CN111440000B - Preparation method of large-size rotary ceramic target - Google Patents
Preparation method of large-size rotary ceramic target Download PDFInfo
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- CN111440000B CN111440000B CN202010333199.5A CN202010333199A CN111440000B CN 111440000 B CN111440000 B CN 111440000B CN 202010333199 A CN202010333199 A CN 202010333199A CN 111440000 B CN111440000 B CN 111440000B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention discloses a preparation method of a large-size rotary ceramic target, belonging to the technical field of target preparation, and comprising the following steps of 1) preparing a target blank, 2) forming a mold, 3) degreasing the target blank, 4) pre-sintering the target blank, and 5) sintering the target. The preparation method of the large-size rotary ceramic target material provided by the invention has the advantages that the yield of the target material is improved, the rejection rate of raw materials is reduced, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a preparation method of a large-size rotary ceramic target.
Background
In order to improve the utilization rate of the target material, the target material is prepared into a cylindrical rotary target material, so that the utilization rate of the target material is improved to 80 percent from 30 to 35 percent of a plane target material. The limitation of the process and the production condition is that the ultra-long target material which can be directly used in a single section cannot be prepared, but a multi-section assembling mode of 200 mm and 600 mm is used, and the industry generally believes that the gap between the sections of the rotary target material has an important influence on the quality of the transparent conductive film, and in order to further improve the film coating quality of the rotary target material, the number of the abutted seams needs to be reduced, so that the length of the single section of the target material needs to be increased. The short rotary target material is formed by sintering the axis vertical to the horizontal plane, after the length of the rotary target material is increased to a certain value, because the self weight of the rotary target material is too large, the bell mouth phenomenon and the ellipse phenomenon appear on the cross section, which are caused by the inconsistent contraction of the upper and lower large diameters due to the friction force between the rotary target material and a burning bearing plate, can appear, and meanwhile, the density deviation of the target material is overproof due to the overlarge temperature difference generated by too high furnace body, and in addition, the furnace bottom has different temperature and pressure resistance due to the density deviation, so the target material has different degrees of deformation under high temperature and heavy pressure, the center of gravity of the target material is inclined, and the straightness deviation of the target material in the length direction is overlarge.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a large-size rotary ceramic target, and corresponding research and change are made from powder preparation, a forming mode, a processing method, a degreasing and pre-sintering process and the like, so that the yield of the target is improved, and the production cost is reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a large-size rotary ceramic target comprises the following steps:
1) manufacturing a target blank, wherein the target raw material is spherical particles added with enough binder for spray granulation so as to ensure the uniformity and strength of the blank during molding;
2) the forming die adopts the structure of an inner cylinder steel core outer cylinder rubber sleeve to ensure the roundness and the straightness of an inner hole of a target blank;
3) degreasing the target blank, putting the target blank into a pre-sintering furnace in a vertical mode, and keeping the degreasing temperature for 10 hours at 600 ℃;
4) pre-sintering a target blank, heating to 1100 ℃ in a pre-sintering furnace, keeping for 10 hours for pre-sintering, then cooling to room temperature along with the furnace, and enabling the target to be partially sintered to improve the strength, wherein the strength of the target blank is not lower than 20 MPa;
5) sintering the target material, horizontally placing the pre-sintered target material on two parallel sintering roller rods with the same diameter and length in a sintering furnace, wherein the sintering roller rods can synchronously and reversely rotate by being supported by a bearing outside the furnace, and the rotating speed of the sintering roller rods is maintained at 3-20 revolutions per minute; in the sintering process, oxygen is conveyed to the inner hole of the target by an air inlet pipe which is coaxial with the target, the axes of other air inlet pipes are also parallel to the axis of the target, the distance between the other air inlet pipes and the outer surface of the target is kept to be more than 5 cm, and the air inlet pipes cannot be directly blown to the surface of the target; the temperature in the sintering furnace is raised to 1500-;
the technical scheme of the invention is further improved as follows: step 1), after the target blank is subjected to cold isostatic pressing at 200MPa, the three-point bending strength of the target blank is not less than 6 MPa; bending strength, that is, flexural strength, is the ability of a material to resist bending without breaking, and is used mainly to examine the strength of brittle materials such as ceramics. The evaluation is generally carried out by a three-point bending resistance test or a four-point test method. The four-point test requires two loading forces and is relatively complex; three-point testing is most commonly used, and the value is directly proportional to the maximum pressure to be borne, which is known as three-point bending strength.
The technical scheme of the invention is further improved as follows: the binder in the step 1) comprises PVA and polymer emulsion.
The technical scheme of the invention is further improved as follows: and 2) processing the target blank by taking the inner hole as a positioning reference until the thickness deviation is less than 0.2 mm and the straightness is less than 0.2 mm.
The technical scheme of the invention is further improved as follows: and 3) heating up at a speed of less than 0.5 ℃ per minute in the target blank degreasing process.
The technical scheme of the invention is further improved as follows: step 5) the sintering roller rods are made of recrystallized silicon carbide or sintered silicon carbide, the sintering roller rods are subjected to finish machining through a diamond grinding wheel before use, the straightness is less than 0.1 mm, the sintering roller rods are supported by an outer bearing of a sintering furnace, the parallelism of the sintering roller rods is less than 0.2 mm, the levelness of the sintering roller rods is less than one thousandth, a pair of gears with the same diameter and the same number of teeth are meshed at the same ends of the two sintering roller rods, the gears are connected with a speed reducer through chains, and the speed of the gears is adjusted through a frequency converter; two ends of the sintering roller rod in the sintering furnace are provided with a stop ring for preventing the target material from colliding with the furnace wall.
The technical scheme of the invention is further improved as follows: the temperature rise speed in the pre-sintering furnace is preferably 0.2 ℃ per minute in the degreasing process of the target blank, the temperature in the sintering furnace is preferably 1520 ℃ in the target sintering process, and the rotation speed of the target is preferably 6 revolutions per minute.
Due to the adoption of the technical scheme, the invention has the technical progress that:
according to the preparation method of the large-size rotary ceramic target, the three-point bending strength of the target blank is not less than 6MPa after the target blank is subjected to cold isostatic pressing at 200MPa, and the unsintered target blank has enough strength, which is important for ensuring that the yield is enough in the subsequent operation process.
According to the preparation method of the large-size rotary ceramic target provided by the invention, the binder of the target blank body comprises PVA and polymer emulsion, and spherical particles added with enough binder for spray granulation can ensure the uniformity and strength of the target blank body during molding.
According to the preparation method of the large-size rotary ceramic target, the forming die adopts the structure of the inner cylinder, the steel core and the outer cylinder rubber sleeve, so that the roundness and the straightness of the inner hole of the target blank are ensured as the core; when the target blank is processed by taking the inner hole as a positioning reference, the standards that the concentricity of the inner part and the outer part is not more than 0.1 mm and the straightness is not more than 0.2 mm are met.
According to the preparation method of the large-size rotary ceramic target, the target blank is placed in a sintering furnace in a vertical mode to prevent the target blank from deforming; the degreasing temperature is kept for 10 hours at 600 ℃, the temperature rising speed is slow during degreasing so as to avoid the defect caused by too fast decomposition of organic matters, the common binder can be removed completely when the temperature reaches 600 ℃, the strength of the target is very low at this time, the target cannot be moved, and the pre-sintering aims at improving the strength of the target blank so as to ensure that the target blank cannot be cracked and abraded in the subsequent rolling sintering process.
The invention provides a preparation method of a large-size rotary ceramic target, which is characterized in that a pre-sintered target blank is placed on two parallel sintering roller rods with the same diameter and length, the sintering roller rods are supported by a bearing seat outside a furnace and can synchronously and reversely rotate, the rotating speed is maintained at 3-20 r/min, and the target can still normally and stably rotate to be good when the sintering roller rods are spaced and the target is sintered and shrunk; the material of the sintering roller rod is preferably recrystallized silicon carbide or sintered silicon carbide, and the two materials can still keep higher elastic modulus and bending strength at the high temperature of 1550 ℃ so as to resist deformation under high load.
According to the preparation method of the large-size rotary ceramic target, oxygen is conveyed to the inner hole of the target through the air inlet pipe which is coaxial with the target in the sintering process, the axes of other air inlet pipes are also parallel to the axis of the target, the distance between the other air inlet pipes and the outer surface of the target is kept to be more than 5 cm, and the oxygen cannot be directly blown to the surface of the target, so that the target blank is prevented from being deformed or cracked under stress to cause defective products.
According to the preparation method of the large-size rotary ceramic target material, the rotation speed of the target material is 2-20 rpm, preferably 6 rpm, in the sintering process, so that the target material can be uniformly heated, and the yield is improved.
Drawings
FIG. 1 is a schematic structural diagram of a sintering furnace used in the method for preparing a large-size rotary ceramic target material according to the present invention;
the device comprises a sintering furnace 1, a sintering furnace 2, a target 3, a gear 4, a bearing 5, a sintering roller 6 and an air inlet pipe.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings 1 and examples:
a preparation method of a large-size rotary ceramic target material is disclosed, wherein FIG. 1 is a schematic diagram of the method, mainly comprising a sintering furnace and a schematic diagram of the internal structure of the sintering furnace; the method specifically comprises the following steps:
1) manufacturing a target blank, wherein the raw material of the target blank is spherical particles added with enough binder for spray granulation so as to ensure the uniformity and strength of the blank during molding;
2) the forming die adopts the structure of an inner cylinder steel core outer cylinder rubber sleeve;
3) degreasing the target blank, putting the target blank into a pre-sintering furnace in a vertical mode, and keeping the degreasing temperature for 10 hours at 600 ℃;
4) pre-sintering the target blank, heating the target blank to 1100 ℃ in a pre-sintering furnace, keeping the temperature for 10 hours for pre-sintering, then cooling the pre-sintering furnace to room temperature, and partially sintering the target 2 to improve the strength in the process, wherein the strength of the target blank is not lower than 20 MPa;
5) sintering the target material, wherein the temperature in the sintering furnace 1 is raised to 1500-;
in the embodiment provided by the invention, the three-point bending strength of the target blank is not less than 6MPa after the target blank is subjected to cold isostatic pressing at 200MPa, and the sufficient strength is achieved, so that the reliability of subsequent processing operation can be ensured. Bending strength, that is, flexural strength, is the ability of a material to resist bending without breaking, and is used mainly to examine the strength of brittle materials such as ceramics. The evaluation is generally carried out by a three-point bending resistance test or a four-point test method. The four-point test requires two loading forces and is relatively complex; three-point testing is most commonly used, and the value is directly proportional to the maximum pressure to be borne, which is known as three-point bending strength.
Furthermore, the adhesive comprises PVA and polymer emulsion, and the PVA has the characteristics of high adhesive strength, high decomposition speed in high temperature, convenient synthesis, safety, low toxicity, easy control of product quality, low price, convenient use and the like.
Further, the forming die adopts a structure of an inner cylinder steel core outer cylinder rubber sleeve to ensure the roundness and straightness of an inner hole of a blank body as a core; when the target blank is processed by taking the inner hole as a positioning reference, the standards that the concentricity of the inner part and the outer part is not more than 0.1 mm and the straightness is not more than 0.2 mm are met, so that the target blank is not easy to deform in the later sintering process, and the precision is ensured.
Further, the target blank is placed in a pre-sintering furnace in a vertical mode to prevent the blank from deforming; the degreasing temperature is kept for 10 hours at 600 ℃, the heating speed is slow during degreasing so as to avoid the defect caused by too fast decomposition of organic matters, the binder used when the temperature is raised to 600 ℃ can be completely removed, at the moment, the strength of the target 2 is very low and cannot be moved, the aim of pre-sintering is to improve the strength of the target blank so as to ensure that the target blank is not cracked and abraded in the subsequent rolling sintering process, the slow heating speed is adopted during degreasing so as to avoid the internal defect, the heating speed is less than 0.5 ℃ per minute, the heating speed is better at 0.1-0.3 ℃ per minute, and the optimal temperature is 0.2 ℃ per minute. The degreasing temperature was maintained at 600 degrees celsius for 10 hours. Then the temperature is raised to 1100 ℃ at the heating rate of 0.5 ℃ per minute, the temperature is preserved for 10 hours, then the temperature is reduced to the room temperature along with the furnace, the process causes the target 2 to be partially sintered to improve the strength, and the strength of the target blank is not lower than 20 MPa.
Further, the pre-sintered target blank is placed on two parallel sintering roller rods 5 with the same diameter and length, the sintering roller rods 5 are supported by a bearing 4 outside the sintering furnace and can synchronously and reversely rotate, the rotating speed is maintained at 3-20 revolutions per minute, and the target 2 can still normally and stably rotate better when the distance between the sintering roller rods 5 is equal to the sintering shrinkage of the target 2; the material of the sintering roller rod 5 is preferably recrystallized silicon carbide or sintered silicon carbide, the two materials can still keep higher elastic modulus and bending strength at the high temperature of 1550 ℃ to resist deformation under high load, and the deformation degree is less than 0.2 mm; before use, the sintering roller rods 5 are subjected to finish machining by a diamond grinding wheel, the straightness is less than 0.1 mm, the sintering roller rods are supported by an external bearing 4, the parallelism is less than 0.2 mm, the levelness is less than one thousandth, a pair of gears 3 with the same diameter and the same number of teeth are meshed at the same ends of the two sintering roller rods 5, the gears 3 are connected with a speed reducer by chains, and the speed is adjusted by a frequency converter. Two ends of the sintering roller rod 5 in the furnace are provided with a stop ring for preventing the target material 2 from colliding with the furnace wall.
Further, in the sintering process, oxygen is conveyed to the inner hole of the target 2 through the air inlet pipe 6 which is coaxial with the target 2, the axes of other air inlet pipes 6 are also parallel to the axis of the target 2, the distance between the other air inlet pipes and the outer surface of the target 2 is kept to be more than 5 cm, and the air inlet pipes cannot be directly blown to the surface of the target 2, so that the target blank is prevented from being deformed or cracked under stress to cause defective products.
Further, the rotation speed of the target 2 in the sintering process is 2-20 rpm, preferably 6 rpm, so that the target 2 can be heated uniformly, and the yield is improved.
In the embodiment, ITO powder containing 1.2% PVA binder is filled into a rotating target 2 blank forming die to obtain a target 2 blank with the inner diameter of 166 +/-0.1 mm, the outer diameter of 191 +/-0.5 mm and the length of 1300 mm, and the outer diameter of 189.6 +/-0.1 mm is obtained after the outer circle of the target 2 blank is turned on a special lathe by using a special tool after the inner hole is used as a reference for positioning; and vertically placing the target blank into a pre-sintering furnace, uniformly heating to 600 ℃ at a speed of 12 ℃ per hour, keeping for 10 hours for degreasing, then heating to 1100 ℃ at a speed of 30 ℃ per hour, keeping for 10 hours, and cooling to room temperature along with the furnace. The pre-sintered target material 2 is horizontally placed on a sintering roller rod 5 of a rolling sintering furnace 1, the diameter of the sintering roller rod 5 is 63 mm, the center distance is 110 +/-0.1 mm, the temperature is raised to 1520 ℃ at the speed of 0.5 ℃ per minute under flowing pure oxygen, the sintering is carried out for 10 hours under the condition that the temperature is kept, the inner diameter is detected to be 134.4 +/-0.15 mm, the outer diameter is detected to be 153.6 +/-0.15 mm, the length is detected to be 1053 mm, the straightness of the target material 2 is 0.2 mm, the weight is 32.629 kg, and the density of a sintered body is measured to be 7.135 g per cubic centimeter by an Archimedes method.
In particular, in the embodiment provided by the invention, the invention discloses a preparation method of a large-size rotary ceramic target, and provides a method for preparing the large-size rotary ceramic target by manufacturing a target blank, a forming die, degreasing the target blank, pre-sintering the target blank and sintering the target.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are intended to be within the scope of the invention.
Claims (2)
1. A preparation method of a large-size rotary ceramic target is characterized by comprising the following steps: the method specifically comprises the following steps:
1) manufacturing a target blank, wherein the raw material of the target (2) is spherical particles added with enough binder for spray granulation; the three-point bending strength of the target blank is not less than 6MPa after the target blank is subjected to cold isostatic pressing at 200 MPa;
2) the forming die adopts the structure of an inner cylinder steel core outer cylinder rubber sleeve; the thickness deviation of the target blank body is less than 0.2 mm and the straightness is less than 0.2 mm when the target blank body is processed by taking an inner hole as a positioning reference;
3) degreasing the target blank, putting the target blank into a pre-sintering furnace in a vertical mode, and keeping the degreasing temperature for 10 hours at 600 ℃; the temperature rise speed in the pre-sintering furnace is 0.1-0.3 ℃ per minute in the degreasing process of the target blank;
4) pre-sintering a target blank, heating to 1100 ℃ at the speed of 30 ℃ per hour in a pre-sintering furnace, keeping for 10 hours for pre-sintering, and then cooling to room temperature along with the furnace, wherein the target (2) is partially sintered to improve the strength, and the strength of the target blank is not lower than 20 MPa;
5) sintering the target material (2), horizontally placing the pre-sintered target material (2) on two parallel sintering roller rods (5) with the same diameter and length in a sintering furnace (1), wherein the sintering roller rods (5) are supported by a bearing (4) outside the furnace and can synchronously and reversely rotate, and the rotating speed is maintained at 3-20 revolutions per minute; in the sintering process, oxygen is conveyed to an inner hole of the target (2) by an air inlet pipe (6) which is coaxial with the target (2), the axes of other air inlet pipes (6) are also parallel to the axis of the target (2), the distance between the other air inlet pipes and the outer surface of the target (2) is kept more than 5 cm, and the air inlet pipes cannot be directly blown to the surface of the target (2); a pair of gears (3) with the same diameter and the same number of teeth are meshed at the same end of the two sintering roller rods (5), the gears (3) are connected with a speed reducer through chains and the speed is adjusted through a frequency converter, and the rotating speed of the target (2) is 6 revolutions per minute in the sintering process; two ends of a sintering roller rod (5) in the sintering furnace (1) are provided with a stop ring for preventing the target material (2) from colliding with the furnace wall; the temperature in the sintering furnace (1) rises to 1520 ℃, the temperature rise speed is 0.5 ℃ per minute, the sintering is kept for 10 hours, the sintering roller rod (5) ensures that the deformation is less than 0.2 mm under the condition that the target (2) is loaded at 1550 ℃, the sintering roller rod (5) is made of recrystallized silicon carbide or sintered silicon carbide, the sintering roller rod (5) is finely processed by a diamond grinding wheel before being used, the straightness is less than 0.1 mm, the parallelism is less than 0.2 mm, and the levelness is less than one thousandth.
2. The method for preparing a large-size rotary ceramic target according to claim 1, wherein the method comprises the following steps: the binder in the step 1) comprises PVA and polymer emulsion.
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| CN204620744U (en) * | 2015-05-11 | 2015-09-09 | 基迈克材料科技（苏州）有限公司 | Sputtering rotary target material straightener |
| CN105712719A (en) * | 2016-04-19 | 2016-06-29 | 北京冶科纳米科技有限公司 | Normal-pressure sintering and manufacturing method for large-sized high-density fine-grain ITO target material |
| CN106631049A (en) * | 2016-09-28 | 2017-05-10 | 广西晶联光电材料有限责任公司 | Method for sintering ITO (indium tin oxide) rotating target material used in touch screen and solar cell fields under normal pressure |
| CN107244911A (en) * | 2017-01-13 | 2017-10-13 | 昆明理工大学 | A kind of preparation method of ITO tubular targets |
| CN106977179A (en) * | 2017-04-07 | 2017-07-25 | 中国船舶重工集团公司第七二五研究所 | A kind of method that two steps multi-steps sintering method prepares high fine and close ITO target |
| CN106985261A (en) * | 2017-04-07 | 2017-07-28 | 中国船舶重工集团公司第七二五研究所 | The centrifugal pressure method of ITO rotary target base substrate one sides and mould |
| CN107010940A (en) * | 2017-04-07 | 2017-08-04 | 中国船舶重工集团公司第七二五研究所 | A kind of control oxygen content prepares methods of the TFT LCD with ITO sputtering targets |
| CN107522483A (en) * | 2017-06-26 | 2017-12-29 | 广西新未来信息产业股份有限公司 | A kind of preparation method of AZO targets |
| CN110270689A (en) * | 2018-03-13 | 2019-09-24 | 东莞杰宇机械有限公司 | A kind of bimetal tube sleeve forming technique |
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