CN111549310B - Ceramic powder, mask and manufacturing method thereof - Google Patents
Ceramic powder, mask and manufacturing method thereof Download PDFInfo
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- CN111549310B CN111549310B CN202010285665.7A CN202010285665A CN111549310B CN 111549310 B CN111549310 B CN 111549310B CN 202010285665 A CN202010285665 A CN 202010285665A CN 111549310 B CN111549310 B CN 111549310B
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- C—CHEMISTRY; METALLURGY
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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- C—CHEMISTRY; METALLURGY
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
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Abstract
The invention relates to the technical field of OLED display, in particular to ceramic powder, a mask and a manufacturing method thereof, wherein the ceramic powder is composed of the following raw materials in parts by weight: al (Al)2O344-48 parts of AlN 3-3.5 parts of SiC 1-2 parts of SiO25-10 parts of TiO25-6 parts of ZrO22.3-2.8 parts of ZnO, 1-1.5 parts of ZnO and 0.2-0.4 part of rare earth oxide, and can form an insulating and corrosion-resistant coating on the surface of the mask plate, thereby prolonging the service life of the mask plate and reducing the cost in the production of the OLED display device.
Description
Technical Field
The invention relates to the technical field of OLED display, in particular to ceramic powder, a mask and a manufacturing method thereof.
Background
The OLED is also called as a third generation display technology, and is thinner, low in power consumption, high in brightness, good in light emitting efficiency, capable of displaying pure black, and capable of being bent, such as a current curved screen television, a mobile phone, and the like. Nowadays, international manufacturers strive for terribly and increasingly, research and development investment on the OLED technology is strengthened, so that the OLED technology is more and more widely applied in the fields of television, computer (display), mobile phone, tablet and the like.
The principle of OLED display is essentially different from that of LCD, and OLED mainly realizes light emission by driving organic semiconductor material and light emitting material through electric field and injecting and compounding excess carriers. In essence, an ITO glass transparent electrode is used as an anode of the device, a metal electrode is used as a cathode, electrons are transmitted to an electron transmission layer from the cathode through power supply driving, holes are injected to the hole transmission layer from the anode and then are respectively transferred to a light-emitting layer, excitons are generated after the holes meet each other, luminous molecules are excited, and a light source is generated after radiation. In short, an OLED screen consists of hundreds of millions of "small bulbs".
Although the OLED display technology has a great market application prospect, there are still many problems, such as: complex production technology, large equipment investment, complex process, low yield and the like. The SiNx material for blocking water and air in the evaporation process needs to be deposited on the conductive glass substrate through a PECVD technology in combination with a mask (CVD mask), and the mask is strict in position precision requirement, and meanwhile, the mask needs to be in contact with conductive glass, so that the product is prone to being ignited to lose efficacy, and therefore the mask needs to meet the requirements of insulation and corrosion resistance. In the long-term service process, the accuracy is reduced due to the fact that a large amount of SiNx materials are accumulated on the surface of the mask plate, the OLED packaging performance is affected, in order to reduce the accumulation of the SiNx materials in the mask plate and the cavity, NF3 plasma is adopted for cleaning in the production process, when the SiNx materials are efficiently removed by NF3 plasma, F-containing plasma severely corrodes the mask plate material, and how to further improve the service life of the mask plate and the product performance is the key research point of OLED enterprises at home and abroad.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems, the invention provides the ceramic powder, the mask and the manufacturing method thereof, which can form an insulating and corrosion-resistant ceramic coating on the surface of the mask, prolong the service life of the mask and reduce the cost in the production of the OLED display device.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O344-48 parts of AlN 3-3.5 parts of SiC 1-2 parts of SiO25-10 parts of TiO25-6 parts of ZrO22.3-2.8 parts, 1-1.5 parts of ZnO and 0.2-0.4 part of rare earth oxide.
Further, the ceramic powder consists of the following raw materials in parts by weight;
Al2O345 parts of AlN 3.5 parts of SiC 1.2 parts of SiO25.2 parts of TiO26 parts of ZrO22.4 parts, 1 part of ZnO and 0.22 part of rare earth oxide.
Further, the rare earth oxide is CeO2、La2O3、Y2O3One or more combinations thereof.
Further, the rare earth oxide is La2O3、Y2O3According to the weight ratio of 1: 0: 03-0.15.
The mask comprises a mask body, a bonding layer and a ceramic coating, wherein the ceramic coating is formed by depositing ceramic powder in a plasma spraying mode.
Wherein, the thickness of the bonding layer is 0.1-0.5 μm, and the thickness of the ceramic coating is 4-10 μm.
Furthermore, the bonding layer is formed by depositing bonding powder on the surface of the version surface of the mask in a plasma spraying mode.
Further, the mask body is made of Invar 36 alloy.
Further, the bonding powder is made of Cr2O3、Al2O3、CoO2According to the weight ratio of 7-10: 1: 0.1-0.2.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 50-60L/min for 30-40S, preheating the mask version body to 650-700 ℃ by using plasma flame flow, and then feeding the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 60-80kW, the spraying current is 350-400A, the argon flow is 3.5-3.8m3H, the spraying distance is 80-100mm, and the powder feeding amount is 10-15 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, raising the temperature to 400 ℃ at the speed of 15-25 ℃/min, preserving the temperature for 1-5h, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon with the flow of 50-60L/min for 30-40S, preheating the semi-finished mask to 800-900 ℃ by using plasma flame flow, and then sending the semi-finished mask into ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of the spray gun is 60-80kW, the spraying current is 350-400A, and the argon flow is 4-4.2m3H, the spraying distance is 50-60mm, and the powder feeding amount is 40-50 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
The invention has the beneficial effects that:
the invention provides a ceramic powder, which is prepared from Al2O3、AlN、SiC、SiO2、TiO2、ZrO2ZnO, rare earth oxide, Al2O3The coating has compact structure, high hardness, good erosion corrosion resistance and high temperature oxidation resistance, but single Al2O3The coating has large brittleness, poor toughness and low bonding strength, and AlN, SiC and SiO are added to improve the performance of a single coating2、TiO2、ZrO2ZnO, rare earth oxide and other hard phases form composite ceramic powder, the defect of a single coating is overcome, AlN has good thermal conductivity and small thermal expansion coefficient, is a good thermal shock resistant material, SiC has stable chemical property, high thermal conductivity, small thermal expansion coefficient, good wear resistance and SiO2The rigid chain structure of (A) can be used as Al2O3Reinforced basic skeleton, TiO2Has higher thermal conductivity, less brittleness, stress release, crack reduction and ZrO2The addition of the rare earth oxide can lead the coating substrate to show continuous change on the composition, structure, density and function of the coating surface, relieve the thermal stress generated by the difference of thermo-physical properties among various ceramic materials, effectively improve the coating quality, lead the rare earth oxide to be capable of uniformly strengthening the structure and be distributed on Al2O3In addition, the mask plate prepared by the invention can further improve the bonding strength between the mask plate body and the ceramic coating, avoid the falling off of the ceramic coating caused by external force friction in the processes of evaporation, cleaning and the like, prolong the service life of the mask plate and reduce the cost in the production of an OLED display device.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O345 parts of AlN 3.5 parts of SiC 1.2 parts of SiO25.2 parts of TiO26 parts of ZrO22.4 parts, ZnO 1 part and La2O3、Y2O3According to the weight ratio of 1: 0.1 part of rare earth oxide.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.2 μm, and a ceramic coating with a thickness of 5 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 8: 1: 0.1, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 50L/min for 35S, preheating the mask body to 700 ℃ by using plasma flame flow, and then feeding the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 65kW, the spraying current is 400A, and the argon flow is 3.8m3H, the spraying distance is 85mm, and the powder feeding amount is 15 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, heating to 350 ℃ at the speed of 20 ℃/min, preserving heat for 2 hours, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon at the flow rate of 60L/min for 30 seconds, preheating the semi-finished mask to 880 ℃ by using plasma flame flow, and feeding ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: power of spray gun80kW, spraying current of 360A, argon flow of 4.2m3H, the spraying distance is 60mm, and the powder feeding amount is 40 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Example 2:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O348 parts of AlN 3 parts, SiC 1.5 parts and SiO25 parts of TiO25.2 parts of ZrO22.8 parts, ZnO 1 part and La2O30.3 part.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.1 μm, and a ceramic coating with a thickness of 10 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 8: 1: 0.1, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 60L/min for 35S, preheating a mask version body to 660 ℃ by using plasma flame flow, and then feeding the mask version body into the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of a spray gun is 60kW, the spraying current is 380A, and the argon flow is 3.8m3H, the spraying distance is 100mm, and the powder feeding amount is 12 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, heating to 300 ℃ at the speed of 25 ℃/min, preserving the heat for 5 hours, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon at the flow rate of 50L/min for 35S, preheating the semi-finished mask to 900 ℃ by using plasma flame flow, and then sending the semi-finished mask into ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of the spray gun is 65kW,the spraying current is 400A, and the argon flow is 4m3H, spraying distance is 55mm, and powder feeding amount is 50 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Example 3:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O344 parts of AlN 3 parts, SiC 1 part and SiO25 parts of TiO25 parts of ZrO22.3 parts, ZnO 1 part and CeO2、La2O3、Y2O3According to the weight ratio of 1: 1: 1, 0.2 parts of rare earth oxide.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.5 μm, and a ceramic coating with a thickness of 10 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 7: 1: 0.2, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 60L/min for 30S, preheating the mask body to 700 ℃ by using plasma flame flow, and then feeding the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 70kW, the spraying current is 400A, and the argon flow is 3.6m3H, the spraying distance is 100mm, and the powder feeding amount is 12 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, heating to 300 ℃ at the speed of 25 ℃/min, preserving the heat for 5 hours, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon at the flow rate of 60L/min for 40S, preheating the semi-finished mask to 850 ℃ by using plasma flame flow, and then sending the semi-finished mask to a working platform of the plasma spraying equipmentAnd (3) adding ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of the spray gun is 80kW, the spraying current is 370A, and the argon flow is 4.2m3H, the spraying distance is 60mm, and the powder feeding amount is 45 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Example 4:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O344 parts of AlN 3 parts, SiC 1 part and SiO25 parts of TiO25 parts of ZrO22.3 parts, ZnO 1 part and CeO20.2 part.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.1 μm, and a ceramic coating with a thickness of 4 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 7: 1: 0.1, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 50L/min for 30S, preheating a mask version body to 650 ℃ by using plasma flame flow, and then feeding the mask version body into the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 60kW, the spraying current is 350A, and the argon flow is 3.5m3H, the spraying distance is 80mm, and the powder feeding amount is 10 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, heating to 300 ℃ at the speed of 15 ℃/min, preserving heat for 1h, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon at a flow rate of 50L/min for 30S, preheating the semi-finished mask to 800 ℃ by using plasma flame flow, and feeding ceramic powder for secondary treatmentSpraying, wherein the secondary spraying parameters are as follows: the power of a spray gun is 60kW, the spraying current is 350A, and the argon flow is 4m3H, the spraying distance is 50mm, and the powder feeding amount is 40 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Example 5:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O348 parts of AlN 3.5 parts, SiC 2 parts and SiO210 parts of TiO26 parts of ZrO22.8 parts, ZnO 1.5 parts, La2O3、Y2O3According to the weight ratio of 1: 0.4 parts of rare earth oxide compounded by 0.15.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.5 μm, and a ceramic coating with a thickness of 10 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 10: 1: 0.2, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 60L/min for 40S, preheating the mask body to 700 ℃ by using plasma flame flow, and then feeding the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 80kW, the spraying current is 400A, and the argon flow is 3.8m3H, the spraying distance is 100mm, and the powder feeding amount is 15 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, heating to 400 ℃ at the speed of 25 ℃/min, preserving the heat for 5 hours, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon at the flow rate of 60L/min for 40S, and using plasma flame flow to conductPreheating the semi-finished product mask to 900 ℃, and then feeding the semi-finished product mask into ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of the spray gun is 80kW, the spraying current is 400A, and the argon flow is 4.2m3H, the spraying distance is 60mm, and the powder feeding amount is 50 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Example 6:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O344 parts of AlN 3.5 parts of SiC 1 part of SiO210 parts of TiO25 parts of ZrO22.8 parts, ZnO 1 part and La2O3、Y2O3According to the weight ratio of 1: 0:04 and 0.4 part of rare earth oxide.
A mask comprises a mask body made of Invar 36 alloy, a bonding layer with a thickness of 0.1 μm, and a ceramic coating with a thickness of 10 μm, wherein the bonding powder is Cr2O3、Al2O3、CoO2According to the weight ratio of 7: 1: 0.2, and mixing.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 50L/min for 40S, preheating a mask version body to 650 ℃ by using plasma flame flow, and then feeding the mask version body into the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 80kW, the spraying current is 350A, and the argon flow is 3.8m3H, the spraying distance is 80mm, and the powder feeding amount is 15 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, raising the temperature to 400 ℃ at the speed of 15 ℃/min, preserving the heat for 1h, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on the workbench of the plasma spraying equipment, replacing air in the plasma spraying equipment with argon, and then using argon to replace airVentilating a spray gun for 30 seconds by argon gas with the flow of 60L/min, preheating a semi-finished mask to 900 ℃ by using plasma flame flow, and then sending the semi-finished mask into ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of a spray gun is 60kW, the spraying current is 400A, and the argon flow is 4m3H, the spraying distance is 60mm, and the powder feeding amount is 40 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Comparative example:
the ceramic powder comprises the following raw materials in parts by weight:
Al2O345 parts of AlN 3.5 parts of SiC 1.2 parts of SiO25.2 parts of TiO26 parts of ZrO22.4 parts, ZnO 1 part and La2O3、Y2O3According to the weight ratio of 1: 0.1 part of rare earth oxide.
A mask comprises a mask body made of Invar 36 alloy and a ceramic coating with the thickness of 5 mu m.
The manufacturing method of the mask is as follows:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon with the flow of 60L/min for 30S, preheating a mask version body to 880 ℃ by using plasma flame flow, and then sending the mask version body into ceramic powder for spraying, wherein the spraying parameters are as follows: the power of a spray gun is 80kW, the spraying current is 360A, and the argon flow is 4.2m3H, the spraying distance is 60mm, and the powder feeding amount is 40 g/min;
s5: and after the spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
The comparative example was substantially the same as example 1 except that no bonding layer was provided in the finished mask of the comparative example.
Performance test 1:
the relevant performance of the mask finished product prepared in the embodiment 1 of the invention is detected, and the detection results are shown in the following table 1:
table 1:
in conclusion, the mask prepared by the invention has excellent insulating, wear-resisting and corrosion-resisting properties, and the ceramic coating on the surface of the mask has insulating and corrosion-resisting properties, so that the service life of the mask can be effectively prolonged, and the cost in the production of the OLED display device can be reduced.
Performance test 2:
10 round test pieces made of Invar 36 alloy were divided into an experimental group and a comparative group, the experimental group was sprayed with the bonding layer and the ceramic coating by the method of example 1, the comparative group was sprayed with the ceramic coating by the method of comparative example, the test equipment was an Instron1195 type tensile tester, the test loading rate was 1mm/min, the bonding strength was obtained by dividing the load at break by the sectional area of the coating sample, and the bonding strength was the average value of the test pieces of each group, and the results are shown in Table 2 below.
Table 2:
experimental group | Comparison group | |
Bonding strength/MPa | 101.6 | 68.1 |
In conclusion, the bonding layer is additionally arranged between the mask plate body and the ceramic coating, so that the bonding strength between the mask plate body and the ceramic coating can be effectively improved, and the ceramic coating is prevented from falling off due to external force friction in the processes of evaporation, cleaning and the like.
Claims (2)
1. The ceramic powder is characterized by comprising the following raw materials in parts by weight:
Al2O3 45 parts of AlN 3.5 parts of SiC 1.2 parts of SiO2 5.2 parts of TiO2 6 parts of ZrO22.4 parts, 1 part of ZnO and 0.22 part of rare earth oxide;
the rare earth oxide is La2O3、Y2O3According to the weight ratio of 1: 0: 03-0.15.
2. A mask is characterized by comprising a mask body, a bonding layer and a ceramic coating, wherein the ceramic coating is formed by depositing the ceramic powder in claim 1 in a plasma spraying manner;
the thickness of the bonding layer is 0.1-0.5 μm, and the thickness of the ceramic coating is 4-10 μm;
the bonding layer is formed by depositing bonding powder on the surface of the version surface of the mask in a plasma spraying mode;
the mask body is made of Invar 36 alloy;
the bonding powder is made of Cr2O3、Al2O3、CoO2According to the weight ratio of 7-10: 1: 0.1-0.2;
the manufacturing method of the mask specifically comprises the following steps:
s1: coarsening the surface of the version surface of the mask and fixing the version surface of the mask on a workbench of plasma spraying equipment;
s2: replacing air in the plasma spraying equipment with argon, ventilating the spray gun with argon with the flow of 50-60L/min for 30-40S, preheating the mask version body to 650-700 ℃ by using plasma flame flow, and then feeding the combined powder for primary spraying, wherein the primary spraying parameters are as follows: the power of the spray gun is 60-80kW, the spraying current is 350-400A, the argon flow is 3.5-3.8m3H, the spraying distance is 80-100mm, and the powder feeding amount is 10-15 g/min;
s3: taking out the semi-finished product mask after the primary spraying, transferring the semi-finished product mask to heat treatment equipment, raising the temperature to 400 ℃ at the speed of 15-25 ℃/min, preserving the temperature for 1-5h, and naturally recovering the room temperature;
s4: fixing the heat-treated semi-finished mask on a workbench of plasma spraying equipment, replacing air in the plasma spraying equipment with argon, ventilating a spray gun with argon with the flow of 50-60L/min for 30-40s, preheating the semi-finished mask to 800-900 ℃ by using plasma flame flow, and then sending the semi-finished mask into ceramic powder for secondary spraying, wherein the secondary spraying parameters are as follows: the power of the spray gun is 60-80kW, the spraying current is 350-400A, and the argon flow is 4-4.2m3H, the spraying distance is 50-60mm, and the powder feeding amount is 40-50 g/min;
s5: and after the secondary spraying is finished, naturally cooling to room temperature to obtain a mask plate finished product.
Priority Applications (1)
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CN105316619A (en) * | 2015-10-29 | 2016-02-10 | 中国科学院宁波材料技术与工程研究所 | Method for preparing abrasion-resistant super-hydrophobic ceramic coating through thermal spraying technology and product |
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KR20100063216A (en) * | 2008-12-03 | 2010-06-11 | 주식회사 디에프텍 | Ceramic Coating Film Formation Method by Plasma Spraying |
EP2196555A1 (en) * | 2008-12-03 | 2010-06-16 | Siemens Aktiengesellschaft | Powder mixture made from ceramic and glass, component with masking and method for application |
EP2330230A1 (en) * | 2009-12-04 | 2011-06-08 | Siemens Aktiengesellschaft | Masking material, masking device, method for masking a substrate and method for coating a substrate |
CN101782106A (en) * | 2010-03-18 | 2010-07-21 | 苏州至顺表面科技有限公司 | Insulation bearing with ceramic coating and preparation method thereof |
US9865434B2 (en) * | 2013-06-05 | 2018-01-09 | Applied Materials, Inc. | Rare-earth oxide based erosion resistant coatings for semiconductor application |
CN104451520B (en) * | 2014-12-04 | 2017-08-01 | 中国船舶重工集团公司第十二研究所 | A kind of zirconia polycrystalline rolls into a ball the preparation method of ceramic coating |
CN105369195A (en) * | 2015-10-14 | 2016-03-02 | 南京高光半导体材料有限公司 | Mask plate preparation method for preparing OLED device |
CN105449126B (en) * | 2015-12-22 | 2018-03-16 | 上海天马有机发光显示技术有限公司 | A kind of Vapor deposition mask plate and preparation method thereof |
WO2017201669A1 (en) * | 2016-05-24 | 2017-11-30 | Applied Materials, Inc. | A shadow mask with plasma resistant coating |
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JPH07166318A (en) * | 1994-09-22 | 1995-06-27 | Toshiba Corp | Mask for forming coating pattern |
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