CN101864555A - Conductive niobium oxide target and preparation method and application thereof - Google Patents
Conductive niobium oxide target and preparation method and application thereof Download PDFInfo
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- CN101864555A CN101864555A CN200910049242A CN200910049242A CN101864555A CN 101864555 A CN101864555 A CN 101864555A CN 200910049242 A CN200910049242 A CN 200910049242A CN 200910049242 A CN200910049242 A CN 200910049242A CN 101864555 A CN101864555 A CN 101864555A
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Abstract
The invention relates to a conductive niobium oxide target and a preparation method and application thereof. The niobium oxide target consists of NbOx, wherein x is more than 0.05 and less than 2.5, and according to the Archimedes method, the relative density of the niobium oxide target is not lower than 99 weight percent, the crystal structure is of a cubic crystal shape, the tensile strength is 10-20MPa, the Young's modulus is 1500-2800MPa and the resistivity is 0.03-1Omega.cm. The average transmittance of the film prepared with the conductive niobium oxide target is more than 94 percent within the visible spectral range. The preparation method comprises the following steps: mixing niobium pentoxide powder and niobium powder; filling the mixture into a die, placing the die into a sintering furnace, and carrying out pressure sintering in the inert or vacuum environment; and maintaining the temperature for 8-15 hours under the constant temperature and the constant pressure, and releasing the pressure, thereby obtaining the niobium oxide target. The invention has the advantages that the prepared niobium oxide target has excellent electrical conductivity, and the film with a high refractive index can be prepared through DC sputtering and intermediate-frequency sputtering.
Description
Technical field
The present invention relates to a kind of photoelectric material, relate to a kind of conductive niobium oxide target, preparation method and application thereof specifically.
Background technology
High refractive index film has higher transmissivity to visible light, can be applied in aspects such as liquid-crystal display (LCD), plasma display (PDP), touch-screen (Touch Panel), electroluminescent display (LED), thin-film solar cells, optical mirror slip.At present, people have developed multiple high-index materials such as metal titanium, metal niobium, metal zirconium, titanium dioxide and Niobium Pentxoxide, prepare high refractive index film by adopting magnetron sputtering method.Magnetron sputtering generally is divided into two kinds: d.c. sputtering and radio-frequency sputtering, and wherein d.c. sputtering is merely able to the sputter electro-conductive material, but its equipment principle is simple, and when splash-proofing sputtering metal, its speed is also fast; And the use range of radio-frequency sputtering is more extensive, but except that the sputter electro-conductive material, but the also non-conductive material of sputter also can carry out reactive sputtering simultaneously and prepare compound-materials such as oxide compound, nitride and carbide.Because metal targets need adopt reduction reaction could generate sull when adopting sputtering method to produce high refractive index film, technology more complicated and be difficult to obtain the film of excellent properties, and ordinary oxide is insulating material in the ordinary course of things, can only adopt radio-frequency sputtering technology if adopt titanium dioxide or Niobium Pentxoxide target to prepare high refractive index film, be difficult to obtain higher sputter rate.
Summary of the invention
The purpose of this invention is to provide a kind of conductive niobium oxide target, this target can adopt intermediate frequency or the direct current method of penetrating to prepare high refractive index film.
Another object of the present invention provides a kind of method for preparing above-mentioned conductive niobium oxide target.
The present invention also provides the purposes of above-mentioned niobium oxide target.
The object of the present invention is achieved like this:
A kind of conductive niobium oxide target, described target is by NbO
xConstitute, 0.05＜X＜2.5, described target is measured its relative density by Archimedes's method and is not less than 99wt%, crystalline structure is a cubic-crystal, tensile strength is 10～20Mpa, young's modulus is 1500～2800Mpa, and target resistivity is 0.03～1 Ω cm, the film of making at the visible spectrum range average transmittance more than 94%.
Above-mentioned preparation method is as follows:
(1) material mixing
Take by weighing purity and be not less than 99.99% Niobium Pentxoxide powder and purity and be not less than 99.99% metal niobium powder, mix mutually, wherein: the Niobium Pentxoxide content of powder is 90～99wt%, and the metal niobium content of powder is 1～10wt%;
(2) sintering
With the mould of packing into of gained mixture in the step (1), put into sintering oven, under inertia or vacuum environment, carry out pressure sintering, wherein:
Sintering temperature is 950～1100 ℃,
Sintering pressure is 15～30Mpa,
Sintering time is 20～30 hours;
(3) release
Holding temperature, pressure are constant, constant temperature and pressure insulation 8～15 hours down, and release obtains niobium oxide target.
Wherein, inert environments is helium or argon gas described in the step (2).
The prepared conductive niobium oxide target of the present invention can be used for the d.c. sputtering method and prepares high refractive index film.
The prepared conductive niobium oxide target of the present invention can be used for the intermediate frequency sputtering method and prepares high refractive index film.
The preparation method of niobium oxide target provided by the present invention, by reducing the content of oxygen in the chemical molecular formula, make the niobium oxide target with satisfactory electrical conductivity, the target that makes can prepare in the visible spectrum range average light transmittance by the method for d.c. sputtering and middle RF sputtering at the high refractive index film more than 94%.
The enforcement of above-mentioned niobium oxide target obtains checking in an embodiment.
Embodiment
Further describe the present invention by the following examples, but be not limited thereto.
Embodiment 1
(1) material mixing
Take by weighing purity and be 20 kilograms in 99.99% Niobium Pentxoxide powder, purity is 1.6 kilograms in 99.99% metal niobium powder, and thorough mixing ball milling 3 hours mixes it mutually;
(2) sintering
With the graphite jig of packing into of gained mixture in the step (1), put into sintering oven, under vacuum environment, carry out pressure sintering, wherein: sintering temperature is 1100 ℃, and sintering pressure is 19Mpa, and sintering time is 25 hours.
(3) release
1100 ℃ of holding temperatures, pressure 19Mpa, constant temperature and pressure insulation 10 hours, release obtains niobium oxide target.
Analyze:
(1) testing the relative density that draws target by Archimedes's method is 99.3%;
(2) chemical molecular formula of target being analyzed the gained target by XRD is Nb
2O
4.93So, x=5-4.93, x=0.07;
(3) adopting 4 probe resistance instrument test gained target resistivity is 0.15 Ω cm.
Embodiment 2
(1) material mixing
Take by weighing purity and be 30 kilograms in 99.99% Niobium Pentxoxide powder, purity is 1.5 kilograms in 99.99% metal niobium powder, and thorough mixing ball milling 5 hours mixes it mutually;
(2) sintering
With the graphite jig of packing into of gained mixture in the step (1), put into sintering oven, under vacuum environment, carry out pressure sintering, wherein: sintering temperature is 980 ℃, and sintering pressure is 25Mpa, and sintering time is 22 hours.
(3) release
980 ℃ of holding temperatures, pressure 25Mpa, constant temperature and pressure insulation 12 hours, release obtains niobium oxide target.
Analyze:
(1) testing the relative density that draws target by Archimedes's method is 99.2%;
(2) chemical molecular formula of target being analyzed the gained target by XRD is Nb
2O
4.9So, x=0.1;
(3) adopting 4 probe resistance instrument test gained target resistivity is 0.06 Ω cm.
Embodiment 3
(1) material mixing
Take by weighing purity and be 40 kilograms in 99.99% Niobium Pentxoxide powder, purity is 3 kilograms in 99.99% metal niobium powder, and thorough mixing ball milling 5 hours mixes it mutually;
(2) sintering
With the graphite jig of packing into of gained mixture in the step (1), put into sintering oven, under ar gas environment, carry out pressure sintering, wherein: sintering temperature is 1050 ℃, and sintering pressure is 20Mpa, and sintering time is 21 hours.
(3) release
1050 ℃ of holding temperatures, pressure 20Mpa, constant temperature and pressure insulation 14 hours, release obtains niobium oxide target.
Analyze:
(1) testing the relative density that draws target by Archimedes's method is 99.25%;
(2) chemical molecular formula of target being analyzed the gained target by XRD is Nb
2O
4.32So, x=0.18;
(3) adopting 4 probe resistance instrument test gained target resistivity is 0.08 Ω cm.
Embodiment 4
(1) material mixing
Take by weighing purity and be 40 kilograms in 99.99% Niobium Pentxoxide powder, purity is 4 kilograms in 99.99% metal niobium powder, and thorough mixing ball milling 5 hours mixes it mutually;
(2) sintering
With the graphite jig of packing into of gained mixture in the step (1), put into sintering oven,
VacuumCarry out pressure sintering under (vacuum, argon gas or helium) environment, wherein: sintering temperature is 1080 ℃, and sintering pressure is 28Mpa, and sintering time is 28 hours.
(3) release
1080 ℃ of holding temperatures, pressure 20Mpa, constant temperature and pressure insulation 11 hours, release obtains niobium oxide target.
Analyze:
(1) testing the relative density that draws target by Archimedes's method is 99.5%;
(2) chemical molecular formula of target being analyzed the gained target by XRD is Nb
2O
4.985So, x=0.015;
(3) adopting 4 probe resistance instrument test gained target resistivity is 0.06 Ω cm.
Claims (5)
1. conductive niobium oxide target, it is characterized in that: described target is by NbO
xConstitute, 0.05＜X＜2.5, described target is measured its relative density by Archimedes's method and is not less than 99wt%, crystalline structure is a cubic-crystal, tensile strength is 10～20Mpa, young's modulus is 1500～2800Mpa, and target resistivity is 0.03～1 Ω cm, the film of making at the visible spectrum range average transmittance more than 94%.
2. the preparation method of conductive niobium oxide target as claimed in claim 1 is characterized in that this preparation method is as follows:
(1) material mixing
Take by weighing purity and be not less than 99.99% Niobium Pentxoxide powder and purity and be not less than 99.99% metal niobium powder, mix mutually, wherein: the Niobium Pentxoxide content of powder is 90～99wt%, and the metal niobium content of powder is 1～10wt%;
(2) sintering
With the mould of packing into of gained mixture in the step (1), put into sintering oven, under inertia or vacuum environment, carry out pressure sintering, wherein:
Sintering temperature is 950～1100 ℃,
Sintering pressure is 15～30Mpa,
Sintering time is 20～30 hours;
(3) release
Holding temperature, pressure are constant, constant temperature and pressure insulation 8～15 hours down, and release obtains niobium oxide target.
3. preparation method as claimed in claim 2 is characterized in that: inert environments is helium or argon gas described in the step (2).
4. niobium oxide target as claimed in claim 1 or 2 prepares application in the high refractive index film in the d.c. sputtering method.
5. niobium oxide target as claimed in claim 1 or 2 prepares application in the high refractive index film at the intermediate frequency sputtering method.
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| CN102659405A (en) * | 2012-04-06 | 2012-09-12 | 西北稀有金属材料研究院 | Preparation method of high-density niobium oxide sputtering target material |
| CN103045995A (en) * | 2012-12-19 | 2013-04-17 | 西北稀有金属材料研究院 | Rotary niobium oxide target material and preparation method thereof |
| CN103572236A (en) * | 2013-11-06 | 2014-02-12 | 河北东同光电科技有限公司 | High-performance niobium oxide target material and preparation method thereof |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN104831243A (en) * | 2015-04-16 | 2015-08-12 | 厦门映日新材料科技有限公司 | Low resistivity niobium-doped niobium oxide sputtering rotation target material and preparation method thereof |
| CN105074046A (en) * | 2013-02-26 | 2015-11-18 | 三菱综合材料株式会社 | Niobium oxide sputtering target, production method therefor, and niobium oxide film |
| WO2016056352A1 (en) * | 2014-10-06 | 2016-04-14 | Ｊｘ金属株式会社 | Niobium oxide sintered compact, sputtering target comprising sintered compact, and method for manufacturing niobium oxide sintered compact |
| CN105506549A (en) * | 2015-12-30 | 2016-04-20 | 中国建材国际工程集团有限公司 | Method for preparing niobium pentoxide thin film through pulse direct current sputtering |
| US10347471B2 (en) * | 2012-11-13 | 2019-07-09 | Jx Nippon Mining & Metals Corporation | NbO2 sintered compact, sputtering target comprising the sintered compact, and method of producing NbO2 sintered compact |
| CN110643967A (en) * | 2019-10-24 | 2020-01-03 | 苏师大半导体材料与设备研究院(邳州)有限公司 | Semiconductor film and preparation method thereof |
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| CN102659405A (en) * | 2012-04-06 | 2012-09-12 | 西北稀有金属材料研究院 | Preparation method of high-density niobium oxide sputtering target material |
| US10347471B2 (en) * | 2012-11-13 | 2019-07-09 | Jx Nippon Mining & Metals Corporation | NbO2 sintered compact, sputtering target comprising the sintered compact, and method of producing NbO2 sintered compact |
| CN103045995A (en) * | 2012-12-19 | 2013-04-17 | 西北稀有金属材料研究院 | Rotary niobium oxide target material and preparation method thereof |
| CN103045995B (en) * | 2012-12-19 | 2015-08-05 | 西北稀有金属材料研究院 | A kind of Rotary niobium oxide target material and preparation method thereof |
| CN105074046A (en) * | 2013-02-26 | 2015-11-18 | 三菱综合材料株式会社 | Niobium oxide sputtering target, production method therefor, and niobium oxide film |
| CN103572236B (en) * | 2013-11-06 | 2016-03-02 | 河北东同光电科技有限公司 | A kind of High-performance niobium oxide target material and preparation method thereof |
| CN103572236A (en) * | 2013-11-06 | 2014-02-12 | 河北东同光电科技有限公司 | High-performance niobium oxide target material and preparation method thereof |
| WO2016056352A1 (en) * | 2014-10-06 | 2016-04-14 | Ｊｘ金属株式会社 | Niobium oxide sintered compact, sputtering target comprising sintered compact, and method for manufacturing niobium oxide sintered compact |
| JPWO2016056352A1 (en) * | 2014-10-06 | 2017-04-27 | Ｊｘ金属株式会社 | Niobium oxide sintered body, sputtering target comprising the sintered body, and method for producing niobium oxide sintered body |
| US20170309460A1 (en) * | 2014-10-06 | 2017-10-26 | Jx Nippon Mining & Metals Corporation | Niobium oxide sintered compact, sputtering target formed from said sintered compact, and method of producing niobium oxide sintered compact |
| KR101913052B1 (en) * | 2014-10-06 | 2018-10-29 | 제이엑스금속주식회사 | Niobium oxide sintered compact, sputtering target comprising sintered compact, and method for manufacturing niobium oxide sintered compact |
| US10593524B2 (en) | 2014-10-06 | 2020-03-17 | Jx Nippon Mining & Metals Corporation | Niobium oxide sintered compact, sputtering target formed from said sintered compact, and method of producing niobium oxide sintered compact |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN104831243A (en) * | 2015-04-16 | 2015-08-12 | 厦门映日新材料科技有限公司 | Low resistivity niobium-doped niobium oxide sputtering rotation target material and preparation method thereof |
| CN105506549A (en) * | 2015-12-30 | 2016-04-20 | 中国建材国际工程集团有限公司 | Method for preparing niobium pentoxide thin film through pulse direct current sputtering |
| CN110643967A (en) * | 2019-10-24 | 2020-01-03 | 苏师大半导体材料与设备研究院(邳州)有限公司 | Semiconductor film and preparation method thereof |
| CN111606708A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Low-resistivity niobium pentoxide hot-pressing target material and preparation method thereof |
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Application publication date: 20101020 |