CN115959897A - Method for preparing low-density ITO target material for evaporation by sand milling process - Google Patents
Method for preparing low-density ITO target material for evaporation by sand milling process Download PDFInfo
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- CN115959897A CN115959897A CN202211473793.XA CN202211473793A CN115959897A CN 115959897 A CN115959897 A CN 115959897A CN 202211473793 A CN202211473793 A CN 202211473793A CN 115959897 A CN115959897 A CN 115959897A
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- 239000013077 target material Substances 0.000 title claims abstract description 55
- 238000001704 evaporation Methods 0.000 title claims abstract description 44
- 230000008020 evaporation Effects 0.000 title claims abstract description 44
- 239000004576 sand Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000003801 milling Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 238000005238 degreasing Methods 0.000 claims abstract description 14
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- 235000015895 biscuits Nutrition 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 11
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 11
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000004537 pulping Methods 0.000 claims abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 7
- 238000003825 pressing Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 239000010408 film Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000007740 vapor deposition Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000011164 primary particle Substances 0.000 description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps: uniformly mixing indium oxide with the particle size D50 of 0.1-0.5 um and tin oxide powder; calcining the mixed powder; pulping the calcined powder, and adding the pulp and the binder into a sand mill for sand milling; spray drying and granulating the sanded slurry; performing cold press molding on the granulated powder to obtain a cold press biscuit; degreasing the cold-pressed biscuit; and (3) placing the degreased cold-pressed biscuit in an oxygen atmosphere to carry out normal-pressure sintering to obtain the low-density ITO target material for evaporation. The invention can obtain the low-density ITO target material with uniform grain size and low volume resistivity for evaporation, and the relative density of the low-density ITO target material is 55-65%; the prepared low-density ITO target material is not easy to crack when in evaporation use, the utilization rate of the target material is high, and a uniform conductive film with low resistivity and high light transmittance can be obtained after evaporation.
Description
Technical Field
The invention relates to the technical field of target manufacturing, in particular to a method for preparing a low-density ITO target for evaporation by a sand milling process.
Background
Indium Tin Oxide (ITO) coated glass is one of key materials for flat panel display preparation, and the material has excellent photoelectric characteristics such as high light transmittance and low resistivity in a visible light region, and various researches prove that the resistivity of the material can reach 10 -3 ～10 -4 Ω · cm, and visible light transmittance of 85% or more, so the ITO transparent conductive film is widely used in the field of optoelectronics, such as Liquid Crystal Displays (LCDs), thin film transistor displays (tft.lcds), and the like, in the display industry.
The existing preparation method of the ITO film mainly comprises a magnetron sputtering method and a vacuum evaporation method, wherein the magnetron sputtering method is mainly used for a high-density ITO target material, the relative density of the target material is more than 99 percent, and the vacuum evaporation principle is that the low-density ITO target material is heated, so that the ITO target material is evaporated and deposited on a substrate needing film coating due to the low density of the ITO target material.
The bulk resistance of the conventional ITO target for vapor deposition is generally 1.4X 10 -4 Omega cm, density of 3.93g/cm 3 ～4.65g/cm 3 The square resistance of the evaporated film is about 20-30 omega/□, and the blue light transmittance is 90%. The common method for preparing the indium tin oxide target material is to obtain the ITO target material with required performance by the processes of powder preparation, mould pressing-isostatic pressing, sintering and the like of indium tin oxide mixed powder, but the target material has higher resistance, and the performance of the obtained target material and the film is not ideal.
The prior patent CN102731068A discloses a preparation method of a low-density ITO evaporation target, which adopts a method of powder high-temperature pre-firing, fat doping, granulation, molding, degreasing and sintering to prepare the evaporation target; however, in the powder treatment of the preparation method, excessive reagents such as a binder, a release agent and a parting agent cannot be completely removed in a subsequent degreasing process, and the subsequent target coating is easy to form nodules and crack due to the excessively high impurity content of the sintered target.
The prior patent CN107200562A discloses a preparation method of an ITO evaporation target, which adopts powder heat treatment, mixing, wet grinding, drying, compression molding, cold isostatic pressing, degreasing and sintering methods to prepare the evaporation target; however, in the method, ethanol is used as a ball milling medium for powder treatment, the ethanol is flammable and explosive in the using process, potential safety hazards of the production process exist, and simultaneously the ethanol is volatile in the ball milling process, so that the solid content ratio is changed, and the powder performance is influenced. In addition, the cold isostatic pressing procedure is added in the forming process, so that the target is easy to deform after being formed, the machining procedure is required to be added, and the preparation period and the cost of the target are increased.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing a low-density ITO target material for evaporation by a sand milling process, wherein the prepared low-density ITO target material has higher conductivity, and an ITO film obtained by evaporation by using the low-density ITO target material has higher conductivity and light transmittance.
The invention discloses a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps:
uniformly mixing indium oxide with the particle size D50 of 0.1-0.5 um and tin oxide powder;
calcining the mixed powder;
pulping the calcined powder, and adding the pulp and the binder into a sand mill for sand grinding;
spray drying and granulating the sanded slurry;
performing cold press molding on the granulated powder to obtain a cold press biscuit;
degreasing the cold-pressed biscuit;
and (3) placing the degreased cold-pressed biscuit in an oxygen atmosphere to perform normal-pressure sintering to obtain the low-density ITO target material for evaporation.
As a further improvement of the invention, the mixing time of the indium oxide and the tin oxide powder isIn the mixed powder for 4 to 8 hours 2 O 3 And SnO 2 The mass percentage of (90-95): (10-5).
As a further improvement of the invention, the calcination temperature of the mixed powder is 800-1250 ℃, and the calcination time is 2-6 h.
As a further improvement of the invention, the slurry is prepared from calcined powder and water, and the solid content of the slurry is 40-80%.
As a further improvement of the invention, the binder is polyvinyl alcohol, and the addition amount of the binder is 0.5-4 wt% of the slurry.
As a further improvement of the invention, the rotation speed of the sand grinding is 1000-3000 rpm, and the time is 0.5-2 h.
As a further improvement of the invention, the temperature of the spray drying is 80-200 ℃, and the rotating speed is 10000-25000 rpm.
As a further improvement of the invention, the pressure of the cold press molding is 100-200 MPa.
As a further improvement of the invention, the degreasing temperature is 500-700 ℃, and the time is 10-40 h.
As a further improvement of the invention, the oxygen pressure required by the normal pressure sintering is 0.05-0.15 MPa, the sintering temperature is 1000-1400 ℃, and the heat preservation time is 4-10 h.
Compared with the prior art, the invention has the beneficial effects that:
the invention can obtain the low-density ITO target material with uniform grain size and low volume resistivity for evaporation, and the relative density of the low-density ITO target material is 55-65%; the prepared low-density ITO target material is not easy to crack when in evaporation use, the utilization rate of the target material is high, and a uniform conductive film with low resistivity and high light transmittance can be obtained after evaporation.
Drawings
FIG. 1 is a flow chart of a method for preparing a low-density ITO target material for evaporation by a sanding process disclosed in one embodiment of the present invention;
FIG. 2 is a sectional SEM image of a low-density ITO target for vapor deposition prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention is described in further detail below with reference to the attached drawing figures:
as shown in fig. 1, the present invention provides a method for preparing a low-density ITO target for evaporation by a sand milling process, comprising:
step 1, uniformly mixing indium oxide with the particle size D50 of 0.1-0.5 um and tin oxide powder; wherein, the first and the second end of the pipe are connected with each other,
the mixing time of the indium oxide and the tin oxide powder is 4 to 8 hours, and In the mixed powder 2 O 3 And SnO 2 The mass percentage of (90-95): (10-5);
step 2, calcining the mixed powder; wherein the content of the first and second substances,
the calcining temperature is 800-1250 ℃, and the calcining time is 2-6 h;
step 3, pulping the calcined powder, and adding the pulp and the binder into a sand mill for sand milling; wherein the content of the first and second substances,
the slurry is prepared from calcined powder and water, and the solid content of the slurry is 40-80%; the binder is preferably polyvinyl alcohol (PVA), and the addition amount of the binder is 0.5-4 wt% of the slurry; the rotational speed of sanding is 1000-3000 rpm, and the time is 0.5-2 h;
step 4, performing spray drying and granulation on the sanded slurry; wherein, the first and the second end of the pipe are connected with each other,
the temperature of spray drying is 80-200 ℃, and the rotating speed is 10000-25000 rpm;
step 5, performing cold press molding on the granulated powder to obtain a cold-pressed biscuit; wherein the content of the first and second substances,
the pressure of cold press molding is 100-200 MPa;
step 6, degreasing the cold-pressed biscuit; wherein the content of the first and second substances,
the degreasing temperature is 500-700 ℃, and the time is 10-40 h;
step 7, placing the degreased cold-pressed biscuit in an oxygen atmosphere for normal-pressure sintering to obtain a low-density ITO target material for evaporation; wherein the content of the first and second substances,
the oxygen pressure required by the normal pressure sintering is 0.05-0.15 MPa, the sintering temperature is 1000-1400 ℃, and the heat preservation time is 4-10 h.
Example 1
The invention provides a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps:
s11, mixing indium oxide and tin oxide powder with primary particle diameter D50 of 0.3um and purity of 99.99% according to In 2 O 3 With SnO 2 The mass percentage of 90;
s12, placing the mixed powder obtained in the S11 into a calcining furnace, and calcining for 5 hours at 1150 ℃;
s13, preparing the powder obtained in the S12 into slurry with the solid content of 60%, adding 1.5% of polyvinyl alcohol, and carrying out sand grinding for 0.8h in a sand mill at the rotating speed of 1500 rpm;
s14, carrying out spray drying treatment on the slurry obtained in the step S13, wherein the drying temperature is 100 ℃, and the rotation speed of an atomizer is 13000rpm;
s15, placing the powder treated in the S14 into a cold pressing die, and pressing under the pressure of 100Mpa to obtain a cold pressing blank with the density of 53%;
s16, degreasing the pressed blank in the S15 at 600 ℃ for 30h;
s17, sintering the degreased target blank in the step S16, wherein the atmosphere in the furnace is oxygen and the pressure is 0.1MPa; and during sintering, heating to 900 ℃ at the speed of 200 ℃/h, preserving heat for 2h, heating to 1300 ℃ at the speed of 200 ℃/h, preserving heat for 6h, and finally cooling to room temperature at the speed of 60 ℃/h to obtain the low-density ITO target material for evaporation, wherein the purity of the low-density ITO target material is 99.99%.
The low-density ITO target for vapor deposition prepared according to the example had a relative density of 61.3% and a resistivity of 1.6X 10 -4 Omega cm, section of low density ITO target materialThe SEM image is shown in FIG. 2.
Example 2
The invention provides a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps:
s21, mixing indium oxide and tin oxide powder with primary particle size D50 of 0.3um and purity of 99.99% according to In 2 O 3 With SnO 2 The mass percentage of 90;
s22, placing the mixed powder obtained in the S21 into a calcining furnace, and calcining for 5 hours at 1150 ℃;
s23, preparing the powder obtained in the step S22 into slurry with the solid content of 60%, adding 1.5% of polyvinyl alcohol, and carrying out sand milling for 0.8h in a sand mill at the rotating speed of 1500 rpm;
s24, carrying out spray drying treatment on the slurry obtained in the S23, wherein the drying temperature is 100 ℃, and the rotation speed of an atomizer is 13000rpm;
s25, placing the powder treated in the S24 into a cold pressing die, and pressing at 100Mpa to obtain a cold pressing blank with the density of 53%;
and S26, degreasing the pressed compact in the S25 at 600 ℃ for 30h.
S27, sintering the degreased target blank in the step S26, wherein the atmosphere in the furnace is oxygen, and the pressure is 0.1Mpa; and during sintering, heating to 900 ℃ at the speed of 200 ℃/h, preserving heat for 2h, heating to 1400 ℃ at the speed of 200 ℃/h, preserving heat for 6h, and finally cooling to room temperature at the speed of 60 ℃/h to obtain the low-density ITO target material for evaporation, wherein the purity of the low-density ITO target material is 99.99%.
The low-density ITO target for vapor deposition prepared according to this example had a relative density of 62.5% and a resistivity of 1.6X 10 -4 Ω·cm。
Example 3
The invention provides a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps:
s31, mixing indium oxide and tin oxide powder with primary particle diameter D50 of 0.3um and purity of 99.99% according to In 2 O 3 With SnO 2 Uniformly mixing the components in percentage by mass 95;
s32, placing the mixed powder obtained in the S31 into a calcining furnace, and calcining for 5 hours at 1150 ℃;
s33, preparing the powder obtained in the S32 into slurry with the solid content of 60%, adding 1.5% of polyvinyl alcohol, and carrying out sand grinding for 0.5h in a sand mill at the rotating speed of 1500 rpm;
s34, carrying out spray drying treatment on the slurry obtained in the S33, wherein the drying temperature is 100 ℃, and the rotation speed of an atomizer is 13000rpm;
s35, placing the powder treated in the S34 into a cold pressing die, and pressing at 100Mpa to obtain a cold pressing blank with the density of 53%;
s36, degreasing the pressed blank in the S35 at 600 ℃ for 30h;
s37, sintering the degreased target blank in the step S36, wherein the atmosphere in the furnace is oxygen and the pressure is 0.1MPa; and during sintering, heating to 900 ℃ at the speed of 200 ℃/h, preserving heat for 2h, heating to 1300 ℃ at the speed of 200 ℃/h, preserving heat for 8h, and finally cooling to room temperature at the speed of 60 ℃/h to obtain the low-density ITO target material for evaporation, wherein the purity of the low-density ITO target material is 99.99%.
The low-density ITO target for vapor deposition prepared according to the example had a relative density of 61.8% and a resistivity of 1.7X 10 -4 Ω·cm。
Example 4
The invention provides a method for preparing a low-density ITO target material for evaporation by a sand milling process, which comprises the following steps:
s41, indium oxide and tin oxide powders with the primary particle size D50 of 0.3um and the purity of 99.99 percent are mixed according to the proportion of In 2 O 3 With SnO 2 The mass percentage of 95;
s42, placing the mixed powder obtained in the S41 into a calcining furnace, and calcining for 5 hours at 1150 ℃;
s43, preparing the powder obtained in the step S42 into slurry with the solid content of 60%, adding 1.5% of polyvinyl alcohol, and carrying out sand milling for 0.5h in a sand mill with the rotating speed of 1500 rpm;
s44, carrying out spray drying treatment on the slurry obtained in the S43, wherein the drying temperature is 100 ℃, and the rotation speed of an atomizer is 13000rpm;
s45, putting the powder treated in the S44 into a cold pressing die, and pressing under the pressure of 100Mpa to obtain a cold pressing blank with the density of 53%;
s46, degreasing the pressed blank in the S45 at 600 ℃ for 30h;
s47, sintering the degreased target blank in the S46, wherein the atmosphere in the furnace is oxygen and the pressure is 0.1MPa; and during sintering, heating to 900 ℃ at the speed of 200 ℃/h, preserving heat for 2h, heating to 1400 ℃ at the speed of 200 ℃/h, preserving heat for 8h, and finally cooling to room temperature at the speed of 60 ℃/h to obtain the low-density ITO target material for evaporation, wherein the purity of the low-density ITO target material is 99.99%.
The low-density ITO target for vapor deposition prepared according to this example had a relative density of 62.8% and a resistivity of 1.6X 10 -4 Ω·cm。
The invention has the advantages that:
the invention can obtain the low-density ITO target material for evaporation with uniform grain size and low volume resistivity, and has simple production process flow, the purity of the ITO target material is more than or equal to 99.99 percent, and the relative density is 55-65 percent; the prepared low-density ITO target material is not easy to crack when in evaporation use, the utilization rate of the target material is high, and a uniform conductive film with low resistivity and high light transmittance can be obtained after evaporation.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a low-density ITO target material for evaporation by a sand milling process is characterized by comprising the following steps:
uniformly mixing indium oxide with the particle size D50 of 0.1-0.5 um and tin oxide powder;
calcining the mixed powder;
pulping the calcined powder, and adding the pulp and the binder into a sand mill for sand milling;
spray drying and granulating the sanded slurry;
performing cold press molding on the granulated powder to obtain a cold-pressed biscuit;
degreasing the cold-pressed biscuit;
and (3) placing the degreased cold-pressed biscuit in an oxygen atmosphere to perform normal-pressure sintering to obtain the low-density ITO target material for evaporation.
2. The method for preparing the low-density ITO target material for evaporation by using the sand milling process as claimed In claim 1, wherein the mixing time of the indium oxide and the tin oxide powder is 4-8 h, and In the mixed powder 2 O 3 And SnO 2 The mass percentage of (90-95): (10-5).
3. The method for preparing the low-density ITO target material for evaporation through the sand milling process as claimed in claim 1, wherein the calcination temperature of the mixed powder is 800-1250 ℃, and the calcination time is 2-6 h.
4. The method for preparing the low-density ITO target material for evaporation by using the sand milling process as claimed in claim 1, wherein the slurry is prepared from calcined powder and water, and the solid content of the slurry is 40-80%.
5. The method for preparing the low-density ITO target material for evaporation by using the sand milling process as claimed in claim 1, wherein the binder is polyvinyl alcohol, and the addition amount of the binder is 0.5-4 wt% of the slurry.
6. The method for preparing a low-density ITO target material for evaporation according to claim 1, wherein the rotational speed of the sand mill is 1000-3000 rpm, and the time is 0.5-2 h.
7. The method for preparing the low-density ITO target material for evaporation by using the sand milling process as claimed in claim 1, wherein the temperature of the spray drying is 80-200 ℃, and the rotating speed is 10000-25000 rpm.
8. The method for preparing the low-density ITO target material for evaporation by the sand milling process according to claim 1, wherein the pressure of the cold press molding is 100-200 MPa.
9. The method for preparing the low-density ITO target material for evaporation by using the sand milling process as claimed in claim 1, wherein the degreasing temperature is 500-700 ℃ and the time is 10-40 h.
10. The method for preparing the low-density ITO target material for evaporation through the sand milling process as claimed in claim 1, wherein the oxygen pressure required by the normal-pressure sintering is 0.05-0.15 MPa, the sintering temperature is 1000-1400 ℃, and the heat preservation time is 4-10 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211473793.XA CN115959897A (en) | 2022-11-22 | 2022-11-22 | Method for preparing low-density ITO target material for evaporation by sand milling process |
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Application publication date: 20230414 |