CN115747734A - Die filling method and preparation method of large-size and high-density nickel-chromium target - Google Patents
Die filling method and preparation method of large-size and high-density nickel-chromium target Download PDFInfo
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- CN115747734A CN115747734A CN202211611665.7A CN202211611665A CN115747734A CN 115747734 A CN115747734 A CN 115747734A CN 202211611665 A CN202211611665 A CN 202211611665A CN 115747734 A CN115747734 A CN 115747734A
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- 238000011049 filling Methods 0.000 title claims abstract description 63
- 229910018487 Ni—Cr Inorganic materials 0.000 title claims abstract description 35
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000007872 degassing Methods 0.000 claims abstract description 68
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000013077 target material Substances 0.000 claims abstract description 21
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 18
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 90
- 239000010439 graphite Substances 0.000 claims description 90
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 89
- 239000000843 powder Substances 0.000 claims description 57
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims description 39
- 239000011265 semifinished product Substances 0.000 claims description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910001120 nichrome Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 238000005477 sputtering target Methods 0.000 abstract description 2
- 238000003466 welding Methods 0.000 description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- 229910052786 argon Inorganic materials 0.000 description 9
- 239000010408 film Substances 0.000 description 7
- 238000005192 partition Methods 0.000 description 7
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- 238000003723 Smelting Methods 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
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Abstract
The invention belongs to the field of sputtering targets of electronic devices, and discloses a die filling method and a preparation method of a large-size and high-density nickel-chromium target. The method comprises the following steps: preparing a sheath with a rectangular structure; then, filling the mold; placing the sheath after the mold filling into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, stopping heating and degassing when the vacuum degree in the sheath meets the requirement, and sealing the degassing pipe; placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization, heating sintering, cooling and pressure recovery; and discharging the nickel-chromium target material from the furnace, and removing the sheath to obtain the nickel-chromium target material. The nickel-chromium target material manufactured by the die filling mode is a single-piece product and can also be divided into two parts in the length/width direction, a sheath can process 2~6 products, and after the sheath is removed, a target blank machine is simple. The invention adopts a hot isostatic pressing method for sintering, can prepare a large-size and high-density target material, the size can be 350-550mm, and the density is more than or equal to 99%.
Description
Technical Field
The invention belongs to the field of sputtering targets of electronic devices, relates to a die filling method and a preparation method of a nickel-chromium target, and more particularly relates to a die filling method and a preparation method of a large-size and high-density nickel-chromium target.
Background
With the continuous development of science and technology, electronic devices are further required to have small size, good stability and small resistance temperature coefficient, and a nichrome film has the characteristics of high resistivity, low resistance temperature coefficient, higher sensitivity coefficient, small dependence on temperature and the like, and is mainly applied to the preparation of thin film resistance strain gauges in thin film resistors and thin film capacitors; in addition, the nickel-chromium alloy resistance film is easy to prepare, mature in process and stable in performance, so that the nickel-chromium alloy resistance film is widely applied to the preparation of precise resistance films in hybrid integrated circuits and can meet the performance requirements of sensitive films of resistance strain gauges; in addition, in the coating industry, ni-Cr series binary alloy target materials and films are widely applied to surface strengthening films with wear resistance, wear reduction, heat resistance, corrosion resistance and the like, and high-end technology industries such as low-emissivity glass, microelectronics, magnetic recording, semiconductors, thin film resistors and the like.
The existing preparation methods of the nickel-chromium target material comprise a smelting method and a powder metallurgy method. The smelting method is easy to cause the phenomenon of uneven micro-distribution of finished product components. Chinese patent CN102732845B discloses a high-purity, high-composition uniformity nichrome target and a preparation method thereof, which is based on the results of material science and process calculation simulation to precisely control the technological parameters of melting, solidification, thermal mechanical processing and annealing heat treatment of a nichrome series alloy target, but the technical scheme has complicated processes and is not suitable for batch production in factories; powder metallurgy methods include cold pressing, vacuum hot pressing, hot isostatic pressing and the like, and the hot pressing method has certain difficulty in sintering large-size and high-density target materials due to equipment limitation.
Disclosure of Invention
In view of the above problems in the prior art, the present invention is directed to a method for die-filling a nickel-chromium target.
Therefore, the invention provides a die filling method of a nickel-chromium target, which is used for preparing the nickel-chromium target with large size and high density by sintering through a hot isostatic pressing method, is simple in machining and processing, and is suitable for batch production of the target
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a die filling method and a preparation method of a large-size and high-density nickel-chromium target material comprise the following steps:
(1) Preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a supporting plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, the cover plate is provided with a through hole, the degassing pipe is arranged at the through hole, and the supporting plate and the graphite paper are arranged in a rectangular accommodating space formed by the bottom plate, the outer side plate and the cover plate;
(2) Assembling the bottom plate and the outer side plate to form a sheath semi-finished product with an opening at one end, laying graphite paper on the side wall of the sheath semi-finished product, laying graphite paper, a support plate and graphite paper at the bottom of the sheath semi-finished product in sequence, weighing nickel-chromium alloy powder, placing the nickel-chromium alloy powder in the sheath, tamping the nickel-chromium alloy powder, and laying the graphite paper, the support plate and the graphite paper on the nickel-chromium alloy powder in sequence; repeatedly setting up the die filling sequence of graphite paper, a support plate, graphite paper, nickel-chromium alloy powder, graphite paper, the support plate and graphite paper until the last layer of nickel-chromium alloy powder is filled;
(3) And ensuring that graphite paper, a supporting plate and graphite paper are sequentially filled on the last layer of nickel-chromium alloy powder, sealing and fixing the opening of the sheathed semi-finished product by using a cover plate, and installing a degassing pipe at the through hole of the cover plate to finish mold filling.
A die filling method of a nickel-chromium target comprises the following steps:
(1) Preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a supporting plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, the outer side plate is provided with a through hole, the degassing pipe is arranged at the through hole, and the supporting plate and the graphite paper are arranged in a rectangular accommodating space formed by the bottom plate, the outer side plate and the cover plate;
(2) Assembling a bottom plate and an outer side plate to form a sheathed semi-finished product with an opening at one end, filling graphite paper, a supporting plate, graphite paper, a supporting plate and graphite paper at the inner wall of the outer side plate with a through hole, filling graphite paper at the inner wall of the outer side plate without the through hole, filling the graphite paper, the supporting plate and the graphite paper at the bottom of the sheathed semi-finished product in sequence, weighing nickel-chromium alloy powder, placing the nickel-chromium alloy powder in a sheath, tamping the nickel-chromium alloy powder, and filling the graphite paper, the supporting plate and the graphite paper on the nickel-chromium alloy powder in sequence; repeatedly setting up the die filling sequence of graphite paper, a support plate, graphite paper, nickel-chromium alloy powder, graphite paper, the support plate and graphite paper until the last layer of nickel-chromium alloy powder is filled;
(3) And ensuring that graphite paper, a supporting plate and graphite paper are sequentially arranged on the last layer of nickel-chromium alloy powder in a cushioning mode, sealing and fixing the opening of the sheathed semi-finished product by using a cover plate, and installing a degassing pipe at the through hole of the outer side plate to finish mold filling.
Preferably, the outer side plate is a rectangular column structure.
Preferably, the installation modes of the bottom plate and the outer side plate, the cover plate and the outer side plate, and the cover plate and the degassing pipe are all welded and fixed.
Preferably, in the step (3), the plane of the topmost graphite paper is flush with the opening of the semi-finished wrapping sleeve.
Preferably, the graphite paper can be replaced with ceramic fiber paper.
Preferably, the thickness of the support plate is 4 to 16mm; the thickness of the graphite paper is 0.3 to 1mm; the outer diameter of the degassing pipe is 12 to 18mm, and the wall thickness of the degassing pipe is 4 to 7mm; the bottom plate, the outer side plate, the supporting plate, the cover plate and the degassing pipe are made of low-carbon steel or stainless steel.
Preferably, the purity of the nickel-chromium alloy powder is required to be more than 99.95 percent, wherein the mass of the nickel accounts for 10 to 90 percent, and the balance is chromium.
The invention also discloses a preparation method of the nickel-chromium target, which uses the die filling method and also comprises the following steps:
(4) Putting the sheath after the mold filling into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, stopping heating and degassing when the vacuum degree in the sheath meets the requirement, and sealing the degassing pipe;
(5) Placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization, heating sintering, cooling and pressure recovery;
(6) And discharging the nickel-chromium target material from the furnace, and removing the sheath to obtain the nickel-chromium target material.
Preferably, in the step (4), the degassing temperature is 450 to 650 ℃; and when the vacuum degree in the sheath is less than 5 × 10-3Pa, stopping heating and degassing, and sealing the degassing pipe.
Preferably, in the step (5), in the heating sintering process, the heating rate is 1~8 ℃/mins, the sintering temperature is 750 to 1000 ℃, the pressure is 110 to 160MPa, and the maintaining time is 3 to 5h; and after the temperature rise sintering is finished, cooling and pressure recovery are carried out until the temperature is less than 200 ℃, and the pressure of the hot isostatic pressing sintering furnace reaches the furnace discharge standard when the pressure is 0 MPa.
Compared with the prior art, the invention has the beneficial effects that:
(1) The nickel-chromium target material manufactured by the die filling mode is a single-piece product and can also be divided into two parts in the length/width direction, a sheath can process 2~6 products, and after the sheath is removed, a target blank machine is simple.
(2) The invention adopts a hot isostatic pressing method for sintering, can prepare a target material with large size and high density, the size (length/width direction) can reach 350 to 550mm, and the density is more than or equal to 99 percent.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a die-filling structure of the present invention;
FIG. 2 is a block diagram of the outer panel of the present invention;
wherein: 1-except the trachea, 2-apron, 3-outside plate, 4-backup pad, 5-graphite paper, 6-bottom plate, 31-first outside plate, 32-second outside plate, 33-third outside plate, 34-fourth outside plate.
Detailed Description
In order to facilitate an understanding of the invention, reference will now be made in detail to the present preferred embodiments of the invention, examples of which are illustrated in the accompanying drawings, and the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
The embodiment discloses a preparation method of a nickel-chromium target, which comprises the following steps:
(1) Referring to fig. 1 and 2, preparing a sheath, preparing a bottom plate 6, a first outer side plate 31, a second outer side plate 32, a third outer side plate 33, a fourth outer side plate 34, a low carbon steel support plate 4 and a cover plate 2 which are 2.3mm thick, wherein the bottom plate 6, the first outer side plate 31, the second outer side plate 32, the third outer side plate 33, the fourth outer side plate 34, the middle partition plate 4 and the cover plate 2 are all made of low carbon steel; preparing a low-carbon steel degassing pipe 1 with graphite paper 5 of 0.38mm thickness, an outer diameter of 14mm and a wall thickness of 4 mm; welding a first outer side plate 31, a second outer side plate 32, a third outer side plate 33 and a fourth outer side plate 34 into a rectangular columnar outer side plate 3 by argon arc welding, and welding a bottom plate 6 at the bottom of the outer side plate 3 by argon arc welding to manufacture a semi-finished sheath for nickel-chromium alloy powder die filling;
(2) Filling a mold, filling graphite paper on the side wall of the sheathed semi-finished product, sequentially filling graphite paper 5, a support plate 4 and graphite paper 5 at the bottom of the sheathed semi-finished product, and weighing 2300g of nickel-chromium alloy powder with the powder purity of 99.95 percent, wherein the mass ratio of nickel is 40wt percent, and the balance is chromium; putting the powder into the sheath for 5 times, tamping and leveling the powder after each time of powder putting, filling graphite paper 5, a middle partition plate 4 and graphite paper 5 on the powder in sequence after 2300g of nickel-chromium alloy powder is completely put into and tamped, wherein the plane of the graphite paper 5 at the topmost layer is basically flush with the opening at the top of the sheath semi-finished product, fixing the cover plate 2 at the top of the sheath semi-finished product by using a C-shaped clamp, welding the cover plate by using argon arc welding, and welding a degassing pipe 1 at the through hole of the cover plate 2;
(3) Degassing, namely putting the sheath after mold filling into a trolley furnace, heating while vacuumizing and degassing the sheath through a degassing pipe 1, wherein the degassing temperature is 600 ℃; when the vacuum degree in the sheath reaches the requirement, stopping heating and degassing, and sealing the degassing pipe 1;
(4) Hot isostatic pressing sintering, namely placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization and temperature rise sintering; the heating rate is 5 ℃/mins, the sintering temperature is 900 ℃, the pressure is 150MPa, and the maintaining time is 4h; after sintering, cooling and recovering pressure, and discharging when the temperature is lower than 200 ℃ and the pressure of a hot isostatic pressing sintering furnace is 0 MPa;
(5) Removing the sheath, cutting the sheath along the edge of the weld joint after the sheath is sintered and discharged from the furnace, taking out the sintered and molded nickel-chromium target material, and subsequently carrying out plane grinding and excircle processing to obtain the finished nickel-chromium target material.
And (3) measuring the density of the nickel-chromium target obtained in the step (5) by adopting an Archimedes method, measuring the size of the blank by adopting a steel plate ruler and a caliper, and detailing detection data in a table 1.
Example 2
The embodiment discloses a preparation method of a nickel-chromium target, which comprises the following steps:
(1) Preparing a sheath, preparing a bottom plate 6, a first outer side plate 31, a second outer side plate 32, a third outer side plate 33, a fourth outer side plate 34 and a low-carbon steel support plate 4 and a cover plate 2 which are 2.3mm thick, wherein the bottom plate 6, the first outer side plate 31, the second outer side plate 32, the third outer side plate 33, the fourth outer side plate 34, the middle partition plate 4 and the cover plate 2 are all made of low-carbon steel; preparing a low-carbon steel degassing pipe 1 with graphite paper 5 of 0.38mm thickness, an outer diameter of 14mm and a wall thickness of 4 mm; welding a first outer side plate 31, a second outer side plate 32, a third outer side plate 33 and a fourth outer side plate 34 into a rectangular columnar outer side plate 3 by argon arc welding, and welding a bottom plate 6 at the bottom of the outer side plate 3 by argon arc welding to manufacture a semi-finished sheath for nickel-chromium alloy powder die filling;
(2) Filling a mold, filling graphite paper on the side wall of the sheathed semi-finished product, sequentially filling graphite paper 5, a support plate 4 and graphite paper 5 at the bottom of the sheathed semi-finished product, and weighing 2300g of nickel-chromium alloy powder with the powder purity of 99.95 percent, wherein the mass ratio of nickel is 40wt percent, and the balance is chromium; putting the powder into a jacket by 5 times, tamping and leveling the powder after each time of putting the powder, and filling graphite paper 5, a middle partition plate 4 and graphite paper 5 on the powder in sequence after 2300g of nickel-chromium alloy powder is completely put into the jacket and tamped. And weighing 2300g of nickel-chromium alloy powder with the purity of 99.95 percent, wherein the mass ratio of nickel is 40wt percent, and the balance of chromium is put into the jacket by 5 times, tamping the powder with a mold filling tool after each time of putting the powder, and filling graphite paper 5, a middle partition plate 4 and graphite paper 5 on the powder in sequence after all 2300g of nickel-chromium alloy powder is put into the jacket and tamped. At the moment, the plane of the topmost graphite paper 5 is basically flush with the opening at the top of the semi-finished wrapping sleeve, finally the cover plate 2 is fixed at the top of the semi-finished wrapping sleeve by a C-shaped clamp, the cover plate is welded by argon arc welding, and the degassing pipe 1 is welded at the through hole of the cover plate 2;
(3) Degassing, namely putting the sheath after mold filling into a trolley furnace, heating while vacuumizing and degassing the sheath through a degassing pipe 1, wherein the degassing temperature is 600 ℃; when the vacuum degree in the sheath reaches the requirement, stopping heating and degassing, and sealing the degassing pipe 1;
(4) Hot isostatic pressing sintering, namely placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization and temperature rise sintering; the heating rate is 5 ℃/mins, the sintering temperature is 900 ℃, the pressure is 150MPa, and the maintaining time is 4h; after sintering, cooling and recovering pressure, and discharging when the temperature is lower than 200 ℃ and the pressure of a hot isostatic pressing sintering furnace is 0 MPa;
(5) Removing the sheath, cutting the sheath along the edge of the weld joint after the sheath is sintered and discharged from the furnace, taking out the sintered and molded nickel-chromium target material, and subsequently carrying out plane grinding and excircle processing to obtain the finished nickel-chromium target material.
And (3) measuring the density of the nickel-chromium target obtained in the step (5) by adopting an Archimedes method, measuring the size of the blank by adopting a steel plate ruler and a caliper, and detailing detection data in a table 1.
Example 3
The embodiment discloses a preparation method of a nickel-chromium target, which comprises the following steps:
(1) Preparing a sheath, preparing a bottom plate 6 with the thickness of 2.5mm, a first outer side plate 31, a second outer side plate 32, a third outer side plate 33, a fourth outer side plate 34, a low-carbon steel support plate 4 with the thickness of 10mm and a cover plate 2, wherein the bottom plate 6, the first outer side plate 31, the second outer side plate 32, the third outer side plate 33, the fourth outer side plate 34, the middle partition plate 4 and the cover plate 2 are all made of low-carbon steel; preparing a low-carbon steel degassing pipe 1 with graphite paper 5 of 0.38mm thickness, an outer diameter of 14mm and a wall thickness of 4 mm; welding a first outer side plate 31, a second outer side plate 32, a third outer side plate 33 and a fourth outer side plate 34 into a rectangular columnar outer side plate 3 by argon arc welding, and welding a bottom plate 6 at the bottom of the outer side plate 3 by argon arc welding to manufacture a semi-finished sheath for nickel-chromium alloy powder die filling;
(2) Filling a mold, sequentially filling a support plate 4, graphite paper 5, a support plate 4 and graphite paper 5 on the inner wall of a first outer side plate 31 of a sheathed semi-finished product, filling the graphite paper 5 on the inner walls of a second outer side plate 32, a third outer side plate 33 and a fourth outer side plate 34 of the sheathed semi-finished product, sequentially filling the graphite paper 5, the support plate 4 and the graphite paper 5 on the bottom of the sheathed semi-finished product, and weighing 2300g of nickel-chromium alloy powder with the purity of 99.95 percent, wherein the mass ratio of nickel is 40wt percent, and the balance is chromium; putting the powder into the jacket for 5 times, tamping and leveling the powder after each time of putting the powder, after 2300g of nickel-chromium alloy powder is completely put into the jacket and tamped, sequentially filling graphite paper 5, a middle partition plate 4 and graphite paper 5 on the powder, wherein the plane of the graphite paper 5 at the topmost layer is basically flush with an opening at the top of the jacket semi-finished product, fixing the cover plate 2 at the top of the jacket semi-finished product by using a C-shaped clamp, welding the cover plate by argon arc welding, and welding a degassing pipe 1 at a through hole of the first outer side plate 31;
(3) Degassing, namely putting the sheath after mold filling into a trolley furnace, heating while vacuumizing and degassing the sheath through a degassing pipe 1, wherein the degassing temperature is 550 ℃; when the vacuum degree in the sheath reaches the requirement, stopping heating and degassing, and sealing the degassing pipe 1;
(4) Hot isostatic pressing sintering, namely placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization and temperature rise sintering; the heating rate is 5 ℃/mins, the sintering temperature is 850 ℃, the pressure is 150MPa, and the maintaining time is 4h; after sintering, cooling and recovering pressure, and discharging when the temperature is lower than 200 ℃ and the pressure of a hot isostatic pressing sintering furnace is 0 MPa;
(5) Removing the sheath, cutting the sheath along the edge of the weld joint after the sheath is sintered and discharged from the furnace, taking out the sintered and molded nickel-chromium target material, and subsequently carrying out plane grinding and excircle processing to obtain the finished nickel-chromium target material.
And (3) measuring the density of the nickel-chromium target obtained in the step (5) by adopting an Archimedes method, measuring the size of the blank by adopting a steel plate ruler and a caliper, and detailing detection data in a table 1.
As can be seen from the data in Table 1, the invention can prepare the target material with large size and high density, the size (length/width direction) can reach 350 to 550mm, and the density is more than or equal to 99 percent.
TABLE 1
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A die filling method for a large-size and high-density nickel-chromium target is characterized by comprising the following steps:
(1) Preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a supporting plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, the cover plate is provided with a through hole, the degassing pipe is arranged at the through hole, and the supporting plate and the graphite paper are arranged in a rectangular accommodating space formed by the bottom plate, the outer side plate and the cover plate;
(2) Assembling a bottom plate and an outer side plate to form a sheathed semi-finished product with an opening at one end, filling graphite paper on the side wall of the sheathed semi-finished product, sequentially filling graphite paper, a supporting plate and graphite paper at the bottom of the sheathed semi-finished product, weighing nickel-chromium alloy powder, placing the nickel-chromium alloy powder in a sheath, tamping the nickel-chromium alloy powder, and sequentially filling the graphite paper, the supporting plate and the graphite paper on the nickel-chromium alloy powder; repeatedly setting up the die filling sequence of graphite paper, a support plate, graphite paper, nickel-chromium alloy powder, graphite paper, the support plate and graphite paper until the last layer of nickel-chromium alloy powder is filled;
(3) And ensuring that graphite paper, a supporting plate and graphite paper are sequentially filled on the last layer of nickel-chromium alloy powder, sealing and fixing the opening of the sheathed semi-finished product by using a cover plate, and installing a degassing pipe at the through hole of the cover plate to finish mold filling.
2. A die filling method for a large-size and high-density nickel-chromium target is characterized by comprising the following steps:
(1) Preparing a sheath, wherein the sheath comprises a bottom plate, an outer side plate, a supporting plate, graphite paper, a cover plate and a degassing pipe, the bottom plate is arranged at the bottom of the outer side plate, the cover plate is arranged at the top of the outer side plate, the outer side plate is provided with a through hole, the degassing pipe is arranged at the through hole, and the supporting plate and the graphite paper are arranged in a rectangular accommodating space formed by the bottom plate, the outer side plate and the cover plate;
(2) Assembling the bottom plate and the outer side plate to form a sheathed semi-finished product with an opening at one end, filling graphite paper, a supporting plate, graphite paper, a supporting plate and graphite paper on the inner wall of the outer side plate with a through hole, filling graphite paper on the inner wall of the outer side plate without the through hole, filling the graphite paper, the supporting plate and the graphite paper at the bottom of the sheathed semi-finished product in sequence, weighing nichrome powder, placing the nichrome powder in the sheath, tamping the nichrome powder, and filling the graphite paper, the supporting plate and the graphite paper on the surface in sequence; repeatedly setting up the die filling sequence of graphite paper, a support plate, graphite paper, nickel-chromium alloy powder, graphite paper, the support plate and graphite paper until the last layer of nickel-chromium alloy powder is filled;
(3) And ensuring that graphite paper, a supporting plate and graphite paper are sequentially arranged on the last layer of nickel-chromium alloy powder in a cushioning mode, sealing and fixing the opening of the sheathed semi-finished product by using a cover plate, and installing a degassing pipe at the through hole of the outer side plate to finish mold filling.
3. A mold filling method according to claim 1 or 2, wherein said outer panel is a rectangular columnar structure; the installation modes of the bottom plate and the outer side plate, the cover plate and the outer side plate, and the cover plate and the degassing pipe are all welded and fixed.
4. A method as claimed in claim 1 or 2, wherein in step (3), the topmost graphite paper is in a plane flush with the opening of the jacket semi-finished product.
5. A method as claimed in claim 1 or claim 2, in which the graphite paper is replaced by ceramic fibre paper.
6. A mould filling method as claimed in claim 1 or 2, wherein the support plate has a thickness of 4 to 16mm; the thickness of the graphite paper is 0.3 to 1mm; the outer diameter of the degassing pipe is 12 to 18mm, and the wall thickness of the degassing pipe is 4 to 7mm; the bottom plate, the outer side plate, the supporting plate, the cover plate and the degassing pipe are made of low-carbon steel or stainless steel.
7. A die filling method as claimed in claim 1 or 2, wherein the purity of the nickel-chromium alloy powder is required to be more than 99.95%, wherein the mass ratio of nickel is 10-90%, and the balance is chromium.
8. A method for preparing a large-size and high-density nickel-chromium target, which is characterized by using the die filling method of any one of claims 1~7, and further comprising the following steps:
(4) Putting the sheath after the mold filling into a furnace, heating while vacuumizing and degassing the sheath through a degassing pipe, stopping heating and degassing when the vacuum degree in the sheath meets the requirement, and sealing the degassing pipe;
(5) Placing the sheath subjected to degassing into a hot isostatic pressing sintering furnace, and performing vacuum pumping, pressurization, heating sintering, cooling and pressure recovery;
(6) And discharging the nickel-chromium target material from the furnace, and removing the sheath to obtain the nickel-chromium target material.
9. The method of claim 8The preparation method is characterized in that in the step (4), the degassing temperature is 450 to 650 ℃; when the vacuum degree in the sheath is less than 5 x 10 -3 And when Pa, stopping heating and degassing, and sealing the degassing pipe.
10. The preparation method according to claim 8, wherein in the step (5), the temperature rise rate is 1~8 ℃/mins, the sintering temperature is 750-1000 ℃, the pressure is 110-160MPa, and the holding time is 3-5h; and after the temperature rise sintering is finished, cooling and pressure recovery are carried out until the temperature is less than 200 ℃, and the pressure of the hot isostatic pressing sintering furnace is 0MPa, so that the furnace discharge standard is reached.
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| CN103785838A (en) * | 2012-11-01 | 2014-05-14 | 宁波江丰电子材料有限公司 | Chromium target production method |
| US20160184895A1 (en) * | 2013-05-22 | 2016-06-30 | Aubert & Duval | Method of fabricating a steel part by powder metallurgy, and resulting steel part |
| CN110256080A (en) * | 2019-06-28 | 2019-09-20 | 先导薄膜材料（广东）有限公司 | Indium selenide target prepares mold and preparation method |
| WO2021134972A1 (en) * | 2020-01-02 | 2021-07-08 | 宁波江丰电子材料股份有限公司 | Chromium-silicon alloy sputtering target material and preparation method therefor |
| CN113088901A (en) * | 2021-03-31 | 2021-07-09 | 宁波江丰电子材料股份有限公司 | Nickel-chromium alloy sputtering target material and hot isostatic pressing preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103785838A (en) * | 2012-11-01 | 2014-05-14 | 宁波江丰电子材料有限公司 | Chromium target production method |
| US20160184895A1 (en) * | 2013-05-22 | 2016-06-30 | Aubert & Duval | Method of fabricating a steel part by powder metallurgy, and resulting steel part |
| CN110256080A (en) * | 2019-06-28 | 2019-09-20 | 先导薄膜材料（广东）有限公司 | Indium selenide target prepares mold and preparation method |
| WO2021134972A1 (en) * | 2020-01-02 | 2021-07-08 | 宁波江丰电子材料股份有限公司 | Chromium-silicon alloy sputtering target material and preparation method therefor |
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