CN114717456A - High-temperature soluble aluminum alloy, preparation method and application - Google Patents

Abstract

The invention discloses a high-temperature soluble aluminum alloy, a preparation method and use thereof. The composition of each element of the aluminum alloy is calculated by weight percentage: Mg 1.5wt%, Ga 0.1wt%, In 0.7wt%, Sn 0.6wt%, the balance For Al and inevitable impurity elements. The soluble aluminum alloy is obtained by smelting each component and then performing heat treatment and aging treatment after ingot casting. The soluble aluminum alloy material can be used as the material of the fracturing tool used for shale oil and gas development. The soluble aluminum alloy prepared by the invention has controllable dissolution and good mechanical properties and dissolution rate in a high temperature environment.

Description

A kind of high temperature soluble aluminum alloy, preparation method and use

technical field

The invention belongs to the technical field of alloy preparation, in particular to a high-temperature soluble aluminum alloy, a preparation method and an application.

Background technique

In the oil and gas exploration in recent years, my country has abundant unconventional oil and gas resources, among which the reserves of shale gas and shale oil rank among the top in the world. Relying on hydraulic fracturing and other technologies, the development of bridge plugs is one of the most important technologies in multi-layer and multi-stage fracturing technology. Tools made of soluble materials can dissolve in the underground environment by themselves after completing the operation, eliminating the need for manual drilling, grinding and recycling processes, reducing engineering risks and improving construction efficiency.

The expansion ring is a component that can fix objects by expanding and contracting. Because the expansion ring has a simple structure and easy disassembly and assembly operations, it is widely used in mechanical parts in many industries.

my country's aluminum alloy production is abundant, and has low density, high specific strength and excellent electrical conductivity, thermal conductivity and corrosion resistance, and at the same time its plasticity is good, can be processed into various profiles, widely used in aviation, aerospace, automobiles, ships, etc. field. When the soluble aluminum alloy all-metal bridge plug expansion ring is used in a high temperature environment, due to the poor high temperature resistance of ordinary soluble aluminum alloys, the mechanical properties such as tensile strength and hardness of the material are reduced. The aluminum alloy has an accelerated dissolution rate and poor controllability. It cannot provide the mechanical index requirements required for work and the effective time required to complete the operation, which limits its application range. Therefore, the rational design of the element ratio and process parameters of high-temperature soluble aluminum alloy materials is an important technical problem. Solving this problem is expected to promote the development of high-temperature and high-performance soluble aluminum alloy materials, and improve my country's shale oil and gas. The technical level of unconventional energy mining.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a high temperature soluble aluminum alloy, preparation method and application. High temperature soluble aluminum alloy materials can be prepared by melting casting, hot extrusion, heat treatment, etc., which realizes the controlled degradation of soluble aluminum alloy materials in high temperature environment, and also has good mechanical properties and stable dissolution in high temperature environment. rate.

In order to achieve the above purpose, the technical solution adopted in the present invention is a high-temperature soluble aluminum alloy material. The composition of each element is calculated by weight percentage: Mg 1.5wt%, Ga 0.1wt%, In 0.7wt%, Sn 0.6wt%, and the rest The amount is Al and inevitable impurity elements.

Preferably, the tensile strength of the high temperature soluble aluminum alloy is 120-140 MPa, and the elongation is 25-30%.

The present invention also provides a preparation method of high temperature soluble aluminum alloy, comprising the following steps:

Step 1), each element is weighed according to the proportion by weight, Mg is introduced with Al-Mg master alloy, Ga is introduced with Al-Ga master alloy, In is introduced with Al-In master alloy, Sn is introduced with Al-Sn master alloy, Insufficient Al is introduced with pure aluminum ingots;

Step 2), smelting and casting: under the protection of argon, pure aluminum is first melted, and when the temperature of the melt reaches 715-735 ° C, Al-Mg master alloy, Al-Ga master alloy, Al- In master alloy and Al-Sn master alloy are smelted; heated to 850-900°C and kept for 1-2 hours, all melted and then refined, and the obtained aluminum alloy liquid was kept at 850-870°C for 5-10 minutes Rapidly cool down 50-80°C at 5-8°C/s, then heat up to 850-870°C, keep warm for 30-40 minutes, and cast at constant temperature; the molten liquid is cast in the mold, and rapidly cooled to 300°C, after cooling, the temperature is 300°C. -400 ℃ for 7-8 hours to obtain aluminum alloy ingots;

Step 3) Hot extrusion treatment: the ingot is made into a bar by hot extrusion;

Step 4) Solution heat treatment: keep at 440°C for 1-2h, and then keep at 500°C for 1-2h;

Step 5) Aging treatment: keep the temperature at 80° C. for 8-12 hours, and air-cool to room temperature.

Preferably, in step 2), an impurity remover is added to remove impurities and refine, and the impurities remover is composed of sodium fluoride, sodium chloride, potassium chloride, and the mass ratio is 1:1:1; the addition amount of the impurity remover is the melt 2-3% of the total mass.

Preferably, in step 2), adding a slag agent to remove slag, the slag agent is aluminum titanium boron wire, and the components of the aluminum titanium boron wire are, in mass percentage, Ti 4.5-5.5%, B0.8-1.0 %, the remainder is Al, of which impurities: Si < 0.20%, Fe < 0.30%, V < 0.25%, other elements < 0.03%, the total content of impurity elements < 0.10%; the amount of slag agent added is 2 of the total mass of the melt -3%.

Preferably, in step 4), the extrusion temperature is 380-420°C, the extrusion ratio is 10-20, and the extruded aluminum alloy is kept at 150°C for 7-8 hours.

The invention also provides the use of a high temperature soluble aluminum alloy in preparing a fracturing tool for shale oil and gas exploitation. Such as all-metal bridge plug expansion ring.

Compared with the traditional soluble aluminum alloy, the soluble aluminum alloy prepared by the present invention has the following beneficial effects:

(1) The high temperature soluble aluminum alloy of the present invention can refine the grain size of the ingot through the addition of elements Ga, In and Sn, reduce the segregation of the ingot, and ensure the refinement of the ingot structure and stable solubility to a certain extent. sex. At the same time, a refiner is added to further refine the grain size of the ingot.

(2) The high-temperature soluble aluminum alloy of the present invention is prepared by the melting and casting method. Compared with the powder metallurgy method, the internal pores of the material are eliminated, thereby significantly improving the mechanical properties of the material.

(3) There is no low temperature phase in the soluble aluminum alloy material of the present invention, and the high temperature resistance performance is good.

(4) The high temperature soluble aluminum alloy prepared by the present invention has a tensile strength of 120-140 MPa, an elongation of 25-30%, and a good dissolution rate in a high temperature environment of 90°C.

Detailed ways

The reagents or raw materials used in the present invention can be obtained commercially. Unless otherwise specified, the reagents or raw materials used in the present invention are used in a conventional manner in the art or in accordance with product instructions.

The high-temperature soluble aluminum alloy used in the present invention is composed of elements by weight percentage: Mg 1.5wt%, Ga0.1wt%, In 0.7wt%, Sn 0.6wt%, and the balance is Al and inevitable impurity elements.

The preparation method of the high temperature soluble aluminum alloy of the present invention comprises the following steps:

Step 1), each element is weighed according to the weight percentage ratio of each component of the above-mentioned soluble aluminum alloy, Mg is introduced with Al-Mg master alloy, Ga is introduced with Al-Ga master alloy, and In is introduced with Al-In master alloy , Sn is introduced by Al-Sn master alloy, and insufficient AL is introduced by pure aluminum ingot;

Step 2), under the protection of argon gas, first melt pure aluminum, and when the temperature of the molten metal reaches 715-735 ° C, add Al-Mg master alloy, Al-Ga master alloy, and Al-In master alloy to the aluminum liquid in turn. , Al-Sn master alloy is smelted; heated to 850-900 ℃ and kept for 1-2 hours, all melted and then refined, and the obtained aluminum alloy liquid was kept at 850-870 ℃ for 5-10 minutes and then 5- 8°C/s to rapidly cool down to 50-80°C, then heat up to 850-870°C, keep warm for 30-40 minutes, and cast at constant temperature; the melt is cast in the mold, and rapidly cooled to 300°C, and then cooled to 300-400°C Under heat preservation for 7-8 hours to obtain aluminum alloy ingots;

Add impurity remover to remove impurities and refine, and the ingredients of impurity remover are sodium fluoride, sodium chloride and potassium chloride, and the mass ratio is 1:1:1; the added amount of impurity remover is 2-3% of the total mass of the melt.

Add a slag agent to remove slag, the slag agent is aluminum titanium boron wire, and the components of the aluminum titanium boron wire are, in terms of mass percentage, Ti4.5-5.5%, B0.8-1.0%, and the rest is Al, among which impurities : Si < 0.20%, Fe < 0.30%, V < 0.25%, other elements < 0.03%, the total content of impurity elements < 0.10%; the amount of slagging agent added is 2-3% of the total mass of the melt.

Step 3) Hot extrusion treatment: the extrusion temperature is 380-420°C, the extrusion ratio is 10-20, the extruded aluminum alloy is kept at 150°C for 7-8 hours, and the ingot is made by hot extrusion. bar;

Step 4) Solution heat treatment: keep at 440°C for 1-2h, and then keep at 500°C for 1-2h;

Step 5) Aging treatment: keep the temperature at 80° C. for 8-12 hours, and air-cool to room temperature.

Below, some preferred embodiments are given for detailed description.

Example 1

High temperature soluble aluminum alloy, in weight percent, each element composition: Mg 1.5wt%, Ga 0.1wt%, In0.7wt%, Sn 0.6wt%, the balance is Al and inevitable impurity elements.

Its preparation method is as follows:

Step 1), weighing raw materials according to the above-mentioned proportions: weighing pure aluminum ingot, Al-Mg master alloy, Al-Ga master alloy, Al-In master alloy, and Al-Sn master alloy.

After weighing the raw material, sand the surface of the raw material to remove the surface oxide layer.

Step 2), smelting and casting: first place pure aluminum in a graphite crucible for heating and melting, and use argon gas protection during the melting process. After all the pure aluminum is melted, the temperature of the melt is raised to 715 ° C and each master alloy is added, and the temperature is continued to 850 ℃ and hold for 2 hours, confirm that all melting is carried out for refining treatment; after the aluminum alloy melt is kept at 850 ℃ for 10 minutes, it is rapidly cooled by 50 ℃ at 5 ℃/s, and then heated to 850 ℃, and the temperature is maintained for 40 minutes. Casting; the molten liquid is cast in the mold, and rapidly cooled to 300°C, and then kept at 300°C for 8 hours after cooling to obtain an aluminum alloy ingot;

Refining treatment: adding impurity remover to remove impurities and refining, the ingredients of impurity remover are sodium fluoride, sodium chloride, potassium chloride, the mass ratio is 1:1:1; the addition amount of impurity remover is 2% of the total mass of the melt.

Add slag agent to remove slag, the slag agent is aluminum titanium boron wire, the composition of aluminum titanium boron wire is, in terms of mass percentage, Ti4.5%, B1.0%, and the rest is Al, wherein impurities: Si<0.20 %, Fe < 0.30%, V < 0.25%, other elements < 0.03%, the total content of impurity elements < 0.10%; the amount of slagging agent added is 3% of the total mass of the melt.

Step 3) Hot extrusion treatment: the extrusion temperature is 420°C, the extrusion ratio is 20, the extruded aluminum alloy is kept at 150°C for 7 hours, and the ingot is made into a bar by hot extrusion;

Step 4) Solution heat treatment: keep at 440°C for 1 hour, and then keep at 500°C for 1 hour;

Step 5) Aging treatment: keeping at 80° C. for 8 hours, and air-cooled to room temperature.

The high temperature soluble aluminum alloy obtained through the above steps was tested, and the room temperature tensile strength was 130MPa, the elongation was 27.5%, and in the high temperature environment of 90 °C, the 3% KCl solution had a good dissolution rate.

Example 2

High temperature soluble aluminum alloy, in weight percent, each element composition: Mg 1.5wt%, Ga 0.1wt%, In0.7wt%, Sn 0.6wt%, the balance is Al and inevitable impurity elements.

Its preparation method is as follows:

Step 1), weighing raw materials according to the above-mentioned proportions: weighing pure aluminum ingot, Al-Mg master alloy, Al-Ga master alloy, Al-In master alloy, and Al-Sn master alloy.

After weighing the raw material, sand the surface of the raw material to remove the surface oxide layer.

Step 2), smelting and casting: first place pure aluminum in a graphite crucible for heating and melting, and use argon protection during the melting process. After all the pure aluminum is melted, the temperature of the melt is raised to 735 ° C and each master alloy is added, and the temperature is continued to 900 ℃ and hold for 1 hour, confirm that all melting is carried out for refining; after the aluminum alloy melt is kept at 870 ℃ for 5 minutes, it is rapidly cooled to 80 ℃ at 8 ℃/s, and then heated to 870 ℃ and kept for 30 minutes, and then constant temperature casting is carried out. ; The molten liquid is cast in the mold, and rapidly cooled to 300°C, and then kept at 350°C for 7.5 hours to obtain an aluminum alloy ingot;

Refining treatment: adding impurity remover to remove impurities and refining, the ingredients of impurity remover are sodium fluoride, sodium chloride, potassium chloride, the mass ratio is 1:1:1; the addition amount of impurity remover is 3% of the total mass of the melt.

Add slag agent to remove slag, the slag agent is aluminum-titanium-boron wire, and the components of aluminum-titanium-boron wire are, in mass percentage, Ti5.5%, B0.8%, and the rest is Al, wherein impurities: Si<0.20 %, Fe < 0.30%, V < 0.25%, other elements < 0.03%, the total content of impurity elements < 0.10%; the amount of slagging agent added is 2% of the total mass of the melt.

Step 3) Hot extrusion treatment: the extrusion temperature is 400°C, the extrusion ratio is 15, the extruded aluminum alloy is kept at 150°C for 7 hours, and the ingot is made into a bar by hot extrusion;

Step 4) Solution heat treatment: keep at 440°C for 1.5h, and then keep at 500°C for 1.5h;

Step 5) Aging treatment: heat preservation at 80° C. for 10 hours, and air-cool to room temperature.

The high temperature soluble aluminum alloy obtained by the above steps was tested, and the room temperature tensile strength was 140MPa, the elongation was 30%, and in the high temperature environment of 90 °C, the 3% KCl solution had a good dissolution rate.

Example 3

High temperature soluble aluminum alloy, in weight percent, each element composition: Mg 1.5wt%, Ga 0.1wt%, In0.7wt%, Sn 0.6wt%, the balance is Al and inevitable impurity elements.

Its preparation method is as follows:

Step 1), weighing raw materials according to the above-mentioned proportions: weighing pure aluminum ingot, Al-Mg master alloy, Al-Ga master alloy, Al-In master alloy, and Al-Sn master alloy.

After weighing the raw material, sand the surface of the raw material to remove the surface oxide layer.

Step 2), smelting and casting: first place pure aluminum in a graphite crucible for heating and melting, and use argon gas protection during the melting process. After all the pure aluminum is melted, the melt temperature is raised to 725 ° C and each intermediate alloy is added, and the temperature is continued to rise to 880 ℃ and hold for 2 hours, confirm that all melting is carried out for refining; after the aluminum alloy melt is kept at 860 ℃ for 10 minutes, it is rapidly cooled by 70 ℃ at 7 ℃/s, and then heated to 865 ℃, and the temperature is kept for 40 minutes, and the constant temperature is carried out. Casting; the molten liquid is cast in a mold, and rapidly cooled to 300°C, and then kept at 400°C for 7 hours to obtain an aluminum alloy ingot;

Refining treatment: adding impurity remover to remove impurities and refining, the ingredients of impurity remover are sodium fluoride, sodium chloride, potassium chloride, the mass ratio is 1:1:1; the addition amount of impurity remover is 2.5% of the total mass of the melt.

Add slag agent to remove slag, the slag agent is aluminum titanium boron wire, the components of aluminum titanium boron wire are, in terms of mass percentage, Ti5%, B0.9%, and the rest is Al, wherein impurities: Si<0.20%, Fe < 0.30%, V < 0.25%, other elements < 0.03%, the total content of impurity elements < 0.10%; the amount of slag agent added is 2.5% of the total mass of the melt.

Step 3) Hot extrusion treatment: the extrusion temperature is 380°C, the extrusion ratio is 10, the extruded aluminum alloy is kept at 150°C for 8 hours, and the ingot is made into a bar by hot extrusion;

Step 4) Solution heat treatment: keep at 440°C for 2 hours, and then keep at 500°C for 2 hours;

Step 5) Aging treatment: keep the temperature at 80° C. for 12 hours, and air-cool to room temperature.

The high temperature soluble aluminum alloy obtained by the above steps was tested, and the room temperature tensile strength was 120MPa, the elongation was 25%, and in the high temperature environment of 90°C, the 3% KCl solution had a good dissolution rate.

It can be seen from the above that the high temperature soluble aluminum alloy prepared by the present invention has a tensile strength of 120-140 MPa, an elongation of 25-30%, and a good dissolution rate in a 3% KCl solution in a high temperature environment of 90°C. The controlled dissolution of the material when used in a high temperature environment is achieved, and it also has good mechanical properties and a stable dissolution rate in a high temperature environment.

The high-temperature soluble aluminum alloy prepared by the invention can be used for making fracturing tools for shale oil and gas development, such as all-metal bridge plug expansion rings.

Claims (7)

1. A high temperature soluble aluminum alloy material, each element composition, in weight percentage: Mg 1.5wt%, Ga 0.1wt%, In 0.7wt%, Sn 0.6wt%, the balance is Al and inevitable impurity elements . 2 . The high temperature soluble aluminum alloy according to claim 1 , wherein the tensile strength of the high temperature soluble aluminum alloy is 120-140 MPa, and the elongation is 25-30%. 3 . 3. the preparation method of the arbitrary described high temperature soluble aluminum alloy of claim 1 or 2, comprises the following steps: Step 1), each element is weighed according to the proportion by weight, Mg is introduced with Al-Mg master alloy, Ga is introduced with Al-Ga master alloy, In is introduced with Al-In master alloy, Sn is introduced with Al-Sn master alloy, Insufficient Al is introduced with pure aluminum ingots; Step 2), smelting and casting: under the protection of argon, pure aluminum is first melted, and when the temperature of the melt reaches 715-735 ° C, Al-Mg master alloy, Al-Ga master alloy, Al- In master alloy and Al-Sn master alloy are smelted; heated to 850-900°C and kept for 1-2 hours, all melted and then refined, and the obtained aluminum alloy liquid was kept at 850-870°C for 5-10 minutes Rapidly cool down 50-80°C at 5-8°C/s, then heat up to 850-870°C, keep warm for 30-40 minutes, and cast at constant temperature; the molten liquid is cast in the mold, and rapidly cooled to 300°C, after cooling, the temperature is 300°C. -400 ℃ for 7-8 hours to obtain aluminum alloy ingots; Step 3) Hot extrusion treatment: the ingot is made into a bar by hot extrusion; Step 4) Solution heat treatment: keep at 440°C for 1-2h, and then keep at 500°C for 1-2h; Step 5) Aging treatment: keep the temperature at 80° C. for 8-12 hours, and air-cool to room temperature. 4. the preparation method of high temperature soluble aluminum alloy according to claim 3, is characterized in that, in step 2), add impurity remover refining, impurity remover composition is sodium fluoride, sodium chloride, chlorine Potassium, the mass ratio is 1:1:1; the addition amount of the impurity remover is 2-3% of the total mass of the melt. 5. the preparation method of high temperature soluble aluminum alloy according to claim 3, is characterized in that, in step 2), add slag agent to remove slag, and slag agent is aluminum-titanium-boron wire, the group of aluminum-titanium-boron wire Divided into, by mass percentage, Ti 4.5-5.5%, B0.8-1.0%, and the rest is Al, wherein impurities: Si<0.20%, Fe<0.30%, V<0.25%, other elements<0.03%, impurities The total content of elements is less than 0.10%; the added amount of slag agent is 2-3% of the total mass of the melt. 6. The preparation method of high temperature soluble aluminum alloy according to claim 3, characterized in that, in step 4), the extrusion temperature is 380-420 DEG C, the extrusion ratio is 10-20, and the extruded aluminum alloy is Incubate at 150°C for 7-8h. 7. Use of the high temperature soluble aluminum alloy according to any one of claims 1 or 2 in the preparation of a fracturing tool for shale oil and gas exploitation.