planar target is affected, and the inventor researches that the obtained titanium dioxide planar target has enough purity and the density can reach 4.2g/cm by adopting the parameter interval defined by the invention 3 The above.
Preferably, in the step (2), the heating rate is 5 to 10 ℃/min.
The temperature rising rate is moderate, so that the pre-pressed coarse target material can be heated uniformly, and the situation that the coarse target material is cracked due to uneven local heating is avoided.
Preferably, in the step (3), the temperature after cooling is less than 500 ℃, and a protective atmosphere is introduced until the temperature of the graphite mold is cooled to room temperature.
Preferably, in the step (4), the heating rate during heating is 1-10 ℃/min, and the cooling rate during cooling is 5-10 ℃/min.
Preferably, in the step (4), the obtained high-purity titanium dioxide planar target is further subjected to the following treatment: the high-purity titanium dioxide planar target is subjected to cutting and CNC surface grinding treatment, and then is bound on the backboard by adopting indium metal.
The invention further aims at providing the planar target prepared by the preparation method of the high-purity titanium dioxide planar target.
Preferably, the density of the high-purity titanium dioxide planar target material is more than or equal to 4.2g/cm 3 The purity is more than or equal to 4N.
According to the preparation method of the product, other chemical additives are not introduced in the whole process, so that the high-purity planar target product can be prepared by using raw material titanium dioxide powder with sufficient purity, and the density of the obtained product is relatively high due to a specific pressure maintaining and heat preserving processing procedure, so that the use requirements of most planar targets can be met.
The invention has the beneficial effects that the invention provides the preparation method of the high-purity titanium dioxide planar target, which is a method for preparing the high-purity titanium dioxide planar target by steps of sintering, pressing and the like without adding any auxiliary agent. The method also does not need special equipment or complicated processing procedures, and can ensure that the density and purity of the finally prepared product reach the use level after ensuring that the purity of the raw materials reaches the standard.
Detailed Description
The present invention will be further described with reference to specific examples/comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and is intended to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents, raw materials and instruments designed in the practice and comparative examples of the present invention are common reagents, raw materials and instruments unless otherwise specified.
Example 1
An embodiment of the preparation method of the high-purity titanium dioxide planar target material comprises the following steps:
(1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 5 minutes under the pressure of 80T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, then heating is carried out at 5 ℃/min to 1000 ℃ for 30min, and then heating is carried out at 10 ℃/min to 1100 ℃ for 60min;
(3) Pressurizing the graphite mold to 250T, maintaining the pressure for 1h, cooling to below 500 ℃, closing an extraction valve, a Roots pump and a mechanical pump, introducing nitrogen into the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(4) Placing the coarse target material obtained in the step (3) into a sintering furnace, sealing the sintering furnace under normal pressure, heating to 1550 ℃ at a speed of 5 ℃/min, preserving heat for 10 hours, cooling to room temperature at a speed of 5 ℃/min after preserving heat, and obtaining the high-purity titanium dioxide planar target material, cutting the high-purity titanium dioxide planar target material, grinding the CNC surface, and binding indium metal on a backboard.
Example 2
An embodiment of the preparation method of the high-purity titanium dioxide planar target material comprises the following steps:
(1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 10 minutes under the pressure of 100T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, then heating is carried out at 10 ℃/min to 1000 ℃ for 30min, and then heating is carried out at 10 ℃/min to 1200 ℃ for 120min;
(3) Pressurizing the graphite mold to 280T, maintaining the pressure for 1h, cooling to below 500 ℃, closing an exhaust valve, a Roots pump and a mechanical pump, introducing nitrogen into the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(4) And (3) placing the crude target obtained in the step (3) into a sintering furnace, sealing the sintering furnace at normal pressure, heating to 1580 ℃ at 8 ℃/min, preserving heat for 20 hours, cooling to room temperature at a speed of 5 ℃/min after preserving heat, and obtaining the high-purity titanium dioxide planar target, cutting the high-purity titanium dioxide planar target, grinding the CNC surface, and binding indium metal on the backboard.
Example 3
An embodiment of the preparation method of the high-purity titanium dioxide planar target material comprises the following steps:
(1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 10 minutes under the pressure of 100T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, then heating is carried out at 5 ℃/min to 900 ℃ for 30min, and then heating is carried out at 10 ℃/min to 1150 ℃ for 60min;
(3) Pressurizing the graphite mold to 300T, maintaining the pressure for 1h, cooling to below 500 ℃, closing an extraction valve, a Roots pump and a mechanical pump, introducing nitrogen into the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(4) Placing the coarse target material obtained in the step (3) into a sintering furnace, sealing the sintering furnace under normal pressure, heating the coarse target material to 1600 ℃ at 8 ℃/min, preserving heat for 40 hours, cooling the coarse target material to room temperature at the rate of 8 ℃/min after the heat preservation is finished, and obtaining the high-purity titanium dioxide planar target material, cutting the high-purity titanium dioxide planar target material, grinding the CNC surface of the high-purity titanium dioxide planar target material, and binding indium metal on a backboard.
Comparative example 1
The only difference between the preparation method of the titanium dioxide planar target material and the embodiment 1 is that the preparation method is as follows: (1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 5 minutes under the pressure of 80T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, and then heating is carried out at 5 ℃ per minute to 1000 ℃ for 90min;
(3) Pressurizing the graphite mold to 250T, maintaining the pressure for 1h, cooling to below 500 ℃, closing an extraction valve, a Roots pump and a mechanical pump, introducing nitrogen into the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(4) Placing the coarse target material obtained in the step (3) into a sintering furnace, sealing the sintering furnace under normal pressure, heating to 1550 ℃ at a speed of 5 ℃/min, preserving heat for 10 hours, cooling to room temperature at a speed of 5 ℃/min after preserving heat, and obtaining the high-purity titanium dioxide planar target material, cutting the high-purity titanium dioxide planar target material, grinding the CNC surface, and binding indium metal on a backboard.
Comparative example 2
The preparation method of the titanium dioxide planar target material only differs from example 2 in that the temperature in the heat preservation of the step (4) is 1400 ℃ and the time is 5 hours.
Comparative example 3
The only difference between the preparation method of the titanium dioxide planar target and the embodiment 2 is that the temperature in the heat preservation of the step (4) is 1700 ℃.
Comparative example 4
The preparation method of the high-purity titanium dioxide planar target material only differs from the embodiment 1 in that the preparation method comprises the following steps:
(1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 5 minutes under the pressure of 80T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, and then heating is carried out at 5 ℃/min to 1100 ℃ and heat preservation is carried out for 60min;
(3) Pressurizing the graphite mold to 250T, maintaining the pressure for 1h, cooling to below 500 ℃, closing an extraction valve, a Roots pump and a mechanical pump, introducing nitrogen into the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(4) Placing the coarse target material obtained in the step (3) into a sintering furnace, sealing the sintering furnace under normal pressure, heating to 1550 ℃ at a speed of 5 ℃/min, preserving heat for 10 hours, cooling to room temperature at a speed of 5 ℃/min after preserving heat, and obtaining the high-purity titanium dioxide planar target material, cutting the high-purity titanium dioxide planar target material, grinding the CNC surface, and binding indium metal on a backboard.
Comparative example 5
The preparation method of the high-purity titanium dioxide planar target material only differs from the embodiment 1 in that the pressurizing pressure in the step (3) is 200T.
Comparative example 6
The preparation method of the high-purity titanium dioxide planar target material only differs from the embodiment 1 in that the preparation method comprises the following steps:
(1) 5.8kg of 4N titanium dioxide powder is placed into a graphite die with the diameter of D350mm, the pressure is maintained for 5 minutes under the pressure of 80T, and then the pressure is relieved to 10T;
(2) Vacuum processing is carried out on the graphite mould until the vacuum degree is less than 10Pa, then heating is carried out at 5 ℃/min to 1000 ℃ for 30min, and then heating is carried out at 10 ℃/min to 1100 ℃ for 60min; pressurizing the graphite mold to 250T while maintaining the pressure for 60min, then cooling to below 500 ℃, closing an exhaust valve, a Roots pump and a mechanical pump, introducing nitrogen gas to the graphite mold, cooling to room temperature, and cutting and polishing the obtained coarse target;
(3) Placing the coarse target material obtained in the step (3) into a sintering furnace, sealing the sintering furnace under normal pressure, heating to 1550 ℃ at a speed of 5 ℃/min, preserving heat for 10 hours, cooling to room temperature at a speed of 5 ℃/min after preserving heat, and obtaining the high-purity titanium dioxide planar target material, cutting the high-purity titanium dioxide planar target material, grinding the CNC surface, and binding indium metal on a backboard.
Effect example 1
In order to verify the quality of the high-purity titanium dioxide planar target prepared by the preparation method, the purity of each example and comparative example product is tested by ICP, the density is tested by a drainage method, the thickness of the product is measured, and the surface condition of the target is observed, and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the titanium dioxide planar target prepared by the preparation method of the invention has higher density which is more than or equal to 4.2g/cm 3 At the same time, the purity of the product is higher because no processing aid is introduced. In contrast, the same effect of the product could not be obtained by processing the titanium dioxide planar target using the parameter conditions outside the range defined by the present invention, as shown in comparative examples 1 to 6.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. The preparation method of the high-purity titanium dioxide planar target material is characterized by comprising the following steps of:
(1) Placing 4N titanium dioxide powder into a graphite die, maintaining the pressure for 5-10 min under 50-100T pressure, and then decompressing to 5-10T;
(2) Carrying out vacuum treatment on the graphite mold until the vacuum degree is less than 10Pa, then heating to 900-1000 ℃ and preserving heat for 10-60 min, and then heating to 1000-1200 ℃ and preserving heat for 30-120 min;
(3) Pressurizing the graphite mold to 250-300T, maintaining the pressure for 1-3 h, cooling and introducing protective atmosphere, and cutting and polishing the obtained coarse target;
(4) And (3) heating the crude target obtained in the step (3) to 1500-1600 ℃ in a sealing way under normal pressure, preserving heat for 10-50 h, cooling to room temperature to obtain the high-purity titanium dioxide planar target, cutting and CNC surface grinding the high-purity titanium dioxide planar target, and binding indium metal on the backboard.
2. The method for preparing a high-purity titanium dioxide planar target according to claim 1, wherein in the step (2), the heating rate is 5-10 ℃/min.
3. The method for preparing a high-purity titanium dioxide planar target according to claim 1, wherein in the step (3), the temperature after cooling is less than 500 ℃, and protective atmosphere is introduced until the temperature of the graphite mold is cooled to room temperature.
4. The method for preparing a high-purity titanium dioxide planar target according to claim 1, wherein in the step (4), the heating rate is 1-10 ℃/min during heating, and the cooling rate is 5-10 ℃/min during cooling.
5. The high-purity titanium dioxide planar target prepared by the method for preparing the high-purity titanium dioxide planar target according to any one of claims 1 to 4.
6. The high purity titanium dioxide planar target according to claim 5, wherein the density of the high purity titanium dioxide planar target is not less than 4.2g/cm 3 The purity is more than or equal to 4N.
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| JPH11172423A (en) * | 1997-12-10 | 1999-06-29 | Mitsubishi Materials Corp | Production of electrically conductive high-density titanium oxide target |
| CN1951873A (en) * | 2005-10-18 | 2007-04-25 | 北京有色金属研究总院 | Thermocompressed sintering and forming method for large size ceramic sputtering target material |
| CN104557021A (en) * | 2015-01-14 | 2015-04-29 | 河北东同光电科技有限公司 | High-compactness titanium oxide target material and preparation method thereof |
| CN105734508A (en) * | 2016-04-08 | 2016-07-06 | 有研亿金新材料有限公司 | Oxide target material and preparation method thereof |
| CN106587940A (en) * | 2016-12-02 | 2017-04-26 | 有研亿金新材料有限公司 | High-purity compact magnesium oxide target material and preparation method thereof |
| CN108203297A (en) * | 2016-12-19 | 2018-06-26 | 宁波森利电子材料有限公司 | A kind of conductive titanium oxide ceramic sputtering target material and preparation method thereof |
| CN107267930A (en) * | 2017-07-21 | 2017-10-20 | 张治国 | A kind of TiO based on electron beam evaporation technique2High transmittance high conductivity method for manufacturing thin film |
| CN107759215A (en) * | 2017-11-01 | 2018-03-06 | 苏州大学 | The method for preparing huge dielectric constant low-loss ceramic capacitor |
| CN110627481A (en) * | 2019-10-18 | 2019-12-31 | 先导薄膜材料（广东）有限公司 | High-purity Ga2O3Preparation method of target material |
| CN115124330A (en) * | 2022-07-04 | 2022-09-30 | 宁波江丰电子材料股份有限公司 | Preparation method of silicon oxide ceramic target blank |
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