Preparation method of AZO target material grain size used for thin-film solar cell
阅读说明：本技术 薄膜太阳能电池使用的azo靶材晶粒尺度的制备方法 (Preparation method of AZO target material grain size used for thin-film solar cell ) 是由 盖伟 古建国 尹凯 张立新 于 2021-03-04 设计创作，主要内容包括：本发明提供了薄膜太阳能电池使用的AZO靶材晶粒尺度的制备方法,属于光电材料制备技术领域,该薄膜太阳能电池使用的AZO靶材晶粒尺度的制备方法包括S1,湿法磨粉、S2,混合粉浆料干燥制粒、S3,冷等静压氧化锌铝靶材成形、S4,氧化锌铝靶材脱离橡胶模、S5,精整形和S6,烧结致密等步骤,其中,S1,湿法磨粉：在搅拌球磨机中加入一定量的研磨球、SDN6800湿法球磨用分散剂和一定比例的去离子水,并在搅拌球磨机中加入纯度大于99.95％氧化锌粉和纯度大于99.95％氧化铝粉进行混合搅拌,搅拌数小时后加入聚乙烯醇粘结剂水溶液持续搅拌得到氧化锌铝粉浆料；依据本发明实施例能够获得氧化锌铝靶材晶粒达到小于25um的水平,能够在薄膜太阳能电池中发挥优良的电学和光学性能。(The invention provides a preparation method of an AZO target material grain size used for a thin-film solar cell, which belongs to the technical field of photoelectric material preparation, and comprises the following steps of S1, wet grinding, S2, mixed powder slurry drying and granulating, S3, cold isostatic pressing zinc-aluminum oxide target material forming, S4, separation of the zinc-aluminum oxide target material from a rubber mold, S5, fine shaping and S6, sintering and compacting, and the like, wherein S1 is formed by wet grinding: adding a certain amount of grinding balls, a dispersing agent for SDN6800 wet ball milling and a certain proportion of deionized water into a stirring ball mill, adding zinc oxide powder with the purity of more than 99.95% and alumina powder with the purity of more than 99.95% into the stirring ball mill for mixing and stirring, adding a polyvinyl alcohol binder aqueous solution after stirring for several hours, and continuously stirring to obtain zinc oxide-aluminum powder slurry; according to the embodiment of the invention, the level of the zinc-aluminum oxide target material crystal grain less than 25um can be obtained, and excellent electrical and optical properties can be exerted in a thin-film solar cell.)
1. The preparation method of the AZO target material grain size used by the thin-film solar cell is characterized by comprising the following steps:
s1, wet grinding: adding a certain amount of grinding balls, a dispersing agent for SDN6800 wet ball milling and a certain proportion of deionized water into a stirring ball mill, adding zinc oxide powder with the purity of more than 99.95 percent and alumina powder with the purity of more than 99.95 percent into the stirring ball mill for mixing and stirring, adding a polyvinyl alcohol binder aqueous solution after stirring for several hours, and continuously stirring to obtain zinc oxide-aluminum mixed powder slurry;
s2, drying and granulating the mixed powder slurry: setting the grinding time in a control system of a stirring grinder, pouring the ground zinc-aluminum oxide powder slurry into a spray storage drying device, and operating spray atomization drying granulation equipment to prepare zinc-aluminum oxide spherical powder;
s3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming;
s4, separating the zinc-aluminum oxide target from the rubber mold: firstly, hoisting a die frame from a cold isostatic pressing hydraulic cylinder, taking out a die from the die frame, and finally taking out a formed blank zinc-aluminum oxide target from the die;
s5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the fine-shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is larger than or equal to 35mm, the distance between the zinc-aluminum oxide target is larger than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence.
2. The method for preparing the AZO target material with the grain size for the thin-film solar cell according to claim 1, wherein the grinding balls in the step S1 are zirconia balls.
3. The method for preparing AZO target material with crystal grain size for the thin-film solar cell according to claim 1, wherein the weight ratio of the grinding balls to the deionized water in the step S1 is (2.5-2): (1-1.5).
4. The method for preparing the AZO target material used for the thin-film solar cell according to claim 1, wherein the weight ratio of the zinc oxide powder to the aluminum oxide powder in the step S1 is (97-99.5): (3-0.5).
5. The method for preparing AZO target material with crystal grain size for the thin-film solar cell according to claim 1, wherein the grinding time range of the zinc oxide powder and the aluminum oxide powder in the step S1 is 3-6 h.
6. The method for preparing AZO target material with crystal grain size for the thin-film solar cell according to claim 1, wherein the size range of the spherical zinc aluminum oxide powder in the step S2 is 80-120 meshes.
7. The method for preparing the AZO target material used for the thin-film solar cell according to claim 1, wherein the isostatic compaction pressure in the step S3 is in a range of 150MPa to 250 MPa.
8. The method for preparing the AZO target material with the grain size for the thin-film solar cell according to claim 1, wherein the maximum sintering temperature range of the zinc-aluminum oxide target material in the step S6 is 1200-1500 ℃.
9. The method for preparing AZO target material with crystal grain size for the thin-film solar cell according to claim 1, wherein the sintering time of the zinc-aluminum oxide target material in the step S6 is 6-12 h.
Technical Field
The invention belongs to the technical field of photoelectric material preparation, and particularly relates to a preparation method of an AZO target material grain size used for a thin-film solar cell.
Background
AZO target (component composition: ZnO + Al)2O3) The Transparent Conductive Oxide (TCO) film is prepared, belongs to semiconductor photoelectron materials, has the characteristics of wider band gap, ultraviolet absorption, visible light transparency, infrared reflection, lower resistivity and the like, and can be applied to the fields of luminescent devices, solar cells, optical waveguides, sensors, flat liquid crystal displays, infrared reflectors and the like.
AZO target (component composition: ZnO: Al)2O3) Is ZnO doped Al2O3The ZnO-based transparent conductive film can be prepared by various deposition technologies; such as thermal evaporation, sputtering, ion plating; in addition, ZnO has the advantages of rich raw materials, low price, no toxicity and the like, and the deposition temperature is relatively low, so that the ZnO is green and environment-friendly, and is an excellent TCO film material.
At present, AZO target materials are mainly applied to LOW-emissivity (LOW-E) glass films and amorphous silicon thin-film solar cells. The two types of the AZO film have different requirements on the quality of the AZO target material when being applied to the AZO film function; the technical requirement of the LOW-E film on the AZO target is lower than that of an amorphous silicon thin film solar cell.
The target produced by most of the existing target enterprises can only be used for LOW-E coating, the AZO target used on the amorphous silicon thin-film solar cell has small requirement on the grain size, the general requirement is less than 25um, and the production process parameters of the AZO target are difficult to control.
Disclosure of Invention
The embodiment of the invention provides a preparation method of an AZO target material grain size used for a thin-film solar cell, and aims to solve the problem that the existing AZO target material production process parameters are difficult to control.
In view of the above problems, the technical solution proposed by the present invention is:
the invention provides a preparation method of AZO target material grain size used for a thin film solar cell, which comprises the following steps:
s1, wet grinding: adding a certain amount of grinding balls, a dispersing agent for SDN6800 wet ball milling and a certain proportion of deionized water into a stirring ball mill, adding zinc oxide powder with the purity of more than 99.95 percent and alumina powder with the purity of more than 99.95 percent into the stirring ball mill for mixing and stirring, adding a polyvinyl alcohol binder aqueous solution after stirring for several hours, and continuously stirring to obtain zinc oxide-aluminum mixed powder slurry;
s2, drying and granulating the mixed powder slurry: setting grinding time in a control system of a stirring grinder, pouring the ground zinc-aluminum oxide powder slurry into a spray drying storage device, and operating spray atomization drying granulation equipment to prepare zinc-aluminum oxide spherical powder;
s3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for isostatic pressing;
s4, separating the zinc-aluminum oxide target from the rubber mold: firstly, hoisting a die frame from a cold isostatic pressing hydraulic cylinder, taking out a die from the die frame, and finally taking out a formed blank zinc-aluminum oxide target from the die;
s5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the fine-shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is larger than or equal to 35mm, the distance between the zinc-aluminum oxide target is larger than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence.
In a preferred embodiment of the present invention, the grinding balls in step S1 are zirconia balls.
As a preferred technical solution of the present invention, the weight ratio range of the grinding balls and the deionized water in step S1 is (2.5-2): (1-1.5).
As a preferable technical scheme of the present invention, the weight ratio range of the zinc oxide powder and the alumina powder in step S1 is (97-99.5): (3-0.5).
As a preferable technical solution of the present invention, the grinding time of the zinc oxide powder and the alumina powder in the step S1 is in a range of 3h to 6 h.
In a preferred embodiment of the present invention, the size range of the spherical zinc aluminum oxide powder in step S2 is 80 to 120 meshes.
In a preferred embodiment of the present invention, the isostatic compaction pressure in step S3 is in a range of 150MPa to 250 MPa.
In a preferred embodiment of the present invention, the maximum sintering temperature range of the zinc-aluminum oxide target in step S6 is 1200-1500 ℃.
In a preferred embodiment of the present invention, the sintering time of the zinc-aluminum oxide target in step S6 is 6 to 12 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention achieves the performance requirements of the thin film solar cell by optimizing and controlling the shape and size of the zinc aluminum oxide powder, the sintering temperature and the sintering time.
(2) According to the embodiment of the invention, the crystal grain of the zinc-aluminum oxide target material can reach the level less than 25um, and the zinc-aluminum oxide target material can play excellent electrical and optical properties in a thin-film solar cell.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
Fig. 1 is a work flow chart of a method for preparing an AZO target material grain size for a thin film solar cell disclosed by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of 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 any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the equipment or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Examples
Referring to the attached figure 1, the invention provides a technical scheme: the preparation method of the AZO target material grain size used by the thin-film solar cell comprises the following steps;
the first embodiment is as follows:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 3 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: firstly setting the inlet temperature of a spray drying granulation tower to be 270 ℃, the outlet temperature to be 110 ℃, starting the heating spray drying granulation tower to ensure that the actual temperature of the inlet and the actual temperature of the outlet reach the set temperature, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, then adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower; the rotating speed control value of the atomizing disc of the spray drying granulation tower is 40.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
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S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, the sintering section temperature is 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, the time of the highest sintering temperature is 12 hours, the fracture surface of the section of the zinc-aluminum oxide target material is rough when the highest sintering temperature reaches 1500 ℃, and the grain size is more than 60 um.
Example two:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 2 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: firstly setting the inlet temperature of a spray drying granulation tower to be 270 ℃, the outlet temperature to be 110 ℃, starting the heating spray drying granulation tower to ensure that the actual temperature of the inlet and the actual temperature of the outlet reach the set temperature, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, then adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower; the rotating speed control value of the atomizing disc of the spray drying granulation tower is 40.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
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S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, the sintering section temperature is 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, the time of the highest sintering temperature is 12 hours, the fracture surface of the section of the zinc-aluminum oxide target material is rough when the highest sintering temperature reaches 1500 ℃, and the grain size is more than 60 um.
Example three:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 3 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: firstly setting the inlet temperature of a spray drying granulation tower to be 270 ℃, the outlet temperature to be 110 ℃, starting the heating spray drying granulation tower to ensure that the actual temperature of the inlet and the actual temperature of the outlet reach the set temperature, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, then adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower; the rotating speed control value of the atomizing disc of the spray drying granulation tower is 30.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
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S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, the sintering section temperature is 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, the time of the highest sintering temperature is 12 hours, the fracture surface of the section of the zinc-aluminum oxide target material is rough when the highest sintering temperature reaches 1500 ℃, and the grain size is more than 60 um.
Example four:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 3 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: firstly setting the inlet temperature of a spray drying granulation tower to be 270 ℃, the outlet temperature to be 110 ℃, starting the heating spray drying granulation tower to ensure that the actual temperature of the inlet and the actual temperature of the outlet reach the set temperature, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, then adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower; the rotating speed control value of the atomizing disc of the spray drying granulation tower is 20.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
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S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, the sintering section temperature is 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, the time of the highest sintering temperature is 12 hours, the fracture surface of the section of the zinc-aluminum oxide target material is rough when the highest sintering temperature reaches 1500 ℃, and the grain size is more than 60 um.
Example five:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 3 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: setting the inlet temperature of a spray drying granulation tower to be 270 ℃, setting the outlet temperature to be 110 ℃, starting a heating spray drying granulation tower to ensure that the actual inlet and outlet temperatures reach the set temperatures, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
item segment
1
2
3
4
5
6
7
Pressure (MPa)
60
60
100
100
160
160
200
Time(s)
Random value
180
Random value
180
Random value
180
Random value
Item segment
8
9
10
11
1
13
14
Pressure (MPa)
200
160
160
100
100
60
60
Time(s)
300
Random value
60
Random value
60
Random value
60
S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, the sintering segment temperature is 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, the time of the highest sintering temperature is 12 hours, the roughness of the fracture section of the zinc-aluminum oxide target material is obviously reduced when the highest sintering temperature is 1470 ℃, the grain size is less than 60um, the fracture section of the zinc-aluminum oxide target material is continuously reduced from the highest sintering temperature of 1470 ℃ to 1300 ℃, the fracture section of the zinc-aluminum oxide target material after sintering is rough to fine, and the grain size of the AZO target material is reduced from more than 60um to less than 25 um.
Specifically, it can be seen that the maximum sintering temperature in this embodiment can significantly reduce the grain size of the zinc aluminum oxide target, and the fracture section of the target is observed to become fine from coarse along with the reduction of the maximum sintering temperature.
Example six:
s1, wet grinding: adding 200Kg of zirconium oxide grinding balls, 37.5Kg of deionized water and 0.3Kg of SDN6800 dispersant for wet ball milling into the stirring ball mill in sequence, starting the stirring ball mill, and adjusting the control table value of the stirring ball mill to be 20; stirring for several minutes, adjusting the control table value of a stirring ball mill to be 15, adding alumina powder with the purity of more than 99.95 percent and the weight of 1.53Kg, adjusting the control table value of the stirring ball mill to be 40, returning a stirring barrel to control the table value to be 15 after stirring the alumina powder for 2 minutes, adding zinc oxide powder with the purity of more than 99.95 percent and the weight of 75Kg, adjusting the control table value of the stirring barrel to be 50 after stirring for 5 minutes, continuing stirring for 3 hours according to the control table value of 50, stopping stirring, then adding 12.5Kg of polyvinyl alcohol binder aqueous solution, slowly adjusting the control table value to be 50 from 5 within 1 minute, and continuing stirring for 1 hour according to the control table value of 50.
S2, drying and granulating the mixed powder slurry: setting the inlet temperature of a spray drying granulation tower to be 270 ℃, setting the outlet temperature to be 110 ℃, starting a heating spray drying granulation tower to ensure that the actual inlet and outlet temperatures reach the set temperatures, filtering the zinc oxide aluminum powder slurry subjected to ball milling in the step S1 by using a 300-mesh sieve, adding the filtered zinc oxide aluminum powder slurry into a material barrel of the spray drying granulation tower, continuously operating the spray drying granulation tower, and collecting dry spherical zinc oxide and aluminum oxide mixed powder, namely zinc oxide aluminum spherical powder, from a discharge port of the spray drying granulation tower.
S3, forming the zinc aluminum oxide target by cold isostatic pressing: filling the prepared zinc-aluminum oxide spherical powder into an assembled special rubber mold, placing the rubber mold in a special mold frame, and hoisting the mold frame into a cold isostatic pressing hydraulic cylinder by using a hoisting mechanical device for carrying out static pressure forming. The sectional forming pressing pressure and time values are set on the cold isostatic pressing control panel as follows:
item segment
1
2
3
4
5
6
7
Pressure (MPa)
60
60
100
100
160
160
200
Time(s)
Random value
180
Random value
180
Random value
180
Random value
Item segment
8
9
10
11
1
13
14
Pressure (MPa)
200
160
160
100
100
60
60
Time(s)
300
Random value
60
Random value
60
Random value
60
S4, separating the zinc-aluminum oxide target from the rubber mold: firstly, the mould frame is lifted out of the cold isostatic pressing hydraulic cylinder, the mould is taken out of the mould frame, and finally the formed blank zinc-aluminum oxide target material is taken out of the mould.
S5, finishing: clamping the formed blank zinc aluminum oxide target on a fine shaping lathe, and customizing the specification and the size of the fine shaping according to the size requirement required by a user;
s6, sintering and compacting: the method comprises the following steps that a precisely shaped zinc-aluminum oxide target is placed on a sintering furnace charging platform, the distance between the zinc-aluminum oxide target and a sintering furnace heating element is more than or equal to 35mm, the distance between the zinc-aluminum oxide target is more than or equal to 5mm, a sintering furnace control system sets segmented sintering temperature and time, and the two processes of heating, glue discharging and sintering of the sintering furnace are completed in the same furnace in sequence; the glue discharging temperature is as follows: at the room temperature of 100-600 ℃ for 26 hours, discharging the glue in 6 sections, wherein the sectional temperature of the glue discharging is 100 ℃, 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 600 ℃ in sequence; the sintering temperature is as follows: 600-1500 ℃ for 24 hours, sintering section temperatures of 800 ℃, 1000 ℃, 1200 ℃, 1300 ℃ and 1500 ℃ in sequence, and the time of the highest sintering temperature of 10, 8 and 6 hours in sequence, wherein the cross section and the roughness of the zinc-aluminum oxide target material are obviously reduced along with the reduction of the high-temperature sintering time when the highest sintering temperature of 1500 ℃ is reached, the grain size is reduced from more than 60um to less than 25um, and the fracture cross section of the target material is observed from rough to fine.
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 may be made to the present invention by 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.