CN116023127A - YBCO target manufacturing method and target mold - Google Patents
YBCO target manufacturing method and target mold Download PDFInfo
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- CN116023127A CN116023127A CN202211700069.6A CN202211700069A CN116023127A CN 116023127 A CN116023127 A CN 116023127A CN 202211700069 A CN202211700069 A CN 202211700069A CN 116023127 A CN116023127 A CN 116023127A
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Abstract
The invention discloses a method for manufacturing a YBCO target and a target mould, wherein the method comprises the following steps: preparing target material powder by adopting a solid phase reaction method; placing the target powder in a target mould and then performing thermal sintering to obtain a target; wherein the density of the target material is more than 95%. According to the manufacturing method of the YBCO target and the target die, raw material granularity is reduced through repeated grinding and presintering, and the target prepared through the spark plasma assisted hot-pressing sintering or cold pressing method is smooth in surface and has the compactness of more than 95%.
Description
Technical Field
The invention relates to the technical field of targets, in particular to a method for manufacturing a YBCO target and a target die.
Background
The compactness is a key performance index of the target material and is the ratio of the actual density to the theoretical density of the target material. The low-density target material has more pores and more adsorbed impurities, and meanwhile, in the film growth process, loose particle clusters are easy to fall off due to the instant high temperature of the sputtering surface of the target material, so that the surface of a substrate is polluted, and the film plating quality is influenced. The prior target manufacturing method has the problems that the density (70-80%) of the target is low and the surface particles are large when the target with large size (such as 2 inches) is manufactured, and the surface of the manufactured film has a large number of large liquid drop particles, as shown in figure 1, and the surface fluctuation is very large.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for manufacturing a YBCO target, wherein the target is manufactured by a spark plasma assisted hot press sintering or cold pressing method, and has a smooth surface and a compactness of more than 95%.
According to an aspect of the present invention, there is provided a method for manufacturing a YBCO target, including: preparing target material powder by adopting a solid phase reaction method; placing the target powder in a target mould and then performing thermal sintering to obtain a target; wherein the density of the target material is more than 95%.
Optionally, the step of preparing the target powder by a solid phase reaction method comprises: preparing a plurality of raw materials with high purity according to a chemical dosage ratio; grinding and mixing a plurality of raw materials; presintering various raw material powders in an atmosphere; repeating the steps of grinding, mixing and presintering a plurality of times; grinding the raw material after the last presintering to obtain target powder.
Optionally, the method for thermally sintering the target powder in the mold to obtain the target comprises the following steps: a hot-press sintering method and a cold-press method assisted by discharge plasma.
Optionally, the step of obtaining the target material by adopting a spark plasma assisted hot press sintering method comprises the following steps: placing target material powder in a mould, prepressing, and placing the mould in discharge plasma sintering equipment; inserting a thermocouple into the die, and vacuumizing the sintering environment in the sintering equipment to a preset value; setting a pressure value and a temperature rise process system of sintering equipment; sintering the target powder in the die to obtain the target.
Optionally, the sintering environment within the sintering apparatus is evacuated to 10Pa.
Optionally, the sintering equipment is set to a pressure value of 30-70MPa.
Optionally, setting a temperature rise process system of the sintering equipment as follows: heating to 900 ℃ at the heating speed of 100-200 ℃/min, and rapidly cooling after heat preservation for 5-10 min.
Optionally, the step of obtaining the target material by cold pressing comprises: placing target powder in a target mould and prepressing the target powder by a tablet press; sintering the cold-pressed blank according to preset temperature and time to obtain the target material.
Optionally, the target powder is pre-pressed by a tablet press at a pressure of 300-1450MPa.
Alternatively, the sintering temperature is 900 ℃ and the sintering time is 24 hours.
Optionally, in the step of pre-sintering the plurality of raw material powders under an atmosphere, the sintering temperature is 900 ℃ and the sintering time is 24 hours.
Optionally, the steps of milling and pre-sintering are repeated a number of times, the number of times the steps of milling and pre-sintering are repeated between 2 and 5 times.
Alternatively, when the plurality of raw materials of the target material have a volatile raw material, the number of repetition of the grinding mixing and pre-sintering steps can be reduced.
Alternatively, when the target has a volatile raw material among a plurality of raw materials, the sintering time of the pre-sintering step may be reduced.
According to another aspect of the present invention, there is provided a target mold comprising: a first base having a first protrusion; a restriction ring having a first hollow portion at a center thereof for accommodating the first protrusion; an open annulus having a second hollow portion in the center thereof, which can be placed in the first hollow portion of the restriction ring; a compression sheet which can be placed in the second hollow part of the valve opening ring; and a second base having a second protrusion, wherein the second protrusion is accommodated in a second hollow portion of the valve opening ring, wherein the valve opening ring is composed of a plurality of valve portions, and the second hollow portion of the valve opening ring is used for placing target powder.
Optionally, the open annulus comprises 3-5 petals.
Optionally, the pressing sheets include a first pressing sheet and a second pressing sheet, after the first pressing sheet is placed in the second hollow part of the valve opening ring, target powder is placed in the second hollow part of the valve opening ring, and then the second pressing sheet is placed above the target powder in the second hollow part of the valve opening ring.
Optionally, the first protrusion of the first base, the valve opening ring, the pressing sheet and the second protrusion of the second base are made of Cr12 steel.
Optionally, the material of the limiting ring is 304 steel, and the first base and the second base further comprise a housing made of 304 steel.
Optionally, the maximum pressure that the target mold can withstand is 1450Mpa.
According to the method for manufacturing the YBCO target, disclosed by the invention, raw materials of the target are ground and sintered for multiple times, the obtained powder is fine enough, and the powder is sufficiently and uniformly mixed, so that the powder granularity of the target is reduced, and the surface smoothness of the target can be further improved.
Further, the YBCO target material provided by the application is prepared by adopting a plasma discharge assisted sintering process, has the characteristics of high heating speed (100-300 ℃/min), short sintering time, low sintering temperature, uniform crystal grains and the like, and is beneficial to controlling the fine microstructure of sintered blocks and obtaining high-density block materials, so that the YBCO target material prepared by the application has uniform component distribution and has the density of more than 95%.
Further, the YBCO target provided by the application is subjected to cold press molding through the split die, and then is subjected to hot sintering preparation, and as the pressure which can be born by the split die is 300 tons (1450 MPa) or less, the density of the YBCO target subjected to cold press molding is high, and the components of the YBCO target prepared finally are distributed uniformly, and the density of the YBCO target reaches over 95 percent.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent from the following description of embodiments of the present invention with reference to the accompanying drawings, in which:
FIG. 1 shows a thin film surface prepared from a low density (75%) target according to the prior art;
fig. 2 shows a flow chart of a method of manufacturing a YBCO target according to an embodiment of the present invention;
fig. 3 shows a flow chart of sintering steps of a method of manufacturing a YBCO target according to a first embodiment of the present invention;
FIG. 4 shows a target sintering ramp up process diagram according to a first embodiment of the present invention;
fig. 5 shows a flow chart of sintering steps of a method of manufacturing a YBCO target according to a second embodiment of the present invention;
fig. 6 shows an open-die diagram of a target according to a second embodiment of the invention.
Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings. Like elements are denoted by like reference numerals throughout the various figures. For clarity, the various features of the drawings are not drawn to scale. Furthermore, some well-known portions may not be shown. The device structure obtained after several steps may be depicted in one figure for simplicity.
So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized below, may be had by reference to the appended drawings and examples.
Fig. 2 shows a flow chart of a method of manufacturing a YBCO target according to an embodiment of the present invention; fig. 3 shows a flow chart of sintering steps of a method of manufacturing a YBCO target according to a first embodiment of the present invention; fig. 4 shows a target sintering temperature rise process diagram according to a first embodiment of the present invention.
Referring to fig. 2, the steps of one embodiment of a method of manufacturing a YBCO target of the present application are as follows, wherein the manufactured target is, for example, a YBCO polycrystalline target.
Step S10: preparing target material powder from various raw materials with high purity according to stoichiometric ratio.
Step S20: grinding with a ball mill, mixing the powder thoroughly and reducing the powder particle size.
Step S30: presintering is carried out in the atmosphere.
Step S40: steps S20 and S30 are repeated a plurality of times.
Step S50: and grinding the powder pre-sintered for the last time again to finish the target powder.
Step S60: sintering the target powder in a mould.
In this example, the target produced is a YBCO polycrystalline target, and the starting material comprises BaCO with a purity of 99.99% 3 CuO, and Y 2 O 3 . Raw materials with the same purity are prepared according to the stoichiometric ratio, and then are ground by a ball mill, so that the granularity of the various raw materials is reduced and the raw materials are fully mixed. The mixed target raw material powder is presintered in an atmosphere at a temperature of, for example, 900 ℃ for a time of, for example, 24 hours. Further, grinding is performed again by the ball mill, and pre-sintering is performed under an air atmosphere, i.e., steps S20 and S20 are repeatedStep S30 is repeated so that the particle sizes of the various raw materials are further reduced and sufficiently mixed. And after the steps of multiple grinding and presintering, fully grinding the target material after the last presintering to finish the preparation of YBCO target powder.
In step S40, the number of repetition of pre-sintering and grinding of the raw material may be set differently according to the raw material. In this embodiment, the steps S20 pre-sintering and S30 grinding are repeated, for example, 2 to 5 times, depending on the target being manufactured as YBCO polycrystalline target.
In another embodiment, the target preparation method provided by the application can be used for preparing targets of other materials, and the targets of other materials comprise BiFeO 3 ，SrTiO 3 ，Ga 2 O 3 And the like, and only the preparation steps are required to be adaptively modified according to the corresponding target materials.
Furthermore, in other embodiments, if the starting material of the target is produced with a volatile substance, e.g. to produce a ferroelectric target BiFeO 3 The material having Bi element is a volatile raw material, and in order to reduce the loss of the volatile raw material, volatilization can be reduced by adopting measures such as reducing the number of pre-sintering reactions, the reaction time, and the like. Furthermore, the target pressing process can be added after grinding, and then the presintering process is carried out, so that the presintering reaction is more sufficient. Wherein, in the target pressing process of the presintering stage, the pressure of less than 100MPa can be adopted.
Further, after the manufacture of the target powder is completed, the method further comprises the step of sintering the target powder in a mold to obtain the formed target. In this example, the methods employed in this step include spark plasma assisted hot press sintering (Spark Plasma Sintering Technology, SPS) and cold pressing.
In the spark plasma assisted sintering (Spark Plasma Sintering), an ON-OFF dc pulse voltage generated by a special power supply control device is applied to a powder sample, so that a sintering acceleration effect (discharge impact pressure and joule heating) caused by usual electric discharge machining is utilized, and a sintering acceleration effect caused by a spark discharge phenomenon (instantaneous generation of high-temperature plasma) generated between powders at the initial stage of pulse discharge is effectively utilized to realize densification by an instantaneous high-temperature field. In the SPS process, besides the sintering process is promoted by the Joule heat of hot-pressed sintering and plastic deformation caused by pressurization, direct-current pulse voltage is generated among powder particles, and the self-heating effect generated by discharge among powder particles is effectively utilized; because the pulse is generated instantaneously, intermittently and at high frequency, the discharge part and the Joule heating part in the powder can move rapidly, the diffusion of powder particle atoms is greatly promoted, and the diffusion coefficient is much larger than that of the powder under the normal hot pressing condition, so that the rapid sintering of the powder is achieved.
In this example, the procedure for preparing the target using the plasma assisted hot pressed sintering method is shown in fig. 3.
Step S611: and (3) placing the target powder into a die, and placing the die into sintering equipment.
Step S612: a thermocouple is inserted into the mold and the sintering environment within the sintering apparatus is evacuated to a predetermined value.
Step S613: setting the pressure value and the temperature rise process system of sintering equipment, and starting sintering.
Step S614: and (5) ending sintering to obtain the target material.
In the application, the target material prepared by adopting the plasma assisted hot-pressed sintering method can have high density, and the density is more than 95%. In this embodiment, the target powder prepared in the steps S10 to S50 is placed into a mold of a sintering device, and is pre-pressed under a pressure of 5MPa and then placed into the sintering device, and the pre-pressing step makes the target powder have a certain density and shape in the mold, so that the subsequent sintering is facilitated. In this embodiment, the mold of the sintering apparatus is a graphite mold.
Further, a thermocouple is inserted into a die in which the target powder is placed, and a sintering chamber of the sintering equipment is vacuumized to a vacuum degree of 10Pa; or the sintering chamber is filled with argon.
Further, parameters of the sintering equipment are set, including pressure values and a temperature rise process regime. Wherein, the pressure value of the sintering equipment is set to be 30-70MPa, the temperature rise process system of the sintering equipment is set as shown in figure 4, and then the sintering of the target powder in the die is started.
Referring to FIG. 4, in the heating process system, heating starts at time t1 until reaching a preset temperature at time t2, wherein the heating speed is, for example, 100-200 ℃/min; the time period from the time t2 to the time t3 is a heat preservation time, and the time between the time t3 and the time t4 is a rapid cooling time. Specifically, the time period of t1-t2 is 4-9min, the time period of t2-t3 is 5-10min, and the time period of t1-t4 is within 30 min.
In this embodiment, during the rapid cooling time of t3-t4, the sintering apparatus can rapidly cool the sintered target by circulating water.
And further, after sintering and cooling, unloading the pressure loaded by the sintering equipment, and removing a sintered finished product after inflating the sintering chamber of the sintering equipment to the normal atmosphere, namely the prepared YBCO target.
According to the manufacturing method of the YBCO target, raw materials of the target are ground and sintered for many times, powder is obtained, the powder is fine enough, the powder is sufficiently and uniformly mixed, and the powder granularity of the target is reduced.
Further, the target material provided by the application is prepared by adopting a plasma discharge assisted sintering process, has the characteristics of high heating speed (100-300 ℃/min), short sintering time, low sintering temperature, uniform crystal grains and the like, and is beneficial to controlling the fine microstructure of sintered blocks and obtaining high-density block materials, so that the target material prepared by the application has uniform component distribution and has the density of more than 95%.
Fig. 5 shows a flow chart of sintering steps of a method of manufacturing a YBCO target according to a second embodiment of the present invention; fig. 6 shows an open-die diagram of a target according to a second embodiment of the invention.
Referring to fig. 5, the method for preparing a target material using cold press sintering is as follows.
Step S621: and (5) installing a split die, and placing target powder into the split die.
Step S622: and (3) putting the split die with the target powder into a tablet press, and cold-pressing and molding.
Step S623: sintering the cold-pressed blank according to preset temperature and time.
Step S624: and (5) ending sintering to obtain the target material.
In the embodiment, the prepared target powder is placed in a split die, the split die with the target powder is placed in a tablet press, the pressure of 300-1450MPa is loaded, and the target powder is subjected to cold press molding, so that a blank is obtained. And further taking out the formed blank from the split die, placing the blank in an environment of 900 ℃, sintering for 24 hours, and cooling to obtain the target material with the density of more than 95%.
In this example, the split mold used in cold press molding the target powder is shown in fig. 6. The split die comprises: a first base 10, a confinement ring 20, an open annulus 30, a compression tab 40 and a second base 50. In this embodiment, the split die is, for example, a 2 inch die, i.e., the size of the cold formed target is 2 inches.
The first base 10 includes three parts, a first housing 11, a bottom 12 wrapped by the first housing 11, and a first protrusion 13 connected to the bottom 12. Wherein, the bottom 12 and the first bulge 13 are integrally formed parts, and the material of the parts is Cr12 steel; the first housing 11 wraps at least the side surface of the bottom 12 and the bottom surface far from the first protrusion 13, and the material of the first housing 11 is 304 steel.
The intermediate portion of the confinement ring 20 is a first hollow portion, as indicated by the dashed line 21 in fig. 6. Specifically, the diameter of the first hollow portion of the confinement ring 20 is equal to or slightly smaller than the diameter of the first protrusion 13 in the first base 10. Further, the first hollow portion of the restriction ring 20 has a stepped column shape, that is, the diameter of the first hollow portion on the side close to the first base 10 shown in fig. 6 is larger than the diameter on the side away from the first base 10. In this embodiment, the angle of inclination of the side wall of the first hollow portion of the confinement ring 20 is, for example, 1.5 °.
The ring 30 is entirely hollow and annular, and the dashed line 31 in fig. 6 illustrates that the second hollow portion of the ring 30 has an outermost diameter of the ring 30 that is equal to or slightly smaller than the diameter of the second hollow portion of the ring 20, i.e. the ring 30 can be entirely placed in the first hollow portion of the ring 20, so that the outermost side wall of the ring 30 also has an inclination angle of 1.5 °. Further, the open annulus 30 comprises a plurality of petals that combine to form a hollow open annulus 30. In this embodiment, the number of petals of the open annulus 30 is, for example, 3-5.
The compression sheet 40 is a cylinder with a diameter equal to or slightly smaller than the diameter of the second hollow portion of the valve ring 30, i.e. the compression sheet 40 can be integrally placed in the second hollow portion of the valve ring 30. In addition, the height of the sheeting 40 is also less than the height of the open annulus 30. In this embodiment, the preform 40 comprises a first preform 41 and a second preform 42, the first preform 41 and the second preform 42 being of the same size, diameter, thickness.
The second base 50 includes three parts, a second housing 51, a top 52 surrounded by the second housing 51, and a second protrusion 53 connected to the top 52. Wherein, the top 52 and the second bulge 53 are integrally formed parts, and the material of the parts is Cr12 steel; the second housing 51 is made of 304 steel material and wraps at least the side surface of the top 52 and the bottom surface far from the second protrusion 53. Wherein the diameter of the second protrusion 53 is the same as the diameter of the compression sheet 40, and is equal to or slightly smaller than the diameter of the second hollow portion of the valve opening ring 30.
The application method of the split die comprises the following steps: placing the first protrusion 13 of the first base 10 upward; placing the side of the first hollow portion of the confinement ring 20, the diameter of which matches the diameter of the first protrusion 13 of the first base 10, downward, and positioning the first protrusion 13 of the first base 10 in the first hollow portion of the confinement ring 20; placing the open annulus 30 in the first hollow portion of the confinement ring 20; placing a first compression sheet 41 into the second hollow portion of the open annulus 30; filling the second hollow portion of the valve ring 30 with target powder above the first pressing piece 41; placing a second press sheet 42 over the target powder in the second hollow portion of the split ring 30; placing the second protrusion 53 of the second base 50 downward on the second base 50 such that the second protrusion 53 of the second base 50 is located in the second hollow portion of the open annulus 30; and (3) putting the whole split die into a tablet press, and carrying out cold press molding on the target powder by loading pressure. In this embodiment, the usage of the split mold can be simply seen as the sequential nesting of the five components in fig. 6 from bottom to top.
In another embodiment, the split mold may be used by first placing the split ring 30 in the first hollow portion of the confinement ring 20, then placing the split ring 30 and the confinement ring 20 together on the first base 10, so that the first protrusion 13 in the first base 10 is located in the first hollow portion of the confinement ring 30,
the split die provided by the application can bear the weight below 300 tons (1450 MPa), so that the cold-press formed target can be thermally sintered to form a 2-inch large-size target, the density of the target is not less than 95%, and the components of the target are uniformly distributed.
Embodiments in accordance with the present invention, as described above, are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention and various modifications as are suited to the particular use contemplated. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (20)
1. The method for manufacturing the YBCO target is characterized by comprising the following steps of:
preparing target material powder by adopting a solid phase reaction method;
placing the target powder in a target mould and then performing thermal sintering to obtain a target;
wherein the density of the target material is more than 95%.
2. The manufacturing method according to claim 1, wherein the step of preparing the target powder by a solid phase reaction method comprises:
preparing a plurality of raw materials with high purity according to a chemical dosage ratio;
grinding and mixing a plurality of raw materials;
presintering various raw material powders in an atmosphere;
repeating the steps of grinding, mixing and presintering a plurality of times;
grinding the raw material after the last presintering to obtain target powder.
3. The manufacturing method according to claim 1, wherein the method of thermally sintering the target powder in the mold to obtain the target includes: a hot-press sintering method and a cold-press method assisted by discharge plasma.
4. The manufacturing method according to claim 3, wherein the step of obtaining the target material by using a spark plasma assisted hot press sintering method comprises:
placing target material powder in a mould, prepressing, and placing the mould in discharge plasma sintering equipment;
inserting a thermocouple into the die, and vacuumizing the sintering environment in the sintering equipment to a preset value;
setting a pressure value and a temperature rise process system of sintering equipment;
sintering the target powder in the die to obtain the target.
5. The manufacturing method according to claim 4, wherein the sintering atmosphere in the sintering apparatus is evacuated to 10Pa.
6. The manufacturing method according to claim 4, wherein the pressure value of the sintering apparatus is set to 30 to 70MPa.
7. The manufacturing method according to claim 4, wherein the temperature rise process regime of the sintering equipment is set to be: heating to 900 ℃ at the heating speed of 100-200 ℃/min, and rapidly cooling after heat preservation for 5-10 min.
8. A method of manufacturing according to claim 3, wherein the step of obtaining the target material using cold pressing comprises:
placing target powder in a target mould and prepressing the target powder by a tablet press;
sintering the cold-pressed blank according to preset temperature and time to obtain the target material.
9. The manufacturing method according to claim 8, wherein the target powder is pre-pressed by a tablet press at a pressure of 300 to 1450MPa.
10. The manufacturing method according to claim 8, wherein the sintering temperature is 900 ℃ and the sintering time is 24 hours.
11. The production method according to claim 2, wherein in the step of pre-sintering the plurality of raw material powders under an atmosphere, the sintering temperature is 900 ℃ and the sintering time is 24 hours.
12. The manufacturing method according to claim 2, wherein the steps of grinding, mixing and presintering are repeated a plurality of times, the steps of grinding, mixing and presintering being repeated a plurality of times ranging from 2 to 5 times.
13. The manufacturing method according to claim 11, wherein when the plurality of raw materials of the target material have a volatile raw material, the number of repetition of the steps of grinding mixing and presintering can be reduced.
14. The manufacturing method according to claim 11, wherein when the plurality of raw materials of the target material have a volatile raw material, a sintering time of the pre-sintering step can be reduced.
15. A target die, comprising:
a first base having a first protrusion;
a restriction ring having a first hollow portion at a center thereof for accommodating the first protrusion;
an open annulus having a second hollow portion in the center thereof, which can be placed in the first hollow portion of the restriction ring;
a compression sheet which can be placed in the second hollow part of the valve opening ring;
a second base having a second protrusion, the second hollow portion of the open annulus being adapted to receive the second protrusion,
the valve opening ring consists of a plurality of valve parts, and the second hollow part of the valve opening ring is used for placing target powder.
16. The target mold of claim 15, wherein the split ring comprises 3-5 petals.
17. The target mold of claim 15, wherein the preforms comprise a first preform and a second preform, the first preform being placed into the second hollow portion of the open annulus, followed by placing target powder into the second hollow portion of the open annulus, and then placing the second preform over the target powder in the second hollow portion of the open annulus.
18. The target mold of claim 15, wherein the first protrusion of the first base, the split ring, the preform, and the second protrusion of the second base are of Cr12 steel.
19. The target mold of claim 15, wherein the confinement ring is of 304 steel, and the first base and the second base further comprise a housing of 304 steel.
20. The target mold of claim 15, wherein the maximum pressure that the target mold can withstand is 1450Mpa.
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| CN202211700069.6A CN116023127A (en) | 2022-12-28 | 2022-12-28 | YBCO target manufacturing method and target mold |
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