CN111441021A - Preparation method of rotary target and spraying equipment thereof - Google Patents
Preparation method of rotary target and spraying equipment thereof Download PDFInfo
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- CN111441021A CN111441021A CN202010451974.7A CN202010451974A CN111441021A CN 111441021 A CN111441021 A CN 111441021A CN 202010451974 A CN202010451974 A CN 202010451974A CN 111441021 A CN111441021 A CN 111441021A
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- 238000005507 spraying Methods 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000155 melt Substances 0.000 claims abstract description 88
- 238000003723 Smelting Methods 0.000 claims abstract description 87
- 238000010438 heat treatment Methods 0.000 claims abstract description 57
- 239000011248 coating agent Substances 0.000 claims abstract description 55
- 238000000576 coating method Methods 0.000 claims abstract description 55
- 229910052738 indium Inorganic materials 0.000 claims abstract description 38
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000002347 injection Methods 0.000 claims abstract description 13
- 239000007924 injection Substances 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 37
- 239000000758 substrate Substances 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 27
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- 230000001105 regulatory effect Effects 0.000 claims description 20
- 239000013077 target material Substances 0.000 claims description 17
- 230000001681 protective effect Effects 0.000 claims description 10
- 238000005275 alloying Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 17
- 229910052718 tin Inorganic materials 0.000 abstract description 11
- 238000004544 sputter deposition Methods 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 47
- 239000011159 matrix material Substances 0.000 description 16
- 239000011261 inert gas Substances 0.000 description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000004321 preservation Methods 0.000 description 7
- 238000011049 filling Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 208000032325 CEBPE-associated autoinflammation-immunodeficiency-neutrophil dysfunction syndrome Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 238000010309 melting process Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/123—Spraying molten metal
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The invention relates to the technical field of sputtering coating, in particular to a preparation method of a rotary target and spraying equipment thereof, which comprises a smelting furnace; the heating device is used for heating the smelting furnace; the spraying device comprises a nozzle and a melt conveying pipeline; wherein, the nozzle includes the fuse-element pipeline and the gas pipeline of locating the fuse-element pipeline outside of cover, forms gas injection clearance between the lateral wall of fuse-element pipeline and the inside wall of gas pipeline, and the fuse-element pipeline passes through fuse-element conveying pipeline and smelting furnace intercommunication. The smelting spraying equipment provided by the invention has the characteristics of simple structure and low manufacturing cost; by coating the indium coating on the surface of the base material, the spray coating is uniformly and reliably adhered to the surface of the base material by utilizing the stronger adhesive force between indium and Sn, In, InSn and other particles, and the uniformity of the target sputtering formed film layer is improved.
Description
Technical Field
The invention relates to the technical field of sputtering coating, and particularly provides a preparation method of a rotary target and spraying equipment thereof.
Background
Low melting point materials such as: tin, indium tin alloy and the like are important raw materials of glass coating and copper indium gallium selenide solar cells. The low-melting-point alloy material is mainly used in the sputtering coating industry in the form of a target material, the target material mainly comprises a planar target and a cylindrical (rotating target) target according to different sputtering coating equipment, and the utilization rate of the raw materials of the cylindrical (rotating target) target is up to 70-80% relative to the planar target, so that the rotating target is often used as the raw material for large-scale coating equipment.
In the prior art, molten metal is usually directly cast on a substrate, and then the molten metal is controlled to be condensed to obtain a metal rotating target, in order to obtain a good condensation effect, vertical casting is usually adopted, a large-size rotating target casting platform and a large-size rotating target casting mold need 4-5 m in height, the operation risk degree is high, and the investment of equipment is also large.
Disclosure of Invention
The invention aims to provide a preparation method of a rotary target and spraying equipment thereof, which are beneficial to simplifying the equipment structure and ensuring that the process is relatively safe, and meanwhile, the prepared target is beneficial to improving the uniformity of a sputtering formed film layer.
In order to achieve the above object, the present invention provides a method for preparing a rotary target, comprising the steps of:
s1: uniformly coating metal indium on the surface of a base material to form an indium coating;
s2: smelting low-melting-point metal in an inert protective atmosphere environment to obtain a metal melt;
s3: and (4) uniformly spraying the metal melt obtained in the step S2 on the surface of the substrate obtained in the step S1 in an inert protective atmosphere environment to obtain the target material.
Optionally, the target material obtained in step S3 is subjected to a surface alloying heat treatment.
Optionally, in step S3, the substrate reciprocates at a speed of 20 to 70mm/min relative to a nozzle of a spraying device during the spraying process, and the substrate rotates at a speed of 60 to 150 r/min.
Based on the object of the invention, there is also provided a spraying apparatus of a rotary target, comprising:
a smelting furnace;
a heating device for heating the smelting furnace;
the spraying device comprises a nozzle and a melt conveying pipeline;
the nozzle comprises a melt pipeline and a gas pipeline sleeved outside the melt pipeline, a gas injection gap is formed between the outer side wall of the melt pipeline and the inner side wall of the gas pipeline, and the melt pipeline is communicated with the smelting furnace through the melt conveying pipeline.
Optionally, the smelting furnace is fitted with a switch assembly for replacing the furnace gases.
Optionally, the switch assembly comprises a vacuum valve and an air inlet valve.
Optionally, the heating device includes a heating box and a heating unit, the melting furnace is disposed in the heating box, and the heating unit is disposed in the heating box and used for heating the melting furnace.
Optionally, the melt conveying pipeline is provided with a melt regulating valve for regulating the melt flow.
Optionally, the gas pipeline is connected with a gas conveying pipeline, and a gas regulating valve is arranged on the gas conveying pipeline.
Optionally, the width of the air injection gap is 0.5-1 mm, and the pipe diameter of the opening end of the melt pipeline is 1-3 mm.
The embodiment of the invention has the following technical effects:
according to the smelting and spraying equipment provided by the invention, the smelting furnace is arranged to smelt metal, the heating device is used for continuously and stably heating the smelting furnace in the metal smelting process, and in addition, the smelted metal melt is sprayed out through the nozzle to realize the spraying of the melt, so that the smelting and spraying equipment has the characteristics of simple structure and low manufacturing cost; in the process that the melt is sprayed out through the melt pipeline, high-speed high-pressure gas is introduced into the gas pipeline, the high-speed high-pressure gas is sprayed out from the gas spraying gap, meanwhile, liquid flow of the melt is instantaneously crushed into micron-sized particles, the melt particles sprayed out from the melt pipeline are pushed to strike the surface of the substrate, and after the melt particles touch the back pipe, plastic deformation is generated to adhere to the substrate to form a compact coating, so that the spraying processing of the substrate is realized.
In addition, the indium coating is coated on the surface of the base material, and the spraying layer is uniformly and reliably adhered to the surface of the base material by utilizing the stronger adhesive force between the indium and the particles of Sn, In, InSn and the like, so that the uniformity of the target sputtering formed film layer is improved.
Drawings
FIG. 1 is a schematic structural diagram of a preferred embodiment of the present invention;
FIG. 2 is a schematic view of the structure of a nozzle in a preferred embodiment of the present invention;
fig. 3 is a schematic diagram of the steps in a preferred embodiment of the invention.
Description of reference numerals:
1. the device comprises a smelting furnace 11, a first pressure gauge 12, a pressure relief valve 13, an air inlet valve 14, a vacuum valve 15, an exhaust valve 16, a heat preservation base 17 and a detection unit;
2. a heating device 21, a heating box body 22 and a heating unit;
3. the spraying device comprises a spraying device 31, a nozzle 311, a melt pipeline 312, a gas pipeline 313, a gas spraying gap 32, a melt conveying pipeline 33, a melt regulating valve 34, a gas conveying pipeline 35, a gas regulating valve 36 and a second pressure gauge.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description herein, reference to the description of the terms "one embodiment/mode," "some embodiments/modes," "example," "specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/mode or example is included in at least one embodiment/mode or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to be the same embodiment/mode or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/aspects or examples and features of the various embodiments/aspects or examples described in this specification can be combined and combined by one skilled in the art without conflicting therewith.
In addition, the terms "first", "second", and the like are employed in the present invention to describe various information, but the information should not be limited to these terms, which are used only to distinguish the same type of information from each other. For example, "first" information may also be referred to as "second" information, and similarly, "second" information may also be referred to as "first" information, without departing from the scope of the present invention.
Example 1:
one embodiment of the present invention provides a rotary target spray coating device including:
a smelting furnace 1;
a heating device 2 for heating the melting furnace 1;
the spraying device 3 comprises a nozzle 31 and a melt conveying pipeline 32;
the nozzle 31 comprises a melt pipeline 311 and a gas pipeline 312 sleeved outside the melt pipeline 311, a gas injection gap 313 is formed between the outer side wall of the melt pipeline 311 and the inner side wall of the gas pipeline 312, and the melt pipeline 311 is communicated with the smelting furnace 1 through a melt conveying pipeline 32.
According to the smelting and spraying equipment provided by the invention, metal is smelted by the smelting furnace 1, the smelting furnace 1 is continuously and stably heated by the heating device 2 in the metal smelting process, and in addition, the smelted metal melt is sprayed out through the nozzle 31, so that the melt is sprayed, and the smelting and spraying equipment has the characteristics of simple structure and low manufacturing cost; when the melt is sprayed out through the melt pipeline 311, the gas pipeline 312 is filled with high-speed high-pressure gas, the high-speed high-pressure gas is sprayed out from the gas spraying gap 313, liquid flow of the melt is instantly crushed into micron-sized particles, the melt particles sprayed out from the melt pipeline 311 are pushed to strike the surface of the substrate, and after the melt particles touch the back pipe, plastic deformation is generated to adhere to the substrate to form a compact coating, so that the spraying processing of the substrate is realized.
Specifically, the smelting furnace 1 in this embodiment is made of alloy steel, and may be made of stainless steel such as 304, 304L, 316, etc., and the smelting furnace 1 needs to satisfy an operating pressure of 0.7 to 1.0MPa, and a start pressure of the pressure relief valve 12 on the smelting furnace 1 is 0.6 to 0.9 MPa.
Further, in order to avoid the reaction between the metal and the oxygen in the air during the melting process, the furnace space of the melting furnace 1 in this embodiment is closed, so that the inert gas is conveniently charged into the furnace to replace the air in the furnace, wherein the melting furnace 1 in this embodiment is provided with a switch assembly for replacing the gas in the furnace.
Specifically, the switch assembly in this embodiment includes a vacuum valve 14 and an air inlet valve 13, and the vacuum pumping device is arranged to connect the vacuum valve 14 to perform vacuum pumping in the melting furnace 1, so as to pump out air in the melting furnace 1, and the air inlet valve 13 is filled with inert gas, so as to form an inert gas environment in the melting furnace 1 to prevent oxidation of the metal melt.
Also comprises an exhaust valve 1 for exhausting gas in the furnace after production is finished.
Further, in order to guarantee the safety of the use of the smelting furnace 1, the switch assembly of the embodiment further comprises a pressure release valve 12 and a first pressure gauge 11, so that the pressure in the smelting furnace is conveniently adjusted and monitored.
The heating device 2 in this embodiment includes a heating box 21 and a heating unit 22, the smelting furnace 1 is disposed in the heating box 21, and the heating unit 22 is disposed in the heating box 21 and used for heating the smelting furnace 1, specifically, the heating unit 22 is a plurality of heating pipes, and the plurality of heating pipes are uniformly arranged on the inner side wall of the heating box 21, so as to uniformly heat the smelting furnace 1; wherein, the heating box body 21 is made of high-purity graphite.
In order to reduce the energy consumption and stabilize the temperature in the heating box, the bottom of the heating box body 21 is provided with a heat preservation base 16 to reduce the heat transfer, and the heat preservation base 16 is made of aluminum silicate heat preservation cotton and has the thickness of 30 mm.
The embodiment also comprises a detection unit 17 for detecting the temperature of the smelting furnace 1, which is convenient for monitoring the temperature in the smelting furnace 1 and adjusting the temperature at any time, specifically, the detection unit 17 in the embodiment is a K-type thermocouple, and the type of the thermocouple is OMEGA NB 3-CAIN-18E-12.
Further, the melt conveying pipeline 32 of the embodiment is provided with a melt adjusting valve 33 for adjusting the melt flow, so that the flow and the pressure of the output melt can be conveniently adjusted, in addition, the melt conveying pipeline 32 adopts a BA-grade 304L or 316L pipeline, the melt conveying pipeline 32 is connected with the smelting furnace 1 by adopting a stainless steel bayonet joint or a VCR joint, and the CV value of the flow coefficient of the melt adjusting valve 33 for controlling the melt conveying is 0.09-0.37.
In order to further ensure that the temperature of the melt is kept stable during the output process, the melt conveying pipeline 32 comprises a conveying pipe and a pipeline heating unit 22 for heating the conveying pipe, so that the melt is kept warm or heated by the pipeline heating unit 22 during the output process, and the temperature of the melt when being sprayed out from the nozzle 31 is controlled, and specifically, the pipeline heating unit 22 is a heating sheet coated on the surface of the conveying pipe.
In this embodiment, the gas pipeline 312 is connected with the gas transmission pipeline 34, the gas transmission pipeline 34 is provided with a gas regulating valve 35 and a second pressure gauge 36, the pressure of the output gas on the gas transmission pipeline 34 is monitored through the second pressure gauge 36, and the gas is regulated through the gas regulating valve 35, so that the use is more convenient.
Specifically, the width of the gas injection gap 313 in this embodiment is 0.5-1 mm, and the pipe diameter of the opening end of the melt pipe 311 is 1-3 mm, so that the gas injected from the gas injection gap 313 forms a stable annular air flow channel, and the melt injected from the melt pipe 311 in the flow channel is pushed to impact the substrate.
Based on the smelting spraying equipment, the invention provides a preparation method of a rotating target in one embodiment, which comprises the following steps:
s1: the indium coating is formed by uniformly coating metal indium on the surface of the base material, in order to ensure a strong bonding effect between the indium coating and the spray coating, the thickness of the indium coating is 0.05-0.4 mm, the thickness of the indium coating is too thin, the bonding effect between the spray coating and the indium coating is poor, the indium coating is too thick, the cost is increased, and the uniformity is difficult to ensure, so that the thickness of the indium coating in the embodiment is 0.2 mm;
s2: weighing 20Kg of 4N metallic indium (melting point 156.61 ℃) and putting into a smelting furnace 1, in order to avoid the oxidation of materials in the smelting furnace 1 in the smelting process, melting low-melting-point metals under an inert protective atmosphere environment to obtain a metal melt, specifically, in the embodiment, the operation of vacuumizing and inflating is repeated;
wherein, the vacuum-inflation process comprises:
opening a vacuum valve 14, closing an air inlet valve 13 and an exhaust valve 1, vacuumizing until the pressure in the smelting furnace is less than 1pa, closing the vacuum valve 14, opening the air inlet valve 13, filling inert gas until the pressure in the smelting furnace 1 is recovered to normal pressure, repeating the operation for 3 times to completely replace the air in the smelting furnace 1, and then filling the inert gas into the smelting furnace 1 to ensure that the pressure in the smelting furnace reaches 0.3 Mpa;
the final temperature of the smelting furnace 1 is set to be 200 ℃, then the smelting furnace 1 enters a heat preservation stage, the pipeline heating unit 22 is opened while the smelting furnace 1 is heated, and the final temperature is set to be 180 ℃ and 23.39 ℃ higher than the melting point of metal.
S3: uniformly spraying the metal melt obtained in the step S2 on the surface of the substrate obtained in the step S1 in an inert protective atmosphere environment to obtain a target material;
in the spraying process, the melt is sprayed out through the melt pipeline 311, the gas pipeline 312 is filled with high-speed high-pressure gas, the high-speed high-pressure gas is sprayed out from the gas spraying gap 313, and meanwhile, the liquid flow of the melt is instantly crushed into micron-sized particles, so that the obtained target material has uniform grain size, the uniformity of a film layer formed by sputtering the target material is improved, the melt particles sprayed out from the melt pipeline 311 are pushed to strike the surface of a substrate, and after the melt particles touch a back pipe, the melt particles are plastically deformed and adhered to the substrate to form a compact coating, so that the spraying processing of the substrate is realized, preferably, the relative position of the nozzle 31 and the substrate meets:
A. the direction of the nozzle 31 is vertical and is opposite to the central line of the matrix, and the tolerance of the levelness of the nozzle 31 is controlled within +/-5 degrees, so that the melt sprayed out from the nozzle 31 is hit on the matrix as much as possible, a higher deposition rate in the spraying process is ensured, the loss of materials is reduced, and further, the tolerance of the levelness of the nozzle 31 in the embodiment is controlled within 2 degrees;
B. on one hand, in order to prevent the loss of kinetic energy after the melt is sprayed out from the nozzle 31 and cause poor compactness of a formed spray coating, on the other hand, in order to avoid the excessive kinetic energy after the melt is sprayed out from the nozzle 31 and cause the low material deposition rate of the melt particles after colliding with the matrix, the distance d between the nozzle 31 and the outer side of the matrix is controlled to be 3-10 cm, and further, the distance d between the nozzle 31 and the outer side of the matrix in the embodiment is controlled to be 4-8 cm;
C. the spraying is started by aligning the nozzle 31 with the starting point of the indium coating spraying of the substrate
D. In the spraying process, the moving speed of the matrix relative to the nozzle 31 is 30mm/min, and the matrix rotates at the same time, the rotation speed is 70r/min, so that the melt sprayed out from the nozzle 31 is uniformly adhered to the surface of the matrix;
E. the air injection pressure of the air injection gap 313 is controlled to be 0.5Mpa, and the melt regulating valve 33 on the melt conveying pipeline 32 is opened to the valve opening degree of 20 degrees;
F. in the spraying process, because the liquid level in the smelting furnace is continuously reduced, the static pressure of the melt at the nozzle is always reduced, inert gas needs to be continuously supplemented into the smelting furnace 1, and the pressure in the smelting furnace 1 is controlled to be 0.35 Mpa;
when the sprayed coating reaches a preset thickness, the melt regulating valve 33 and the gas regulating valve 35 are sequentially closed.
The rotary target obtained in the embodiment comprises a substrate, and an indium coating which are sequentially covered on the substrate, wherein the relative density of the rotary target is 98.5%, and the oxygen content is 240 pm.
Example 2:
based on the smelting spraying equipment provided in the embodiment 1, the invention provides a preparation method of a rotary target for spraying production of low-melting-point materials, which comprises the following steps:
s1: the indium tin coating is formed by uniformly coating metal indium on the surface of a base material, in order to ensure a strong bonding effect between the indium tin coating and a spray coating, the thickness of the indium tin coating is 0.05-0.4 mm, the thickness of the indium coating is too thin, the bonding effect between the spray coating and the indium coating is poor, the indium coating is too thick, the cost is increased, and the uniformity is difficult to ensure, so that the thickness of the indium coating in the embodiment is 0.3 mm;
s2: weighing 15Kg4N In30Sn70 (30 atomic percent In: 70% Sn, melting point 173 ℃) and putting into a smelting furnace 1, In order to avoid the oxidation of materials In the smelting furnace 1 In the smelting process, melting low-melting-point metal In an inert protective atmosphere environment to obtain a metal melt, specifically, In the embodiment, the operation of vacuumizing and inflating is repeated;
wherein, the vacuum-inflation process comprises:
opening a vacuum valve 14, closing an air inlet valve 13 and an exhaust valve 1, vacuumizing until the pressure in the smelting furnace is less than 1pa, closing the vacuum valve 14, opening the air inlet valve 13, filling inert gas until the pressure in the smelting furnace 1 is recovered to normal pressure, repeating the operation for 3 times to completely replace the air in the smelting furnace 1, and then filling the inert gas into the smelting furnace 1 to ensure that the pressure in the smelting furnace reaches 0.35 Mpa;
the final temperature of the smelting furnace 1 is set to 223 ℃, then the smelting furnace 1 enters a heat preservation stage, and the pipeline heating unit 22 is opened while the smelting furnace 1 is heated, and the final temperature is set to 200 ℃ and is 27 ℃ higher than the melting point of metal.
S3: uniformly spraying the metal melt obtained in the step S2 on the surface of the substrate obtained in the step S1 in an inert protective atmosphere environment to obtain a target material;
during the spraying process, the relative position of the nozzle 31 and the substrate preferably satisfies the following condition:
A. the direction of the nozzle 31 is vertical and is opposite to the central line of the matrix, and the tolerance of the levelness of the nozzle 31 is controlled within 3 degrees;
B. the distance d between the nozzle 31 and the outer side of the matrix is controlled to be 6-10 cm;
C. spraying is started by aligning the nozzle 31 with the starting point of the indium coating spraying of the substrate;
D. in the spraying process, the moving speed of the matrix relative to the nozzle 31 is 25mm/min, and the matrix rotates at the same time, wherein the rotating speed is 100 r/min;
E. the air injection pressure of the air injection gap 313 is controlled to be 0.65Mpa, and the melt regulating valve 33 on the melt conveying pipeline 32 is opened to the valve opening degree of 30 degrees;
F. in the spraying process, because the liquid level in the smelting furnace is continuously reduced, the static pressure of the melt at the nozzle is always reduced, inert gas needs to be continuously supplemented into the smelting furnace 1, and the pressure in the smelting furnace 1 is controlled to be 0.45 Mpa;
when the sprayed coating reaches a preset thickness, the melt regulating valve 33 and the gas regulating valve 35 are sequentially closed.
S4: and (4) carrying out surface alloying heat treatment on the target material obtained in the step (S3), taking down the sprayed indium tin target material, and placing the indium tin target material in an annealing furnace, wherein the optimal alloying temperature is preferably 170 ℃, and the annealing time is 5 hours.
The rotary target obtained in this example includes a substrate, and an indium coating layer and an indium tin alloy layer sequentially covering the substrate, and the relative density of the rotary target is 97.2%, and the oxygen content is 238 pm.
Example 3:
based on the smelting spraying equipment provided in the embodiment 1, the invention provides a preparation method of a rotary target for spraying production of low-melting-point materials, which comprises the following steps:
s1: the method comprises the following steps of uniformly coating indium metal on the surface of a base material to form a tin coating, wherein in order to ensure a strong bonding effect between the tin coating and a spray coating, the thickness of the tin coating is 0.05-0.4 mm, the thickness of the indium coating is too thin, the bonding effect between the spray coating and the indium coating is poor, the indium coating is too thick, the cost is increased, and the uniformity is difficult to ensure, so that the thickness of the indium coating in the embodiment is 0.2 mm;
s2: weighing 20kg of 4N metallic tin (melting point 231.89 ℃) and putting into a smelting furnace 1, wherein in order to avoid the oxidation of materials in the smelting furnace 1 in the smelting process, low-melting-point metal needs to be smelted in an inert protective atmosphere environment to obtain a metal melt, specifically, in the embodiment, the operation of vacuumizing and inflating is repeated;
wherein, the vacuum-inflation process comprises:
opening a vacuum valve 14, closing an air inlet valve 13 and an exhaust valve 1, vacuumizing until the pressure in the smelting furnace is less than 1pa, closing the vacuum valve 14, opening the air inlet valve 13, filling inert gas until the pressure in the smelting furnace 1 is recovered to normal pressure, repeating the operation for 3 times to completely replace the air in the smelting furnace 1, and then filling the inert gas into the smelting furnace 1 to ensure that the pressure in the smelting furnace reaches 0.4 Mpa;
the final temperature of the smelting furnace 1 is set to 280 ℃, then the smelting furnace 1 enters a heat preservation stage, and the pipeline heating unit 22 is opened while the smelting furnace 1 is heated, and the final temperature is set to 262 ℃ which is 30.11 ℃ higher than the melting point of metal.
S3: uniformly spraying the metal melt obtained in the step S2 on the surface of the substrate obtained in the step S1 in an inert protective atmosphere environment to obtain a target material;
during the spraying process, the relative position of the nozzle 31 and the substrate preferably satisfies the following condition:
A. the direction of the nozzle 31 is vertical and is opposite to the central line of the matrix, and the tolerance of the levelness of the nozzle 31 is controlled within 3 degrees;
B. the distance d between the nozzle 31 and the outer side of the matrix is controlled to be 5 cm-10 cm;
C. the spraying is started by aligning the nozzle 31 with the starting point of the indium coating spraying of the substrate
D. In the spraying process, the moving speed of the matrix relative to the nozzle 31 is 30mm/min, and the matrix rotates at the same time, wherein the rotating speed is 80 r/min;
E. the air injection pressure of the air injection gap 313 is controlled to be 0.65Mpa, and the melt regulating valve 33 on the melt conveying pipeline 32 is opened to the opening degree of the valve of 45 degrees;
F. in the spraying process, because the liquid level in the smelting furnace is continuously reduced, the static pressure of the melt at the nozzle is always reduced, inert gas needs to be continuously supplemented into the smelting furnace 1, and the pressure in the smelting furnace 1 is controlled to be 0.5 Mpa;
when the sprayed coating reaches a preset thickness, the melt regulating valve 33 and the gas regulating valve 35 are sequentially closed.
S4: and (4) carrying out surface alloying heat treatment on the target material obtained in the step S3, preferably, taking down the sprayed tin target material, putting the tin target material into an annealing furnace, heating to 180 ℃, preserving heat for 3 hours, cooling to room temperature, and taking out.
The rotating target obtained in this example comprises a substrate, and an indium coating and a tin layer sequentially covering the substrate, and the rotating target has a relative density of 96.5% and an oxygen content of 185 ppm.
In conclusion, the smelting and spraying equipment provided by the invention has the advantages that metal is smelted by the smelting furnace 1, the smelting furnace 1 is continuously and stably heated by the heating device 2 in the metal smelting process, and in addition, the smelted metal melt is sprayed out through the nozzle 31, so that the melt spraying is realized, and the smelting and spraying equipment has the characteristics of simple structure and low manufacturing cost; when the melt is sprayed out through the melt pipeline 311, the gas pipeline 312 is filled with high-speed high-pressure gas, the high-speed high-pressure gas is sprayed out from the gas spraying gap 313, liquid flow of the melt is instantaneously crushed into micron-sized particles, the melt particles sprayed out from the melt pipeline 311 are pushed to strike the surface of the substrate, and after the melt particles touch the substrate, plastic deformation is generated to adhere to the substrate to form a compact coating, so that the spraying processing of the substrate is realized.
In addition, the invention ensures that the spray coating is reliably adhered to the surface of the base material by utilizing the stronger adhesive force between indium and Sn, In, InSn and other particles by coating the indium coating on the surface of the base material, and carries out surface alloying heat treatment on the spray coating formed after spraying, thereby enhancing the adhesive force between the coating layer and the spray coating.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for preparing a rotary target, comprising the steps of:
s1: uniformly coating metal indium on the surface of a base material to form an indium coating;
s2: smelting low-melting-point metal in an inert protective atmosphere environment to obtain a metal melt;
s3: and (4) uniformly spraying the metal melt obtained in the step S2 on the surface of the substrate obtained in the step S1 in an inert protective atmosphere environment to obtain the target material.
2. The method of manufacturing a rotary target according to claim 1, wherein in S1, the target material obtained in step S3 is subjected to surface alloying heat treatment.
3. The method for producing a rotary target according to claim 1, wherein in step S3, the base material is reciprocated at a speed of 20 to 70mm/min relative to a nozzle of a spray equipment during the spray coating, and the base material is rotated at a speed of 60 to 150 r/min.
4. A rotary target spray coating device, comprising:
a smelting furnace;
a heating device for heating the smelting furnace;
the spraying device comprises a nozzle and a melt conveying pipeline;
the nozzle comprises a melt pipeline and a gas pipeline sleeved outside the melt pipeline, a gas injection gap is formed between the outer side wall of the melt pipeline and the inner side wall of the gas pipeline, and the melt pipeline is communicated with the smelting furnace through the melt conveying pipeline.
5. The rotary target spraying apparatus of claim 4, wherein the melting furnace is equipped with a switch assembly for replacing the furnace gas.
6. The rotary target coating apparatus of claim 5 wherein the switch assembly comprises a vacuum valve and an air inlet valve.
7. The rotary target spraying apparatus according to claim 4, wherein the heating device comprises a heating box and a heating unit, the melting furnace is disposed in the heating box, and the heating unit is disposed in the heating box for heating the melting furnace.
8. The rotary target coating apparatus of claim 4 wherein the melt delivery conduit is provided with a melt regulating valve for regulating melt flow.
9. The rotary target coating apparatus according to claim 4, wherein a gas delivery pipe is connected to the gas pipe, and a gas regulating valve is provided on the gas delivery pipe.
10. The rotary target coating apparatus of claim 4 wherein the gas jet gap has a width of 0.5-1 mm and the melt conduit has an open end pipe diameter of 1-3 mm.
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