CN106380188A - Sintered body and amorphous thin film - Google Patents
Sintered body and amorphous thin film Download PDFInfo
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- CN106380188A CN106380188A CN201610702480.5A CN201610702480A CN106380188A CN 106380188 A CN106380188 A CN 106380188A CN 201610702480 A CN201610702480 A CN 201610702480A CN 106380188 A CN106380188 A CN 106380188A
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- 239000010409 thin film Substances 0.000 title claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 43
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 12
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 12
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 12
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 115
- 239000000843 powder Substances 0.000 claims description 104
- 239000000463 material Substances 0.000 claims description 48
- 238000007733 ion plating Methods 0.000 claims description 40
- 238000009413 insulation Methods 0.000 claims description 28
- 230000008033 biological extinction Effects 0.000 claims description 26
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 11
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052733 gallium Inorganic materials 0.000 claims description 10
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000005477 sputtering target Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 229910003069 TeO2 Inorganic materials 0.000 claims description 5
- 229910009973 Ti2O3 Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 5
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 150000002835 noble gases Chemical class 0.000 claims description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 abstract description 26
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 110
- 239000011787 zinc oxide Substances 0.000 description 53
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 32
- 229910052786 argon Inorganic materials 0.000 description 16
- 239000007789 gas Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 11
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- 238000003754 machining Methods 0.000 description 9
- 238000000576 coating method Methods 0.000 description 8
- 210000004379 membrane Anatomy 0.000 description 8
- 239000012528 membrane Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 6
- 230000000149 penetrating effect Effects 0.000 description 6
- 208000037656 Respiratory Sounds Diseases 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- 238000004017 vitrification Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 210000004276 hyalin Anatomy 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 210000000713 mesentery Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
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- 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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention discloses a sintered body and an amorphous thin film. The sintered body is characterized by containing zinc (Zn), trivalent metallic elements, germanium (Ge) and/or silicon (Si), oxygen (O). When the total content of trivalent metallic elements in terms of oxides is set as A mol%, and the total content of Ge and/or Si in terms of GeO2 and/or SiO2 is set as B mol%, 15 <= A + B <= 70. According to the present invention, the bulk resistance is low and DC sputtering may be performed. The sintered body can be used to form the amorphous thin film with low refractive index.
Description
The application be the applying date be on July 3rd, 2013, the Chinese patent application of Application No. 201310276943.2 point
Case application.
Technical field
The present invention relates to the sintered body possessing the nesa coating of good transmission of visible light and electric conductivity can be obtained
And the amorphous film with low-refraction using the making of this sintered body.
Background technology
In the past, as nesa coating, in Indium sesquioxide. add stannum obtained from film be ITO (Indium-Tin-oxide,
Indium tin oxide) film transparent and electrically conductive is excellent, is used for the purposes of the wide scopes such as various display.But, due to as master
Want the indium of composition expensive, therefore this ITO is with the presence of the problem of inferior position in terms of manufacturing cost.
In view of the foregoing, the succedaneum as ITO is it is proposed that for example using the film of zinc oxide (ZnO).Made with zinc oxide
For main component film have the advantages that cheap.Known this film exists due to the oxygen defect of the ZnO as main component
And lead to the enhanced phenomenon of electric conductivity, and if the membrane property such as electric conductivity and transmitance is approximate with ITO, the application of this material
There is the probability of increase.
In the case of utilizing visible ray in display etc., this material needs to be transparent, particularly preferably entirely visible
Optical range has high-transmission rate.In addition, light loss increases or so that the view angle dependency of display is deteriorated when refractive index is high, therefore also
Expecting refraction rate is low, and in order to improve the crackle of film and etching performance also it is desirable to be amorphous film.
The stress of amorphous film is little, is therefore not likely to produce crackle compared with crystalline film, from now on it is believed that aobvious towards flexibility
Show in device purposes and require as amorphous film.In addition, for ITO before, in order to improve resistance value and absorbance, needing to make it
Crystallization, and, when being made into amorphous, there is in short wavelength range absorption and hyaline membrane can not be formed, be therefore not suitable for
This purposes.
As the material using zinc oxide it is known that IZO (Indium sesquioxide .-zinc oxide), GZO (gallium oxide/zinc oxide), AZO (oxygen
Change aluminum-zinc oxide) etc. (patent documentation 1～3).But, although IZO can form low-resistance amorphous film, exist in shortwave
Also there is in long scope absorption and the high problem of refractive index.In addition, GZO, AZO are easily formed because ZnO is easily orientated along c-axis
Crystalline film, the stress of this crystalline film increases, and therefore haves such problems as that film is peeled off and film rupture.
In addition, Patent Document 4 discloses and wanting composition based on ZnO and fluorination alkaline earth metal compound, achieve wide cut
The transparent conductive material of refractive index.But, this material is crystalline film, cannot get the effect of amorphous film as the present invention described later
Really.In addition, Patent Document 5 discloses that refractive index is little and ratio resistance is little and the nesa coating for amorphous, but itself and this
Bright compositional system is different, there is a problem of can not adjusting refractive index and resistance value simultaneously.
Prior art literature
Patent documentation
Patent documentation 1：Japanese Unexamined Patent Publication 2007-008780 publication
Patent documentation 2：Japanese Unexamined Patent Publication 2009-184876 publication
Patent documentation 3：Japanese Unexamined Patent Publication 2007-238375 publication
Patent documentation 4：Japanese Unexamined Patent Publication 2005-219982 publication
Patent documentation 5：Japanese Unexamined Patent Publication 2007-035342 publication
Content of the invention
Invent problem to be solved
The problem of the present invention is that offer can obtain maintaining good transmission of visible light and the transparent of electric conductivity to lead
The sintered body of the amorphous film of electrolemma, particularly low-refraction.The absorbance of this thin film is high and mechanical property is excellent, accordingly, as
The protecting film of the nesa coating of display or optical device is useful.Thus, it is an object of the invention to improve optical device characteristic,
Reduce equipment cost, greatly improve the characteristic of film forming.
Means for solving the problem
In order to solve the above problems, present inventor has performed furtheing investigate, result is found as follows：By will be conventional
The nesa coatings such as ITO are substituted for material system as follows, can arbitrarily adjust resistivity and refractive index, can be true
Protect and carry out stable film forming with conventional peer-level or while higher than conventional optical characteristics using sputtering or ion plating, and then
By forming amorphous film, the characteristic of the optical device possessing this thin film can be improved and improve productivity ratio.
The present invention provides following inventions based on this discovery.
1) a kind of sintered body is it is characterised in that by zinc (Zn), trivalent metallic element, germanium (Ge) and/or silicon (Si), oxygen (O)
Constitute, if the total content of trivalent metallic element is scaled the total content of A mole of %, Ge and/or Si with GeO with oxide2And/or
SiO2When being scaled B mole of %, 15≤A+B≤70.
2) sintered body as described in above-mentioned 1) is it is characterised in that the total content of above-mentioned Ge and/or Si is 5≤B≤30.
3) as above-mentioned 1) or 2) as described in sintered body it is characterised in that the total content of above-mentioned trivalent metallic element is with trivalent
The atomic number ratio of metallic element/(Zn+ trivalent metallic element) is calculated as more than 0.1.
4) as above-mentioned 1)～3) any one of sintered body it is characterised in that above-mentioned trivalent metallic element be selected from
One or more of the group being made up of aluminum (Al), gallium (Ga), boron (B), yttrium (Y) and indium (In) element.
5) a kind of sintered body is it is characterised in that be made up of the oxide of zinc (Zn), gallium (Ga), germanium (Ge), if the content of Ga
With Ga2O3The content being scaled A mole of %, Ge is with GeO2When being scaled B mole of % and balance of ZnO, meet 15≤A+B≤50
And the condition of A >=3B/2.
6) as above-mentioned 1)～5) any one of sintered body it is characterised in that also contain with oxide weight conversion
For metal 0.1～5 weight %, forming the oxide that fusing point is less than 1000 DEG C.
7) sintered body as described in above-mentioned 6) it is characterised in that oxide that above-mentioned fusing point is less than 1000 DEG C be selected from
By B2O3、P2O5、K2O、V2O5、Sb2O3、TeO2、Ti2O3、PbO、Bi2O3、MoO3One or more of the group of composition oxide.
8) as above-mentioned 1)～7) any one of sintered body it is characterised in that relative density be more than 90%.
9) as above-mentioned 1)～8) any one of sintered body it is characterised in that bulk resistance be below 10 Ω cm.
10) a kind of sputtering target it is characterised in that use above-mentioned 1)～9) any one of sintered body.
11) a kind of ion plating material is it is characterised in that use the sintered body described in above-mentioned 5).
12) a kind of thin film is it is characterised in that by zinc (Zn), trivalent metallic element, germanium (Ge) and/or silicon (Si), oxygen (O)
Constitute, if the total content of trivalent metallic element is scaled the total content of A mole of %, Ge and/or Si with GeO with oxide2And/or
SiO2When being scaled B mole of %, 15≤A+B≤70, and be amorphous film.
13) a kind of thin film is it is characterised in that be made up of the oxide of zinc (Zn), gallium (Ga), germanium (Ge), if the content of Ga
With Ga2O3The content being scaled A mole of %, Ge is with GeO2When being scaled B mole of % and balance of ZnO, meet 15≤A+B≤50
And the condition of A >=3B/2, and it is amorphous film.
14) as above-mentioned 12) or 13) as described in thin film be scaled 0.1～5 it is characterised in that also containing with oxide weight
Weight %, formation are selected from B2O3、P2O5、K2O、V2O5、Sb2O3、TeO2、Ti2O3、PbO、Bi2O3、MoO3In the group of composition
The metal of more than one oxides.
15) as above-mentioned 12)～14) any one of thin film it is characterised in that extinction coefficient under wavelength 450nm
For less than 0.01.
16) as above-mentioned 12)～15) any one of thin film it is characterised in that the refractive index under wavelength 550nm is
2.00 it is following.
17) as above-mentioned 12)～16) any one of thin film it is characterised in that specific insulation be 1 × 10-3～1
×109Ω·cm.
18) a kind of manufacture method of sintered body, its be above-mentioned 1)～9) any one of sintered body manufacture method,
It is characterized in that, material powder is mixed, by obtained mixed-powder under noble gases or vacuum atmosphere, 1000 DEG C～
Carry out pressure sintering at 1500 DEG C, or by after obtained mixed-powder press molding, by this formed body in noble gases or
Under vacuum atmosphere, carry out at 1000 DEG C～1500 DEG C normal pressure-sintered.
Invention effect
The present invention has following excellent results：By the nesa coatings such as conventional ITO are substituted for material as implied above
Material, can arbitrarily adjust resistivity and refractive index, can guarantee and conventional peer-level or higher than conventional optical characteristics
While using sputtering or ion plating carry out stable film forming, and then by formed amorphous film, the light possessing this film can be improved
The characteristic of device simultaneously improves productivity ratio.
Specific embodiment
The present invention is with zinc (Zn), trivalent metallic element, germanium (Ge) and/or silicon (Si), the sintering as constitution element for the oxygen (O)
Body it is characterised in that set the total content of trivalent metallic element with oxide be scaled the total content of A mole of %, Ge and/or Si with
GeO2And/or SiO2When being scaled B mole of %, meet 15≤A+B≤70.
During raw material preparation, so that composition reaches balance of ZnO and the ratio of each oxide is calculated as 100 moles of % with its total amount
Mode be prepared, therefore, the content of Zn can be obtained by the conversion of such surplus ZnO.By using this composition, can
Form the amorphous film of low-refraction, thus obtaining the effect above of the present invention.
In addition, in the present invention, carry out the content of each metal in regulation sintered body with oxide conversion, but each in sintered body
Part or all of metal is presented in composite oxides.In addition, in the component analyses of the sintered body being usually used,
The form of the non-oxidized substance respective content of mensure in a metallic form.
Germanium oxide (the GeO containing in the sintered body of the present invention2) and silicon dioxide (SiO2) it is vitrification composition (glass shape
Become oxide), it is the effective ingredient for making film decrystallized (vitrification).On the other hand, this vitrification composition sometimes with oxidation
Zinc (ZnO) reaction forms ZnGe2O4Such material and become crystalline film, the membrane stress of this crystalline film increases and causes film to shell
From or film rupture.Therefore, it can expect form mullite composition (3M by introducing trivalent metallic element (being denoted as M)2O3-2GeO2、
3M2O3-2SiO2) and suppress the generation of this material.
In addition, germanium oxide (GeO2), silicon oxide (SiO2) such network former and trivalent metallic element oxidation
Thing is the refractive index material lower than zinc oxide (ZnO), therefore, by adding these oxides, can reduce the refractive index of film.Separately
On the one hand, when adjusting composition in the way of reducing refractive index (when reducing ZnO), resistance value has the tendency of rising.
Therefore, if the total addition level of the oxide of trivalent metallic element is always adding of (A), germanium oxide and/or silicon dioxide
When dosage is (B), make 15≤A+B≤70.It is difficult to form amorphous during A+B ＜ 15, therefore not preferred, when making A+B ＞ 70, ZnO's
Content reduces and forms the film of insulating properties, therefore not preferred.
In the present invention, carry out the content of regulation trivalent metallic element with oxide conversion, oxide said here represents and sets
Trivalent metallic element is by M during M2O3The oxide constituting.
For example, in the case that trivalent metallic element is for aluminum (Al), represent by Al2O3The oxide constituting.As trivalent gold
Belong to element, be particularly preferably selected from one or more of group that aluminum (Al), gallium (Ga), boron (B), yttrium (Y) and indium (In) form
Element.
Trivalent metallic element contributes to electric conductivity, the wherein folding of Al, Ga, B, Y, In as the dopant of zinc oxide (ZnO)
Rate of penetrating is low, can easily adjust refractive index and resistance value by combining with above-mentioned network former, is therefore especially to have
The material of effect.The oxide being made up of these metallic elements can each individually add or compound interpolation, is capable of the application
The purpose of invention.
In the present invention, the total content of Ge and/or Si constituting network former is with GeO2And/or SiO2Conversion is preferably
It is set as 5 moles of more than % and 30 mole of below %, be more preferably set as 5 moles of more than % and 20 mole of below %.This be because
For, during less than 5 moles of %, the effect reducing refractive index reduces and cannot sufficient decrystallized effect.On the other hand, exceed
During 30 moles of % (20 moles of %), the bulk resistance of sintered body easily rises it is difficult to carry out stable DC sputtering.
In addition, in the present invention, the total content of above-mentioned trivalent metallic element is with trivalent metallic element/(Zn+ trivalent metal unit
Element) atomic number be preferably set to more than 0.1 than meter, be more preferably set as more than 0.15.In this case, to low-refraction
Effective with decrystallized.In order to play this effect, it is set as more than 0.1 in terms of atomic number ratio, is more preferably set as more than 0.15.
In addition, the present invention provides a kind of sintered body, it is made up of the oxide of zinc (Zn), gallium (Ga), germanium (Ge), if Ga's contains
Amount is with Ga2O3The content being scaled A mole of %, Ge is with GeO2When being scaled B mole of % and balance of ZnO, satisfaction 15≤A+B≤
50 and A >=3B/2 condition.The sintered body constituting is grouped into by this one-tenth particularly useful as the material of ion plating.
Ion plating method is to be made evaporation of metal, made its ionizing using high-frequency plasma etc. using electron beam etc. in a vacuum
(cation), this cation is made to accelerate postadhesion to form the technology of film by applying nagative potential to substrate.Compared with sputtering, from
Son plating has the advantages that high, the estimated productivity ratio of the service efficiency of material improves.
The sintered body of the present invention, can be used as ion plating materials'use when using part composition as above.This
It is because, by selecting to Ga, Ge element and ratio of components, so that vapour pressure etc. is reduced such that it is able to carry out ion plating.
In the case of as ion plating materials'use, except using tabular material obtained from sintered body polish
Beyond material, can also use make after this sintered body is pulverized further powder or granular obtained from material.Make after pulverizing
Powder or granular obtained from material than tabular material be easier evaporate, therefore from the viewpoint of production efficiency more preferably.
The sintered body of the present invention can also contain with oxide weight be scaled 0.1～5 weight %, formed fusing point be
The metal of less than 1000 DEG C of oxide (low melting point oxide).Due to zinc oxide (ZnO) easily reduction, evaporation, therefore cannot
Excessively rise high sintering temperature, be sometimes difficult to make the density of sintered body to improve.But, by adding this low melting point oxide, tool
There is the effect that can realize densification in the case of excessively not raising sintering temperature.
Less than during 0.1 weight % it is impossible to play this effect, in addition, during more than 5 weight %, characteristic may be made to become
Change thus preferred, be therefore set as above-mentioned numerical range.
As above-mentioned low melting point oxide, such as B can be enumerated2O3、P2O5、K2O、V2O5、Sb2O3、TeO2、Ti2O3、PbO、
Bi2O3、MoO3.These oxides can each individually add or compound interpolation, is capable of the purpose of the present application.This
Bright sintered body can use as sputtering target, in this case, preferably makes relative density be more than 90%.The increase meeting of density
Improve the uniformity of sputtered film, and there is the effect producing powder when can suppress to sputter.
It is below 10 Ω cm that the sintered body of the present invention is capable of its bulk resistor.By reducing bulk resistance, Neng Gouli
Carry out high speed film forming with direct current (DC) sputtering.Need to carry out high frequency (RF) sputtering or magnetron sputtering according to the selection of material, at this
Also film forming speed can be improved in the case of kind.By improving film forming speed, production capacity can be improved such that it is able to go far towards
Cut down cost.
It is important that film obtained from spatter film forming or logical is carried out by the target that obtain processed to sintered body in the present invention
The film crossing above-mentioned ion plating formation is amorphous film.Whether obtained film is that amorphous film can be by for example using X-ray diffraction
Diffracted intensity near 2 θ=34.4 ° at the peak to (002) face ZnO for the method carries out observing judging.With ZnO for main one-tenth
The problems such as membrane stress of the thin film dividing is big, therefore, can crack or rupture when for crystalline film, and then generation film is peeled off, but
By making this thin film be amorphous film, there are the excellent results it can be avoided that the problems such as the rupture that caused by membrane stress or crackle.
By film that the machined target obtaining of sintered body of the present invention is sputtered and formed or by above-mentioned from
The extinction coefficient that the film that son plating is formed is capable of under wavelength 450nm are less than 0.01.The thin film of display needs whole
Transparent in visible-range, but the oxide mesentery such as IZO film typically has absorption in short wavelength range, therefore, it is difficult to sending distinctness
Blueness.According to the present invention, when the extinction coefficient under wavelength 450nm are less than 0.01, almost do not inhale in short wavelength range
Receive, it can be said that being extremely suitable material as transparent material.
In addition, film by the machined target obtaining of sintered body of the present invention is sputtered and formed or by upper
The refractive index that the film stating ion plating formation is capable of under wavelength 550nm is less than 2.00 (preferably less than 1.90).And, above-mentioned
The specific insulation of film is capable of 1 × 10-3～1 × 109Ω·cm.
By germanium oxide (GeO2), silicon dioxide (SiO2), oxide (the wherein preferably Al that constitutes of trivalent metallic element2O3、
Ga2O3、B2O3、Y3O2、In2O3) for refractive index be less than zinc oxide (ZnO) material, therefore, by adding these oxides, can
Obtain refractive index film low than ever.
In addition, film by the machined target obtaining of sintered body of the present invention is sputtered and formed or by upper
Nesa coating or formation optical information record that the film stating ion plating formation can be used in the various display such as organic EL television set
The optical thin film of the protective layer of recording medium.In the case of the protective layer of optical information recording medium, especially because not using
ZnS, therefore, have the pollution that there is not S and cause, will not thus make recording layer deterioration remarkable result.
Embodiment
Hereinafter, illustrated based on embodiment and comparative example.In addition, the present embodiment is one at most, the present invention is not
Any restriction by this.That is, the present invention is limited only by the appended claims, and comprises each beyond contained embodiment in the present invention
Plant deformation.
(embodiment 1)
Prepare ZnO powder, Al2O3Powder, SiO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into the proportioning described in table 1, after being mixed, by dusty material in a vacuum, 1100 DEG C of temperature, pressure
250kgf/cm2Under conditions of carry out hot pressed sintering.
Then, by machining, this sintered body is finish-machined to sputter target shape.The bulk resistor of the target obtained by measuring
And relative density, as shown in table 1, relative density reaches 99.3% to result, and bulk resistor is 2.1m Ω cm, can carry out stable
DC sputters.
In addition, being sputtered using the target after above-mentioned polish.It is being set as DC sputtering, sputtering power 500W, containing 2 bodies
The O of long-pending %2The sputtering condition of Ar air pressure 0.5Pa under, film forming isThickness.Measure into the amorphous of membrane sample
Property, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, formed by sputtering
Thin film is amorphous film, and its refractive index is 1.80 (wavelength 550nm), and specific insulation is 2 × 108Ω cm, extinction coefficient are less than
0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(embodiment 2)
Prepare ZnO powder, Ga2O3Powder, SiO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into the proportioning described in table 1, after being mixed, by dusty material in argon gas atmosphere, 1100 DEG C of temperature, pressure
250kgf/cm2Under conditions of carry out hot pressed sintering.Then, by machining, this sintered body is finish-machined to sputter target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density reaches 98.5% to result, and bulk resistor is
1.6m Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, by splashing
The thin film penetrating formation is amorphous film, and its refractive index is 1.89 (wavelength 550nm), and specific insulation is 2 × 10-1Ω cm, delustring
Coefficient is less than 0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(embodiment 3)
Prepare ZnO powder, Al2O3Powder, GeO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into the proportioning described in table 1, after being mixed, by dusty material in argon gas atmosphere, 1100 DEG C of temperature, pressure
250kgf/cm2Under conditions of carry out hot pressed sintering.Then, by machining, this sintered body is finish-machined to sputter target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density reaches 98.6% to result, and bulk resistor is
3.6m Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, by splashing
The thin film penetrating formation is amorphous film, and its refractive index is 1.79 (wavelength 550nm), and specific insulation is 5 × 106Ω cm, delustring
Coefficient is less than 0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(embodiment 4)
Prepare ZnO powder, Y2O3Powder, GeO2Powder and the B as low melting point oxide2O3Powder.Then, by these powder
End is deployed into the proportioning described in table 1, after being mixed, by dusty material in argon gas atmosphere, 1000 DEG C of temperature, pressure
250kgf/cm2Under conditions of carry out hot pressed sintering.Then, by machining, this sintered body is finish-machined to sputter target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density reaches 98.3% to result, and bulk resistor is
7.6m Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, by splashing
The thin film penetrating formation is amorphous film, and its refractive index is 1.88 (wavelength 550nm), and specific insulation is 7 × 104Ω cm, delustring
Coefficient is less than 0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(embodiment 5)
Prepare ZnO powder, In2O3Powder, GeO2Powder.Then, these powder are deployed into the proportioning described in table 1, will
After its mixing, by dusty material in argon gas atmosphere, 1050 DEG C of temperature, pressure 250kgf/cm2Under conditions of carry out hot pressing burning
Knot.Then, by machining, this sintered body is finish-machined to sputter target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density reaches 98.7% to result, body
Resistance is 1.3m Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).
As shown in table 1, by sputtering the thin film being formed for amorphous film, its refractive index is 1.88 (wavelength 550nm), volume electricity
Resistance rate is 2 × 10-3Ω cm, extinction coefficient are less than 0.01 (wavelength 450nm), have obtained the amorphous film of low-refraction.
(embodiment 6)
Prepare ZnO powder, B2O3Powder, SiO2Powder and the Bi as low melting point oxide2O3Powder.Then, by these
Powder is deployed into the proportioning described in table 1, after being mixed, by dusty material in 500kgf/cm2Pressure under press molding,
By this formed body in a vacuum, carry out under conditions of 1300 DEG C of temperature normal pressure-sintered.Then, by machining by this sintered body
It is finish-machined to sputter target shape.The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density reaches result
To 96.5%, bulk resistor is 2.3 Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, by splashing
The thin film penetrating formation is amorphous film, and its refractive index is 1.73 (wavelength 550nm), and specific insulation is 3 × 10 Ω cm, delustring system
Number is less than 0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(embodiment 7)
Prepare ZnO powder, Ga2O3Powder, GeO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into the proportioning described in table 1, after being mixed, by dusty material in 500kgf/cm2Pressure under press molding,
By this formed body in argon gas atmosphere, carry out under conditions of 1100 DEG C of temperature normal pressure-sintered.Then, by machining, this is burnt
Knot body is finish-machined to sputter target shape.The bulk resistor of target obtained by measuring and relative density, result is as shown in table 1, relatively close
Degree reaches 99.8%, and bulk resistor is 0.9m Ω cm, can carry out stable DC sputtering.
In addition, using the target after above-mentioned polish, being sputtered under conditions of similarly to Example 1, measure film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm).As shown in table 1, by splashing
The thin film penetrating formation is amorphous film, and its refractive index is 1.89 (wavelength 550nm), and specific insulation is 2 × 10-3Ω cm, delustring
Coefficient is less than 0.01 (wavelength 450nm), has obtained the amorphous film of low-refraction.
(comparative example 1)
Prepare ZnO powder, Ga2O3Powder, GeO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into A+B as described in Table 1<15 proportioning, after being mixed, by dusty material in argon gas atmosphere, temperature 1050
DEG C, pressure 250kgf/cm2Under conditions of carry out hot pressed sintering.Then, by machining, this sintered body is finish-machined to sputter
Target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density is 95.8% to result, body electricity
Hinder for 1.2m Ω cm, DC sputtering can be carried out.
But, using the target after above-mentioned polish, sputtered under conditions of similarly to Example 1, measured film forming sample
The amorphism of product, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength 450nm), result as shown in table 1, is led to
The thin film crossing sputtering formation does not form amorphous film.In addition, refractive index is 1.98 (wavelength 550nm), specific insulation is 3 × 10-3
Ω cm, extinction coefficient are less than 0.01 (wavelength 450nm).
(comparative example 2)
Prepare ZnO powder, Al2O3Powder, SiO2Powder and the B as low melting point oxide2O3Powder.Then, by these
Powder is deployed into A+B as described in Table 1>70 proportioning, after being mixed, by dusty material in argon gas atmosphere, temperature
1100 DEG C, pressure 250kgf/cm2Under conditions of carry out hot pressed sintering.Then, by machining, this sintered body is finish-machined to
Sputtering target shape.
The bulk resistor of target obtained by measuring and relative density, as shown in table 1, relative density is 96.4% to result, body electricity
Hinder for 40m Ω cm, DC sputtering can be carried out.But, using the target after above-mentioned polish, in condition similarly to Example 1
Under sputtered, measure into the amorphism of membrane sample, refractive index (wavelength 550nm), specific insulation, extinction coefficient (wavelength
450nm), as shown in table 1, the specific insulation of the thin film being formed by sputtering is more than 1 × 10 for result9Ω cm and show absolutely
Edge.In addition, its for refractive index be 1.66 (wavelength 550nm), extinction coefficient be less than 0.01 (wavelength 450nm) amorphous film.
(embodiment 8)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=80.0:13.0:The proportioning of 7.0 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result as shown in table 2, can carry out stable ion plating, made film
Refractive index reach 1.87 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), the specific insulation of thin film
For 1 × 10-2Ω cm and show electric conductivity.In addition, confirming as amorphous film.
(embodiment 9)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=52.7:29.4:The proportioning of 17.9 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850
℃、250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating, and the refractive index of made film reaches
To 1.71 (wavelength 550nm).
In addition, extinction coefficient are less than 0.01 (wavelength 450nm), the specific insulation of thin film is 3 × 106Ω cm and show
Go out electric conductivity.In addition, confirming as amorphous film.
(embodiment 10)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=66.3:20.6:The proportioning of 13.1 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850
℃、250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating it is thus identified that made film is non-
Epitaxial.In addition, the refractive index of this film reaches 1.75 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), thin
The specific insulation of film is 6 × 104Ω cm and show electric conductivity.
(embodiment 11)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=74.5:16.9:The proportioning of 8.6 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating it is thus identified that made film is non-
Epitaxial.In addition, refractive index reaches 1.82 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), the body of thin film
Long-pending resistivity is 8 × 10-2Ω cm and show electric conductivity.
(embodiment 12)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=67.7:23.4:The proportioning of 8.9 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating it is thus identified that made film is non-
Epitaxial.In addition, the refractive index of this film reaches 1.77 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), thin
The specific insulation of film is 3 × 10-1Ω cm and show electric conductivity.
(embodiment 13)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=50.2:41.9:The proportioning of 7.9 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating it is thus identified that made film is non-
Epitaxial.In addition, the refractive index of this film reaches 1.66 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), thin
The specific insulation of film is 3 × 103Ω cm and show electric conductivity.
(comparative example 3)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=85.0:2.2:The proportioning of 12.8 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body, result can carry out stable ion plating, and the refractive index of made film is
1.94 (wavelength 550nm).In addition, extinction coefficient are less than 0.01 (wavelength 450nm), the specific insulation of thin film is 4 × 10-3Ω·
Cm and show electric conductivity.But, confirm that film there occurs crystallization.
(comparative example 4)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=44.0:34.0:The proportioning of 22.0 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850
℃、250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Although implementing ion plating using this sintered body as a result, made film is amorphous film, the refractive index of film is 1.68
(wavelength 550nm), extinction coefficient are less than 0.01 (wavelength 450nm), the specific insulation of thin film>1×109Ω cm, electric conductivity
Significantly reduce.
(comparative example 5)
Prepare be equivalent to less than 5 μm of the ZnO powder of 3N, be equivalent to the Ga of below 5 μm of the mean diameter of 3N2O3Powder, phase
As the GeO below 5 μm of the mean diameter of 3N2Powder.Then, by ZnO powder, Ga2O3Powder and GeO2Powder is deployed into ZnO:
Ga2O3:GeO2=90.0:7.0:The proportioning of 3.0 moles of %, after being mixed, by dusty material in argon gas atmosphere, 850 DEG C,
250kgf/cm2Pressure under carry out hot pressed sintering and make ion plating sintered body.
Implement ion plating using this sintered body as a result, the refractive index of film is 1.93 (wavelength 550nm), extinction coefficient are less than
0.01 (wavelength 450nm), the specific insulation of thin film is 1 × 10-3Ω cm and show electric conductivity, but the film made there occurs
Crystallization.
Industrial applicability
The sintered body of the present invention can make sputtering target or ion plating material, using these sputtering targets or ion plating material shape
The thin film becoming has the effect that：By forming the protecting film of the nesa coating in various display or optical device, in transmission
Rate, refractive index, electric conductivity aspect have extremely excellent characteristic.In addition, the one of the present invention is characterised by greatly by forming amorphous
Film and there are the excellent results of the crackle that can significantly improve film and etching performance.
In addition, using the present invention sputtering target obtained from sintered body bulk resistance is low and relative density up to 90% with
On, therefore, it is possible to carry out stable DC sputtering.And, have and can easily play the control that the feature of this DC sputtering sputters
Property, improve film forming speed thus improving the remarkable result of sputtering yield.Also considerable in the case of implementing RF sputtering as needed
Observe the raising of film forming speed.In addition, the powder producing in sputtering during film forming, dross can be reduced, quality fluctuation is made to reduce
And improve mass productivity.
Additionally, the amorphous film of low-refraction can be formed using ion plating material obtained from the sintered body of the present invention, because
This, have the effect that can suppress the generation of crackle or rupture and film stripping caused by membrane stress.This amorphous film is as shape
The optical thin film of protective layer of one-tenth optical information recording medium, organic EL used as television thin film, transparency electrode are particularly useful with thin film.
Claims (14)
1. a kind of sintered body is it is characterised in that comprise zinc (Zn), trivalent metallic element, germanium (Ge) or germanium (Ge) and silicon (Si), oxygen
(O), if the total content of trivalent metallic element is scaled the total content of A mole of %, Ge or Ge and Si with GeO with oxide2Or GeO2
And SiO2When being scaled B mole of %, 15≤A+B≤70, described trivalent metallic element is selected from aluminum (Al), gallium (Ga), boron
(B), one or more of group that yttrium (Y) and indium (In) form element, the total content of this trivalent metallic element is with trivalent metal unit
The atomic number ratio of element/(Zn+ trivalent metallic element) is calculated as more than 0.1.
2. sintered body as claimed in claim 1 is it is characterised in that the total content of described Ge or Ge and Si is with GeO2Or GeO2With
SiO2It is scaled 5≤B≤30.
3. a kind of sintered body is it is characterised in that comprise zinc (Zn), gallium (Ga), germanium (Ge), oxygen (O), if the content of Ga is with Ga2O3Change
Calculate content for A mole of %, Ge with GeO2When being scaled B mole of %, meet the condition of 15≤A+B≤50 and A >=3B/2.
4. sintered body as claimed in claim 1 or 2 is scaled 0.1～5 weight it is characterised in that also containing with oxide weight
Metal amount %, forming the oxide that fusing point is less than 1000 DEG C, this fusing point be less than 1000 DEG C of oxide be selected from
B2O3、P2O5、K2O、V2O5、Sb2O3、TeO2、Ti2O3、PbO、Bi2O3、MoO3One or more of the group of composition oxide.
5. sintered body as claimed in claim 1 or 2 is it is characterised in that relative density is more than 90%.
6. sintered body as claimed in claim 1 or 2 is it is characterised in that bulk resistance is below 10 Ω cm.
7. a kind of sputtering target is it is characterised in that usage right requires the sintered body any one of 1～6.
8. a kind of ion plating material is it is characterised in that usage right requires the sintered body described in 3.
9. a kind of thin film is it is characterised in that comprise zinc (Zn), trivalent metallic element, germanium (Ge) or germanium (Ge) and silicon (Si), oxygen
(O), if the total content of trivalent metallic element is scaled the total content of A mole of %, Ge or Ge and Si with GeO with oxide2Or GeO2
And SiO2When being scaled B mole of %, 15≤A+B≤70, described trivalent metallic element is selected from aluminum (Al), gallium (Ga), boron
(B), one or more of group that yttrium (Y) and indium (In) form element, the total content of this trivalent metallic element is with trivalent metal unit
The atomic number ratio of element/(Zn+ trivalent metallic element) is calculated as more than 0.1, and is amorphous film.
10. thin film as claimed in claim 9 is scaled 0.1～5 weight % it is characterised in that also containing with oxide weight
, formed be selected from B2O3、P2O5、K2O、V2O5、Sb2O3、TeO2、Ti2O3、PbO、Bi2O3、MoO3One of group of composition with
The metal of upper oxide.
11. thin film as described in claim 9 or 10 are it is characterised in that the extinction coefficient under wavelength 450nm are less than 0.01.
12. thin film as described in claim 9 or 10 are it is characterised in that the refractive index under wavelength 550nm is less than 2.00.
13. thin film as described in claim 9 or 10 are it is characterised in that specific insulation is 1 × 10-3～1 × 109Ω·cm.
A kind of 14. manufacture methods of sintered body, it is the manufacture method of the sintered body any one of claim 1～6, its
Be characterised by, material powder mixed, by obtained mixed-powder under noble gases or vacuum atmosphere, 1000 DEG C～
Carry out pressure sintering at 1500 DEG C, or by after obtained mixed-powder press molding, by this formed body in noble gases or
Under vacuum atmosphere, carry out at 1000 DEG C～1500 DEG C normal pressure-sintered.
Applications Claiming Priority (7)
| Application Number | Priority Date | Filing Date | Title |
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| JP2012-149357 | 2012-07-03 | ||
| JP2012149357 | 2012-07-03 | ||
| JP2012287729 | 2012-12-28 | ||
| JP2012-287729 | 2012-12-28 | ||
| JP2013119611A JP5550768B1 (en) | 2012-07-03 | 2013-06-06 | Sintered body and amorphous film |
| JP2013-119611 | 2013-06-06 | ||
| CN201310276943.2A CN103524119A (en) | 2012-07-03 | 2013-07-03 | Sintered compact and amorphous film |
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| CN201310276943.2A Division CN103524119A (en) | 2012-07-03 | 2013-07-03 | Sintered compact and amorphous film |
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| CN201610702480.5A Pending CN106380188A (en) | 2012-07-03 | 2013-07-03 | Sintered body and amorphous thin film |
| CN202010396262.XA Pending CN111620687A (en) | 2012-07-03 | 2013-07-03 | Sintered body and amorphous film |
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| CN107207356A (en) * | 2015-02-27 | 2017-09-26 | 捷客斯金属株式会社 | Oxidate sintered body, oxide sputtering target and sull |
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| WO2015118724A1 (en) * | 2014-02-07 | 2015-08-13 | リンテック株式会社 | Transparent conductive laminate, method for producing transparent conductive laminate, and electronic device formed using transparent conductive laminate |
| JP5688179B1 (en) * | 2014-09-10 | 2015-03-25 | Jx日鉱日石金属株式会社 | Oxide sintered body, sputtering target, thin film, and method for producing oxide sintered body |
| JP6409588B2 (en) * | 2015-01-21 | 2018-10-24 | Tdk株式会社 | Transparent conductor and touch panel |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN103524119A (en) | 2014-01-22 |
| TWI631579B (en) | 2018-08-01 |
| KR101841791B1 (en) | 2018-03-23 |
| KR20140004586A (en) | 2014-01-13 |
| TW201405580A (en) | 2014-02-01 |
| CN111620687A (en) | 2020-09-04 |
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