CN117778883A - Ultra-high purity clean steel for manufacturing semiconductor and manufacturing method thereof - Google Patents
Ultra-high purity clean steel for manufacturing semiconductor and manufacturing method thereof Download PDFInfo
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- CN117778883A CN117778883A CN202311854733.7A CN202311854733A CN117778883A CN 117778883 A CN117778883 A CN 117778883A CN 202311854733 A CN202311854733 A CN 202311854733A CN 117778883 A CN117778883 A CN 117778883A
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Abstract
The application discloses ultra-high purity clean steel for manufacturing semiconductors and a manufacturing method thereof, wherein the ultra-high purity clean steel comprises 0.01MAX weight percent of carbon, 0.15MAX weight percent of silicon, 0.05MAX weight percent of manganese, 0.02MAX weight percent of phosphorus, 0.002MAX weight percent of sulfur, 0.01MAX weight percent of aluminum, 0.01MAX weight percent of niobium, 0.01MAX weight percent of titanium, 0.01MAX weight percent of cesium, 0.01MAX weight percent of calcium, 0.2MAX weight percent of copper, 14.50-15.00 weight percent of nickel, 16.5-17.00 weight percent of chromium, 2.20-2.50 weight percent of molybdenum and the balance of iron.
Description
Technical Field
The invention relates to ultra-high purity steel, in particular to ultra-high purity steel for manufacturing semiconductors and a manufacturing method thereof.
Background
At present, with the development of the semiconductor field, ultra-high purity clean steel has become a trend material for manufacturing semiconductor materials. Research shows that the manufacture of the semiconductor cavity and the parts is not separated from the material.
The ultra-high purity clean steel is used as a first-choice material of the high-end semiconductor, and has certain corrosion resistance and ultra-high cleanliness, and improves the use balance and safety of the high-end semiconductor. The vacuum induction furnace and the vacuum consumable furnace are adopted for smelting, the functional part is changed into the structural part, the development trend is biased to thin-wall parts, integrated and structurally complicated ultra-pure clean steel, and the materials are required to be high in strength and high in extension, so that the stability of part welding can be met.
However, at present, many ultra-pure clean steels cannot meet the preset performance requirements, especially, the uncontrollable factors in the process of smelting raw materials are more, and the deformation, low yield and high cost of the ultra-pure clean steel structural members are finally caused. However, the semiconductor in China is free from ultra-high purity clean steel, but in the currently used Japanese Datong special material, the sulfur-aluminum content is controlled to be very low in order to ensure the plasticity of the material, so that the regenerated raw material is difficult to produce.
With the deep advancement of semiconductors and semiconductor parts, ultra-high purity clean steel has become available in the future, and has shown remarkable advantages in domestic use, so as to get rid of the dependence of Japanese Dazhong on "exclusive supply". However, the properties such as hardness, area shrinkage and corrosion resistance of the ultra-high purity steel in China are still different from those of the ultra-high purity steel produced in large scale in Japan.
Disclosure of Invention
An advantage of the present invention is to provide an ultra-pure clean steel for manufacturing semiconductors and a working method thereof, wherein the ultra-pure clean steel is heat treated after forging to obtain a tensile strength >450Mpa, a yield strength >175Mpa, a section elongation >29%, an area reduction >45%, a hardness >187HB, while obtaining good corrosion resistance and a high-odor use.
Another advantage of the present invention is to provide an ultra-high purity steel for manufacturing semiconductors and a method of operating the same, wherein the ultra-high purity steel for manufacturing semiconductors has high hardness and plasticity.
To achieve at least one of the above advantages, the present invention provides an ultra-high purity steel for manufacturing semiconductors, characterized in that the ultra-high purity steel comprises:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
the balance being iron.
According to an embodiment of the invention, the ratio of the nickel content to the molybdenum content is: 6.0:1-6.14:1.
According to an embodiment of the present invention, the ratio of the chromium content to the molybdenum content is: 6.8:1-7.2:1.
According to an embodiment of the present invention, the ultra-high purity steel includes: 0.03 to 0.05 percent of manganese.
According to an embodiment of the invention, the ultra-high purity steel comprises 0.012-0.015% phosphorus.
According to an embodiment of the present invention, the ultra-high purity steel includes 0.0015 to 0.019% sulfur.
To achieve at least one of the above advantages, the present invention provides a method for manufacturing ultra-high purity clean steel, comprising the steps of:
s1, melting 4N9 pure iron raw materials;
s2, the ultra-high purity steel comprises the following components:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
and (3) adding high-purity nickel, 4N9 pure iron, high-purity molybdenum and high-purity chromium into the filtrate, and melting the added components by heating molten steel.
Drawings
FIG. 1 is a mirror phase diagram at 100um for ultra-high purity clean steel used to fabricate semiconductors.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and this summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
An ultra-high purity steel for manufacturing a semiconductor according to a preferred embodiment of the present invention will be described in detail below, wherein the ultra-high purity steel comprises:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
the balance being iron.
It is worth mentioning that the share of sulfur and aluminum in ultra-high purity clean steel is at most 0.012 wt.%, because the regenerated elements can be maximally used, preferably the iron is kept high purity and grade 4N9 is ensured.
It is worth mentioning that the ratio of nickel content to molybdenum content is: 6.0:1-6.14:1, wherein the ratio of the chromium content to the molybdenum content is as follows: 6.8:1-7.2:1, thus, the ultra-high purity clean steel for manufacturing semiconductors has good tensile strength, yield strength, section elongation and the like, and also has good corrosion resistance and high-odor acid use scene. As shown in fig. 1.
It is worth mentioning that in the ultra-high purity steel, low carbon reduces yield point and tensile strength, but plasticity and impact are improved, and when the carbon content is 0.01% exceeded, the welding performance of the steel is better, but the yield strength and tensile strength of the ultra-high purity steel are affected.
Silicon is added as a reducing agent and a deoxidizing agent in the refining process of the ultra-high purity steel, and silicon with the content of less than 0.15% is added into the ultra-high purity steel, so that the corrosion resistance and the oxidation resistance are improved, and the welding performance is improved.
Manganese is a good deoxidizer and desulfurizing agent in the refining process of the ultra-high purity steel, and the high purity steel preferably contains 0.03 to 0.05% manganese. The manganese content is maintained in this range, which can improve corrosion resistance and improve welding performance. Improving hot workability of steel
In the refining of said ultra-high purity steel, phosphorus is generally a detrimental element in the steel. The ultra-high purity clean steel adopts 0.02 percent MAX, preferably 0.012 to 0.015 percent of low phosphorus so as to improve the cold brittleness of the steel, improve the welding performance and the plasticity and improve the cold bending performance.
Sulfur in the ultra-high purity steel is also a detrimental element in the normal case. The high-purity steel adopts MAX with low sulfur content of 0.002 percent, preferably 0.0015 to 0.019 percent, avoids the phenomenon of thermal embrittlement and improves the ductility and toughness of the steel. The low sulfur steel is advantageous in forging and rolling processes. In addition, the low sulfur is favorable for welding performance and improves corrosion resistance.
Chromium can significantly improve strength, hardness, and wear resistance, but at the same time reduces plasticity and toughness in structural and tool steels. Chromium can also improve the oxidation resistance and corrosion resistance of steel, so that the chromium is an important alloy element of stainless steel and heat-resistant steel.
Nickel can improve the strength of the steel while maintaining good plasticity and toughness. Nickel has high corrosion resistance to acid and alkali, and has rust resistance and heat resistance at high temperature. However, too much Ni element addition may reduce the conductivity of the ultra-pure clean steel finally formed. Thus, the electrical properties of the final semiconductor formed are affected. Thus, in a preferred embodiment, by limiting the ratio of nickel content to molybdenum content and the ratio of chromium content to molybdenum content, on the one hand, it is possible to control the improvement of the electrical properties of the semiconductor, but also its corrosion resistance and other mechanical properties.
Molybdenum can refine the crystal grains of steel, improve hardenability and heat strength, and maintain sufficient strength and creep resistance at high temperature (long-term stress at high temperature, deformation, and creep). Molybdenum is added into the structural steel, so that the mechanical property can be improved. It is also possible to suppress brittleness of the alloy steel due to fire.
Titanium is a strong deoxidizer in the ultra-high purity steel. It can compact the internal structure of steel and refine the grain force; reducing ageing sensitivity and cold brittleness. Improving the welding performance. The addition of suitable titanium to chromium 18 nickel 9 austenitic stainless steel avoids intergranular corrosion.
Niobium refines the grains and reduces the susceptibility to overheating and temper embrittlement of the steel, increasing strength, but with some reduction in plasticity and toughness. Niobium is added into the common low alloy steel to improve the resistance to atmospheric corrosion and hydrogen, nitrogen and ammonia corrosion at high temperature. Niobium may improve the welding properties. Niobium is added to austenitic stainless steel to prevent intergranular corrosion.
Copper can improve strength and toughness, particularly atmospheric corrosion performance. The disadvantage is that thermal embrittlement is easy to occur during hot working, the plasticity of copper content exceeding 0.2% is significantly better, but thermal embrittlement is easy to occur. When the copper content is less than 0.2%, there is no effect on weldability.
Aluminum is a commonly used deoxidizer in steel. The addition of a small amount of aluminum into the steel can refine grains, improve impact toughness, and has oxidation resistance and corrosion resistance, and the combination of aluminum, chromium and silicon can obviously improve the high-temperature non-skinning performance and the high-temperature corrosion resistance of the steel. The disadvantage of adding aluminum is that it affects the hot workability, weldability and machinability of the steel.
It is worth mentioning that the calcium element is preferably added in an amount of 0.003 to 0.006MAX weight%. The addition of the calcium element not only can consume oxygen in the molten steel in the subsequent manufacturing process.
According to another aspect of the present invention, there is provided a method for manufacturing ultra-high purity clean steel, wherein the method for manufacturing high purity clean steel comprises the steps of:
s1, melting 4N9 pure iron raw materials;
s2, the ultra-high purity steel comprises the following components:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
and (3) adding high-purity nickel, 4N9 pure iron, high-purity molybdenum and high-purity chromium into the filtrate, and melting the added components by heating molten steel.
And (3) forging production verification:
1) Production equipment and auxiliary accessories: a 10 ton air hammer, a heat treatment device,
2) And (3) forging process control: the initial forging temperature of the ultra-pure clean steel is controlled at 1050 ℃, the final forging temperature is controlled at 960 ℃,
3) The following is the test performance of the die-casting test piece with different component proportions according to GBT228 standard test piece wire cutting, using a three-Si tensile machine and an inlet extensometer.
The aluminum alloys for high pressure casting of five examples were manufactured by the above manufacturing processes, respectively, and the properties thereof were examined, and the following table 1 is concrete.
TABLE 1
It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are by way of example only and are not limiting. The advantages of the present invention have been fully and effectively realized. The functional and structural principles of the present invention have been shown and described in the examples and embodiments of the invention may be modified or practiced without departing from the principles described.
Claims (10)
1. An ultra-high purity steel for use in the manufacture of semiconductors, the ultra-high purity steel comprising:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
the balance being iron.
2. The ultra-high purity clean steel for use in manufacturing semiconductors according to claim 1, wherein the ratio of the nickel content to the molybdenum content is: 6.0:1-6.14:1.
3. Ultra-high purity clean steel for use in the manufacture of semiconductors according to claim 1 or 2, characterized in that the ratio of chromium content to molybdenum content is: 6.8:1-7.2:1.
4. The ultra-high purity clean steel for use in manufacturing semiconductors as recited in claim 1, wherein the ultra-high purity clean steel comprises: 0.03 to 0.05 percent of manganese.
5. The ultra-high purity steel for manufacturing semiconductors according to claim 1, wherein the ultra-high purity steel comprises 0.012-0.015% phosphorus.
6. The ultra-high purity steel for manufacturing semiconductors according to claim 1, wherein the ultra-high purity steel comprises 0.0015 to 0.019% sulfur.
7. The manufacturing method of the ultra-high purity clean steel is characterized by comprising the following steps of:
s1, melting 4N9 pure iron raw materials;
s2, the ultra-high purity steel comprises the following components:
0.01MAX weight percent carbon;
0.15MAX weight percent silicon;
0.05MAX weight percent manganese;
0.02MAX weight percent phosphorus;
0.002MAX weight percent sulfur;
0.01MAX weight percent aluminum;
0.01MAX weight percent niobium;
0.01MAX weight percent titanium;
0.01MAX weight percent cesium;
0.01MAX weight percent calcium;
0.2MAX wt% copper;
14.50 to 15.00 weight percent nickel;
16.5 to 17.00 weight percent chromium;
2.20 to 2.50 wt% molybdenum;
and (3) adding high-purity nickel, 4N9 pure iron, high-purity molybdenum and high-purity chromium into the filtrate, and melting the added components by heating molten steel.
8. The method for manufacturing ultra-high purity steel for manufacturing semiconductors according to claim 7, wherein the ratio of the nickel content to the molybdenum content is: 6.0:1-6.14:1.
9. The method for manufacturing ultra-high purity steel for manufacturing semiconductors according to claim 7 or 8, wherein the ratio of chromium content to molybdenum content is: 6.8:1-7.2:1.
10. The method for manufacturing ultra-high purity steel for manufacturing semiconductors according to claim 7, wherein the ultra-high purity steel comprises: 0.03 to 0.05 percent of manganese.
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| CN118064790A (en) * | 2024-04-18 | 2024-05-24 | 浦夕特种合金(上海)有限公司 | Preparation method of ultra-pure steel for semiconductor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118064790A (en) * | 2024-04-18 | 2024-05-24 | 浦夕特种合金(上海)有限公司 | Preparation method of ultra-pure steel for semiconductor |
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