CN112921223B - Fe-containing soluble magnesium alloy and preparation method thereof - Google Patents
Fe-containing soluble magnesium alloy and preparation method thereof Download PDFInfo
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- CN112921223B CN112921223B CN202110142919.4A CN202110142919A CN112921223B CN 112921223 B CN112921223 B CN 112921223B CN 202110142919 A CN202110142919 A CN 202110142919A CN 112921223 B CN112921223 B CN 112921223B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
The invention relates to the technical field of metal materials and processing, in particular to a soluble magnesium alloy containing Fe and a preparation method thereof, wherein the alloy is Mg-Nd-Ce-Fe magnesium alloy and comprises the following elements in percentage by mass: 0.20 to 5.00 wt% of Nd, 0 to 2.00 wt% of Ce, 0.10 to 2.00 wt% of Fe, and the balance of Mg and inevitable impurity elements. The magnesium alloy material can be prepared by casting, extruding and other modes, and the effective regulation and control of the tissue and the components of the material are realized; and also has good mechanical properties and a uniform and stable dissolution rate.
Description
Technical Field
The invention relates to the technical field of metal materials and processing, in particular to a soluble magnesium alloy containing Fe and a preparation method thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the exhaustion of traditional oil and gas resources, shale oil and gas gradually become an important direction for the development of the energy field in the current and future period of time, and have high development prospect and economic value, and related mining technologies have been successful in the United states-6 months in 2019, and the United states surpasses Saudi once and becomes the largest oil export country in the world. According to statistics, the reserves of shale gas and shale oil in China are in the forefront of the world, and the future development prospect is wide. However, related mining technologies are still in a starting price stage, and currently, the mainstream horizontal well mining technology is a staged fracturing technology. One key component of the technology is the fracturing tool, including a temporary plugging ball, a ball seat, a bridge plug, a sliding sleeve and the like. The tool has solubility and good mechanical property in the fracturing process.
Soluble materials commonly used are polymeric materials, aluminum alloys and magnesium alloys. Wherein, the soluble magnesium alloy is mostly added with Cu, Ni, Fe and other elements on the basis of Mg-Zn system, Mg-Al system and Mg-RE system to form a cathode phase, and the rapid dissolution in the water solution is realized through galvanic corrosion. At present, the magnesium alloy containing Cu and Ni can be used for preparing related parts by the traditional casting, hot extrusion, heat treatment and other modes, and the soluble magnesium alloy containing Fe is prepared by adopting a powder metallurgy mode mostly. The reasons are two: firstly, Mg-Fe intermediate alloy is not seen in the market, and the melting point of Fe is high, so that the solubility of Fe in magnesium alloy melt is low in the smelting process, and the Mg-Fe intermediate alloy is difficult to add; and secondly, Fe is easy to form a second phase with various elements such as Al, Zn, Cu, Ni, Mn, Si and the like, so that the size and distribution of the Fe-containing cathode phase are not easy to control, and the product performance is unstable. In addition, for magnesium alloys, Fe has a similar grain refining effect as Zr element. Therefore, reasonably designing the components of the magnesium alloy containing Fe and the adding mode of the Fe element and regulating the distribution of the Fe element in the magnesium alloy are important technical problems. The method solves the problem, is expected to promote the development of high-performance soluble magnesium alloy materials and improve the technical level of shale oil and gas exploitation in China.
Disclosure of Invention
The disclosure provides an Fe-containing soluble magnesium alloy and a preparation method thereof, aiming at the defects of the existing Fe-containing soluble magnesium alloy prepared by a powder metallurgy method. The magnesium alloy material can be prepared by casting, extruding and other modes, and the effective regulation and control of the tissue and the components of the material are realized; and also has good mechanical properties and a uniform and stable dissolution rate.
Specifically, the technical scheme of the present disclosure is as follows:
in a first aspect of the present disclosure, there is provided a Fe-containing soluble magnesium alloy, which is a Mg-Nd-Ce-Fe magnesium alloy, composed of the following elements by mass percent: 0.20 to 5.00 wt% of Nd, 0 to 2.00 wt% of Ce, 0.10 to 2.00 wt% of Fe, and the balance of Mg and inevitable impurity elements.
In a second aspect of the present disclosure, the present disclosure provides a method for preparing an Fe-containing soluble magnesium alloy, comprising:
weighing pure magnesium ingots, Mg-Nd intermediate alloy, Mg-Ce intermediate alloy, pure iron powder or iron oxide powder according to the weight percentage of the Fe-containing soluble magnesium alloy; under the protection of argon, smelting a pure magnesium ingot, an Mg-Nd intermediate alloy and an Mg-Ce intermediate alloy, refining and deslagging, adding pure iron powder or ferric oxide powder, and simultaneously casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; and (5) aging treatment.
In a third aspect of the disclosure, the disclosure provides a use of an Fe-containing soluble magnesium alloy and/or a method of making an Fe-containing soluble magnesium alloy in the preparation of a fracturing tool for shale oil and gas exploration.
One or more technical schemes in the disclosure have the following beneficial effects:
(1) according to the Mg-Nd-Ce-Fe magnesium alloy disclosed by the invention, the grain size of an ingot can be refined by adding light rare earth elements Nd and Ce, and the ingot segregation is reduced; in addition, Nd and Ce can not form a second phase with Fe, so that the existence of Fe simple substance in the alloy can be ensured, and the refinement and the solubility property stability of the ingot casting structure are ensured to a certain extent.
(2) Compared with a powder metallurgy method, the Mg-Nd-Ce-Fe magnesium alloy disclosed by the invention is prepared by a fusion casting method, and internal pores of the material are eliminated, so that the mechanical property of the material is obviously improved.
(3) The material disclosed by the invention does not have a low-temperature phase, so that the high-temperature resistance of the material is better, and the material does not crack in a high-temperature thermal deformation process.
(4) In the preparation process of the material disclosed by the invention, pure iron powder or ferric oxide is added in the form of a refiner, and more Fe is added compared with the traditional smelting method, so that the material has a stable corrosion rate in a low-salt environment.
(5) As Nd has 3.6 wt% solid solubility in the magnesium alloy, the material prepared by the method can be strengthened by heat treatment, so that the regulation and control range of the mechanical property of the material is large, and the requirements of various environments can be met.
(6) The Fe-containing soluble magnesium alloy prepared by the method has the tensile strength of 260-380 MPa, the elongation of 14-30% and a good dissolution rate in a high-salt or low-salt environment at 93 ℃.
Detailed Description
The disclosure is further illustrated with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or starting materials used in the present invention can be purchased from conventional sources, and unless otherwise specified, the reagents or starting materials used in the present invention can be used in a conventional manner in the art or in accordance with the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the present disclosure provides a soluble magnesium alloy containing Fe and a method for preparing the same, in order to solve the above problems, the present disclosure provides a soluble magnesium alloy containing Fe and a method for preparing the same, in which the solubility in a magnesium alloy solution is low due to a high melting point of Fe, which makes it difficult to prepare an Mg — Fe master alloy, and the size and distribution of a cathode phase containing Fe are not easily controlled, which leads to unstable product performance.
In one embodiment of the present disclosure, there is provided a Fe-containing soluble magnesium alloy, which is a Mg-Nd-Ce-Fe magnesium alloy, composed of the following elements by mass percent: 0.20 to 5.00 wt% of Nd, 0 to 2.00 wt% of Ce, 0.10 to 2.00 wt% of Fe, and the balance of Mg and inevitable impurity elements.
Further, the Fe-containing soluble magnesium alloy consists of the following elements in percentage by mass: 0.20 to 3.70 wt% of Nd, 0.50 to 1.00 wt% of Ce, 0.50 to 2.00 wt% of Fe, and the balance of Mg and inevitable impurity elements.
Further, the Fe-containing soluble magnesium alloy consists of the following elements in percentage by mass: 3.60 wt% of Nd, 1.00 wt% of Ce, 1.50 wt% of Fe, and the balance of Mg and inevitable impurity elements.
The Fe element can not form a second phase with the magnesium, so the Fe element has obvious effect of refining grains. In order to fully play the role of heterogeneous nucleation of Fe simple substances and avoid the addition of elements forming a second phase with Fe, Nd and Ce elements are added, belong to light rare earth elements, and have lower cost compared with heavy rare earth. The high-melting-point second phase formed by Nd and Ce and Mg also has the function of refining grains.
In one embodiment of the present disclosure, there is provided a method for preparing an Fe-containing soluble magnesium alloy, including:
weighing pure magnesium ingots, Mg-Nd intermediate alloy, Mg-Ce intermediate alloy, pure iron powder or iron oxide powder according to the weight percentage of the Fe-containing soluble magnesium alloy; under the protection of argon, smelting a pure magnesium ingot, an Mg-Nd intermediate alloy and an Mg-Ce intermediate alloy, refining and deslagging, adding pure iron powder or ferric oxide powder, and simultaneously casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; and (5) aging treatment.
The solubility of Fe in magnesium alloy melt is low, so that the preparation by the conventional smelting process is difficult. The present disclosure adds pure iron powder or iron oxide powder in the form of a refiner to the magnesium alloy solution prior to casting. Wherein, the ferric oxide and the magnesium are subjected to magnesium thermal reaction to produce Fe simple substance and magnesium oxide, and release heat. The released heat can raise the temperature of local magnesium alloy melt, and further improve the solubility of Fe. Fe simple substance is gradually precipitated and sunk along with the casting, thereby achieving the purpose of refining grains. Magnesium oxide, which has a low density, floats to the surface of the magnesium melt and forms slag.
Further, the concrete steps of smelting and casting into an ingot are as follows: under the condition of argon protection, smelting a pure magnesium ingot, an Mg-Nd intermediate alloy and an Mg-Ce intermediate alloy at 720-760 ℃, preserving heat for 40-60 min, and stirring for 5-10 min; refining for 20-30 min, heating to 740-780 ℃ after refining, standing for 30-40 min, adding iron oxide powder at 720-740 ℃, and casting into a semi-continuous ingot.
Further, homogenizing at 500-540 ℃ for 1-16 h, cooling by air cooling, cutting into corresponding blanks, and peeling; preferably, the homogenization treatment condition is that the homogenization treatment is carried out at 520 ℃ for 8 h.
Further, the specific conditions of the extrusion are as follows: the extrusion temperature is 380-460 ℃, the extrusion ratio is 4-10, and the extrusion speed is 0.1-10 m/min; more preferably, the extrusion temperature is 400 ℃, the extrusion ratio is 8, and the extrusion speed is 5 m/min.
Further, the specific conditions of the aging treatment are as follows: keeping the temperature for 1-48h at 150-200 ℃.
In one embodiment of the disclosure, there is provided a use of an Fe-containing soluble magnesium alloy and/or a method of making an Fe-containing soluble magnesium alloy in the preparation of a fracturing tool for shale oil and gas exploration.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific embodiments.
Example 1
The Fe-containing soluble magnesium alloy is Mg-Nd-Ce-Fe magnesium alloy and consists of the following elements in percentage by mass: 3.60 wt% of Nd, 1.00 wt% of Ce, 1.50 wt% of Fe, and the balance of Mg and inevitable impurity elements.
The preparation process comprises the following steps: weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Nd intermediate alloy, Mg-30% Ce intermediate alloy and ferric oxide powder;
under the protection of argon, smelting the pure magnesium ingot, the Mg-Nd intermediate alloy and the Mg-Ce intermediate alloy at 740 ℃, preserving heat for 50min, and stirring for 10 min; refining for 30min, heating to 780 ℃, standing for 40min after refining, adding iron oxide powder at 740 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 540 ℃ for 6h, cooling by air cooling, cutting into corresponding blanks, and peeling;
extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 420 ℃, the extrusion ratio is 8 and the extrusion speed is 5 m/min; aging at 180 deg.C for 7 h.
Example 2
The Fe-containing soluble magnesium alloy is Mg-Nd-Ce-Fe magnesium alloy and consists of the following elements in percentage by mass: nd 5.0 wt%, Ce 2.00 wt%, Fe 2.0 wt%, and Mg and inevitable impurity elements in balance.
Weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Nd intermediate alloy, Mg-30% Ce intermediate alloy and pure iron powder;
under the protection of argon, smelting the pure magnesium ingot, the Mg-Nd intermediate alloy and the Mg-Ce intermediate alloy at 760 ℃, preserving heat for 60min, and stirring for 5 min; refining for 20min, heating to 780 ℃, standing for 30min after refining, adding pure iron powder at 740 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 540 ℃ for 8h, cooling by air cooling, cutting into corresponding blanks, and peeling;
extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 460 ℃, the extrusion ratio is 4 and the extrusion speed is 2 m/min; aging at 170 deg.C for 10 h.
Example 3
The Fe-containing soluble magnesium alloy is Mg-Nd-Ce-Fe magnesium alloy and consists of the following elements in percentage by mass: 0.2 wt% of Nd, 1.00 wt% of Ce, 0.5 wt% of Fe, and the balance of Mg and inevitable impurity elements.
Weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Nd intermediate alloy, Mg-30% Ce intermediate alloy and ferric oxide powder;
under the protection of argon, smelting the pure magnesium ingot, the Mg-Nd intermediate alloy and the Mg-Ce intermediate alloy at 740 ℃, preserving heat for 40min, and stirring for 5 min; refining for 30min, heating to 760 ℃, standing for 35min, adding iron oxide powder at 750 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 500 ℃ for 3h, cooling by air cooling, cutting into corresponding blanks, and peeling;
and extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 400 ℃, the extrusion ratio is 10 and the extrusion speed is 0.5 m/min.
Example 4
The Fe-containing soluble magnesium alloy is Mg-Nd-Fe magnesium alloy and consists of the following elements in percentage by mass: 1.0 wt% of Nd, 0.2 wt% of Fe, and the balance of Mg and inevitable impurity elements.
Weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Nd intermediate alloy and ferric oxide powder;
under the protection of argon, smelting the pure magnesium ingot and the Mg-Nd intermediate alloy at 740 ℃, preserving heat for 40min, and stirring for 8 min; refining for 30min, heating to 760 ℃, standing for 30min, adding iron oxide powder at 750 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 500 deg.C for 2h, cooling by air cooling, cutting into corresponding blanks, and peeling;
and extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 400 ℃, the extrusion ratio is 10 and the extrusion speed is 0.5 m/min.
Comparative example 1
The difference from example 1 is that the fusion casting process is different in the alloy preparation method. The method specifically comprises the following steps:
weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Nd intermediate alloy, Mg-30% Ce intermediate alloy and pure iron powder;
under the protection of argon, smelting the pure magnesium ingot, the Mg-Nd intermediate alloy, the Mg-Ce intermediate alloy and the pure iron powder at 740 ℃, preserving heat for 50min, and stirring for 10 min; refining for 30min, heating to 780 deg.C, standing for 40min, and casting at 740 deg.C to obtain semi-continuous ingot.
Comparative example 2
The Mg-Gd-Y-Fe magnesium alloy consists of the following elements in percentage by mass: 5.0 wt% of Gd, 2.00 wt% of Y, 2.0 wt% of Fe, and the balance of Mg and inevitable impurity elements.
Weighing the following raw materials in proportion: pure magnesium ingot, Mg-30% Gd intermediate alloy, Mg-30% Y intermediate alloy, iron oxide powder;
under the protection of argon, smelting the pure magnesium ingot, the Mg-Gd intermediate alloy and the Mg-Y intermediate alloy at 760 ℃, preserving heat for 60min, and stirring for 5 min; refining for 20min, heating to 780 ℃, standing for 30min after refining, adding iron oxide powder at 740 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 540 ℃ for 8h, cooling by air cooling, cutting into corresponding blanks, and peeling;
extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 460 ℃, the extrusion ratio is 4 and the extrusion speed is 2 m/min; aging at 170 deg.C for 10 h.
Comparative example 3
The Mg-Nd-Ce-Al-Mn-Fe magnesium alloy consists of the following elements in percentage by mass: 0.2 wt% of Nd, 1.00 wt% of Ce, 3 wt% of Al, 1.00 wt% of Mn, 0.5 wt% of Fe and the balance of Mg and inevitable impurity elements.
Weighing the following raw materials in proportion: pure magnesium ingot, pure aluminum ingot, Mg-30% Nd intermediate alloy, Mg-30% Ce intermediate alloy, Mg-10% Mn intermediate alloy, iron oxide powder;
under the protection of argon, smelting the pure magnesium ingot, the pure aluminum ingot, the Mg-Nd intermediate alloy, the Mg-Ce intermediate alloy and the Mg-Mn intermediate alloy at 740 ℃, preserving heat for 40min, and stirring for 5 min; refining for 30min, heating to 760 ℃, standing for 35min, adding iron oxide powder at 750 ℃, and casting into a semi-continuous ingot;
homogenizing the cast ingot at 500 ℃ for 3h, cooling by air cooling, cutting into corresponding blanks, and peeling;
and extruding the blank obtained in the last step into a bar under the conditions that the extrusion temperature is 400 ℃, the extrusion ratio is 10 and the extrusion speed is 0.5 m/min.
Comparative example 4
The difference from example 4 is that the alloy composition is different-Fe element is not contained. The alloy consists of the following elements in percentage by mass: nd 1.0 wt%, and Mg and inevitable impurity elements as the rest.
The mechanical properties and dissolution properties of the alloys of examples 1-4 and comparative examples 1-4 are shown in table 1, and the mechanical property test method was performed according to GB T228.1-2010; the solubility was 93 ℃ and 3% KCl aqueous solution (high salt solution) and 93 ℃ and 0.1% KCl aqueous solution (low salt solution), respectively.
TABLE 1 magnesium alloy room temperature mechanical properties and 93 ℃ dissolution rate
Comparing the examples with the comparative examples it can be seen that: the Fe-containing soluble magnesium alloy prepared by the method has the tensile strength of 260-380 MPa, the elongation of 14-30% and a good dissolution rate in a high-salt or low-salt environment at 93 ℃.
As can be seen from the above specific case comparison, the comparative examples 1-4 are different from the examples 1-4 in preparation process or chemical composition, respectively, and the mechanical properties and dissolution rate of the comparative example preparation material are significantly reduced.
In summary, the soluble magnesium alloy material containing Fe prepared by the method disclosed by the disclosure has good mechanical properties and good solubility in high-salt and low-salt environments, and can meet the requirements of soluble magnesium alloy parts required by shale oil and gas development.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of Fe-containing soluble magnesium alloy is characterized by comprising the following steps: weighing pure magnesium ingots, Mg-Nd intermediate alloy, Mg-Ce intermediate alloy, pure iron powder or iron oxide powder according to the weight percentage of the Fe-containing soluble magnesium alloy; under the protection of argon, smelting a pure magnesium ingot, an Mg-Nd intermediate alloy and an Mg-Ce intermediate alloy, refining and deslagging, adding pure iron powder or ferric oxide powder, and simultaneously casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; aging treatment; the Fe-containing soluble magnesium alloy: the alloy is Mg-Nd-Ce-Fe magnesium alloy and consists of the following elements in percentage by mass: 0.20 to 3.70 wt% of Nd0.50 to 1.00 wt% of Ce0.50 to 1.00 wt% of Fe0.50 to 2.00 wt% of the balance of Mg and inevitable impurity elements;
wherein, the specific conditions of the hot extrusion are as follows: the extrusion temperature is 380-460 ℃, the extrusion ratio is 4-10, and the extrusion speed is 0.1-10 m/min;
the specific conditions of the aging treatment are as follows: keeping the temperature for 1-48h at 150-200 ℃.
2. The method for preparing the Fe-containing soluble magnesium alloy as set forth in claim 1, wherein the Fe-containing soluble magnesium alloy: the material consists of the following elements in percentage by mass: nd3.60wt%, Ce1.00wt% and Fe1.50wt%, and the balance of Mg and inevitable impurity elements.
3. The method for preparing the Fe-containing soluble magnesium alloy according to claim 1, wherein the steps of smelting and casting into an ingot are as follows: under the condition of argon protection, smelting a pure magnesium ingot, an Mg-Nd intermediate alloy and an Mg-Ce intermediate alloy at 720-760 ℃, preserving heat for 40-60 min, and stirring for 5-10 min; refining for 20-30 min, heating to 740-780 ℃ after refining, standing for 30-40 min, adding pure iron powder or ferric oxide powder at 720-740 ℃, and casting into a semi-continuous ingot.
4. The method for preparing the Fe-containing soluble magnesium alloy as claimed in claim 1, wherein the homogenizing treatment is carried out at 500-540 ℃ for 1-16 h, the cooling is air cooling, and then the alloy is cut into corresponding blanks and peeled.
5. The method of claim 1, wherein the homogenization treatment is carried out at 520 ℃ for 8 hours.
6. The method of claim 1, wherein the hot extrusion is performed at an extrusion temperature of 400 ℃, an extrusion ratio of 8, and an extrusion speed of 5 m/min.
7. Use of the method of any one of claims 1 to 6 for the preparation of a fracturing tool for shale oil and gas exploration.
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