CN107619972B - Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material - Google Patents
Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material Download PDFInfo
- Publication number
- CN107619972B CN107619972B CN201711096566.9A CN201711096566A CN107619972B CN 107619972 B CN107619972 B CN 107619972B CN 201711096566 A CN201711096566 A CN 201711096566A CN 107619972 B CN107619972 B CN 107619972B
- Authority
- CN
- China
- Prior art keywords
- aluminum
- neodymium
- alloy
- intermediate alloy
- crucible
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for manufacturing an aluminum-neodymium alloy for a magnetron sputtering target, which comprises two steps, wherein the aluminum-neodymium intermediate alloy is prepared by taking aluminum and neodymium as raw materials in the first step, and the aluminum-neodymium alloy is prepared by taking the aluminum-neodymium intermediate alloy as the raw materials in the second step.
Description
Technical Field
The invention relates to the field of magnetron sputtering target material manufacturing, in particular to a method for manufacturing an aluminum-neodymium alloy for a magnetron sputtering target material.
Background
Magnetron sputtering coating is a novel physical vapor phase coating mode, namely, an electron gun system is used for emitting and focusing electrons on a coated material, so that atoms sputtered out of the material fly away from the material to a substrate by higher kinetic energy according to a momentum conversion principle to deposit and form a film. The plated material is called magnetron sputtering target material. In order to improve the sputtering efficiency and ensure the quality of a deposited film, the quality of the target material must be strictly controlled, and a large number of practical researches show that the main factors influencing the quality of the target material comprise purity, impurity content, density, grain size and size distribution, crystal orientation and structure uniformity, geometric shape and size and the like, and the target material is particularly used in the industries of flat panel display, energy-saving low-radiation glass, LED, semiconductor components and the like and has strict requirements on the purity and the impurity content.
The aluminum-neodymium alloy is a common magnetron sputtering target material, the melting point of aluminum is 660 ℃, the density is 2.7, the heat conductivity coefficient is 0.53, the melting point of neodymium is 1024 ℃, the density is 7.0, and the heat conductivity coefficient is 0.031.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a method for producing an aluminum-neodymium alloy for a magnetron sputtering target, which can improve the purity of the aluminum-neodymium alloy and reduce the impurity content.
The purpose of the invention is realized by the following technical scheme: a method for manufacturing an aluminum-neodymium alloy for a magnetron sputtering target comprises the following steps:
s1: putting an aluminum raw material and a neodymium raw material into a smelting furnace, heating, melting, refining and casting to obtain an aluminum-neodymium intermediate alloy;
s2: and (4) adding the aluminum-neodymium intermediate alloy obtained in the step (S1) into an aluminum raw material, putting into a smelting furnace, heating, melting, refining and casting to obtain the aluminum-neodymium alloy.
Compared with the prior art, the manufacturing method provided by the invention comprises two steps, wherein the aluminum-neodymium intermediate alloy is prepared by taking aluminum and neodymium as raw materials in the first step, and the aluminum-neodymium alloy is prepared by taking the aluminum-neodymium intermediate alloy as the raw materials in the second step, because the aluminum-neodymium intermediate alloy has low melting point, low specific gravity and high purity and is more matched with the physical and chemical properties of aluminum, the aluminum-neodymium intermediate alloy and the aluminum-neodymium intermediate alloy have better cooperation and synergistic effect in the smelting process, the melting time can be shortened, the problems of splashing, segregation and the like are solved, the pollution is reduced, the purity of the aluminum-neodymium alloy is improved, and the content of impurities is reduced, so that the purity of the aluminum-neodymium alloy prepared by the method can reach 99.
Further, the aluminum-neodymium intermediate alloy has a weight ratio of aluminum component to neodymium component of 65: 35. Because the melting point of aluminum is lower than that of neodymium, neodymium begins to melt slowly after aluminum is melted, and because neodymium has low thermal conductivity, the neodymium is internally cooled by external heat, and is brittle, so that the problems of splashing and residual sprue are easily caused. At the weight ratio of aluminum to neodymium of 65:35, the molten pool pressure is increased due to the increase of the amount of aluminum liquid after the aluminum is melted, the melting point of neodymium in the melting process is greatly reduced, the splashing problem is solved, and the residual sprue is reduced.
Further, the particle diameter of the neodymium raw material is less than 0.2 mm. The particle diameter of the neodymium is less than 0.2mm, so that the problem of local coking caused by high temperature in the melting process can be prevented, and the melting is more uniform.
Further, in step S1, when charging, the aluminum material is charged first and then the neodymium material is charged. Firstly, the low melting point aluminum raw material is loaded, then the high melting point neodymium raw material is loaded, the lower part is tight and the upper part is loose, the bridging is prevented, and the melting process is orderly carried out.
Further, before charging, a hearth and a crucible in the smelting furnace are cleaned, and then the crucible is preheated to 300-400 ℃. The hearth and the crucible are cleaned, so that the cleanliness of the smelting furnace can be improved, and the pollution is reduced; preheating the crucible to 300-400 ℃ can prevent the crucible from cracking due to overlarge stress under the condition of sharp heat.
Further, the vacuum degree in the smelting furnace is 0.1-0.2 Pa. Smelting under vacuum is beneficial to removing impurity gas, and simultaneously, impurities brought by the raw materials can be volatilized under a vacuum state, so that the materials are purified.
Further, in step S2, the weight ratio of the aluminum-neodymium intermediate alloy to the aluminum raw material is 5-80: 100. The aluminum neodymium intermediate alloy in the composition range is added to an aluminum matrix, so that the melting point of materials can be reduced, the melting time is shortened, and the prepared aluminum neodymium alloy has high purity.
For a better understanding and practice, the invention is described in detail below with reference to specific examples.
Detailed Description
Example 1
The embodiment provides a method for manufacturing an aluminum-neodymium alloy for a magnetron sputtering target, which comprises the following steps:
(1) preparing an aluminum-neodymium intermediate alloy: selecting high-purity aluminum with the purity of more than 99% and high-purity neodymium as raw materials, weighing and proportioning according to a certain weight ratio, and feeding 44kg of the raw materials in total; before charging, cleaning a hearth and a crucible in a smelting furnace, and preheating the crucible to 300 ℃; putting aluminum into a crucible, vacuumizing, increasing power, slowly adding neodymium particles with the diameter less than 0.2mm after the aluminum is melted, preserving heat at 1000 ℃ for 35min after the neodymium is melted, keeping the vacuum degree at 0.1-0.2Pa and keeping the frequency at 2000 Hz; after the melting is finished, stirring the molten metal to fully mix the alloy, degassing and deslagging, cooling to 900 ℃ after the liquid level is purified, and standing for 20 min; after purification is finished, high-power stirring is continued for 3 times, and then casting is carried out; and after the casting is finished, breaking vacuum for 5min, and discharging to obtain the aluminum-neodymium intermediate alloy.
(2) Preparing aluminum-neodymium alloy: selecting high-purity aluminum with the purity of more than 99% and the aluminum-neodymium intermediate alloy obtained in the step (1) as raw materials, wherein the weight ratio of the aluminum-neodymium intermediate alloy to the aluminum raw materials is 5-80: 100; before charging, cleaning a hearth and a crucible in a smelting furnace, and preheating the crucible to 300 ℃; putting aluminum into a crucible, vacuumizing, increasing power, adding aluminum-neodymium intermediate alloy after the aluminum is melted, preserving heat at 1000 ℃ for 35min after the aluminum-neodymium intermediate alloy is melted, keeping the vacuum degree at 0.1-0.2Pa and keeping the frequency at 2000 Hz; after the melting is finished, stirring the molten metal to fully mix the alloy, degassing and deslagging, cooling to 900 ℃ after the liquid level is purified, and standing for 20 min; after purification is finished, high-power stirring is continued for 3 times, and then casting is carried out; and after the casting is finished, breaking the vacuum for 5min, and discharging to obtain the aluminum-neodymium alloy.
In the preparation process of the aluminum-neodymium intermediate alloy in step (1) of this embodiment, aluminum-neodymium intermediate alloys are prepared according to experiments with aluminum-neodymium weight ratios of 50:50 (abbreviated as 50:50 wt%), 60:40 (abbreviated as 60:40 wt%), and 65:35 (abbreviated as 65:35 wt%), respectively, and the results are as follows:
the first test: during the smelting process, because the melting point of aluminum is 660 ℃, the thermal conductivity coefficient is 0.53, the melting point of neodymium is 1024 ℃, and the thermal conductivity coefficient is 0.031, neodymium is slowly melted after the aluminum is aluminized, external heat and internal cooling are caused due to low thermal conductivity of neodymium, the neodymium is brittle, so that the aluminum-neodymium intermediate alloy splashes seriously and pollutes seriously, and in addition, the melting point of 50:50 wt% of the aluminum-neodymium intermediate alloy is 1205 ℃, so that a lot of gates remain and are not easy to be fed back. Therefore, the effect is not desirable.
And (3) second test: compared with the first test, the method for preparing the 60:40 wt% aluminum-neodymium intermediate alloy reduces the content of neodymium, but the problem of splashing in the smelting process cannot be solved, the melting point of the 60:40 wt% aluminum-neodymium alloy is 1020 ℃, and the problem of gate residue is slightly better than the first test result, but is still not ideal.
For the third test: compared with the first test and the second test, the method for preparing the 65:35 wt% aluminum-neodymium intermediate alloy further reduces the content of neodymium, solves the problem of splashing of neodymium in the melting process due to the increase of the amount of aluminum liquid after aluminizing, avoids pollution, reduces the melting point of the 65:35 wt% aluminum-neodymium alloy to 820 ℃, greatly reduces the residual gate to be below 0.5kg, is very ideal in the whole process, and has very high quality of the intermediate alloy.
Compared with the prior art, the manufacturing method provided by the invention comprises two steps, wherein the aluminum-neodymium intermediate alloy is prepared by taking aluminum and neodymium as raw materials in the first step, and the aluminum-neodymium alloy is prepared by taking the aluminum-neodymium intermediate alloy as the raw materials in the second step, because the aluminum-neodymium intermediate alloy has low melting point, low specific gravity and high purity and is more matched with the physical and chemical properties of aluminum, the aluminum-neodymium intermediate alloy and the aluminum-neodymium intermediate alloy have better cooperation and synergistic effect in the smelting process, the melting time can be shortened, the problems of splashing, segregation and the like are solved, the pollution is reduced, the purity of the aluminum-neodymium alloy is improved, and the content of impurities is reduced, so that the purity of the aluminum-neodymium alloy prepared by the method can reach 99.
The above-mentioned embodiments only express one embodiment of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (1)
1. A manufacturing method of aluminum-neodymium alloy for magnetron sputtering target materials is characterized by comprising the following steps: the method comprises the following steps:
s1: putting an aluminum raw material and a neodymium raw material into a smelting furnace, heating, melting, refining and casting to obtain an aluminum-neodymium intermediate alloy; the method specifically comprises the following steps: selecting high-purity aluminum with the purity of more than 99 percent and high-purity neodymium as raw materials, and weighing and proportioning according to the weight ratio of the aluminum component to the neodymium component of 65: 35; before charging, cleaning a hearth and a crucible in a smelting furnace, and preheating the crucible to 300 ℃; putting aluminum into a crucible, vacuumizing, increasing power, slowly adding neodymium particles with the diameter less than 0.2mm after the aluminum is melted, preserving heat at 1000 ℃ for 35min after the neodymium is melted, keeping the vacuum degree at 0.1-0.2Pa and keeping the frequency at 2000 Hz; after the melting is finished, stirring the molten metal to fully mix the alloy, degassing and deslagging, cooling to 900 ℃ after the liquid level is purified, and standing for 20 min; after purification is finished, high-power stirring is continued for 3 times, and then casting is carried out; after the casting is finished, breaking vacuum for 5min, and discharging to obtain aluminum-neodymium intermediate alloy;
s2: adding the aluminum-neodymium intermediate alloy obtained in the step S1 into an aluminum raw material, loading into a smelting furnace, and heating, melting, refining and casting to obtain an aluminum-neodymium alloy; the method specifically comprises the following steps: selecting high-purity aluminum with the purity of more than 99% and aluminum-neodymium intermediate alloy obtained from S1 as raw materials, wherein the weight ratio of the aluminum-neodymium intermediate alloy to the aluminum raw materials is 5-80: 100; before charging, cleaning a hearth and a crucible in a smelting furnace, and preheating the crucible to 300 ℃; putting aluminum into a crucible, vacuumizing, increasing power, adding aluminum-neodymium intermediate alloy after the aluminum is melted, preserving heat at 1000 ℃ for 35min after the aluminum-neodymium intermediate alloy is melted, keeping the vacuum degree at 0.1-0.2Pa and keeping the frequency at 2000 Hz; after the melting is finished, stirring the molten metal to fully mix the alloy, degassing and deslagging, cooling to 900 ℃ after the liquid level is purified, and standing for 20 min; after purification is finished, high-power stirring is continued for 3 times, and then casting is carried out; and after the casting is finished, breaking the vacuum for 5min, and discharging to obtain the aluminum-neodymium alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711096566.9A CN107619972B (en) | 2017-11-09 | 2017-11-09 | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711096566.9A CN107619972B (en) | 2017-11-09 | 2017-11-09 | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107619972A CN107619972A (en) | 2018-01-23 |
| CN107619972B true CN107619972B (en) | 2020-07-07 |
Family
ID=61098829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711096566.9A Active CN107619972B (en) | 2017-11-09 | 2017-11-09 | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107619972B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959595B (en) * | 2021-12-17 | 2024-03-29 | 常州苏晶电子材料有限公司 | High-purity aluminum neodymium alloy target material for sputtering and manufacturing method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999034028A1 (en) * | 1997-12-24 | 1999-07-08 | Kabushiki Kaisha Toshiba | SPUTTERING TARGET, Al INTERCONNECTION FILM, AND ELECTRONIC COMPONENT |
| CN102776394A (en) * | 2012-07-17 | 2012-11-14 | 南昌大学 | Method for preparing aluminum neodymium intermediate alloy with high-intensity ultrasound |
| CN102978491A (en) * | 2012-12-24 | 2013-03-20 | 郝相臣 | High-conductivity aluminium alloy conductor material for cables and preparation method thereof |
| CN103184419A (en) * | 2013-03-19 | 2013-07-03 | 昆山海普电子材料有限公司 | Production method of aluminum-neodymium alloy target material |
| CN104818411A (en) * | 2015-05-21 | 2015-08-05 | 广西友合铝材有限公司 | Rare-earth aluminum-magnesium alloy material and preparation method thereof |
| CN104831242A (en) * | 2015-04-08 | 2015-08-12 | 无锡舒玛天科新能源技术有限公司 | Large-size integral aluminum-neodymium rotary target material and preparation method thereof |
| CN104894409A (en) * | 2015-03-19 | 2015-09-09 | 中信戴卡股份有限公司 | Refining method for aluminum alloy |
| CN105525114A (en) * | 2014-09-29 | 2016-04-27 | 王晓芳 | Method for optimizing Zl301 alloy by adding mixed rare earth |
| CN106191571A (en) * | 2016-08-16 | 2016-12-07 | 中国科学院宁波材料技术与工程研究所 | Aluminum alloy anode material, its preparation method and application thereof |
-
2017
- 2017-11-09 CN CN201711096566.9A patent/CN107619972B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999034028A1 (en) * | 1997-12-24 | 1999-07-08 | Kabushiki Kaisha Toshiba | SPUTTERING TARGET, Al INTERCONNECTION FILM, AND ELECTRONIC COMPONENT |
| CN102776394A (en) * | 2012-07-17 | 2012-11-14 | 南昌大学 | Method for preparing aluminum neodymium intermediate alloy with high-intensity ultrasound |
| CN102978491A (en) * | 2012-12-24 | 2013-03-20 | 郝相臣 | High-conductivity aluminium alloy conductor material for cables and preparation method thereof |
| CN103184419A (en) * | 2013-03-19 | 2013-07-03 | 昆山海普电子材料有限公司 | Production method of aluminum-neodymium alloy target material |
| CN105525114A (en) * | 2014-09-29 | 2016-04-27 | 王晓芳 | Method for optimizing Zl301 alloy by adding mixed rare earth |
| CN104894409A (en) * | 2015-03-19 | 2015-09-09 | 中信戴卡股份有限公司 | Refining method for aluminum alloy |
| CN104831242A (en) * | 2015-04-08 | 2015-08-12 | 无锡舒玛天科新能源技术有限公司 | Large-size integral aluminum-neodymium rotary target material and preparation method thereof |
| CN104818411A (en) * | 2015-05-21 | 2015-08-05 | 广西友合铝材有限公司 | Rare-earth aluminum-magnesium alloy material and preparation method thereof |
| CN106191571A (en) * | 2016-08-16 | 2016-12-07 | 中国科学院宁波材料技术与工程研究所 | Aluminum alloy anode material, its preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107619972A (en) | 2018-01-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109047783B (en) | Aluminum alloy powder and preparation method thereof | |
| CN113737011B (en) | Preparation method of ultra-high purity copper-manganese alloy | |
| EP2772327B1 (en) | High-purity titanium ingots, manufacturing method therefor, and titanium sputtering target | |
| CN112301241B (en) | Preparation method of scandium-containing aluminum alloy welding wire cast ingot | |
| CN102534316B (en) | Al-Mo-W-Ti intermediate alloy and preparing method thereof | |
| WO2023208249A1 (en) | Preparation method for molybdenum alloy tube target material, molybdenum alloy tube target material, and application | |
| CN113512657A (en) | Preparation method of high-uniformity boron-containing titanium alloy ingot | |
| CN107619972B (en) | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material | |
| CN114774865B (en) | Aluminum scandium alloy target and preparation method thereof | |
| CN113652564A (en) | Method for smelting high-temperature alloy by using return material | |
| CN111321361A (en) | Manufacturing method of copper-chromium-nickel-silicon alloy back plate for sputtering target material | |
| CN111088440B (en) | Vacuum induction smelting manufacturing method of high-purity nickel-boron alloy | |
| JP2015045084A (en) | Copper alloy sputtering target and method of manufacturing copper alloy sputtering target | |
| CN112962070B (en) | Preparation equipment and preparation method of sputtering target material | |
| CN103589912A (en) | Melting method of powder superalloy | |
| CN113684456A (en) | La-Ti alloy target and preparation method thereof | |
| CN114293078A (en) | Aluminum alloy powder and preparation method thereof | |
| WO2019237545A1 (en) | Method for preparing copper indium gallium alloy powder | |
| CN110484743B (en) | Low-cost skull for electron beam cold bed smelting furnace and preparation method thereof | |
| CN103225066A (en) | Copper-gallium alloy target material for sputtering and preparation method thereof | |
| CN111020248B (en) | Ag-Zr-Zn intermediate alloy and preparation method and application thereof | |
| RU2807237C1 (en) | Method for smelting heat-resistant copper base alloys | |
| CN115449656B (en) | Preparation method of high-purity chromium-based alloy | |
| JP2018145518A (en) | Cu-Ni alloy sputtering target | |
| CN109881054B (en) | Aluminum-silicon brazing filler metal and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 512026 Yangshan village committee, Xilian Town, Wujiang District, Shaoguan City, Guangdong Province Patentee after: Guangdong Oulai high tech materials Co.,Ltd. Address before: 512000 in Yangshan Area, Muxi Industrial Park, Shaoguan City, Guangdong Province Patentee before: SHAOGUAN OULAI HI-TECH MATERIAL Co.,Ltd. |
|
| CP03 | Change of name, title or address |