CN116878271A - Plasma smelting furnace and preparation method of high-density MgO target material - Google Patents
Plasma smelting furnace and preparation method of high-density MgO target material Download PDFInfo
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- CN116878271A CN116878271A CN202310826541.9A CN202310826541A CN116878271A CN 116878271 A CN116878271 A CN 116878271A CN 202310826541 A CN202310826541 A CN 202310826541A CN 116878271 A CN116878271 A CN 116878271A
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- 238000003723 Smelting Methods 0.000 title claims abstract description 40
- 239000013077 target material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 254
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 135
- 230000006698 induction Effects 0.000 claims abstract description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 230000000977 initiatory effect Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 63
- 239000007789 gas Substances 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 5
- 235000012431 wafers Nutrition 0.000 description 8
- 238000004663 powder metallurgy Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- -1 argon ions Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- PNHVEGMHOXTHMW-UHFFFAOYSA-N magnesium;zinc;oxygen(2-) Chemical compound [O-2].[O-2].[Mg+2].[Zn+2] PNHVEGMHOXTHMW-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003570 air Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
- F27B14/10—Crucibles
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
- F27B14/14—Arrangements of heating devices
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
- F27B14/20—Arrangement of controlling, monitoring, alarm or like devices
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
- F27B2014/045—Vacuum
Abstract
The invention discloses a plasma smelting furnace and a preparation method of a high-density MgO target material. The smelting furnace has: furnace body, magnesia crucible and induction plasma gun, magnesia crucible inlays and establishes in the furnace body inside, and induction plasma gun is vertical to be set up in magnesia crucible top, and its muzzle is put into in the magnesia crucible. The induction plasma gun comprises a magnesium oxide outer tube, a graphite initiation rod and an induction coil, wherein the graphite initiation rod is arranged in the magnesium oxide outer tube in a penetrating mode, the induction coil is sleeved on the outer wall of the magnesium oxide outer tube, the upper portion of the induction plasma gun is communicated with an argon source, and a muzzle at the lower portion of the induction plasma gun is a plasma flame outlet. The method for preparing the high-density MgO target material by utilizing the plasma smelting process has the advantages of few steps, short period, capability of reducing the mixing of other impurities, capability of ensuring the high purity of the target material and capability of ensuring the density of the MgO target material to be more than 99.99 percent.
Description
Technical Field
The invention relates to the technical field of target manufacturing, in particular to a plasma smelting furnace and a preparation method of a high-density MgO target.
Background
The MgO film has the advantages of high temperature stability, high dielectric property, low dielectric loss, good lattice matching with various substrate materials and the like, and is suitable for layered electronic devices such as a magnetic recording layer of a magnetic recording medium. Usually, an MgO film for electrons is formed by a magnetron sputtering method, mgO molecules are knocked out by a MgO target material source by high-energy ion in the magnetron sputtering to deposit on a bottom layer, and the MgO film is formed; therefore, the quality of the MgO target material is the key of film formation, wherein the higher the compactness of the target material is, the higher the sputtering efficiency is, and the better the film formation quality is. At present, mgO target material is prepared by a powder metallurgy method, for example, the technical scheme described in reference 1:
reference 1: chinese patent document with patent publication No. CN114736013 a.
Reference 1 discloses a zinc oxide magnesium target and a preparation method thereof, and belongs to the technical fields of semiconductor photoelectric materials, magnetron sputtering coating and powder metallurgy sintering. The method comprises the following steps: respectively taking ZnO and MgO powder raw materials according to a design group; the powder raw materials are treated by adopting the processes of sectional ball milling, wet blank making, sectional degreasing, sectional sintering, machining, grinding and the like; according to the method provided by the invention, the zinc oxide magnesium target finished product which has high density, guaranteed purity, no defect, uniform and fine crystal grains and is not easy to crack can be obtained.
The existing powder metallurgy preparation steps have complex flow, impurity elements are very easy to mix in each preparation process, impurities cannot be removed once mixed in, and the compactness of the MgO target material prepared by the powder metallurgy method is difficult to reach 99.99%.
Disclosure of Invention
The invention aims to solve the problem of insufficient compactness of an MgO target material prepared in the prior art, and provides a plasma smelting furnace and a preparation method of a high-compactness MgO target material.
The invention solves the technical problems, and adopts the following technical scheme: a plasma smelting furnace, having:
a furnace body; and
the magnesia crucible is embedded in the furnace body; and
the induction plasma gun is vertically arranged above the magnesia crucible, and the muzzle of the induction plasma gun is arranged in the magnesia crucible;
the induction plasma gun comprises a magnesium oxide outer tube, a graphite initiation rod and an induction coil, wherein the graphite initiation rod is arranged in the magnesium oxide outer tube in a penetrating mode, the induction coil is sleeved on the outer wall of the magnesium oxide outer tube, the upper portion of the induction plasma gun is communicated to an argon source, and a muzzle at the lower portion of the induction plasma gun is a plasma flame outlet.
Further optimization of a plasma smelting furnace as one of the present invention: the bottom of the magnesium oxide crucible is of a hemispherical structure.
Further optimization of a plasma smelting furnace as one of the present invention: the side wall of the magnesia crucible is also provided with an annular storage cavity, the annular storage cavity is communicated with the interior of the magnesia crucible through an inclined overflow channel, and the horizontal position of an opening of the overflow channel positioned on the inner wall of the magnesia crucible is higher than that of the opening of the annular storage cavity.
Further optimization of a plasma smelting furnace as one of the present invention: the furnace body is also provided with a pressure gauge for detecting the gas pressure in the furnace body.
A preparation method of a high-density MgO target material comprises the steps of screening MgO powder, placing screened MgO in a plasma furnace according to claim 3 or 4, smelting in a vacuum environment, cooling after smelting to take out MgO ingots, cutting MgO into wafers, welding MgO wafers with a backboard, and further processing the wafers into the MgO target material.
As a preparation method of the high-density MgO target material, the preparation method is further optimized: mgO powder with the purity of more than 99% is selected and screened by a 100-300 mesh screen.
As a preparation method of the high-density MgO target material, the preparation method is further optimized: sequentially sieving MgO powder with 100-mesh, 200-mesh and 300-mesh sieves, selecting and mixing 20-30% of 100-mesh powder, 50-70% of 200-mesh powder and 10-20% of 300-mesh powder after sieving to obtain mixed MgO powder, and then placing the mixed MgO powder into a plasma furnace for smelting.
As a preparation method of the high-density MgO target material, the preparation method is further optimized: firstly, paving a layer of high-purity MgO powder on the bottom of a magnesium oxide crucible, wherein the purity of the high-purity MgO powder is more than 99.99%, and then paving mixed MgO powder on the high-purity MgO powder.
As a preparation method of the high-density MgO target material, the preparation method is further optimized: sequentially sieving MgO powder with 100 mesh, 200 mesh and 300 mesh sieve, selecting 100 mesh powder 20%, 200 mesh powder 65% and 300 mesh powder 15% for mixing to obtain mixed MgO powder, and smelting in a plasma furnace.
As a preparation method of the high-density MgO target material, the preparation method is further optimized: sequentially sieving MgO powder with 100 mesh, 200 mesh and 300 mesh sieve, selecting 30% of 100 mesh powder, 60% of 200 mesh powder and 10% of 300 mesh powder for mixing to obtain mixed MgO powder, and smelting the mixed MgO powder in a plasma furnace.
The invention has the following beneficial effects: the method for preparing the high-density MgO target material by utilizing the plasma smelting process has the advantages of few steps, short period, capability of reducing the mixing of other impurities, capability of ensuring the high purity of the target material and capability of ensuring the density of the MgO target material to be more than 99.99 percent.
Drawings
FIG. 1 is a schematic view of a plasma melting furnace according to the present invention;
the marks in the figure: 1. furnace body, 2, magnesia crucible, 3, induction plasma gun, 301, magnesia outer tube, 302, graphite initiation rod, 303, induction coil, 201, annular storage cavity, 202, overflow channel.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate, but are not to be construed as limiting the invention.
< plasma melting furnace >
As shown in fig. 1, a plasma smelting furnace has: furnace body 1, magnesia crucible 2 and induction plasma gun 3.
The magnesia crucible 2 is embedded in the furnace body 1. The induction plasma gun 3 is vertically arranged above the magnesia crucible 2, and the muzzle of the induction plasma gun is arranged in the magnesia crucible 2. The furnace body 1 is also provided with a pressure gauge for detecting the gas pressure in the furnace body 1.
The induction plasma gun 3 comprises a magnesium oxide outer tube 301, a graphite initiation rod 302 and an induction coil 303, wherein the graphite initiation rod 302 is arranged in the magnesium oxide outer tube 301 in a penetrating mode, the induction coil 303 is arranged on the outer wall of the magnesium oxide outer tube 301 in a sleeved mode, the upper portion of the induction plasma gun 3 is communicated with an argon source, and a muzzle at the lower portion of the induction plasma gun 3 is a plasma flame outlet.
The plasma is an independent form of a substance, and is composed of free electrons, cations, neutral particles and the like, and is in a form of an electrically neutral substance as a whole. Plasma is a powerful high temperature heat source that can be used as a heat source to melt, refine or remelt metallic or non-metallic materials using a plasma arc. The method for generating the plasma mainly comprises an arc method and a high-frequency induction method, and the high-frequency induction method has the characteristics of high temperature, no pollution of electrode materials and the like and is a smelting method which is rising in the future.
The brief working principle is as follows: after vacuumizing the furnace, introducing argon into an argon port of the induction plasma gun; the induction coil is connected with a high-frequency induction power supply, the graphite induction rod heats and ionizes argon gas to form ions, the argon ions continuously collide with other argon gas under the action of an electric field to generate plasma, the plasma is flushed out of the outlet under the flow of the argon gas to release a large amount of energy to form plasma flame, and MgO powder is smelted by the high heat of the plasma flame.
The plasma formed by the argon has high energy and high density, and the energy is higher than that of nitrogen, oxygen or air, so that the magnesia powder can be smoothly melted. A gas mixture may also be used here as a plasma gas or an additional gas. There may also be a recirculation system for hot gases drawn from the furnace, by means of which recirculation system it is possible to effect the gas again as a circulating plasma gas. The closed loop operation allows for a reduction in the amount of plasma gas that needs to be added, thereby reducing the cost, especially of argon.
As a specific structural design, the bottom of the magnesia crucible 2 has a hemispherical structure. The side wall of the magnesia crucible 2 is also provided with an annular storage cavity 201, the annular storage cavity 201 is communicated with the interior of the magnesia crucible 2 through an inclined overflow channel 202, and the horizontal position of an opening of the overflow channel 202 positioned on the inner wall of the magnesia crucible 2 is higher than that of the annular storage cavity 201. If impurities in the smelting process can form a short-range diffusion passage to gradually diffuse to the solid-liquid boundary, and the overflow passage 202 is arranged to enable liquid phase containing the impurities to enter the annular storage cavity 201 so as to improve the purity of the MgO ingot and facilitate the subsequent processing (cutting off the edge part of the MgO ingot after complete crystallization after smelting).
The plasma can generate a large amount of heat and can smelt various metal and non-metal materials, and the plasma generated by the high-frequency induction method has the characteristics of high temperature, no pollution of electrode materials and the like, and is a smelting method which is emerging in the future. MgO raw materials can be effectively smelted by designing proper plasma gun structures and parameters such as working gas flow, flow velocity, induction coil size, induction power supply frequency and the like, and other structures can be protected from being melted. Compared with the powder metallurgy method, the method for preparing the MgO target material by utilizing the plasma smelting has the advantages of fewer process steps, capability of avoiding generating unnecessary impurities and capability of smelting the MgO target material reaching theoretical density.
< preparation method of highly dense MgO target >
A preparation method of a high-density MgO target material comprises the steps of screening MgO powder, placing screened MgO in a plasma furnace according to claim 3 or 4, smelting in a vacuum environment, cooling after smelting to take out MgO ingots, cutting MgO into wafers, welding MgO wafers with a backboard, and further processing the wafers into the MgO target material.
When the induction coil is connected with a high-frequency induction power supply, the graphite induction rod heats up and ionizes the argon to form ions, the argon ions continuously collide with other argon under the action of an electric field to generate plasma, and the plasma rushes out of an outlet under the flow of the argon to release a large amount of energy to form plasma flame, and the high heat of the plasma flame is enough to smelt MgO powder. In the smelting process, the low-melting-point impurities can be gradually moved or separated out to the edge of a molten pool by utilizing the temperature gradient effect, so that MgO in the central part is purified.
Example 1
MgO powder with the purity of over 99.99 percent is selected and respectively sieved by a 100-mesh sieve, a 200-mesh sieve and a 300-mesh sieve to obtain powder with the granularity of 100-mesh, 200-mesh and 300-mesh accounting for 20 percent, 65 percent and 15 percent respectively, and the powder with different particle sizes is mixed with each other and then is placed in a magnesia crucible; and (3) vacuumizing the plasma furnace, introducing argon with certain flow and flow rate, adjusting proper argon flow and flow rate, induction coil power supply frequency and other parameters, smelting MgO powder, cutting off the edge part of the MgO ingot after complete crystallization after smelting, processing into a wafer, welding with a backboard, and further processing into a high-density MgO target material.
Example 2
MgO powder with the purity of over 99.99 percent is selected and respectively sieved by a 100-mesh sieve, a 200-mesh sieve and a 300-mesh sieve to obtain powder with the granularity of 100-mesh, 200-mesh and 300-mesh accounting for 30%, 60% and 10% respectively, and the powder with different particle sizes is mixed with each other and then is placed in a magnesia crucible; and (3) vacuumizing the plasma furnace, introducing argon with certain flow and flow rate, adjusting proper argon flow and flow rate, induction coil power supply frequency and other parameters, smelting MgO powder, cutting off the edge part of the MgO ingot after complete crystallization after smelting, processing into a wafer, welding with a backboard, and further processing into a high-density MgO target material.
After the powders with different particle sizes are mixed with each other, small-granularity powder fills gaps of large-granularity powder, thereby being beneficial to MgO smelting.
The purity and the density of the MgO target materials in the example 1 and the example 2 are detected, the purity of the example 1 reaches more than 99.994 percent, and the density is 99.992 percent; example 2 had a purity of 99.993% and a density of 99.996%.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (10)
1. A plasma smelting furnace, characterized in that it has:
a furnace body (1); and
the magnesia crucible (2) is embedded in the furnace body (1); and
an induction plasma gun (3) which is vertically arranged above the magnesia crucible (2) and the muzzle of which is arranged in the magnesia crucible (2);
the induction plasma gun (3) comprises a magnesium oxide outer tube (301), a graphite initiation rod (302) and an induction coil (303), wherein the graphite initiation rod (302) is arranged in the magnesium oxide outer tube (301) in a penetrating mode, the induction coil (303) is sleeved on the outer wall of the magnesium oxide outer tube (301), the upper portion of the induction plasma gun (3) is communicated with an argon source, and a muzzle at the lower portion of the induction plasma gun (3) is a plasma flame outlet.
2. A plasma smelting furnace as claimed in claim 1, wherein: the bottom of the magnesium oxide crucible (2) is of a hemispherical structure.
3. A plasma smelting furnace as claimed in claim 2, wherein: the side wall of the magnesia crucible (2) is also provided with an annular storage cavity (201), the annular storage cavity (201) is communicated with the inside of the magnesia crucible (2) through an inclined overflow channel (202), and the horizontal position of an opening of the overflow channel (202) positioned on the inner wall of the magnesia crucible (2) is higher than that of the annular storage cavity (201).
4. A plasma smelting furnace as claimed in claim 1, wherein: the furnace body (1) is also provided with a pressure gauge for detecting the gas pressure in the furnace body (1).
5. A preparation method of a high-density MgO target material is characterized by comprising the following steps: sieving MgO powder, smelting the sieved MgO in the plasma furnace in the vacuum environment, cooling to take MgO ingot out, cutting MgO into disc, welding MgO disc with back plate and further processing to obtain MgO target material.
6. The method for preparing the high-density MgO target material according to claim 5, wherein the method comprises the following steps: mgO powder with the purity of more than 99% is selected and screened by a 100-300 mesh screen.
7. The method for preparing the high-density MgO target material according to claim 6, wherein the method comprises the following steps: sequentially sieving MgO powder with 100-mesh, 200-mesh and 300-mesh sieves, selecting and mixing 20-30% of 100-mesh powder, 50-70% of 200-mesh powder and 10-20% of 300-mesh powder after sieving to obtain mixed MgO powder, and then placing the mixed MgO powder into a plasma furnace for smelting.
8. The method for preparing the high-density MgO target material according to claim 6, wherein the method comprises the following steps: firstly, paving a layer of high-purity MgO powder on the bottom of a magnesium oxide crucible, wherein the purity of the high-purity MgO powder is more than 99.99%, and then paving mixed MgO powder on the high-purity MgO powder.
9. The method for preparing the high-density MgO target material according to claim 6, wherein the method comprises the following steps: sequentially sieving MgO powder with 100 mesh, 200 mesh and 300 mesh sieve, selecting 100 mesh powder 20%, 200 mesh powder 65% and 300 mesh powder 15% for mixing to obtain mixed MgO powder, and smelting in a plasma furnace.
10. The method for preparing the high-density MgO target material according to claim 6, wherein the method comprises the following steps: sequentially sieving MgO powder with 100 mesh, 200 mesh and 300 mesh sieve, selecting 30% of 100 mesh powder, 60% of 200 mesh powder and 10% of 300 mesh powder for mixing to obtain mixed MgO powder, and smelting the mixed MgO powder in a plasma furnace.
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