CN113442000A - Preparation method of metallic bismuth planar target - Google Patents
Preparation method of metallic bismuth planar target Download PDFInfo
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- CN113442000A CN113442000A CN202110640367.XA CN202110640367A CN113442000A CN 113442000 A CN113442000 A CN 113442000A CN 202110640367 A CN202110640367 A CN 202110640367A CN 113442000 A CN113442000 A CN 113442000A
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 136
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 145
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 239000013077 target material Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 24
- 239000000155 melt Substances 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000011810 insulating material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000003746 surface roughness Effects 0.000 abstract description 10
- 239000010935 stainless steel Substances 0.000 description 24
- 229910001220 stainless steel Inorganic materials 0.000 description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 22
- 230000007547 defect Effects 0.000 description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 229910002804 graphite Inorganic materials 0.000 description 18
- 239000010439 graphite Substances 0.000 description 18
- 238000005520 cutting process Methods 0.000 description 17
- 238000003754 machining Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004506 ultrasonic cleaning Methods 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 238000004321 preservation Methods 0.000 description 7
- 238000007514 turning Methods 0.000 description 7
- 229920000742 Cotton Polymers 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 101100352919 Caenorhabditis elegans ppm-2 gene Proteins 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 229910052729 chemical element Inorganic materials 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007516 diamond turning Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002115 bismuth titanate Inorganic materials 0.000 description 1
- 229910021418 black silicon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B27/00—Other grinding machines or devices
- B24B27/033—Other grinding machines or devices for grinding a surface for cleaning purposes, e.g. for descaling or for grinding off flaws in the surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/10—Single-purpose machines or devices
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a preparation method of a metal bismuth planar target. The preparation method of the metal bismuth planar target material comprises the following steps: firstly, carrying out primary coarse grinding on a bismuth ingot by using a first grinding wheel to remove a surface oxide layer, then carrying out secondary coarse grinding on the bismuth ingot by using a second grinding wheel, reserving a fine grinding allowance of 0.3-1 mm, and then carrying out fine grinding on the bismuth ingot by using a third grinding wheel to obtain the metal bismuth plane target material, wherein the mesh number of the first grinding wheel is less than or equal to that of the second grinding wheel and less than or equal to that of the third grinding wheel, and the feed amount of the first grinding wheel is less than that of the second grinding wheel and less than that of the third grinding wheel. The method for preparing the bismuth planar target material is simple, the surface roughness of the bismuth target material is below 1.6 mu m, corners are free of corner collapse, and the surface is smooth and clean.
Description
Technical Field
The invention belongs to the field of metal target materials, and relates to a preparation method of a metal bismuth planar target material.
Background
At present, the scale of the domestic semiconductor material industry and the target material industry is gradually enlarged, the acceleration rate is higher than the global acceleration rate, the share of the target material industry in the global market is gradually increased, the Chinese develops into the emerging market of the semiconductor material with the most potential in the world by virtue of the rapid development of the wafer factory in the continental China.
In recent years, with the development of new electronic industries such as big data, internet of things, artificial intelligence and the like, people increasingly demand new-generation high-density, low-power-consumption and multifunctional information storage technologies, and bismuth composite materials such as bismuth ferrite, bismuth titanate and the like are spotlighted as novel memory materials. Bismuth is a metal with thermal conductivity, and the bismuth alloy have a thermoelectric effect, and the bismuth volume is increased during solidification, so that the expansion rate reaches 3.3%, and therefore, the bismuth target material is also regarded as important in the field of sensors such as electronic refrigeration elements, thermoelectric conversion elements and the like.
At present, a lathe or a milling machine is often used for processing the bismuth target, but bismuth is a brittle material, and corner breakage and cutter sticking phenomena can occur when the lathe or the milling machine is used for processing, so that the required roughness cannot be achieved. Therefore, a more effective method for processing the bismuth target is urgently needed to be developed, so that the corners of the obtained bismuth target have no corner collapse, the surface is smooth and clean, and the roughness is lower.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the metal bismuth planar target material, and the obtained bismuth target material has no corner collapse, smooth surface and very low roughness.
In order to achieve the purpose, the invention provides a preparation method of a metal bismuth planar target material, which comprises the following steps:
(1) carrying out primary coarse grinding on the bismuth ingot by using a first grinding wheel to remove a surface oxide layer to obtain a first polished ingot;
(2) carrying out secondary coarse grinding on the first polished ingot by using a second grinding wheel to obtain a second polished ingot;
(3) fine grinding the second polished bismuth ingot by using a third grinding wheel to obtain a metal bismuth plane target material;
wherein the mesh number of the first grinding wheel is less than or equal to that of the second grinding wheel, the mesh number of the second grinding wheel is less than or equal to that of the third grinding wheel, the feed rate of the first grinding wheel is less than that of the second grinding wheel and less than that of the third grinding wheel, and a fine grinding allowance of 0.3-1 mm is reserved during the second coarse grinding.
The preparation method adopts a grinding machine processing method to prepare the metal bismuth plane target material, the surface roughness of the obtained metal bismuth plane target material is below 1.6 mu m, corners have no corner breakage, and the surface is smooth and clean.
Preferably, the mesh number of the first grinding wheel is 60-100 meshes, and the feed amount is 30-50 mu m; the mesh number of the second grinding wheel is 100-320 meshes, and the feed amount is 10-20 mu m; the mesh number of the third grinding wheel is 320-400 meshes, and the feed amount is 2-10 mu m.
Preferably, the mesh number of the first grinding wheel is 100 meshes, and the feed amount is 30-50 μm; the mesh number of the second grinding wheel is 100 meshes, and the feed amount is 10-20 mu m; the mesh number of the third grinding wheel is 400 meshes, and the feed amount is 2 mu m.
Preferably, the first grinding wheel and the second grinding wheel are both alumina grinding wheels; the third grinding wheel is a diamond grinding wheel.
Preferably, the bismuth ingot to be used for the first rough grinding is subjected to an electrical conductivity test, and if the measured electrical conductivity is not lower than a theoretical value, it is used for the first rough grinding.
Preferably, the preparation method further comprises step (i) before step (1): heating the bismuth ingot to be completely melted, removing impurities on the surface of the melt, uniformly mixing the melt, and casting to form the bismuth ingot.
Preferably, the step (i) is: heating the bismuth ingot at 290-310 ℃ to be completely melted in an atmospheric environment, preserving heat for 5-10 min after the bismuth ingot is completely melted, removing impurities on the surface of the melt, uniformly mixing the melt, and casting to form the bismuth ingot.
Preferably, the mould used for casting is preheated, the temperature of the preheated mould being lower than the temperature of the melt to be cast. More preferably, the temperature of the mold after the preheating treatment is 150-200 ℃.
Preferably, the outer surface of the mould used for casting is wrapped by a heat preservation material.
Preferably, the bismuth ingot is washed with an organic solvent before the step (i) is performed.
Preferably, the preparation method further comprises the following steps: and cleaning the metal bismuth planar target material by using an organic solvent, and drying.
Compared with the prior art, the invention has the beneficial effects that: the method for preparing the metal bismuth planar target material by adopting the grinding machine for processing is very simple, the surface roughness of the obtained bismuth target material is below 1.6 mu m, corners have no broken corners, and the surface is smooth and clean.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
In order to obtain the metal bismuth plane target material with no corner breakage, smooth surface and very low roughness, the invention adopts a grinding machine to process a bismuth ingot. Specifically, the preparation method of the metal bismuth planar target comprises the following steps:
(1) carrying out primary coarse grinding on the bismuth ingot by using a first grinding wheel to remove a surface oxide layer to obtain a first polished ingot;
(2) carrying out secondary coarse grinding on the first polished ingot by using a second grinding wheel to obtain a second polished ingot;
(3) finely grinding the second polished bismuth ingot by using a third grinding wheel to obtain a metal bismuth planar target;
wherein the mesh number of the first grinding wheel is less than or equal to that of the second grinding wheel, the mesh number of the second grinding wheel is less than or equal to that of the third grinding wheel, the feed rate of the first grinding wheel is less than that of the second grinding wheel and less than that of the third grinding wheel, and a fine grinding allowance of 0.3-1 mm is reserved during the second coarse grinding. The surface roughness of the metal bismuth plane target material obtained by the grinding machine is below 1.6 mu m, no corner collapse exists, and the surface is smooth.
In some embodiments, the first grinding wheel has a mesh number of 60 to 100 meshes and a feed amount of 30 to 50 μm; the mesh number of the second grinding wheel is 100-320 meshes, and the feed amount is 10-20 mu m; the third grinding wheel has a mesh size of 320-400 meshes and a feed rate of 2-10 μm. In some preferred embodiments, the first grinding wheel has a mesh number of 100, and the feed amount is 30-50 μm; the mesh number of the second grinding wheel is 100 meshes, and the feed amount is 10-20 mu m; the mesh number of the third grinding wheel is 400 meshes, and the feed amount is 2 mu m. The first grinding wheel and the second grinding wheel can be selected from alumina grinding wheels, and the third grinding wheel can be selected from diamond grinding wheels, but the selection of the materials of the first grinding wheel, the second grinding wheel and the third grinding wheel is not limited to the above, for example, the first grinding wheel can also be selected from 60-80 mesh black silicon carbide grinding wheels, brown corundum grinding wheels and the like, and the third grinding wheel can also be selected from 320-400 mesh microcrystalline corundum grinding wheels, diamond grinding wheels and the like.
Before the bismuth ingot is machined by a grinding machine, the bismuth ingot is usually subjected to a conductivity test, and whether defects exist in the bismuth ingot can be judged according to a conductivity test result. If the measured conductivity is not lower than the theoretical value, the bismuth ingot has no defects inside and can be directly used for processing by a grinding machine; if the measured conductivity is lower than the theoretical value, the bismuth ingot has defects inside, cannot be directly used for machining by a grinding machine, and can be used for machining by the grinding machine after internal defects are eliminated by means of casting and the like.
The more test points, the easier the defects inside the bismuth ingot can be detected. Preferably, more than 50 points are uniformly selected on the bismuth ingot to be used for grinding machine processing to carry out the conductivity test.
In some embodiments, the method for preparing the metallic bismuth planar target further comprises a step (i) before the step (1): heating the bismuth ingot to be completely melted, removing impurities on the surface of the melt, uniformly mixing the melt, and casting to form the bismuth ingot. After the bismuth ingot is heated and melted, the impure slag such as oxide and the like can float on the melt, and the impure slag is removed by a net fishing out and the like, so that the purity of the formed cast ingot can be improved, and the internal defect caused by the fact that the impure slag flows into the cast ingot during casting can be avoided. Step (I) is commonly used to eliminate defects inside bismuth ingots.
In some preferred embodiments, step (i) is: heating the bismuth ingot at 290-310 ℃ to be completely melted in an atmospheric environment, preserving heat for 5-10 min after the bismuth ingot is completely melted, removing impurities on the surface of a melt, uniformly mixing the melt, and casting to form the bismuth ingot. The treatment can reduce oxygen introduced by bismuth ingot smelting in the atmosphere, control the oxygen content of the formed ingot below 50ppm, and simplify the casting condition.
In some preferred embodiments, the mould used for casting in step (i) is preheated before casting, the temperature of the preheated mould being lower than the temperature of the melt to be cast. Therefore, the melt is cast in the mold after the preheating treatment, so that the cooling rate in the casting process can be reduced, and the internal shrinkage cavity of the formed cast ingot is reduced. More preferably, the temperature of the mold after the preheating treatment is 150-200 ℃, namely, the melt is cast in the mold at 150-200 ℃, so that shrinkage cavities formed in the cast ingot can be well avoided, the time for forming the cast ingot is short, and the efficiency is high.
The outer surface of the mould used for casting in the step (I) can be not specially treated, but can be wrapped with a heat-insulating material to further reduce the cooling rate in the casting process and reduce the internal shrinkage cavity of the formed cast ingot.
In some embodiments, before step (i), the bismuth ingot is further washed with an organic solvent to remove impurities such as oil stains on the surface. The organic solvent can be at least one of isopropanol, ethanol and the like; when the bismuth ingot is cleaned by the organic solvent, ultrasonic cleaning can be adopted, and the parameters of the ultrasonic cleaning can be adjusted according to actual conditions.
In some embodiments, the bismuth metal planar target is further washed with an organic solvent and then dried. The organic solvent can be at least one of isopropanol, ethanol and the like; when the metal bismuth planar target is cleaned by the organic solvent, ultrasonic cleaning can be adopted, and parameters of the ultrasonic cleaning can be adjusted according to actual conditions, such as ultrasonic frequency of 40-80 kHz and ultrasonic treatment for 1-10 min; during drying, the solvent traces on the surface of the metal bismuth planar target material can be dried firstly, and then vacuum drying is adopted, wherein the vacuum drying can be selected to be drying at 60-80 ℃ for 60-120 min, but the drying mode is not limited to the above.
Preparing a bismuth planar target material by using a bismuth ingot with the purity of 4N, wherein the conductivity of the obtained bismuth planar target material is 0.78-0.79 MS/m, and the roughness of the bismuth planar target material<1.6, density 9.80g/cm3The impurity content meets the 4N standard, which is shown in Table 1.
TABLE 1
| Chemical elements | Unit of | Standard of merit |
| Ag | ppm | ≤40 |
| As | ppm | ≤3 |
| Cu | ppm | ≤10 |
| Fe | ppm | ≤10 |
| Pb | ppm | ≤10 |
| Sb | ppm | ≤5 |
| Te | ppm | ≤3 |
| Zn | ppm | ≤5 |
Example 1
The embodiment provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace to 290 ℃, preserving the temperature for 10min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 180 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 41ppm and the specification of 267 × 169 × 15.8mm, and weighing the ingot as a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: cutting from the first ingot using a waterjet cutter
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. coarse grinding: carrying out coarse grinding twice on the second cast ingot by using a 100-mesh alumina grinding wheel, wherein the feed amount of the first coarse grinding is 40 mu m, and the reduction amount of the ground surface oxide layer is 4 mm; the feed amount of the second coarse grinding is 10 mu m, a circular cast ingot with the thickness of 10.5mm is required to be obtained, and a fine grinding allowance of 0.5mm is reserved;
7. fine grinding: carrying out the treatment on the cast ingot treated in the step 6 by using a 400-mesh diamond grinding wheelFine grinding, setting the feed amount to 2 μm, and processing to
The surface roughness is 0.779 μm, no corner break exists at the corner, and the surface is smooth and clean;
8. cleaning: putting the milled bismuth target material into isopropanol, and ultrasonically cleaning for 5min at the ultrasonic frequency of 40 kHz;
9. drying: and (3) blowing the solvent traces on the surface of the bismuth target by using an air gun, and drying in a vacuum drying oven at 60 ℃ for 60min to obtain the metal bismuth planar target.
The finished metallic bismuth planar target product obtained in the embodiment has the conductivity of 0.79MS/m, the roughness of 0.779 mu m and the density of 9.83g/cm3The impurity contents are shown in Table 2.
TABLE 2
Example 2
The embodiment provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace at 300 ℃, preserving the temperature for 7min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 200 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 40ppm and the specification of 267 × 169 × 15.8mm, and the ingot is called a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: cutting from the first ingot using a waterjet cutter
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. coarse grinding: carrying out coarse grinding twice on the second cast ingot by using a 100-mesh alumina grinding wheel, wherein the feed amount of the first coarse grinding is 30 mu m, and the reduction amount of the ground surface oxide layer is 4 mm; the feed amount of the second coarse grinding is 20 mu m, a circular cast ingot with the thickness of 10.8mm is required to be obtained, and a fine grinding allowance of 0.8mm is reserved;
7. fine grinding: the ingot after the treatment of step 6 was finely ground using a 400-mesh diamond grinding wheel with a feed rate of 2 μm to be processed
The surface roughness is 0.653 μm, no corner breakage exists, and the surface is smooth and clean;
8. cleaning: putting the milled bismuth target material into isopropanol, and ultrasonically cleaning for 5min at the ultrasonic frequency of 50 kHz;
9. drying: and (3) blowing the solvent traces on the surface of the bismuth target by using an air gun, and drying in a vacuum drying oven at 70 ℃ for 100min to obtain the metal bismuth planar target.
The finished metallic bismuth planar target material obtained in the embodiment has the conductivity of 0.79MS/m, the roughness of 0.653 mu m and the density of 9.83g/cm3The impurity contents are shown in Table 3.
TABLE 3
| Chemical elements | Unit of | Content (wt.) |
| Ag | ppm | 20 |
| As | ppm | 2 |
| Cu | ppm | 8 |
| Fe | ppm | 9 |
| Pb | ppm | 6 |
| Sb | ppm | <5 |
| Te | ppm | 2 |
| Zn | ppm | <3 |
Example 3
The embodiment provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace at 310 ℃, keeping the temperature for 5min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 150 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 46ppm and the specification of 267 × 169 × 15.8mm, and the ingot is called a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: cutting from the first ingot using a waterjet cutter
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. coarse grinding: carrying out coarse grinding twice on the second ingot by using a 100-mesh alumina grinding wheel, wherein the feed amount of the first coarse grinding is 50 mu m, and the reduction amount of the ground surface oxide layer is 3.8 mm; the feed amount of the second coarse grinding is 15 mu m, a circular cast ingot with the thickness of 11mm is required to be obtained, and a fine grinding allowance of 1mm is reserved;
7. fine grinding: the ingot after the treatment of step 6 was finely ground using a 400-mesh diamond grinding wheel with a feed rate of 2 μm to be processed
The surface roughness is 0.731 mu m, no corner break exists at the corner, and the surface is smooth and clean;
8. cleaning: putting the milled bismuth target material into isopropanol, and ultrasonically cleaning for 5min at the ultrasonic frequency of 80 kHz;
9. drying: and (3) blowing the solvent traces on the surface of the bismuth target by using an air gun, and then drying in a vacuum drying oven at 60 ℃ for 120min to obtain the metal bismuth planar target.
The finished metallic bismuth planar target material obtained in the embodiment has the conductivity of 0.79MS/m, the roughness of 0.731 mu m and the density of 9.79g/cm3The impurity contents are shown in Table 4.
TABLE 4
| Chemical elements | Unit of | Content (wt.) |
| Ag | ppm | 15 |
| As | ppm | <2 |
| Cu | ppm | 8 |
| Fe | ppm | 9 |
| Pb | ppm | 6 |
| Sb | ppm | <5 |
| Te | ppm | 2 |
| Zn | ppm | <3 |
Comparative example 1
The comparative example provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace to 290 ℃, preserving the temperature for 10min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 180 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 41ppm and the specification of 267 × 169 × 15.8mm, and weighing the ingot as a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: cutting from the first ingot using a waterjet cutter
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. turning: turning on a common lathe by using a diamond turning tool, wherein the common lathe processing technology comprises the following steps: 240RPM, the automatic feed speed ratio is 1:1, the feed amount is 0.1mm, the surface of the target material obtained by lathe processing is rough, the roughness is 4.32 mu m, and obvious spots are formed.
Comparative example 2
The comparative example provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace to 290 ℃, preserving the temperature for 10min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 180 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 41ppm and the specification of 267 × 169 × 15.8mm, and weighing the ingot as a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: from the first ingot using a waterjet cutterIs cut off
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. turning: turning on a common lathe by using a diamond turning tool, wherein the common lathe processing technology comprises the following steps: 320RPM, 1:1, feed rate of 0.1mm, rough surface of the target material obtained by lathe machining, roughness of 4.122 μm and obvious corner collapse.
Comparative example 3
The comparative example provides a preparation method of a metal bismuth planar target, which comprises the following steps:
1. cleaning: cutting 6.7kg of bismuth ingot with the purity of 4N into blocks by using a sawing machine, and putting the cut bismuth ingot into isopropanol to carry out ultrasonic cleaning for 20 minutes so as to clean oil stains and impurities on the surface of the bismuth ingot, wherein the ultrasonic frequency is 40 kHz;
2. smelting: putting the bismuth ingot into a stainless steel crucible, then placing the stainless steel crucible into a heating furnace, heating the bismuth ingot to be smelted in an atmospheric environment, setting the temperature of the heating furnace to 290 ℃, preserving the temperature for 10min after the bismuth ingot is completely smelted, fishing out oxides on the surface of the melt by using a stainless steel net, and then uniformly stirring by using a stainless steel bar to obtain a first melt;
3. casting: casting the first melt in a graphite mold (the specification of the graphite mold is 370 × 170 × 16mm, the outer surface of the graphite mold is wrapped by heat preservation cotton) at 180 ℃ to obtain an ingot with the purity of 4N, the oxygen content of 41ppm and the specification of 267 × 169 × 15.8mm, and weighing the ingot as a first ingot;
4. detecting defects: uniformly selecting 50 points on the first ingot, testing the electrical conductivity of the points by using an eddy current metal conductivity meter, and finding that the electrical conductivity of the points is 78MS/m or 79MS/m, which indicates that no defect exists in the first ingot;
5. cutting: cutting from the first ingot using a waterjet cutter
For grinding machine machining, the round ingot (hereinafter referred to as the second ingot) of (1);
6. turning: turning on a common lathe by using a hard alloy turning tool, wherein the common lathe processing technology comprises the following steps: 240RPM, the automatic feed speed ratio is 1:1, the feed rate is 0.1mm, the surface of the target material obtained by lathe machining is rough, the roughness is 4.775 mu m, and the target material has obvious broken angles.
The surface roughness and the number of edge chipping of the metallic bismuth planar target material obtained in each example and comparative example are shown in tables 5 and 6.
TABLE 5
| Sample (I) | Surface roughness (μm) |
| Example 1 | 0.779 |
| Example 2 | 0.653 |
| Example 3 | 0.731 |
| Comparative example 1 | 4.320 |
| Comparative example 2 | 4.122 |
| Comparative example 3 | 4.775 |
TABLE 6
As can be seen from tables 3 and 4, the surface roughness of the bismuth target material obtained by the grinding machine is very low and the corner has no corner collapse as compared with the lathe machining.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the metal bismuth planar target is characterized by comprising the following steps of:
(1) carrying out primary coarse grinding on the bismuth ingot by using a first grinding wheel to remove a surface oxide layer to obtain a first polished ingot;
(2) carrying out secondary coarse grinding on the first polished ingot by using a second grinding wheel to obtain a second polished ingot;
(3) fine grinding the second polished bismuth ingot by using a third grinding wheel to obtain a metal bismuth plane target material;
wherein the mesh number of the first grinding wheel is less than or equal to that of the second grinding wheel, the mesh number of the second grinding wheel is less than or equal to that of the third grinding wheel, the feed rate of the first grinding wheel is less than that of the second grinding wheel and less than that of the third grinding wheel, and a fine grinding allowance of 0.3-1 mm is reserved during the second coarse grinding.
2. The method according to claim 1, wherein the first grinding wheel has a mesh size of 60 to 100 mesh and a feed rate of 30 to 50 μm; the mesh number of the second grinding wheel is 100-320 meshes, and the feed amount is 10-20 mu m; the mesh number of the third grinding wheel is 320-400 meshes, and the feed amount is 2-10 mu m.
3. The preparation method according to claim 2, wherein the first grinding wheel has a mesh size of 100 meshes and a feed amount of 30 to 50 μm; the mesh number of the second grinding wheel is 100 meshes, and the feed amount is 10-20 mu m; the mesh number of the third grinding wheel is 400 meshes, and the feed amount is 2 mu m.
4. The production method according to any one of claims 1 to 3, wherein the first grinding wheel and the second grinding wheel are both alumina grinding wheels; the third grinding wheel is a diamond grinding wheel.
5. The production method according to any one of claims 1 to 3, characterized in that a conductivity test is performed on the bismuth ingot to be used for the first rough grinding, and if the measured conductivity is not lower than a theoretical value, it is used for performing the first rough grinding.
6. The production method according to any one of claims 1 to 3, characterized by further comprising, before step (1), step (I): heating the bismuth ingot to be completely melted, removing impurities on the surface of the melt, uniformly mixing the melt, and casting to form the bismuth ingot.
7. The method according to claim 6, wherein the step (I) is: heating the bismuth ingot at 290-310 ℃ to be completely melted in an atmospheric environment, preserving heat for 5-10 min after the bismuth ingot is completely melted, removing impurities on the surface of the melt, uniformly mixing the melt, and casting to form the bismuth ingot.
8. The method according to claim 6, wherein the mold for casting is preheated, and the temperature of the preheated mold is lower than that of the melt to be cast; preferably, the temperature of the mold after the preheating treatment is 150-200 ℃.
9. The method according to claim 8, wherein the outer surface of the mold for casting is coated with a heat insulating material.
10. The method of any one of claims 1-3, further comprising the steps of: and cleaning the metal bismuth planar target material by using an organic solvent, and drying.
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